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SediGraph III Plus Operator Manual Rev A Aug 2021

SEDIGRAPH

Uploaded by

Maria Morariu
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© © All Rights Reserved
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Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
475 views

SediGraph III Plus Operator Manual Rev A Aug 2021

SEDIGRAPH

Uploaded by

Maria Morariu
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 266

SEDIGRAPH III PLUS


PARTICLE SIZE ANALYZER

OPERATOR MANUAL
512-42835-01
Aug 2021
(Rev A )
TRADEMARKS
Buna-N is a registered trademark of Pittway Corporation.
Ertalyte is a registered trademark of Quadrant Engineering Plastic Products.
Kalrez is a registered trademark of DuPont Dow Elastomers L.L.C.
Micromeritics is a registered trademark of Micromeritics Instrument Corporation.
Microsoft and Windows are registered trademarks of Microsoft Corporation.
PharMed is a registered trademark of Norton Company.
SediGraph is a registered trademark of Micromeritics Instrument Corporation.
Sedisperse is a trademark of Micromeritics Instrument Corporation.
Teflon is a registered trademark of E. I. DuPont de Nemours Company.
Tygon is a registered trademark of Norton Company.
Viton is a registered trademark of E. I. DuPont Co., Inc.

This application may contain a binary form of the Info-ZIP tool to create .zip files. That source code is provided under the
following license:
This software is provided "as is," without warranty of any kind, express or implied. In no event shall Info-ZIP or its
contributors be held liable for any direct, indirect, incidental, special or consequential damages arising out of the use of
or inability to use this software.
Permission is granted to anyone to use this software for any purpose, including commercial applications, and to alter it
and redistribute it freely, subject to the following restrictions:
1. Redistributions of source code must retain the above copyright notice, definition, disclaimer, and this list of con-
ditions.
2. Redistributions in binary form must reproduce the above copyright notice, definition, disclaimer, and this list of
conditions in documentation and/or other materials provided with the distribution.
3. Altered versions — including, but not limited to, ports to new operating systems, existing ports with new graph-
ical interfaces, and dynamic, shared, or static library versions — must be plainly marked as such and must not
be misrepresented as being the original source. Such altered versions also must not be misrepresented as
being Info-ZIP releases — including, but not limited to, labeling of the altered versions with the names "Info-ZIP"
(or any variation thereof, including, but not limited to, different capitalizations), "Pocket UnZip," "WiZ" or
"MacZip" without the explicit permission of Info-ZIP. Such altered versions are further prohibited from mis-
representative use of the Zip-Bugs or Info-ZIP e-mail addresses or of the Info-ZIP URL(s).
4. Info-ZIP retains the right to use the names "Info-ZIP," "Zip," "UnZip," "WiZ," "Pocket UnZip," "Pocket Zip," and
"MacZip" for its own source and binary releases.

Copyright

The software described in this manual is furnished under a license agreement and may be used or
copied only in accordance with the terms of the agreement.

____________________________________________________________________________

Copyright © 2021. Micromeritics Instrument Corporation. All rights reserved.


Warranty

WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each instrument it
manufactures to be free from defects in material and workmanship impairing its usefulness under normal use and
service conditions except as noted herein.

Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any
instrument or defective parts when returned prepaid to us and which our examination discloses to have been defective.
The purchaser is responsible for all transportation charges involving the shipment of materials for warranty repairs.
Failure of any instrument or product due to operator error, improper installation, unauthorized repair or alteration, failure
of utilities, or environmental contamination will not constitute a warranty claim. The materials of construction used in
MICROMERITICS instruments and other products were chosen after extensive testing and experience for their
reliability and durability. However, these materials cannot be totally guaranteed against wear and/or decomposition by
chemical action (corrosion) as a result of normal use.

Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of shipment.

No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and authorization
to return the instrument or product. All repairs or replacements are made subject to factory inspection of returned parts.

MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are
made by persons other than its own authorized service personnel unless such work is authorized in writing by
MICROMERITICS.

The obligations of this warranty will be limited under the following conditions:

1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under their
respective brand names or trade names. We, therefore, make no express or implied warranty as to such
products. We shall use our best efforts to obtain from the manufacturer, in accordance with his customary prac-
tice, the repair or replacement of such of his products that may prove defective in workmanship or materials. Ser-
vice charges made by such manufacturer are the responsibility of the ultimate purchaser. This states our entire
liability in respect to such products, except as an authorized person of MICROMERITICS may otherwise agree
to in writing.
2. If an instrument or product is found defective during the warranty period, replacement parts may, at the dis-
cretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, check valves,
seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and
stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects. Such
items which perform satisfactorily during the first 45 days after the date of shipment are assumed to be free of
manufacturing defects.

Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against
MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manufactures a
special product to the purchaser’s specifications.

MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its
products other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including
but not limited to, the implied warranties of merchantability or fitness for use.

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Corporate Profile

CORPORATE PROFILE
Micromeritics Instrument Corporation is the world’s leading supplier of high-performance systems
to characterize particles, powders and porous materials with a focus on physical properties,
chemical activity, and flow properties. Our technology portfolio includes: pycnometry, adsorption,
dynamic chemisorption, particle size and shape, intrusion porosimetry, powder rheology, and
activity testing of catalysts. The company has R&D and manufacturing sites in the USA, UK, and
Spain, and direct sales and service operations throughout the Americas, Europe, and Asia.
Micromeritics systems are the instruments-of-choice in more than 10,000 laboratories of the
world’s most innovative companies, prestigious government, and academic institutions. Our
world-class scientists and responsive support teams enable customer success by applying
Micromeritics technology to the most demanding applications. For more information, please visit
www.Micromeritics.com.

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Contact Us

CONTACT US
Micromeritics Instrument Corporation
4356 Communications Drive
Norcross, GA / USA / 30093-2901
Phone: 1-770-662-3636
Fax: 1-770-662-3696
www.Micromeritics.com

Instrument Service or Repair


Phone: 1-770-662-3666
International — contact your local distributor or call 1-770-662-3666
[email protected]

Micromeritics Learning Center


Phone: 1-770-662-3607
www.Micro.edu

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About this Manual

ABOUT THIS MANUAL


The following can be found on the Micromeritics web page (www.Micromeritics.com).

n Error Messages document (PDF)


n Parts and Accessories
The following symbols or icons indicate safety precautions and/or supplemental information and
may appear in this manual:

NOTE — Notes contain important information applicable to the topic.

CAUTION — Cautions contain information to help prevent actions that may damage
the analyzer or components.

WARNING — Warnings contain information to help prevent actions that may cause
personal injury.

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General Safety

GENERAL SAFETY

Do not modify this instrument without the authorization of a Micromeritics service


personnel.

Any piece of laboratory equipment can become dangerous to personnel when improperly
operated or poorly maintained. All employees operating and maintaining Micromeritics
instruments should be familiar with its operation and should be thoroughly trained and instructed
on safety.

n Read the operator manual for any special operational instructions for the instrument.
n Know how the instrument functions and understand the operating processes.

n Wear the appropriate personal protective equipment when operating this


instrument — such as eye protection, lab coat, protective gloves, etc.
n When lifting or relocating the instrument, use proper lifting and transporting devices
for heavy instruments. Ensure that sufficient personnel are available to assist in
moving the instrument. The 5125 SediGraph II Plus weighs approximately 43 kg
(95 lb). The MasterTech weighs approximately 18 kg (40 lb).

n Always pay attention to the safety instructions provided on each label affixed to the
instrument and do not alter or remove the labels. When inspecting the instrument,
ensure that the safety labels have not become worn or damaged.
n Proper maintenance is critical to personnel safety and smooth instrument
operation and performance. Instruments require regular maintenance to help
promote safety, provide an optimum end test result, and to prevent costly down
time. Failure to practice proper maintenance procedures can lead to unsafe
conditions and shorten the life of the instrument.
n Improper handling, disposing of, or transporting potentially hazardous materials
can cause serious bodily harm or damage to the instrument. Always refer to the
MSDS when handling hazardous materials. Safe operation and handling of the
instrument, supplies, and accessories is the responsibility of the operator.

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General Safety

INTENDED USE
The SediGraph III Plus determines particle size by using the highly accurate and reproducible
sedimentation technique which measures the gravity-induced settling rates of different size
particles in a liquid with known properties. This is a simple yet extremely effective technique for
providing particle size information for a wide variety of materials.

The instrument is intended to be operated by trained personnel familiar with the


proper operation of the equipment recommended by the manufacturer and as well as
relevant hazards involved and prevention methods. Other than what is described in
this manual, all use is seen as unintended use and can cause a safety hazard.

The instrument is intended to be used as per applicable local and national regulations.

TRAINING
It is the customer's responsibility to ensure that all personnel operating or maintaining the
equipment participate in training and instruction sessions. All personnel operating, inspecting,
servicing, or cleaning this instrument must be properly trained in operation and machine safety
before operating this instrument.

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General Safety

ENVIRONMENTALLY FRIENDLY USE PERIOD


Hazardous Substances Table
Hazardous Substances
Part Name Lead Mercury Cadmium Hexavalent Polybrominated Polybrominated
(Pb) (Hg) (Cd) Chromium biphenyls diphenyl ethers
(Cr (VI)) (PBB) (PBDE)
Cover x o o o o o
Power
x o o o o o
Supplies
Printed
Circuit x o o o o o
Boards
Cables, Con-
nectors & x o o o o o
Transducers

o Hazardous substance is below the specified limits as described in SJ/T11363-2006.


x Hazardous substance is above the specified limits as described in SJ/T11363-2006.

The Environmentally Friendly Use Period (EFUP) for all enclosed products
and their parts are per the symbol shown here unless otherwise marked. Cer-
tain parts may have a different EFUP (for example, battery modules) and are
marked to reflect such. The Environmentally Friendly Use Period is valid only
when the product is operated under the conditions defined in the product
manual.

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Table of Contents

Warranty i

Corporate Profile ii

Contact Us iii

About this Manual iv

General Safety v

1 Analyzer Components for SediGraph III Plus 1-1


Equipment Options and Upgrades 1-3
SediGraph Safety 1-4
SediGraph X-ray Certification 1-6
Specifications for the SediGraph III Plus 1-7
MasterTech Components (Optional Accessory) 1-9
Specifications for the MasterTech 1 - 12

2 About the Software 2-1


Menu Structure 2-1
Common Fields and Buttons 2-2
File Status 2-5
Keyboard Shortcuts 2-6
Option Presentation 2-7
Libraries 2-9
Methods 2 - 10
Configure the Analyzer 2 - 11
Unit Configuration 2 - 11
Sieve Table 2 - 14
Reynolds Number 2 - 14
Autorinse 2 - 15
Invert Size Axis 2 - 16

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Unit Selection 2 - 16
Report Style 2 - 17
Instrument Status 2 - 19
Show Instrument Log 2 - 19
Show Instrument Schematic 2 - 20
Show Status 2 - 23
Export Files 2 - 24
List Files 2 - 25
Software Setup 2 - 25
Software Uninstall 2 - 26
Software Updates 2 - 26

3 Sample Files 3-1


Create Sample Files 3-2
Open a Sample File 3-3
Manually Enter Data 3-4
Merge Data 3-7

4 Parameter Files 4-1


Material Properties 4-2
Analysis Options 4-7
Liquid Properties 4 - 10
Report Options 4 - 12

5 Perform an Analysis 5-1


Prepare for Analysis 5-1
Create Sample Files 5-1
Drain and Load Operation 5-2
Baseline Measurement 5-4
MasterTech Automatic 5-6
MasterTech Schedule 5-8
Quick Start Analysis 5 - 11
Perform a Sample Analysis 5 - 13

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Initialize MasterTech 5 - 15
Perform a Rinse Operation 5 - 16
Setup the Rinse and Waste Containers 5 - 17
Rinse SediGraph 5 - 18
Rinse MasterTech 5 - 19
Rinse > Both 5 - 20
Perform a Reference Material Analysis 5 - 21
Advanced Options 5 - 22

6 About Reports 6-1


Start Reports 6-1
Baseline Report 6-2
SPC Report 6-3
MicroActive Reports 6-3
Interactive Reports 6-4
Report Features 6-5
Overlay Multiple Sample Files 6 - 10
Report Examples 6 - 12
Baseline Report 6 - 12
Combined Report 6 - 13
Cumulative Finer Mass Percent vs Diameter 6 - 14
Mass Frequency vs Diameter Report 6 - 15

7 Selected Report Options 7-1


Advanced Reports - Python Module 7-1
Baseline Options Report 7-4
Combined Report 7-5
Cumulative Table 7-6
Graph Options 7-7
Log Probability Report 7-8
Particle Size Table 7-9
Rosin Rammler 7 - 10
Sample Log Report 7 - 10

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Standard Class Size Table Report 7 - 11
Standard Sieve Table 7 - 12
Summary Report Options 7 - 13

8 Diagnostics 8-1
Save Files for Problem Diagnosis 8-1

9 Maintenance and Troubleshooting 9-1


Safe Servicing 9-5
Parts And Accessories 9-5
Power 9-6
Enable Manual Control 9-7
Preventive Maintenance 9-8
Analysis Cell Assembly 9-9
Clean the Collimator Slits 9 - 14
Clean the Air Filter 9 - 16
Clean the Instrument 9 - 17
Clean the Mixing Chamber and Bezel 9 - 17
Replace the Flexible Tubing 9 - 18
Check the Mixing Pump Operation 9 - 19
Check the Cell Pump Operation 9 - 20
Reset the Mixing Pump and Cell Pump 9 - 21
Replace the Cell Windows 9 - 21
Drain the System 9 - 22
Check the Level of the Analyzer 9 - 22
Replace the X-ray Indicator Lamps 9 - 23
Replace the Mixing Pump Tubing 9 - 25
Perform a Reference Material Analysis 9 - 26
Cause of Bubbles 9 - 27
Power Instrument On and Off 9 - 28
Recover from a Power Failure 9 - 29
MasterTech Troubleshooting and Maintenance 9 - 30
Replace the MasterTech Ultrasonic Probe Tip 9 - 31

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Replace the MasterTech Input Power Fuse 9 - 31

A Advanced Reports - Python Module A-1


Advanced Report Options A-2
Scripts A-4
Python Reports A-5
Acquire Basic Information A-9
Acquire Report Results A - 13
Acquire Overlay Sample Data A - 15
Enable the Use of Overlay Data A - 29
MicModule Python Calls A - 30

B Chemical Aids for Particle Dispersion B-1

C Data Reduction C-1

D Exported Data Example D-1

E Sample Dispersion E-1

F SediGraph Results Relative to Other Methods F-1

G Sedimentation Theory G-1

H Sedisperse Particle Dispersion Liquids H-1

I Sources of Dispersing Aids I-1

J Stokes' Law J-1

SediGraph III Plus EU Declaration of Conformity DoC - 1

Index Index - 1

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1 Analyzer Components for SediGraph III Plus

1 ANALYZER COMPONENTS FOR SEDIGRAPH III PLUS


Parts and accessories can be found online at www.Micromeritics.com.

The SediGraph was surveyed for radiation leakage prior to shipping. The radiation
detected was well below the government limits. See SediGraph Safety on page 1 -
4.

FRONT COMPONENTS

A. Mixing chamber
B. X-ray standby
indicator
C. X-ray ON indicator
D. X-ray keyswitch
E. Pump control switch

Front Components
Component Description
Mixing chamber Contains the sample during an analysis and maintains sample dis-
persion throughout the analysis with a built-in stirrer.
Pump control Selects the operational mode of the mixing and cell pumps. The OFF
Off/Auto switch position turns off power to the pumps. The Auto position places the
pumps in automatic mode.

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1 Analyzer Components for SediGraph III Plus

Front Components (continued)


Component Description
X-ray keyswitch Sets the X-ray to either the ON or STANDBY position.
X-ray ON indicator Illuminates when X-rays are being generated. The X-ray keyswitch must
be turned to the X-RAY ON position.
X-ray standby Illuminates when the analyzer is ON and the X-ray keyswitch is turned to
indicator the standby position, when the door to the analysis compartment is
open, or any interlock is disengaged.

SIDE PANEL COMPONENTS

A. Ethernet
port
B. Aux RS-232
C. MasterTech
RS-232

Power switch and electrical inlet

Side Panel Components


Component Description
Aux RS-232 port For Micromeritics use only.
Ethernet Port Port for a shielded Ethernet cable allowing communication between
the analyzer and the computer.
MasterTech RS-232 For connecting the MasterTech to the analyzer.
port

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Equipment Options and Upgrades

EQUIPMENT OPTIONS AND UPGRADES


Parts and accessories can be found online at www.Micromeritics.com.

Option Description
MasterTech An automatic sampling device that operates in conjunction with the
SediGraph.

The MasterTech allows up to 18 predispersed samples to be "queued up" and run consecutively
and unattended. It allows samples to be redispersed either by stirring only or by stirring and
disruption with an ultrasonic probe. The MasterTech transfers each sample to the SediGraph,
then after analysis is complete, rinses the mixing chamber, the connecting tubing, and the stirrer.

The MasterTech 052 consists of three main components: the arm assembly, the body, and the
beaker tray. The arm assembly controls the movement of the stirring rotor, the ultrasonic probe,
and the transfer tube. The body houses the electronics, the transfer pump, the front panel
controls, and supports the beaker tray, which holds up to 18 sample beakers.

During operation, the beaker tray is loaded with beakers containing 60 to 80 mL of predispersed
sample.

When the SediGraph is ready for a sample, the tray rotates until the correct sample is underneath
the head of the arm assembly. The head then lowers until it rests on top of the beaker. Stirring
action begins and continues for a user-specified length of time. The ultrasonic probe can be
activated to aid in redispersion.

When redispersion is complete, the pump transfers most of the sample to the SediGraph, where it
is loaded into the mixing chamber. Analysis now proceeds as if the mixing chamber was filled
manually with predispersed sample. When analysis is complete, the contents of the mixing
chamber are disposed to the waste container, and a small amount of rinsing fluid is back-flushed
to the MasterTech to rinse the tubing. The arm rises so that the rinse liquid removes the sample
residue from the stirrer blades and transfer tube. Once rinsing is complete, the arm rises to the Up
position. The MasterTech is now ready to proceed to the next sample.

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1 Analyzer Components for SediGraph III Plus

SEDIGRAPH SAFETY
In a continuing effort to provide maximum safety to operators of Micromeritics equipment, and to
ensure full compliance with all known government safety regulations regarding X-rays,
Micromeritics provides a high level of X-ray safety on its SediGraph line.

GENERAL
The SediGraph Particle Size Analysis System employs soft X-rays to detect relative particle
concentration because X-ray absorption is directly proportional to particle mass. This X-ray beam
is inaccessible to the operator at all times due to cabinet construction, a door enclosing the cell
compartment, a mechanical shutter that blocks the beam’s entry into the cell compartment when
that door is opened more than 12 mm (0.5 in.), and electrical interlocks that interrupt power to the
X-ray tube when the cell compartment door or top panel is opened.

X-RAY SOURCE
X-rays are generated by a small, air-cooled tube having a tungsten target inclined at 55° to a thin
beryllium window. It is operated at a potential of 13,600 VDC with a power input of less than 41
watts. The greatest value the anode voltage can attain in a malfunction is 15,000 VDC. Only the
tungsten L-lines are excited, of which the L is primary. This primary radiation has an energy of
approximately 10,000 eV and a corresponding wavelength of 0.125 nm (1.25 angstroms). The
integrated radiation density of the direct, unattentuated beam over a 25 mm circular aperture is
between 300 and 400 milliroentgens per hour. The X-ray beam is, for example, 60% blocked by a
51 µm (0.002 in.) thick film of the plastic polyvinyl chloride and essentially completely blocked by
130 µm (0.005 in.) thick steel. Nevertheless, the shutter mechanism should never be defeated.

Radiation levels outside the instrument or in the cell compartment when the compartment door is
open are well below 0.5 milliroentgen per hour. Most jurisdictions require the registration of
radiation producing devices regardless of kind or intensity level. Check with the appropriate
authority in your area1 ) .

Since a potential of 13,600 VDC and a current of up to 3 mA generate the X-rays, the instrument
should be unplugged from the power source before any panel is removed for any purpose. This
ensures that X-ray generation ceases and high voltages are eliminated.

1 ) Based on the above information, SediGraph users in the State of Georgia have regularly been
granted waivers to the State of Georgia “Rules and Regulations for X-ray” by the Radiological
Health Section of the Georgia Department of Human Resources.

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SediGraph Safety

WARNING AND INDICATOR LIGHTS


The SediGraph control switches and indicators are located on the front panel of the analytical unit
and include a keyswitch to turn the X-ray tube on. The key is held captive when the keyswitch is
on. There are two warning lights: An amber X-RAY STANDBY light and a red X-RAY ON light.
With the analytical unit connected to the electric mains and the power switch on, the amber X-RAY
STANDBY light is lit. Turning the keyswitch to the ON position causes the red X-RAY ON light to
illuminate signaling that power is applied to the X-ray tube. When the X-RAY ON light is
illuminated, power is applied to both the filament and anode of the X-ray tube. If the X-RAY ON
lamp filament burns out, then power is interrupted to both the filament and anode of the X-ray
tube. In order for power to be supplied to the X-ray tube filament and anode when a failure (open
circuit) occurs in the X-RAY ON light, concurrent failures must occur in two independent circuits
such that these circuits continue to supply power to the X-ray tube.

The SediGraph has magnetically actuated reed switches. These switches are in series with the X-
RAY ON lamp filament. Whenever the top or rear panel of the SediGraph is removed, the cell-
compartment door is opened, the fluid module is removed, or the X-RAY ON lamp filament burns
out (opens), both filament and anode power to the X-ray tube are interrupted.

These switches are in addition to the mechanical shutter which operates when the cell
compartment door is opened, blocking X-rays and and removes filament power when the top
cover is removed. During the last 12 mm (0.5 in.) of travel of the cell compartment door to the fully
closed position, the sliding pin actuates the gravity-operated, spring-assisted shutter so that the
shutter is opened to allow X-rays to enter the cell compartment. When the cell compartment door
is opened from the fully closed position, the shutter is actuated during the first 12 mm (0.5 in.) of
travel to close and block x-rays from entering the cell compartment. As long as the cell
compartment door remains open, the shutter blocks X-rays from entering the cell compartment
and the X-ray Detection Indicator remains off.

Now, when the cell compartment door is opened, not only does the shutter block the X-ray beam
but the power to the X-ray tube also is interrupted.

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1 Analyzer Components for SediGraph III Plus

SEDIGRAPH X-RAY CERTIFICATION


X-radiation in the Micromeritics SediGraph III Plus is electronically generated by a tungsten target
x-ray tube operated at 13,600 volts of regulated DC. X-ray tube current is nominally 1.0 mA and
cannot exceed 3.5 mA in the event of any failure of circuit components . The x-rays are derived
from excitation of the L electron shell (primarily La). The operating wavelength corresponds to
approximately 8.3KeV of photon energy. The integrated radiation density of the direct,
unattenuated beam over a 25 mm circular aperture is between 300 and 400 milliroentege ns per
hour. By definition, all x-rays consist of ionizing radiation. There is no emission of x-radiation
unless the x-ray tube is supplied with electrical power. When power is removed from the
x-ray tube, there is no generation of x-rays and there is no residual x-ray radiation nor
any other type of radiation.

The SediGraph III Plus is designed to prevent x-radiation exposure of personnel through the use
of interlocks and shielding. All SediGraph Ill Pius instruments are tested for x-radiation leakage.
Maximum allowable external levels are 0.02 mrem/hr (200 nSv/hr) at 0.05 m (5 cm). Typical value
is 0.002 mrem/hr (20 nSv/hr).

Primary electrical power to the x-ray tube is controlled by a master key switch. The key is
removable to prevent unauthorized personnel from operating the instrument.

The SediGraph III Plus has three types of safety interlocks used to prevent x-radiation exposure.
Three interlock switches are located under the top panel of the SediGraph lII Plus and a magnetic
switch is mounted on the sample compartment door. When any of the switches are actuated,
electrical power to the x-ray tube is removed and the emission of x-radiation ceases. Top panel
removal and replacement subsequently requires that the key switch be cycled to restore x-ray
generation.

Redundancy is built into the sample compartment door interlocks. In addition to the electrical door
interlock, the SediGraph III Plus also has a gravity-operated mechanical shutter which blocks the
x-ray beam from entering the sample compartment when the sample compartment door begins to
open. Both of these door interlocks function before the door moves out of the frame grooves.

Two warning lights on the front of the SediGraph III Plus indicate the status of the x-ray tube. The
X-RAY STANDBY light indicates that the potential of emitting x-rays exists but that x-rays are not
now present. X-ray emission from standby status could require only a single switch operation. The
X-RAY ON light indicates that x-rays are being produced. If the X- RAY ON light bums out, this is
detected by the electronics, which will not allow x-rays to be produced until filament continuity is
re-established.

The SediGraph III Plus cabinet, analysis compartment , x-ray compartment cover, and base plate
are designed as x-ray shields . In additional , extra shield panels are mounted inside the
SediGraph lII Plus to further minimize the likelihood of any x-ray exposure if other shields are
removed (e.g., in servicing).

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Specifications for the SediGraph III Plus

SPECIFICATIONS FOR THE SEDIGRAPH III PLUS

Particle Diameter Range 300 to 0.1 micrometers Equivalent Spherical Diameter

Stainless steel, Teflon impregnated anodized aluminum, nickel


plated aluminum, nylon, polypropylene, polystyrene, Tygon and
Wetted Materials
Pharmed tubing, tungsten carbide, Ertalyte, Viton, Buna-n, and
epoxy.

Sample Size 50 mL of dispersed sample. Precise concentration is not required.

Any liquid compatible with sample cell materials and not highly
Suspending Liquids absorptive of X-rays. Typical liquids are water, glycols, mineral oils,
SediSperse, and alcohols.

Electrical

Voltage 100-240 VAC

Power 450VA, maximum

Frequency 50/60Hz

Overvoltage category II

Physical

Height 52 cm (21 in.)

Width 51 cm (20 in.)

Depth 58 cm (23 in.)

Weight 43 kg (95 lbs)

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1 Analyzer Components for SediGraph III Plus

Environment

10 to 40 °C (50 to 104 °F), operating


Temperature
-10 to 55 °C (14 to 131°F), non-operating

Humidity 20 to 80% relative, non-condensing

Indoor only
Indoor or outdoor use Altitude: 2000 m max
Pollution degree of the intended environment: 2

Computer Requirements

Windows 7 Professional or higher operating system is


Operating System
recommended for the best user experience.

The application should not be installed on a network drive with


Desktop Installation
shared access. Multiple users cannot operate the application at the
Required
same time.

If the computer is to be connected to a network, two Ethernet ports


10 Base T or 100 Base T
are required. If more than one Ethernet-based unit is connected to
Ethernet Port
the same computer, an Ethernet switch will also be required.

All application users will need Read/Write permission to all


Read/Write Permissions
directories and subdirectories where the application is installed.

Drives USB port

Due to continuous improvements, specifications are subject to change without notice.

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MasterTech Components (Optional Accessory)

MASTERTECH COMPONENTS (OPTIONAL ACCESSORY)


Parts and accessories can be found online at www.Micromeritics.com.

A. Probe cable
B. Arm assembly
C. Ultrasonic probe
D. Arm
E. Cylinder Slots (one on each side)
F. Ultrasonic power display
G. Tray

The MasterTech is an optional accessory that features an ultrasonic probe with a 1/4 in. probe tip
to supply more dispersion power to the sample. Power to the probe tip is adjustable and the
driving circuit is self-tuning for maintaining efficient and consistent sonic energy from the input
power. A digital readout on the front panel assures that the desired power is reached for
dispersing each sample and that the same power is applied each time the method is repeated.

When the instrument is ready to analyze a sample, the tray rotates until the selected sample is
underneath the arm assembly. The arm assembly lowers and stirring begins. Stirring continues
until the sample is thoroughly resuspended. At a predetermined time (specified through the
software), the ultrasonic probe can be activated to aid in dispersion. After redispersion is
complete, the MasterTech transfers the sample to the mixing chamber of the SediGraph for
analysis.

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FRONT COMPONENTS

A. Intensity display
B. Ultrasonic probe AUTO/ON switch
C. Intensity control
D. Arm AUTO/LOAD switch
E. Pump AUTO/OFF switch
F. Transfer tube connector

Front Components
Component Description
Arm AUTO/LOAD The LEDs on the switch indicate the mode of operation.
switch

Do not press the ARM AUTO/LOAD switch while an auto-


matic operation is in progress.

n AUTO. Places the arm under automatic control.


n LOAD. Raises the arm to remove or load the tray.
This switch will not work unless the computer is installed and the
analyzer software is operating.

Ensure the LOAD switch has been released when finished removing or
loading the beaker tray. The MasterTech will not operate if the arm is in
the Load position.
Intensity control n Turn clockwise to increase the intensity of the probe.
n Turn counterclockwise to decrease the intensity.

Power Display Displays the power being generated by the ultrasonic probe.
Pump The LEDs on the switch indicate the mode of operation.
AUTO/OFF switch
n AUTO. Places the pump under automatic control.
n OFF. Powers off the pump.

Transfer tubing Attach the tubing to the side that coordinates with the one used on the
connectors MasterTech pump during installation of the MasterTech.

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MasterTech Components (Optional Accessory)

Front Components (continued)


Component Description
Ultrasonic probe LEDs on the switch indicate the mode of operation.
AUTO/ON switch
n AUTO position. Places the probe under automatic control.
n ON position. Turns on the probe. Remove the probe from its holder
and place it in the liquid before turning on the probe.

Never turn the probe on unless the tip is submerged in


liquid.

After using the probe, press the switch again to place the probe in
automatic mode. Then replace it in its holder.

REAR COMPONENTS

A. Power switch, power connector, and voltage


selector card
B. +5 and +24 VDC indicators
C. RS-232 connector

Rear Panel Components


Component Description
+5 and +24 Illuminates when appropriate power is present in the MasterTech.
VDC Indicators
Power switch, power Powers the MasterTech on and off.
connector, voltage
selector card
RS-232 Connector Connects the MasterTech to the analyzer.

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SPECIFICATIONS FOR THE MASTERTECH

Sample Capacity 18 per tray; continues indefinitely if tray is replenished

Sample Size 0.5 to 4 g of powder in 60 to 80 mL of liquid

Sample Type Any suitable for SediGraph 5100 analysis

Any liquid compatible with sample cell materials and not highly
Suspending liquids absorptive of X-rays. Typical liquids are water, glycols, kerosene,
mineral oils, alcohols, Sedisperse, and mineral spirits.

Glass, stainless steel, Viton, Tygon, Silicone rubber, Polypro-


Wetted Materials
pylene

Electrical

Voltage 100/120/220/240VAC ± 10%

Frequency 50/60 Hz

Power 180 VA maximum

1.25 A (100/120VAC)
Current
0.75 A (220/240VAC)

Environment

10 to 40 °C (50 to 104 °F), operating


Temperature
-10 to 55 °C (14 to 131 °F), non-operating

Humidity 20 to 80% relative, non-condensing

Indoor only
Indoor or outdoor use Altitude: 2000 m max
Pollution degree of the intended environment: 2

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Specifications for the MasterTech

Physical

Height 69 cm (27.25 in.) maximum at load position

Width 46 cm (18.25 in.)

Depth 54 cm (21.25 in.)

Weight 18 kg (40 lbs)

Due to continuous improvements, specifications are subject to change without notice.

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2 About the Software

2 ABOUT THE SOFTWARE


The analyzer allows other computer programs to run while an automatic operation is in progress.
The Help menu provides access to the online operator manual.

Report options can be specified when creating the sample file. When running an analysis, data
gathered during the analysis process are compiled into predefined reports. Reports can also be
defined and generated after an analysis has been run. Each selected report is displayed on its
own tab and reflects data collected during the analysis.

MENU STRUCTURE
All program functions use standard Windows menu functionality.

Main Menu Bar Options


Selections Description
File Use to manage files used by the application — such as sample files, ana-
lysis conditions files, report options files, etc.
Unit [n] Use to perform analyses, calibrations, and other analyzer operations. Up
to two analyzers can be installed on the same computer.
Reports Use to start or initiate reports and view the results.
Options Use to change presentation options, set the method and active metals
defaults, configure signal calibration, manage libraries, select units, and
create report styles.
Window Use to manage open windows and display a list of open windows. A
checkmark appears to the left of the active window.
Help Use to access the embedded operator manual, the Micromeritics web
page (www.Micromeritics.com), and information about the application.

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COMMON FIELDS AND BUTTONS


The fields and buttons in the following table are located in multiple windows throughout the
analyzer application and have the same description or function. Fields and button descriptions not
listed in this table are found in tables in their respective sections. All entry fields will accept
information when using a bar code reader.

Common Fields and Buttons


Selections Description
Add Adds an item to the list.
Add Log Entry Use to enter information that will display in the sample log report that
cannot be recorded automatically through the application. Click the but-
ton again to enter multiple log entries.
Append Use to insert one row at the end of a table.
Autoscale When enabled on report parameters windows, allows the x- and y-axes
to be scaled automatically. Autoscale means that the x- and y- ranges
will be set to show all the data. If Autoscale is not selected, the entered
range is used.
Axis Range On report parameters windows, the From / To fields are enabled when
Autoscale options are not selected. Enter the starting and ending val-
ues for the x- and/or y-axes.
Bar Code (default field Use to enter additional information about the sample, such as a sample
label name) lot number, sample ID, etc.
Browse Searches for a file.
Cancel Discards any changes or cancels the current process.
Clear Use to clear the table entries and display only one default value.
Close Closes the active window and displays a prompt to either accept or
reject changes.
Close All Closes all active windows. If changes were made and not yet saved, a
prompt displays for each changed file providing the option to save the
file.
Comments Enter comments about the sample or analysis. Comments display in
the report header.
Copies Selects the number of copies to print. This field is only enabled when
Print is selected.
Delete When working with tables, deletes the selected information.
Destination Selects the report destination.

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Common Fields and Buttons

Common Fields and Buttons (continued)


Selections Description
Edit When working with report parameters, highlight the item in the Selected
Reports list box and click Edit to modify the report details.
Exit Exits the application. If a file is open with unsaved changes, a prompt
displays the option to save the changes and exit or exit the application
without saving the changes. If an analyzer is currently operating, an
additional prompt displays to confirm exiting from the software.
Export Exports data in a sample file as a .TXT, .XML or .XLS file. When saved
to a file, the data can be imported into other applications.
File Selects the destination directory. Enter a new file name in the File
name field or accept the default. Select to save the file as a spread-
sheet (.XLS), a portable document format (.PDF), or an ASCII text
(.TXT) file format.
File name Selects a file name from the list shown or enter a file name. If the
required file type is not shown, select the type of file from the list.
From / To Indicates the From and To range for x- and/or y-axes when working
with report parameters windows.
Insert Inserts one row above the selected row in the table.
List Creates a list of samples or other types of files. The list will contain the
file name, date/time the file was created or last edited, file identification,
and file status.
Name Contains a list of files in the selected directory or library.
Next Moves to the next window or next step.
OK Saves and closes the active window.
Open Opens the selected file. Alternatively, double-click the file name in the
Name column to open the file.
Prev Moves to the previous window.
Preview Previews predefined reports. Click the tabs at the top of the window to
preview each selected report. When an analysis has not been run on a
sample, this button is disabled.
Print Sends the report to the selected destination (screen, printer, or file).
Remove Removes the selected file or files from the list.
Replace Selects another file where the values will replace the current file’s val-
ues.

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Common Fields and Buttons (continued)


Selections Description
Replace All Selects another .SMP file where the values will replace all values for
the active sample file. The original file will remain unchanged. No
analysis data is added to the file. The only information added is sample
information, material properties, liquid properties, analysis, and
reporting parameters.
Report Displays a window to specify report output options.
Save Saves changes.
Save As Saves a file in the active window under a different file name. A portion
can be saved as a separate, stand-alone file, such as Analysis Condi-
tions or Report Options, when saving sample information.
Start Starts the report, test, analysis, or operation.
Start Date Displays a calendar to select the start date for the report.
View Operation. Displays the data from the current analysis.

Instrument Log. Displays recent analyses, calibrations, errors, or


messages. Enabled only in Service Test Mode.

Instrument Schematic. Displays a schematic of the analyzer system.

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File Status

FILE STATUS
In the File Selector window, the Mic Description column and the Mic Status column display the file
description and file status. The File Selector incorporates standard Windows features for resizing
windows, reordering and repositioning columns, and right-clicking an entry to display a menu of
standard Windows functions.

File Status
File Status Description
Analyzing Sample files that are currently used for analysis.
Complete Sample files used in an analysis that is completed.
Entered Sample files containing manually entered data.
No Analysis Sample files that have not been used to perform an analysis.

File Type and File Name Extension


File Type File Name
Extension
Analysis Conditions .ANC
Export to Disk (Text) .TXT
Liquid Properties .LIQ
Report Options .RPO
Report to Disk .RPT
Sample Information .SMP

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KEYBOARD SHORTCUTS
Shortcut keys can be used to activate some menu commands. Shortcut keys or key combinations
(when applicable) are listed to the right of the menu item.

Certain menus or functions can also be accessed using the Alt key plus the underlined letter in the
menu command. For example, to access the File menu, press Alt + F, then press the underlined
letter on the submenu (such as pressing Alt + F) then pressing O to open the File Selector).

If the underscore does not display beneath the letter on the menu or window, press
the Alt key on the keyboard.

Keyboard Shortcuts
Selections Description
Alt + F4 Exits the program. If files are open with unsaved changes, a prompt to
save changes displays.
F1 Opens the online help operator manual.
F2 Opens the File Selector window.
F6 Cascades open windows.
F7 Tiles all open application windows.
F8 Opens the File Selector to start a report from a selected .SMP file.
F9 Closes all open reports.

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Option Presentation

OPTION PRESENTATION
Options > Option Presentation
Use to change the way sample files and parameter files display: Advanced, Basic, or Restricted.
Each display option shows sample information and options differently.

Option Presentation Display


Presentation Display Description
Advanced Displays all parts of sample and parameter files. Navigate to para-
meter windows by selecting the tabs across the top of the window.
Basic Displays sample information in a single window. This display option
is used after the parameter files have been created. The previously
entered or default parameter files are then accessible using drop-
down lists.
Restricted Displays the sample file in a single window like the Basic display
option with certain functions disabled. A password is set when the
Restricted option is selected. That same password must be entered
to change to the Basic or Advanced display option. This display type
is typically used in laboratories — such as the pharmaceutical
industry — where analysis conditions must remain constant. The
Advanced option is not available in the view selector at the bottom of
the window when using the Restricted display option.
Always Open Edit View Opens files with a Complete status in the tabbed file editor rather
than in the Peak Editor view.
Show Splash Screen Enables (or disables) the splash screen upon application startup.

To change the view for the selected window, use the drop-down list at the bottom of
the sample file editor.

The following examples show the same sample file in Advanced and Basic display. Basic and
Restricted displays will look the same. A password is required if using Restricted format.

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Advanced view Basic or Restricted view

A sample file must be created for each analysis. The file can be created prior to or at
the time of analysis. The sample file identifies the sample, guides the analysis, and
specifies report options.

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Libraries

LIBRARIES
Options > Manage Libraries

This feature is not available when using Restricted option presentation.

The library provides an easy way to locate and open specific analyzer files. Libraries are located
within the File Selector window and can be viewed only within the application.

The library gathers sample and parameter files stored in multiple locations, such as folders on a C:
drive, a network location, a connected external hard drive, or a connected USB flash drive, and
provides access to all files. Even though libraries do not store actual sample and parameter files,
folders can be added or removed within each library.

One library can include up to 50 folders. Other items, such as saved searches and search
connectors, cannot be included.

When removing a folder from a library, the folder and its contents are not deleted from the original
file storage location. However, when deleting files or folders from within a library, they are deleted
from their original file storage location. Deleted files and folders can be recovered from the
Recycle Bin located on the Windows desktop.

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METHODS
Options > Default Method
File > Open > [.MTH File]
A Method determines the default sample identification format and sequence number. A Method is
a template of specifications that go into a newly created sample file. It allows for the definition of
complete sets of parameters for each type of sample commonly analyzed. Only a single selection
is required for each new sample file created.

The Method drop-down list displays only those methods applicable to the open sample file type.

Default Method Example Sample Information File Example

Default Methods
Selections Description
Sample file name Enter a format for the sample identification. The entry in this field
[text box] becomes a part of the saved sample file name. Include the $ symbol
to have the sample file number included as part of the identification.
Sample These field labels may be renamed, and the new label becomes a
Operator part of all new sample files.
Submitter
Bar Code [text box]
Sequence Number Specify a default numeric string to use as a prefix in the Sample field
[text box] when a new sample file is created. This number increments with
each sample file created.

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Configure the Analyzer

CONFIGURE THE ANALYZER


UNIT CONFIGURATION
Unit [n] > Unit Configuration
Use to display and confirm hardware and software configurations and calibrations of the analyzer.

Unit Configuration
Selections Description
Analyses per tubing set Enable analysis counter. Enables or disables the analyses
[group box] counter. The analysis program keeps a counter of the number of
analyses remaining before the next recommended tubing change.
For every sample information file for which an analysis is started
(excluding service tests or baseline measurements) this counter is
decremented.

Max recommended analyses per tubing set. Maximum number of


analyses to be performed before the application displays this
message:

The maximum number of analyses for this tubing has been


reached. It is time to change the tubing. When the tubing has
been replaced, reset the counter in the unit configuration
dialog.
Analyses remaining on current tubing. Number of analyses
remaining before the maximum recommended number is reached.

Reset button. Resets the counter to the recommended maximum


number.

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Unit Configuration (continued)


Selections Description
Baseline [group box] Displays the Date and the Average Intensity of the last baseline per-
formed.
Board ID [button] Displays the IP address used by the analysis program, serial
number, and type of analyzer.

IP address. Displays the IP address of the analyzer.

Change IP. Displays the Board ID dialog, which describes the circuit
boards in the analyzer. Use the Board drop-down list to select a
board to view.

Board ID. Click to display information from the circuit boards in the
analyzer. Use the drop-down list to select a board to view. The
parameters shown cannot be edited.
Calibration [group box] Displays calibration information for analyzer components.
Configuration Displays the IP address used by the analysis program, serial
[group box] number, and type of analyzer.

IP address. Displays the IP address of the analyzer.

Change IP. Displays the Board ID dialog, which describes the circuit
boards in the analyzer. Use the Board drop-down list to select a
board to view.

Board ID. Click to display information from the circuit boards in the
analyzer. Use the drop-down list to select a board to view. The
parameters shown cannot be edited.
Reset [button] Resets the analysis counter to the recommended maximum number.

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Unit Configuration

Unit Configuration (continued)


Selections Description
Set Temperature Enter the target temperature in the Set Point field.
[button]

Software Versions Version of the installed software application.


[group box]

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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SIEVE TABLE
Options > Sieves
Sieves specifies the default sieve sizes to use when sieve data are presented. The sieve sizes
follow the technical specifications per ASTM Specification E-11.

REYNOLDS NUMBER
Options > Reynolds Number
Specifies the Reynolds number to be used in estimating the maximum measurable diameter
displayed on the Material Properties window.

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Autorinse

AUTORINSE
Options > Autorinse
Use to specify autorinse options. The system default for Autorinse is 3 cycles of 3 rinses per cycle.
The analyzer will rinse a maximum of 9 times in an attempt to reestablish baseline conditions
before displaying an error message.

Autorinse
Selections Description
Number of rinses Number of rinses per cycle to be performed after each analysis
before check [text box] before baseline conditions are checked.
Maximum number of Maximum number of baseline checks to be performed before noti-
checks [text box] fication that baseline conditions have not been met.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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INVERT SIZE AXIS


Options > Invert Size Axis
Use to invert the size axis.

UNIT SELECTION
Options > Units
Use to specify how data should appear on the application windows and reports. This menu option
is not available if using Restricted option presentation in a standard installation environment.

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Report Style

REPORT STYLE
Options > Report Style
A report style can also be configured from an analysis with a Completed status.

Report Style
Selections Description
Curve Thickness Enter a value to indicate the thickness of the curve on reports.
[text box]
Font Options Click Edit to select font type, font style, and font size.
Histogram fill style Select how histograms are to appear on the report.
[drop-down box]
Linear Scale Select major and/or minor lines to display in reports for the log-
Logarithmic Scale arithmic and linear scales. Deselect this option to remove the grid
[check box] lines.
Major Gridline Select if the major and/or minor grid lines should appear as solid or
Minor Gridline [button] dotted lines.
Plot border line Enter a value to indicate the thickness of the plot borders on reports.
thickness [text box]
Show bitmap [text box] Use to show a graphic on the report header.

Height/Width. Enter the height and width of the selected graphic.


These values determine the graphic's appearance on the generated
report.

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Report Style (continued)


Selections Description
Show report title Select then enter a report title to appear on the report header.
[text box]

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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Instrument Status

INSTRUMENT STATUS
SHOW INSTRUMENT LOG
Unit [n] > Show Instrument Log
Use to display a log of recent analyses, calibrations, errors, or messages. The information is
logged for a 7-day period for analyses and a 30-day period for messages and calibrations.

Instrument Log
Selections Description
Add Log Entry [button] Use to enter information to appear in the sample log report that can-
not be recorded automatically through the application. Click the but-
ton again to enter multiple log entries.
Analysis/ Select the logs to display.
Calibration/
Message [check box]
Report [button] Click to select the print destination and the report start date.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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SHOW INSTRUMENT SCHEMATIC


Unit [n] > Show Instrument Schematic
Select this option to display a schematic of the analyzer and the MasterTech (if one is being used).

To operate the valves from this window, manual control must be enabled (Unit [n] > Enable
Manual Control).

A. MasterTech pump
B. Mixing pump
C. Mixing chamber
D. Cell pump
E. Analysis cell
F. MasterTech arm
G. MasterTech stirrer
H. MasterTech Beaker
Items in the red box show only if
MasterTech is installed

The colors of the valves and pumps indicate their state:

n White: Closed or Off (when manual control is disabled)


Valves n Yellow: Closed or Off (when manual control is enabled)
n Green: Opened

n White: Off (when manual control is disabled)


n Yellow: Off (when manual control is enabled)
Pumps
n Green: On
n Red: Indicates the pump is disabled.
Right-click a component to display pop-up menus.

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Show Instrument Schematic

Schematic
Component Description
Air Valve Sets the position of the air valve.
Cell Controls the movement of the analysis cell. An arrow in the cell
symbol indicates the direction of cell movement.

Move Cell Position. Enter the cell position.

Absolute. Move the cell position to an absolute (relative to the last


beamsplit location) number of steps. For example, an absolute move
of 100 steps moves the cell 100 steps above beamsplit.

Relative. Move the cell position to a relative (relative to current


position) number of steps. For example, a relative move of 100 steps
moves the cell up 100 steps from its current position.

Cell Position. Move the cell to the position entered.

Stop Motion. Stop cell movement.

X-ray intensity Normal / Low. Select the X-ray intensity setting.

Find Beamsplit. Zeros the cell position at the proper beamsplit


location.

Start. Progress messages display.

Done. Close the window.


Cell Pump Turn Off / Turn On. Turns the cell pump off or on.

Flow up / Down in a cell. Changes flow direction. Arrows in the


pump symbol display the current direction.

Increase / Decrease Speed. Changes the cell pump speed. The


speed of the cell pump can be set from 1 to 5, with 1 being the
slowest speed.
MasterTech Move Arm Up / Down. MasterTech arm movement control.
(if installed)
Ultrasonic On / Off. Turn the ultrasonic probe on or off.

Stirrer On / Off. Turn the stirrer in the beaker on or off.

Stirrer Speed Fast / Slow. Stirrer speed control.

Move to beaker. Move the beaker to the next beaker position.

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Schematic (continued)
Component Description
Turn On / Off. Turn the MasterTech pump on and off.

Flow Direction Rinse / Load. Set the flow direction of the


MasterTech pump. An arrow in the pump symbol changes to show
the current flow direction.
Mix Pump Turns the mixing pump on or off.
Mixing Chamber The speed of the mixing chamber magnetic stirrer can be set from 1
to 10, with 1 being the lowest speed.

Set Speed. Controls the stirrer speed by entering a value from 1 to


10.

Speed. Displays the Mixing Chamber Speed window.

Turns the stirrer on or off.


Rinse Valve Set the rinse valve position.
Set Temperature Set Temperature. Use to set the target temperature.

Set Point. Enter a temperature set point. Range 25.0 to 50.0 °C. The
set point must be at least 10 °C above ambient temperature for
accurate control.
Waste Valve Set the waste valve position.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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Show Status

SHOW STATUS
Unit [n] > Show Status
Use to show the current status for each port.

Use this option if:

n There is an automatic operation in progress and a sample file needs to be edited.


n There are two units attached to the computer. Select Show Status on each unit menu and have
the status for both units displayed simultaneously.

If multiple units are attached to the computer, select Show Status on each Unit [n] menu. The
status for all units displays.

Selections Description
Cell Temp. Temperature of the liquid in the analysis cell.
Diameter Current particle size in the analysis.
Mass Percent Current mass percent in the analysis.
MasterTech MasterTech status (if installed).
Mode Type of operation being performed.
Sample Sample file involved in the operation.
SediGraph Analyzer status — such as Analysis operation in progress, Idle, Wait-
ing for load, etc.
Time Remaining Time remaining on the analysis if an analysis is in progress.
X-ray Counts Intensity of the X-ray in kilocounts/sec.

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2 About the Software

EXPORT FILES
File > Export
Exported Data Example on page D - 1

Provides the option to print the contents of one or more sample or parameter files to either the
screen, a printer, or a file. Data can be exported as a .PDF, .TXT, .XML, or .XLS file format. The
type of data to include or exclude can be selected during the export process. The data can be
imported into other applications that read these file formats when exported to a file.

1. Click List and open an .SMP file.


2. Select an experiment and the applicable options.
3. Click OK.

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List Files

LIST FILES
File > List
Provides the option to create a list of sample file information —such as file name, date, time the
file was created or last edited, file identification, and file status.

Select one or more files from the file selector, click List, then provide the file destination.

Example of File List

SOFTWARE SETUP

If the computer is to be connected to a network, a second Ethernet port on the


computer must be used for that purpose.

The Setup program is located on the installation media and is used to reinstall the software and
make analyzer changes — such as adding, moving, or removing a unit, etc.

If the IP address needs to be changed on the computer connected to the analyzer,


refer to the computer's operating system manual or the internet for instructions. The
IP address for the computer and the IP address specified in the setup program must
match. The IP address must be 192.168.77.100.

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2 About the Software

SOFTWARE UNINSTALL
The software can be uninstalled in two ways. Either method removes only the files required to run
the software, not the analysis files.

n Click the Windows Start icon. Scroll to the Micromeritics entry. Select the Uninstall [analyzer]
option, then follow the prompts.
n Locate the uninstall.exe file in C:\Program Files (x86)\Micromeritics\[analyzer name] (or
wherever the application was installed). Double-click the uninstall.exe file, then follow the
screen prompts.

SOFTWARE UPDATES

A User Account Control in the Windows operating system must be enabled to ensure
all components of the Micromeritics application are correctly installed. If UAC is not
enabled, right-click the setup.exe installer file and select Run as administrator.

The most current version of the instrument software can be found on the Micromeritics web page
(www.Micromeritics.com).

When performing a software update, existing data files are not overwritten. There are three types
of subsequent installation:

n Later version than the current installation.


n Same version as the current installation.
n Earlier version than the current installation.
Insert the setup media into the media drive. The setup program starts automatically. If the
program does not start automatically, navigate to the installation media drive, locate and double-
click the setup.exe file.

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3 Sample Files

3 SAMPLE FILES
Option Presentation on page 2 - 7

Sample files include the information required by the analyzer to perform analyses and collect data.
A sample file identifies the sample, guides the analysis, specifies report options, and may be
displayed in Advanced, Basic, or Restricted presentation display mode.

A sample file consists of parameter sets; however, parameter sets can also stand alone. A sample
file may be created either before or at the time of analysis.

Parameter files allow for repeated use of parameter sets. For example, if the same analysis
conditions exist for multiple analyses, an Analysis Conditions file containing the recurring
conditions can be created. When the sample file is created, the Analysis Conditions file can be
selected for the analysis conditions. Once it becomes part of the new sample file, the new file can
be edited, as needed, without affecting the original Analysis Conditions file.

The analysis application contains a default method. A method is a template for sample files that
contains the parameters to be used for an analysis. When a new sample file is created, all the
parameters are filled with the values in the default method.

To change the view for the selected window, use the drop-down list at the bottom of
the sample file editor.

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3 Sample Files

CREATE SAMPLE FILES


File > New Sample > [.SMP File]
File > Open > [.SMP File]
Each analysis must be linked with a sample file before the analysis can proceed. A sample file can
consist of parameter files; however, parameter files can also stand alone.

Specify or change the option presentation by selecting Options > Option Presentation or use
the view selector drop-down list at the bottom of the window.

Sample files created in the Basic option presentation are selected from parameter files created in
the Advanced option presentation. The values specified in the parameter portions of the default
method are the defaults for new sample files. To navigate from one set of parameters to another,
select the parameter tab across the top of the window.

A bar code reader may be used to enter text into many of the fields on the Sample
Description window. Use a mouse to click in the field first where information is to be
entered then scan the bar code with the bar code reader.

Sample Files
Selections Description
Add Log Entry [button] Use to enter information that will display in the sample log report that
cannot be recorded automatically through the application. Click the
button again to enter multiple log entries.
Bar Code [text box] * Use to enter additional information about the sample, such as a
sample lot number, sample ID, etc.
Comments [text box] Enter comments about the sample or analysis. Comments display in
the report header.
Method [drop-down box] Select a method from the drop-down list.
Operator [text box] * Enter operator identification information.
Sample [text box] * Enter a sample description.
Submitter [text box] * Enter submitter identification information.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

* This field label may have been renamed or may not display if modified in Options > Default
Methods.

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Open a Sample File

OPEN A SAMPLE FILE


File > Open > [.SMP File]

When working with an existing sample file, consider copying the sample file to
maintain the original configuration options.

File Status Displays


No Analysis Tabbed file editor
Complete MicroActive report window
Analyzing
Entered

Tabbed file editor in


Example of a Report window
Advanced view
If a sample file with a Complete status is opened, return to the tabbed file editor, select Advanced
or Basic from the view selector drop-down list at the bottom of the window.

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3 Sample Files

MANUALLY ENTER DATA


This process allows the manual entry of data from a sample file with a Complete status. There are
two methods for manually entering data into a sample file:

n Copy and paste onto the graph area of the interactive window.
n Import data into the interactive window.

COPY AND PASTE MANUALLY ENTERED DATA

To display the file status in a search window, go to File > Open. Right-click the
column header then click More... Scroll to the MIC entries and enable MIC Status.This
is a snippet

1. Open a sample file with a Complete status. The file will open in the interactive reports win-
dow.
2. Right-click in the graph area of the interactive reports window, then select Copy data.

3. Open another sample file using the Advanced option presentation.


4. On the Sample Description tab, select Manually entered in the Type of Data group box.
5. In the view selector drop-down list at the bottom of the window, click Advanced, then select
Particle Size.

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Manually Enter Data

6. Ensure that all parameter fields are set appropriately, then click Paste.

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3 Sample Files

IMPORT MANUALLY ENTERED DATA


When importing data from an external ASCII text file using the Import button on the interactive
window, the ASCII text file must use the following ASCII text file format rules:

n Data must be in two columns and separated by a comma or white-space.


n Only cumulative distributions can be imported.
n An acceptable header should be in the format shown below where Diameter or Radius and
Cumulative Coarser or Cumulative Finer can be used.
n Size units of micrometers are required.
n The distribution can be Mass, Number, or Area.

Example:

Cumulative Coarser Mass Fraction vs Diameter


Particle (µm) Cumulative Coarser Mass Fraction

To import the ASCII text file

1. Open a new sample file in Advanced option presentation.


2. On the Sample Description tab, select Manually entered.
3. In the view selector drop-down list at the bottom of the window, click Advanced, then select
Particle Size.
4. Ensure that all parameter fields are set appropriately, then click Import.

5. Open the .TXT file. The data from the original sample file is imported and displayed. If an
error message displays instead, verify that the .TXT file format is correct.

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Merge Data

MERGE DATA
Use to merge data collected from an external source.

PASTE DATA FROM AN EXTERNAL SOURCE


1. Open the sample file with a Complete status.
2. Copy the external source data onto the clipboard.
3. On the Report window, click Merge Data, then select Merge with external data, then click
Paste.

IMPORT DATA FROM AN EXTERNAL SOURCE


1. Open the sample file with a Complete status.
2. On the Report window, click Merge Data, then select Merge with external data, then click
Import
3. Locate the .TXT file to import, then click Open.

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4 Parameter Files

4 PARAMETER FILES
Parameter files allow for repeated use of parameter sets. For example, if the same analysis
conditions exist for multiple analyses, an Analysis Conditions file containing the recurring
conditions can be created. When the sample file is created, the Analysis Conditions file can be
selected for the analysis conditions. Once it becomes part of the new sample file, the new file can
be edited, as needed, without affecting the original Analysis Conditions file.

Methods include both analysis conditions and report options, offering the most convenient way to
repeat most analyses.

Predefined parameter files are included with the program and can be edited as needed, or new
parameter files created.

The following file types can exist as part of the sample file as well as individual parameter files.

File Type and File Name Extension


File Type File Name
Extension
Analysis Conditions .ANC
Liquid Properties .LIQ
Report Options .RPO
Sample Information .SMP
Method .MTH

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4 Parameter Files

MATERIAL PROPERTIES
File > Open > Analysis Conditions
Or, click the Material Properties tab when in Advanced option presentation.

Material Properties
Selections Description
Analysis liquid Displays a list of the Liquid Properties files.
[group box]
Description. Enter the name of analysis liquids to add to the list.

X-ray Intensity. Displays the X-ray intensity selected for the analysis
liquid. The intensity is selected in Liquid Properties window.

Add. Click to add analysis liquids to the list and change values for an
analysis liquid.

n To add analysis liquids: In the Description field, enter the name of


the liquid, then click Add.
n To change values of an analysis liquid: Highlight the liquid, then
click Properties. Enter the new values, then click OK. Add changes
to Change; click Change.

Delete. Click to delete the selected liquid from the list.

Properties. Click to edit the properties of the analysis liquid. See Liquid
Properties on page 4 - 10.

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Material Properties

Material Properties (continued)


Selections Description
Analysis Type Specifies if the analysis is standard, high speed or high resolution.
[group box]
n Standard. Provides good resolution and average analysis time.
n High speed. Allows a faster analysis, but a little lower resolution.
n High resolution. Provides high resolution at the smallest diameters,
but takes a longer time.

Starting diameter. Specify the range of sizes to be included in the


analysis. The starting diameter generally should be larger than the
largest particle expected to be in the sample.

Ending diameter. The ending diameter must be less than the smallest
size particle of interest. Each time the values in these fields are
changed, the analysis statistics are updated. A note also is added to the
report header indicating changes have been made since the first
analysis was performed.
Analysis Unit Displays a list of the attached units and their temperatures. The
[group box] displayed temperature is used to compute analysis statistics.

n Reynolds number. Calculated for the starting diameter using the


sample’s density and the liquid’s density and viscosity. If this number
is greater than 0.3, large particles falling through the liquid may cre-
ate turbulence, affecting both their velocity and the velocity of neigh-
boring smaller particles. This results in an incorrect particle size
distribution.
n Maximum diameter. Calculated to have a Reynolds number
equivalent to the one entered as a default (from the Options menu). If
the sample has more than a couple percent mass of particles larger
than this diameter, the sample should be analyzed in a liquid with a
higher viscosity.

The Maximum diameter field should be greater than the starting


diameter specified in step 8. The Reynolds number should be less
than 0.3.

n Analysis time. Calculated based on the sample density, liquid dens-


ity and viscosity, and ending diameter. The actual analysis time may
vary slightly if the analysis compartment temperature is different
when the analysis takes place.

The Reynolds number, Maximum diameter, and Analysis time fields

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4 Parameter Files

Material Properties (continued)


Selections Description

display analysis statistics. These values are updated whenever a


parameter affecting their computation is changed.

If... Then...
the maximum diameter and Reyn- a dispersing liquid with a higher
olds number values are not viscosity must be used.
attained
the maximum diameter is much a lower viscosity liquid (if avail-
greater than the starting diameter able) may be used.
and the Reynolds number is
much less than 0.3
Description [text box] Description of the Analysis Conditions file.
Sample Material Displays a list of available sample materials. When a sample material is
[group box] selected, the description and density display.

Description. Name of sample materials to add to the list.

Density. Density of the sample material selected from the list.

Add. Adds sample materials to the list.

n To add samples materials: In the Description field, enter the name


of the sample material. Click Add.
n To change values of the sample material density: Highlight the
sample material in the list, then enter the density value in the Density
field.

Delete. Deletes sample materials from the list.

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Material Properties

Material Properties (continued)


Selections Description
Update Properties Allows the updating of the material properties of a completed analysis.
[button] This allows the collected data to be reprocessed based upon the new
properties.

The material properties for the original analysis remain unchanged. A


note is added to the report header describing the change.

The contents of the Sample Material and Analysis Liquid group boxes
are described elsewhere in this table.

Set Baseline. Applies a baseline different than the one active in the
original analysis. From the drop-down list, select the instrument
containing the baseline to use, then select Use alternate baseline. The
original baseline is preserved.

From the drop-down list, select the instrument containing the baseline to
use, then select Use alternate baseline. The original baseline is
preserved.

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4 Parameter Files

Material Properties (continued)


Selections Description
Apply Changes. Select to apply all changes to the material properties.

Click Yes at the prompt. All test data will be converted to the new data
reduction options. Do you wish to continue? The data are converted and
this prompt displays: Application of new reduction options [file name] is
complete.

Click OK to close the message box.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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Analysis Options

ANALYSIS OPTIONS
File > Open > Analysis Conditions
Or, click the Analysis Options tab when in Advanced option presentation.

Provides details for setting up the sample analysis conditions file. Analysis options can be edited
as long as the analysis is not in progress and the sample file does not contain manually entered
data. Changes made to analysis parameters are noted in the report header upon completion of
the analysis.

Analysis Options
Selections Description
Full scale scan Pump speed. The speed at which the cell pump should operate
[group box] during the full-scale scan. Use a pump speed of 2 or 3 if analyzing
fine samples since they pump through the tubing easily. If analyzing
coarse particles, especially if dispersed in higher viscosity liquids, a
higher pump speed of 4 to 5 should be used. If the analyzer has the
smaller 5 mm (3/16 in.) OD tubing, higher speeds may be required
for finer particles.

Bubble detection. Types of bubble detection (Fine, Medium, or


Coarse).

The presence of most bubbles in the cell can be detected during the
full-scale scan that takes place at the start of the analysis. Detecting
bubbles, however, is somewhat sample-dependent. Samples, which
contain very large particles, may appear to have bubbles near the
top of the cell, when actually the sudden change in X-ray intensity is
due to incomplete filling of the topmost portion of the analysis cell.

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4 Parameter Files

Analysis Options (continued)


Selections Description
For samples of this type, select Coarse bubble detection.

If only small particles are present in the sample (less than 1 mm),
select Fine bubble detection.

For samples between these two ranges, select Medium bubble


detection.
Leave pump on during Coarse materials tend to settle in the tubing during analysis. This
analysis [check box] option allows the pump to operate during analysis, enabling easier
rinsing and resuspension of the sample.
MasterTech treatment (Applicable only if using a MasterTech.)
[group box]
Samples tend to settle in the beakers while waiting for sample
analysis, especially if samples are prepared ahead of time, as in
most cases when using a MasterTech. Program the MasterTech
stirrer and probe to redisperse the sample using options in the group
box.

Stirrer time. The number of seconds to have the stirrer operate


during resuspension.

Stirrer speed. Options include High and Low. Coarse materials and
less-stable dispersions may require more high-speed stirring than
finer materials. Range: 1 to 10, with 1 being the slowest

Probe time. Length of time for the ultrasonic probe to operate during
resuspension. Coarse materials and less-stable dispersions may
require more high-speed stirring than finer materials.
Mixing chamber stirrer Adjusts the speed of the magnetic stirring bar which stirs the mixture
speed [text box] in the mixing chamber. Select a number between 1 and 10. 1 rep-
resents the lowest speed and 10 the highest.
Number of tests The number of analyses to be performed.
[text box]

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Analysis Options

Analysis Options (continued)


Selections Description
Rinse [group box] Rinse after analysis. Select if a rinse cycle should be performed
after analysis.

Autorinse. Performs up to 3 cycles of 3 rinses each (a total of 9


rinses) in an attempt to re-establish baseline conditions. If conditions
are not re-established after 9 rinses, an error message is displayed.

Rinses. The number of rinses to be performed.

Pump speed. The speed for the cell pump to operate during rinsing.
The range is 1 to 5, with 1 being the slowest.
Stop at selected mass Stops analysis at a specified mass percent finer.
percent [check box]
If unsure of the smallest size particle present in the sample, it may be
difficult to determine an ending diameter which will include the
selected data. With this option, choose to end mass percent at 0%,
after having set the ending diameter at a small value of
approximately 0.1 μm. Using this method, wait time is lessened at
the end of the analysis.

Ending percent finer. Enabled only if Stop at selected mass


percent is selected. Enter the point at which the analysis should stop.

Wait for temperature Select to have the temperature in the analysis compartment and
stabilization [check box] mixing chamber stabilize to within ± 0.5 °C of the setpoint before the
analysis begins.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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4 Parameter Files

LIQUID PROPERTIES
File > Open > Liquid Properties
Or, click the Properties button on the Materials Property tab when in Advanced option
presentation.

Use to edit the properties of an analysis liquid and to specify properties for a new liquid properties
file.

The liquid properties are edited by selecting the Materials Properties window. Click
Properties in the Analysis Liquid group box.

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Liquid Properties

Liquid Properties
Selections Description
Current Cell Conditions Displays the cell conditions of the analysis unit. These conditions are
[group box] based on the temperature of the cell and are used in computing the
analysis statistics displayed on the Material Properties window.

Select either fixed values or interpolated values based on the cell


temperature.

Fixed values. Enter a value in the Viscosity and Density fields.


These values will be maintained regardless of the cell temperature.

Interpolate using cell temperature. Enter three sets of values in


the Temp., Density, and Viscosity fields. These values will be used to
interpolate the density and viscosity at the current cell temperature.

The table requires that the entered values be properly ordered. For
example, enter values from left-to-right and from top-to-bottom.
Temperature is in ascending order.
Description [text box] If editing an existing file, this field contains the name of the selected
file. If defining a new file, enter a name in this field.
X-ray intensity [selec- Normal. Optimized for most applications when using high X-ray
tion] absorption liquids, such as water.

Low. Decreases intensity when using low X-ray absorption liquids,


such as hydrocarbons.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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4 Parameter Files

REPORT OPTIONS
File > Open > [.RPO File]
Or, click the Report Options tab when in Advanced option presentation.

About Reports on page 6 - 1


Selected Report Options on page 7 - 1

Additional reports are available using the Reports menu.

Use to specify report options for data collected from an analysis or manually entered data. Report
Options files also help in customizing report details such as axis scale, axis range, column
headings, and components of thickness curve equations. These files may contain tabular reports,
plots, or both, as well as advanced report tables.

Customized report options files can be created then loaded into a sample file, allowing quick
generation of reports.

Report Options files may be defined to include overlay options. This system allows the overlay of
up to 25 plots of different samples onto a plot of the same type or overlay one plot type onto a
different plot type from the same analysis.

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Report Options

Report Options
Selections Description
Distribution type Select the type of distribution data to report: Area, Number, or Mass.
[selection]
Overlays [button] See Overlay Multiple Sample Files on page 6 - 10.
Reference [button] Specify a reference sample file to compare analysis results of the cur-
rent sample.
Report options Browse for a .RPO file that contains report options parameters to be
[drop-down box] used in the report.
Selected reports Select the report names to include in the report.
[group box]
Specification [button] Select the sample files to be used for the coarse and fine spe-
cification boundaries to determine if the results of the current sample
are within the specified boundaries.
Test [drop-down box] Select the analysis for the report: First, Last, or Average.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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5 Perform an Analysis

5 PERFORM AN ANALYSIS

PREPARE FOR ANALYSIS


It is recommended to perform the tasks in the provided order.

CREATE SAMPLE FILES


File > New Sample > [.SMP File]
File > Open > [.SMP File]
Each analysis must be linked with a sample file before the analysis can proceed. A sample file can
consist of parameter files; however, parameter files can also stand alone.

Specify or change the option presentation by selecting Options > Option Presentation or use
the view selector drop-down list at the bottom of the window.

Sample files created in the Basic option presentation are selected from parameter files created in
the Advanced option presentation. The values specified in the parameter portions of the default
method are the defaults for new sample files. To navigate from one set of parameters to another,
select the parameter tab across the top of the window.

A bar code reader may be used to enter text into many of the fields on the Sample
Description window. Use a mouse to click in the field first where information is to be
entered then scan the bar code with the bar code reader.

Sample Files
Selections Description
Add Log Entry [button] Use to enter information that will display in the sample log report that
cannot be recorded automatically through the application. Click the
button again to enter multiple log entries.
Bar Code [text box] * Use to enter additional information about the sample, such as a
sample lot number, sample ID, etc.
Comments [text box] Enter comments about the sample or analysis. Comments display in
the report header.
Method [drop-down box] Select a method from the drop-down list.
Operator [text box] * Enter operator identification information.
Sample [text box] * Enter a sample description.
Submitter [text box] * Enter submitter identification information.

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5 Perform an Analysis

Sample Files (continued)


Selections Description

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

* This field label may have been renamed or may not display if modified in Options > Default
Methods.

DRAIN AND LOAD OPERATION


Unit [n] > Drain and Load
Drain the System on page 9 - 22
Baseline Measurement on page 5 - 4

Before collecting baseline data or performing an analysis, the cell and mixing chamber must be
drained and the sample (or baseline liquid) loaded.

n Prior to a baseline collection or an analysis, go to Unit > Drain and Load.


n At the beginning of a baseline collection, select the Prepare SediGraph to load baseline liquid
check box on the Baseline Measurement window.
n At the beginning of an analysis, select the Prepare SediGraph to load sample check box on the

Ensure that the outlet tube is in the waste reservoir


and that the rinse tube is in the rinse liquid reservoir.

1. Select to either have the liquid remain in the mixing chamber or leave the mixing chamber
empty. Click Continue. A progress message appears prior to the following window.
2. Ensure the mixing chamber bezel is inserted in the mixing chamber, then load the sample
(or baseline liquid) into the mixing chamber. The mixing speed can be changed using the
Increase or Decrease button. Click Continue.

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Drain and Load Operation

3. Confirm the X-ray intensity reduction over the baseline before it completes:

n Good. Indicates reduction is between 30 and 75% meaning that the concentration level
is appropriate.
n Low. Indicates the reduction is less than 30% meaning that the concentration is too low
and sample should be added.
n High. Indicates the reduction is more than 75% meaning that the concentration is too
high and more dispersant or less sample should be used.
4. When the X-ray reduction level is set, click Continue and the cell will move to the normal
park position and the load operation will be complete.

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5 Perform an Analysis

BASELINE MEASUREMENT
Unit [n] > Baseline
A baseline measurement is required for data collection. Although it is not necessary to measure a
baseline for each analysis, Micromeritics recommends that a baseline measurement be
performed once per shift and when changing dispersing agents. Up to seven baselines can be
measured; however, only the last one may be saved.

Ensure that the outlet tube is in the waste container and that no sample is present in
the system.

1. If the baseline liquid has not been loaded into the mixing chamber:

a. Select Prepare to load baseline liquid.


b. Select to have the liquid remain in the mixing chamber or to leave the mixing chamber
empty.

If planning to use a liquid different from the one used for rinsing, select Leave mixing
chamber empty.

2. To have a baseline report generated, select Report After Analysis then select the report des-
tination.
3. Select the X-ray intensity setting.

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Baseline Measurement

Baseline
Selections Description
Baseline to use Select whether to use the latest or the previous baseline
[drop-down box]
Latest. Uses the last baseline performed.

Previous. Uses the baseline which was active before the last series
of baselines were performed.
Prepare to load Select if the baseline liquid is not loaded. Select if the liquid should
baseline liquid remain in the mixing chamber or leave the mixing chamber empty.
[check box]
If Prepare to load background liquid is selected, a drain and load
operation is performed before the baseline measurement begins.
Load the baseline liquid when prompted. Click Next to begin the
baseline measurement.

If Prepare to load baseline liquid was selected, a drain and load


operation is performed first.

If this baseline is not satisfactory, click Next to perform another


baseline. If another baseline is measured, the current one will
become inaccessible.
X-ray intensity Normal. Increases intensity when using high X-ray absorption
[selection] liquids, such as water.

Low. Decreases intensity when using low X-ray absorption liquids,


such as hydrocarbons.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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5 Perform an Analysis

MASTERTECH AUTOMATIC
Unit[n] > MasterTech Automatic

Option is available only if a MasterTech is connected to the analyzer.

Use to analyze a series of samples of the same type, which contain the same analysis conditions.
Sample files are created automatically.

MasterTech Automatic
Selections Description
Method [drop-down box] Select the method to be used in the analysis. See Methods on
page 2 - 10.
Sample resuspension Enter resuspension parameters. All fields in this group box are
[group box] disabled if an analysis is in progress.

Samples tend to settle in the beaker while waiting for analysis,


especially if samples are prepared ahead of time, as in most cases
when using a MasterTech. Use the options in this group box to
program the MasterTech stirrer and probe to re-disperse the sample
before analysis.

Stirrer time. Enter the number of seconds to have the stirrer operate
during resuspension.

Stirrer speed. Select the stirrer speed. Coarse materials and less-
stable dispersions may require more high-speed stirring time than
finer materials.

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MasterTech Automatic

MasterTech Automatic (continued)


Selections Description
Probe time. Enter how long to have the ultrasonic probe operate
during resuspension. Coarse materials and less-stable dispersions
may require more probe time than finer materials.
Start with beaker Enter the position number of the beaker containing the first sample to
[text box] be analyzed. This field is disabled if an analysis is in progress.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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5 Perform an Analysis

MASTERTECH SCHEDULE
Unit [n] > MasterTech Schedule

Option is available only if a MasterTech is connected to the analyzer.

Use to:

n Analyze a series of samples that may be different in size and shape and require different ana-
lysis conditions.
n Perform a series of baseline measurements.
n Analyze samples and measure a baseline alternately.

MasterTech Schedule
Selections Description
Insert [button] Click to insert sample files to be used for analyses.

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MasterTech Schedule

MasterTech Schedule (continued)


Selections Description
If a sample file is selected, the new file will be inserted before the
selected file; otherwise it will be inserted at the end of the list.

Beaker Number. Enter the beaker number containing the selected


sample (or baseline liquid).

Baseline measurement. Specify either a baseline measurement or


sample analysis for the specified beaker. If Baseline measurement is
selected, select the X-ray intensity.

n Normal. Increases intensity when using high X-ray absorption


liquids, such as water.

n Low. Decreases intensity when using low X-ray absorption


liquids, such as hydrocarbons.

Use this option if planning to change dispersing agents


with one of the samples. A baseline measurement can
then be scheduled using the beaker preceding the one
containing the different dispersant. For example, if plan-
ning to change dispersing liquids in beaker position #4,
schedule a baseline measurement in beaker position #3.

Sample analysis. Click Browse, then choose the sample file or use
with the sample in this beaker position.

n Stirrer time. The number of seconds to have the stirrer operate


during resuspension.
n Stirrer speed. Select the stirrer speed. Coarse materials and
less-stable dispersions may require more probe time than finer
materials.
n Probe time. The length of time to have the ultrasonic probe oper-
ate during resuspension. Coarse materials and less-stable dis-
persions may require more highspeed stirring time than finer
materials.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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5 Perform an Analysis

1. Enter the position number of the beaker containing the current sample.
2. Select Baseline measurement or Sample analysis.

n If Sample analysis is selected, click Browse to select a sample file to use with the sample
in this beaker position. The values contained in the fields for Stirrer time, Stirrer speed, and
Probe time are copied from the selected sample file.
n If Baseline measurement is selected, select the X-ray intensity.
o Normal increases intensity when using high X-ray absorption liquids, such as water.
o Low decreases intensity when using low X-ray absorption liquids, such as hydro-
carbons.

3. Click OK. The beaker information displays in the list box.


4. Repeat step 3 and 4 for each beaker containing sample.
If dispersing liquids will be changed at any time during this series, perform a baseline
measurement using the beaker position preceding the one containing the sample with the
new liquid. For example, if dispersing liquids are changed with the sample contained in
beaker position 4, insert a Baseline measurement for beaker position 3.
5. Click Report Settings to generate a report after analysis. Click OK.
6. Click Start to begin the analysis.

When the analysis begins, the Start button changes to Stop. The Stop button
cancels the remaining analyses. The analysis that is currently in progress will be
completed.

To view the analyses in progress, go to View > Analysis Results.

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Quick Start Analysis

QUICK START ANALYSIS
Unit [n] > Quick Start
Use this mode of operation to analyze a series of samples of the same type that contain the same
analysis conditions. Sample files are created automatically.

QuickStart Analysis
Selections Description
Leave liquid in mixing chamber [button] Select to leave liquid in mixing chamber
after analysis.
Leave mixing chamber empty [button] Select to leave mixing chamber empty
after analysis.
Prepare SediGraph to load sample [button] Select if the sample is not loaded. If
selected, an initial drain and load oper-
ation is performed.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

1. If the analyzer has not been drained, select Prepare SediGraph to load sample to drain the
mixing chamber. Then select to have the liquid remain in the mixing chamber after the drain
and load operation or to leave the mixing chamber empty.
2. Click Report After Analysis to generate a report after analysis is complete.
3. Click Next.

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5 Perform an Analysis

4. Select a Method from the drop-down list.


5. To specify a different file name enter the new file name in the text box.
6. Specify a mixing chamber speed using the Increase or Decrease buttons.
7. Load the sample.
8. Click Next. If Prepare SediGraph to load sample was selected, a drain is performed before
being prompted to load the first sample. Analysis of the first sample begins. The current
baseline and data display as they are collected. When analysis is complete, a prompt to
load the next sample displays. Repeat steps 7 and 8 until all analyses are complete.

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Perform a Sample Analysis

PERFORM A SAMPLE ANALYSIS


Unit [n] > Sample Analysis
1. Click New to create a new sample file, or click Browse to select an existing sample file.

Sample Analysis
Selections Description
Prepare SediGraph to Select if the sample has not been loaded into the mixing chamber. If
load sample [check box] selected, a drain and load operation is performed.

Select if the liquid should remain in the mixing chamber or leave the
mixing chamber empty.
Sample density Enter the sample density.
[text box]
Number of tests Enter the number of tests to be performed.
[text box]
Rinse after analysis Select to perform a rinse after analysis.
[check box]

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

2. Click Start.
3. When the analysis completes, the graph displays.

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5 Perform an Analysis

4. Click the Report button to display the report.

5. Click Next to select another sample file for a new analysis.

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Initialize MasterTech

INITIALIZE MASTERTECH
Unit [n] > Initialize MasterTech

Select this option if:

n Manual operations should be performed with the MasterTech.


n The MasterTech beaker tray has been disturbed.

When the MasterTech is initialized, the tray is aligned so that beaker #1 is in the start position.

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5 Perform an Analysis

PERFORM A RINSE OPERATION


Unit [n] > Rinse > [SediGraph, MasterTech, Both]

n A rinse operation cannot be performed when an analysis is in progress.


n The rinse container should be rinsed thoroughly or replaced after each use.

A rinse operation should be performed to rinse the analysis cell, mixing chamber, and tubing of
any contaminants or sample materials from the previous analysis. It is best to perform a rinse
operation after each analysis. On the Analysis Options window, select that a rinse is to be
performed after an analysis.See Analysis Options on page 4 - 7.

Rinse
Selections Description
SediGraph Rinses the analysis cell, mixing chamber, and the analyzer tubing.
MasterTech Rinses the MasterTech tubing.
Both Rinses the analysis cell, mixing chamber, the analyzer tubing, and
the MasterTech tubing.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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Setup the Rinse and Waste Containers

SETUP THE RINSE AND WASTE CONTAINERS


1. Pour approximately 10 liters of water containing a small amount of surfactant into the rinse
container. For example, use 0.05% sodium metaphosphate (W/W) in deionized water.
2. Insert the rinse tube into the rinse container.
3. Insert the waste and overflow tubes into the waste container.
4. Turn the caps clockwise to secure.

A. Rinse container
B. Tube weight
C. Rinse tube
D. Overflow tube
E. Waste tube
F. Waste container

Ensure that tube weights are attached to the rinse and waste tubes, that the overflow
tube and waste tubes are in the waste container, and that the rinse tube is in the rinse
liquid container.

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5 Perform an Analysis

RINSE SEDIGRAPH
Unit [n] > Rinse > SediGraph

SediGraph Rinse
Selections Description
Rinse Cycles [selection] Autorinse. Performs up to 3 cycles of 3 rinses each (a total of 9
rinses) in an attempt to reestablish baseline conditions. If conditions
are not reestablished after nine rinses, an error message is
displayed. See Autorinse on page 2 - 15.

Rinses. Specifies up to five rinses to be performed.


Cell Pump Speed The speed for the cell pump is to operate during rinsing. The range is
[text box] 1 to 5, with 1 being the slowest.
Continue [button] Begins the rinse operation. A message displays indicating a rinse
operation is in progress. When rinsing is complete, the window
closes.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

1. Ensure the rinse and waste containers have been setup. See Setup the Rinse and Waste
Containers on the previous page.
2. Select either of the following:
n Autorinse. To have the analyzer automatically determine how many rinse cycles to per-
form. Autorinse, in an effort to reestablish baseline conditions, performs three cycles of
three rinses per cycle (default setting) before displaying an error message that baseline
conditions cannot be reestablished.

n Rinses. If Rinses is selected, enter the number of rinse cycles to perform.

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Rinse MasterTech

3. Enter the operating speed of the cell pump. A speed of 2 usually is sufficient unless the
material is difficult to rinse; then it may be necessary to use a higher speed.
4. Click Continue. Progress messages display until rinsing is complete.

RINSE MASTERTECH
Unit [n] > Rinse > MasterTech

MasterTech Rinse
Selections Description
Continue [button] Begins the rinse operation. A message displays indic-
ating a rinse operation is in progress. When rinsing is
complete, the window closes.
Rinse beaker number [text box] Enter the position number of the beaker to rinse into.
Ensure the beaker is empty.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

1. Ensure the rinse and waste containers have been setup. See Setup the Rinse and Waste
Containers on page 5 - 17.
2. Enter the position number of the beaker to catch the rinse liquid.
3. Ensure the beaker is empty.
4. Click Continue. Progress messages display until rinsing is complete.

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5 Perform an Analysis

RINSE > BOTH


Unit [n] > Rinse > Both

1. Ensure the rinse and waste containers have been setup. See Setup the Rinse and Waste
Containers on page 5 - 17.
2. In the SediGraph group box, select:
n Autorinse. To have the analyzer automatically determine how many rinse cycles to per-
form. Autorinse, in an effort to reestablish baseline conditions, performs three cycles of
three rinses per cycle (default setting) before displaying an error message that baseline
conditions cannot be reestablished.

n Rinses. Enter the number of rinse cycles to perform.


3. In the MasterTech group box, enter the position number of the beaker to catch the rinse
liquid.
4. Enter a speed in the Cell pump speed field.
5. Ensure the beaker is empty.
6. Click Continue. Progress messages display until rinsing is complete.

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Perform a Reference Material Analysis

PERFORM A REFERENCE MATERIAL ANALYSIS


A reference material analysis is used to verify the analyzer is operating properly and producing
optimum results. These methods provide specifications for critical report quantities and reporting
of whether quantities are in or out of specification.

When running a reference material analysis, use the appropriate reference material kit. This kit is
available from Micromeritics. The results should match those shown on the label of the reference
material bottle, within the tolerance level.

Parts and accessories can be found online at www.Micromeritics.com.

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5 Perform an Analysis

ADVANCED OPTIONS
Options > Advanced Options

Changing these parameters will affect the performance of the SediGraph III Plus
instrument. This program should only be used after consultation with a Micromeritics
Service Representative

BASELINE/FULLSCALE

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Advanced Options

CELL PROFILING
Cell Profiling is the appropriate choice for particle systems that are readily suspended, such as
most pigments and clays. Readily suspended samples would be characterized by particle
populations mostly below 50 micrometers and having a moderate density less than 4 g/cm3).

Cell Profiling uses baseline and full scale readings taken at each cell position to scale mass
percent data taken at that position. This prevents cell window defects or contamination from
affecting the measured size distribution.

BASELINE/FULLSCALE AVERAGING
Baseline/Fullscale Averaging is a choice provided for the analysis of samples having a significant
mass percentage of particles showing a very high setting velocity because of some combination of
size (50 to 300 micrometers) or density.

Baseline/Fullscale Averaging uses mean baseline and fullscale values to scale mass percent data
taken at all cell positions. This procedure largely eliminates the fullscale fluctuations caused by
flow variations in the presence of a statistically small number population of the more massive
particles. When using this choice, the cell should be checked to verify a flat baseline.

HIGH SPEED ANALYSIS

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5 Perform an Analysis

NORMAL MODE
Normal Mode provides an adjusted cell position schedule that ensures a consistent resolution of
the sedimentation profile for an abbreviated high speed analysis. This increase in accuracy comes
at the cost of an approximately 10 minute increase in runtime compared to an abbreviated high
speed Control Mode run.

CONTROL MODE
Control Mode is provided to obtain the fastest possible results when specifying an ending
diameter greater than 0.2 micrometers (an abbreviated run). Because the short analysis time
does not allow full resolution of the particle sedimentation profile, the results obtained, while
consistent, may not exactly agree with a full range analysis.

Abbreviated runs in Control Mode should not be used to check final product quality without
investigating its effect for the materials being used. Select of Control Mode has no effect on full
range analyses, whether high speed, standard, or high resolution.

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6 About Reports

6 ABOUT REPORTS
Reports can be generated for data collected on a sample that has completed analysis, collected
on a sample currently being analyzed, or manually entered.

Reports > Start Report


Generates a report on a sample analysis.

Reports > Close Reports


Closes all open reports. This option is unavailable if reports are being generated.

START REPORTS
Reports > Start Report
Starts the selected report. Select a file from the Files list. Ensure the selected file has a status of
either Complete or Analyzing.

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6 About Reports

BASELINE REPORT
Reports > Baseline
A graphical report can be generated on an instrument’s baseline. This report generates a graph
illustrating the X-ray intensity versus the cell height. The report header contains baseline
statistics, such as the unit serial number, date the baseline was performed, etc.

Baseline Report
Selections Description
Baseline Date and Time Date and time of the last baseline measurement.
Copies [scroll selection] Specifies the number of copies of the report.
Instrument List of serial numbers of the attached instruments.
[drop-down box]
File [text box] Specifies the location where the report should be saved.
File name [text box] Specifies the name for the report.
File type Indicates the report file type: Spreadsheet (.xls), XML (.xml) or
[drop-down box] Unicode Text (.txt).
Preview [button] Displays a preview of the report.
Print [button] Prints the selected report.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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SPC Report

SPC REPORT
Reports > SPC Report Options
Use to generate reports with various SPC (Statistical Process Control) options. All selected
variables must be computed for each sample file used in an SPC report; therefore, it is more
efficient to select only the necessary variables.

MICROACTIVE REPORTS
MicroActive reports are generated automatically after an analysis is performed. This feature
provides a quick and easy way to investigate and manipulate analysis data using a variety of
reporting methods.

When a report is opened, plots and summary data are displayed, and in some reports certain
parameters are also displayed. Plots may be edited by selecting the data points or data point
range to be included in the plots and modifying the parameters. When a report is edited, the
results are immediately reflected in the plots and summary data.

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6 About Reports

INTERACTIVE REPORTS
When opening a sample file that contains data from a complete or in-progress analysis, the
interactive reporting feature is enabled.

1. From the view selector drop-down list at the bottom of the window, do either of the following:
n Change the option presentation of the sample description window to either Basic or
Advanced to modify certain file parameters.
n Select another plot from the list and edit the data contained in the plot.
2. When ranges are edited, the changes are reflected immediately in the plots and the sum-
mary data displayed in the window. Some editing options are:
n Drag the blue bars to increase or decrease the range of data included in the plot.
n Right-click to display a popup menu to include reports; enable or select overlays; edit
curves, axes, legends, titles; and copy and paste the data in a graph or in tabular
format.
3. Click Save.

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Report Features

REPORT FEATURES
Report Style on page 2 - 17

Click Preview on the MicroActive report window to display additional report information.

n After analysis, reports can be viewed, printed, and/or copied and pasted into other documents.
n The report zoom feature provides the viewing of fine graph details and the ability to shift the
axes.
n All reports contain a header displaying file statistics.
n Tabular and graphical reports contain sample and analyzer statistics such as analysis date/-
time, analysis conditions, etc.
n The headers contain notes of sample file changes occurring after analysis.
n Summary report headers contain the same information as tabular and graphical reports with
the exception of notes.

A. Data display (graph or


text)
B. Report header area
C. Report export options
D. Generated tabs
E. Report graphic
F. Title
G. Print icon
H. Style icon

Report Features and Shortcuts


Selections Description
Display area Displays either graphic or text from the generated report. Click the
tabs across the top to display the selected report. When a tabular
report displays, right-click in the tabular report and select Copy table.
The table data can then be pasted into a document outside of the
analyze application.
Generated tabs Tabs represent the reports selected on the Report Options window.

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6 About Reports

Report Features and Shortcuts (continued)


Selections Description
Print Click to send the report to a designated printer.
Report export options Select a file format option for exported report details.
Report graphic A graphic can be displayed on the report by using the Style button.
Report header area Displays details from the generated report.
Report title A report title be displayed on the report by using the Style button.
Style Click to customize report options, such as font size, graphics, report
title, etc.

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Report Features

REPORT SHORTCUTS
Right-click in the graphic or tabular report area to display report shortcuts.

Report Shortcuts
Selections Description
Autoscale all axes Returns the report to full view after using the zoom feature.
Copy data Copies the report data to the clipboard. It can then be pasted into
other software programs as tab-delimited columns or copied as an
overlay onto another graph.
Copy plot Copies the graph to the clipboard. It can then be pasted into other
software programs.
Copy table Copies the table to the clipboard.
Edit curve Edits available curves from the report.
Reset axis limits to ini- Removes the cross-hair and returns the graph back to the initial set-
tial setting ting.
Set scaling options Edits the axis properties.

Linear / Logarithmic. [button] Select the option to scale the graph


as linear or logarithmic.

Autoscale minimum / maximum. [check box] To manually specify


minimum / maximum autoscale, deselect the option and enter the
new amount in the text box.

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6 About Reports

Report Shortcuts (continued)


Selections Description
Show Gridlines. [check box] Use to enable or disable report
gridlines.

Invert scale. [check box] Use to invert the scale.


Show curve Displays a list of all curves. Select the curve(s) to display.
Show legend Displays or hides the legend.

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Report Features

AXIS CROSS-HAIR
Left-click on the graph to view the cross-hair coordinates.

ZOOM FEATURE
Use the zoom feature to examine graph details. Click, hold, and drag the left mouse button on the
graphical area to be enlarged. A box will display in the area to be enlarged. To return to normal
view, right-click in the graph and select Autoscale all axes.

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6 About Reports

OVERLAY MULTIPLE SAMPLE FILES


To overlay the same type of graph on multiple samples:

1. Go to File > Open.


2. Select a .SMP file, then click Open. If the particle size plot displays, select Advanced from
the view selector drop-down list at the bottom of the window to display the tabbed window
view.
3. Click the Report Options tab.
4. In the Selected Reports list box, highlight a report, then click Overlays.

5. In the Plot Overlay Sample Selection window, move up to 25 files from the Available Files
box to the Selected Files box.
Overlay Sample Selection
Selections Description
Available Files Lists files that meet the selected criteria. Select the files to be com-
[selection] bined, then click Add. The selected files are moved to the Selected
Files list box.
Look in [button] Changes the file folder location. Click the Browse icon.
Reference [button] Compares analysis results for the current sample to those obtained
for a reference sample. Results are shown in the Difference from
Reference Graph report.
Selected Files Lists the files selected to be combined. Click Remove to move a file
[selection] back to the Available Files list box. Click OK to combine the files.

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Overlay Multiple Sample Files

Overlay Sample Selection (continued)


Selections Description
Specification [button] Determines if the results for the current sample are within coarse and
fine specifications. Results are shown in the Out of Specification
Graph report.
Status [drop-down box] Selects the status of files to be combined.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

6. Click OK.
7. Click Preview.

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6 About Reports

REPORT EXAMPLES
BASELINE REPORT

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Combined Report

COMBINED REPORT

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6 About Reports

CUMULATIVE FINER MASS PERCENT VS DIAMETER

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Mass Frequency vs Diameter Report

MASS FREQUENCY VS DIAMETER REPORT

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7 Selected Report Options

7 SELECTED REPORT OPTIONS

To edit reports, open the Sample file then select the Report Options tab. Highlight the
report name in the Selected Reports list box and click Edit.

ADVANCED REPORTS - PYTHON MODULE


The mic Python module is automatically imported when running a user supplied script. The
module provides access to particle size data, and provides support for summary, tabular, and
graphical reports.

n Summary reports. Consist of summary sections, each containing a two-column table of label
and value pairs. Summary reports are created with the mic.summary call.
n Tabular reports. Consist of one or more tables each containing one or more labeled columns
of data. Tabular reports are created with the mic.table call.
n Graphical reports. Consist of a single graph with one or more curves on one or two y-axes.
Graphical reports are created with the mic.graph call.
Calls for accessing the sample file data can be found in the Mic Module Python Calls section of
this appendix. More advanced example python scripts are included in the analyzer software.

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7 Selected Report Options

Advanced Report Options


Up to five Advanced reports, each with up to 10 summary reports, 10 tabular reports, and 10
graphical reports can be created. To use this feature, a file containing a Python script that imports
a "mic" Python module must be created. See MicModule Python Calls on page A - 30 for an
example of a Python script and functions for the "mic" Python module.

1. Create the Python script and save it in the Scripts directory.


2. Open a sample file with a Complete status.
3. Select Advanced in the view selector drop-down list at the bottom of the window to return to
the tabbed view.
4. On the Report Options tab, select Advanced in the Selected Reports list box, then click
Edit.
5. On the Advanced Report Options window, click Add in the Available Scripts group box to
locate and select the Python script. Repeat for each script to be added.

6. In the Selected Reports group box, click the drop-down arrows to select up to five Python
scripts previously added in the Available Scripts box.
7. On the Report Options tab, click Preview. The Python Reports will be included on the tabs
across the top portion of the Reports window.

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Advanced Reports - Python Module

Advanced Reports
Selections Description
Advanced Report 1 Use the drop-down lists to select currently-defined functions used to
through 5 define the report calculations and output.
[drop-down box]
Available Scripts Lists the available reports and provides the option to add, replace,
[group box] edit, or remove reports.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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7 Selected Report Options

BASELINE OPTIONS REPORT
The Baseline report shows a baseline measurement of the x-ray intensity as a function of cell
elevator position.

Select the options to include in the Baseline report.

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Combined Report

COMBINED REPORT
The Combined report combines a selection of any SediGraph report onto a single page.

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7 Selected Report Options

CUMULATIVE TABLE
This tabular report shows the SediGraph's collected data interpolated to a user specified set of
cumulative values rather than being reported at the instrument defined standard particle sizes.
Select which quantities to show in each column of the table.

Cumulative Percent Table


If Percent is selected in Options > Units, then the Cumulative Percent Table is available.

CUMULATIVE FRACTION TABLE


If Percent is selected in Options > Units, then the Cumulative Fraction Table is available.

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Graph Options

GRAPH OPTIONS

n Cumulative Graph Options


n Frequency Graph
n Difference from Ref Graph
n Out of Spec
n Surface Area
n Surface Area Population Options
n Number
n Number Population

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7 Selected Report Options

LOG PROBABILITY REPORT


The Log Probability report plots the particle size distribution with particle size on the x-axis and the
logarithm of the probability on the y-axis

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Particle Size Table

PARTICLE SIZE TABLE


Cumulative Table on page 7 - 6

This tabular report shows the SediGraph's collected data interpolated to a user specified set of
particle sizes rather than being reported at the instrument defined standard particle sizes. Select
which quantities to show in each column of the table.

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7 Selected Report Options

ROSIN RAMMLER

The Rosin Rammler report cannot be edited.

This report shows the sample's particle distribution using a graph of the Rosin Rammler
parameter as a function of the particle diameter.

SAMPLE LOG REPORT

Sample Log reports cannot be edited.

Inserts a log of sample operations in the reports.

This report provides information on:

n Manual control operations performed during analysis.


n Information entered using Add Log Entry on the sample file editor.
n Warnings and/or errors which occurred during analysis.

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Standard Class Size Table Report

STANDARD CLASS SIZE TABLE REPORT


This tabular report shows the SediGraph's collected data measured at the instrument defined
standard set of particle sizes. Select which quantities to show in each column of the table.

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7 Selected Report Options

STANDARD SIEVE TABLE


This tabular report shows the SediGraph's collected data interpolated to a set of standard sieves
rather than reported at the instrument defined standard particle sizes. Select which quantities to
show in each column of the table.

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Summary Report Options

SUMMARY REPORT OPTIONS


The Summary report allows the user to select relevant statistical measures to characterize the
sample and show these results on a single report page.

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8 Diagnostics

8 DIAGNOSTICS
Unit [n] > Diagnostics
Use to display diagnostic readings, start diagnostic tests, and open saved diagnostic reports.
Each test generates a file to the default directory name and path of ...\...\Service\userdiag unless
another directory name was specified. These reports can be sent to a Micromeritics Service
Representative for examination.

SAVE FILES FOR PROBLEM DIAGNOSIS


Unit [n] > Diagnostics > Save Files for Problem Diagnosis
Use to compress pertinent diagnostic information into a single zip file. This file can be sent to a
Micromeritics Service Representative for problem resolution.

1. Complete the form. A default file named Diagnostics-[date].zip is created unless another file
name is specified.
2. Add any files that are related to the problem — such as sample files — and save the file.
3. Send an email to [email protected] for instructions on how to transfer
the .ZIP files to Micromeritics.
Save Files for Problem Diagnostics
Selections Description
Problem description Enter information that would be helpful to the Micromeritics rep-
[text box] resentative.
Include Files Add. Click to select additional files to send with this problem
diagnosis.

Delete. Select the file in the Include Files box, then click Delete to
remove the file from the list.

Clear. Click to clear all files from the Include Files box.

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8 Diagnostics

Save Files for Problem Diagnostics (continued)


Selections Description
Save As [button] Click to specify the name and location of the compressed file. Make a
note of the file name and location. This file will need to be sent to
your Micromeritics representative for problem resolution.
Micromeritics Enter the name of your Micromeritics representative. This inform-
representative [text box] ation will remain on the window each time files for problem diagnosis
need to be submitted (can be modified as necessary).
User Information Enter information for the person to be contacted by a Micromeritics
[text box] representative. This information will remain on the window each time
files for problem diagnosis need to be submitted (can be modified as
necessary).

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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9 Maintenance and Troubleshooting

9 MAINTENANCE AND TROUBLESHOOTING

Do not modify this instrument without the authorization of a Micromeritics service per-
sonnel.

Improper handling, disposing of, or transporting potentially hazardous materials can


cause serious bodily harm or damage to the instrument. Always refer to the MSDS
when handling hazardous materials. Safe operation and handling of the instrument,
supplies, and accessories is the responsibility of the operator.

When lifting or relocating the instrument, use proper lifting and transporting devices for
heavy instruments. Ensure that sufficient personnel are available to assist in moving
the instrument. The 5125 SediGraph II Plus weighs approximately 43 kg (95 lb). The
MasterTech weighs approximately 18 kg (40 lb).

Use of a power cord or power supply not provided with the instrument could cause
personal injury or damage to the equipment. If a replacement is needed, contact your
Micromeritics Service Representative. Detachable power supply cords with an
inadequate rating could cause significant instrument damage or physical harm.

Do not add anything between the power cord and the power source that would
compromise the earth ground.

Do not remove or disable the grounding prong on the instrument power cord.

If the equipment needs to be relocated, check with your Micromeritics service


representative. The equipment must be positioned such that the mains supply is not
obstructed and is easily accessible to disconnect the equipment from the AC main
power supply.

The analyzer has been designed to provide efficient and continuous service; however, certain
maintenance procedures should be followed to obtain the best results over the longest period of
time. When unexpected results occur, some common operational problems not indicated on the
window and their respective causes and solutions are provided.

The following can be found on the Micromeritics web page (www.Micromeritics.com).


n Error Messages document (PDF)
n Parts and Accessories

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9 Maintenance and Troubleshooting

Most operational problems are caused by:


n Deteriorated or blocked tubing
n Air leaks
n An unlevel analyzer
When unexpected analysis results occur, check the above first. Some common operational
problems not indicated on the window and their respective causes and solutions are provided
below:

Cell cannot be filled or drained.

Cause A: Blocked or damaged tubing.


Action A: Locate and replace blocked or damaged tubing. See Replace the Flexible Tubing
on page 9 - 18.
Cause B: Blocked cell input or output port.
Action B: Clean analysis cell. See Replace the Analysis Cell Assembly on page 9 - 9.
Cause C: Valve or pump not working properly.
Action C: From Manual Control window, check pump and valve operation. If either is not work-
ing properly, contact authorized service personnel.
Cause D: Tubing improperly installed.
Action D: Install the tubing. See Replace the Flexible Tubing on page 9 - 18.

Cell cannot be raised or lowered

Cause: Elevator which moves cell is stuck.


Action: Check flexible tubing for possible obstruction to elevator movement. If necessary,
reposition tubing. Also check for any other obstruction to elevator movement.

Mixing chamber cannot be filled or drained.

Cause A: Blocked or damaged tubing.


Action A: Locate and replace blocked or damaged tubing.See Replace the Flexible Tubing
on page 9 - 18.
Cause B: Blocked mixing chamber input or output port.
Action B: Clean mixing chamber. See Clean the Mixing Chamber and Bezel on page 9 -
17.
Cause C: Valve or pump not working properly.
Action C: From Manual Control window, check pump and valve operation. If either is not work-
ing properly, contact authorized service personnel.

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9 Maintenance and Troubleshooting

Cause D: Tubing improperly installed.


Action D: Install the tubing. See Replace the Flexible Tubing on page 9 - 18.

Mixing chamber suspension is turning brown

Cause: Teflon coating on stirring bar is worn.


Action: Replace stirring bar.

X-RAY ON indicator is turned on, but the computer display shows 0 kilocounts.

Cause A: Analysis compartment door not completely closed.


Action A: Close analysis compartment door.
Cause B: Cell is in a position which blocks beam.
Action B: Move cell to proper operating position. Enable Manual Control, access the pop-up
menu on the cell, and select Move Cell Position.
Cause C: Cell is clogged.
Action C: Remove and clean cell. See Clean the Analysis Cell Assembly on page 9 - 11.
Cause D: Slits in collimator blocked.
Action D: Clean the collimator. See Clean the Collimator Slits on page 9 - 14.
Cause E: X-ray source or detector has failed.
Action E: Contact authorized service personnel.

X-RAY STANDBY indicator was turned on, but when keyswitch is placed in X-RAY
ON position, XRAY ON indicator does not turn on.

Cause A: Keyswitch is between positions.


Action A: Move keyswitch to X-RAY STANDBY position and then back to X-RAY ON position
while observing indicator.
Cause B: X-RAY ON indicator lamp is burned out.
Action B: Replace lamp. See Replace the X-ray Indicator Lamps on page 9 - 23.
Cause C: X-ray filament supply not available or X-ray unit damaged.
Action C: Contact authorized service personnel in accordance with service contract.
Cause D: Rear panel is off, the top cover is off, or the fluid module is not fully installed.
Action D: Replace all panels.
See Cause of Bubbles on page 9 - 27 first to determine the cause of the bubbles. Perform the

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9 Maintenance and Troubleshooting

outlined procedure then return to this table for corrective action.

Bubble elimination problem.

Cause A: Windows are dirty or misaligned.


Action A: Clean or replace the windows.See Clean the Analysis Cell Assembly on page 9
- 11.
Cause B: Inlet port on the cell assembly is loose.
Action B: Replace the cell assembly. See Replace the Analysis Cell Assembly on page 9
- 9.
Cause C: A valve has failed.
Action C: Contact authorized service personnel.

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Safe Servicing

SAFE SERVICING

Do not modify this instrument without the authorization of a Micromeritics service per-
sonnel.

To ensure safe servicing and continued safety of the instrument after servicing, service personnel
should be aware of the following risks:

Product specific risks that may affect service personnel:


n Electrical. Servicing or repair could require opening the outer panels and exposing ener-
gized electrical components.
n MasterTech Fuses. Only use fuses rated as:

Power Source Required Fuses


100/120VAC Single fuse, 3AG (Slo-Blo) 250V, 2.5A, 6.35mm x
31.75mm. Single pole input.
220/240VAC Double fuse, Time-lag (Slo-Blo), 250V, 1.25A, 5mm x
20mm. Double pole input.

Protective measures for these risks:


n Electrical. The majority of electrical components operate at low voltage (24V or less) and
pose low risk when energized. Maintenance, troubleshooting, and repairs should be per-
formed with the instrument de-energized whenever possible, in accordance with standard
electrical safety guidelines.
n MasterTech Fuses. Use of improperly rated fuses could cause damage to the equipment.
n Power off and unplug the analyzer from the power outlet prior to servicing.

Verification of the safe state of the instrument after repair:


n All instrument panels and covers installed.

PARTS AND ACCESSORIES


Parts and accessories can be found online at www.Micromeritics.com.

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9 Maintenance and Troubleshooting

POWER
The SediGraph is designed to operate with universal input power supply (100/120/220/240VAC,
47/63 Hz, 450VA). The power outlet should be able to supply 15 amps@ 100 or 115VAC ±10% or
7.5 amps @ 240VAC ±10%. These requirements can be checked by using a circuit analyzer
(available at most hardware or electronic supply houses) or a multimeter. There should also be
sufficient outlets for the computer, monitor, printer, and any other peripheral devices. The power
cord, IEC, 300V, 10A (available in the accessories kit) should be connected to noise-free power of
the correct voltage and frequency, with a safety earth ground, through a standard wall receptacle.

The MasterTech 052 leaves the factory set for 120VAC and with the line fuse removed. The
correct setting of the universal power entrance must be checked, and the appropriate fuse
installed before the MasterTech can be operated. The MasterTech is designed to operate with
either 100/120/220/240VAC at 50/ 60 Hz. Voltage selection and fusing are made at the power
connector which is located on the rear panel of the unit.

The instrument should be connected to a switch which meets relevant requirements of IEC 60947-
3 or a circuit breaker which meets the relevant requirements of IEC 60947-2.

Noise-free power of the correct voltage and frequency, with a safety earth ground, should be
available through a standard wall receptacle. There should be a minimum 15A rated breaker
@ 100/120VAC and a minimum 7.5A @ 240VAC.

The analyzer and peripheral devices must be installed on their own dedicated power
line. Other devices — such as motors, generators, or ovens — should not be placed
on the same power line.

Replacement power supply cords must be rated for the specifications stated above.

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Enable Manual Control

ENABLE MANUAL CONTROL


Unit [n] > Enable Manual Control
Show Instrument Schematic on page 2 - 20

Use to enable the manual control of certain system valves and pump components on the analyzer
schematic. When this option is enabled, a checkmark appears to the left of Unit [n] > Enable
Manual Control. If the analyzer schematic is not immediately visible, go to Unit [n] > Show
Instrument Schematic.

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9 Maintenance and Troubleshooting

PREVENTIVE MAINTENANCE
Perform the following preventive maintenance procedures to keep the analyzer operating at peak
performance. Micromeritics also recommends that preventive maintenance procedures and
calibration be performed by a Micromeritics Service Representative every 12 months.

A Micromeritics service technician should perform the following procedures every 12 months. Do
not attempt to perform these procedures yourself.

n Clean the high voltage area


n Calibrate the X-ray control system
n Calibrate the fluid control system
n Calibrate the temperature control system

Maintenance Required Frequency


Perform a reference material run Every week
Clean the analyzer Every 30 days*
Clean the mixing chamber and bezel As needed
Clean the analysis cell Every 30 days*
Replace the mixing pump and cell pump tubing Every 30 days*
Replace the analysis cell tubing As needed
Clean the air filter Every 30 days*
Check the operation of the mixing pump Every 30 days*
Check the operation of the cell pump Every 30 days*
Check the level of the analyzer Every 30 days*
Clean the collimating slits As needed

* Or every 160 analyses, which ever comes first

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Analysis Cell Assembly

ANALYSIS CELL ASSEMBLY

Replace the Analysis Cell Assembly


If the analysis cell assembly becomes damaged, it may be necessary to replace it.

1. Go to Unit [n] > Drain and Load.


2. Select Leave mixing chamber empty.
3. Click Continue.
4. When prompted to load the sample, click Cancel.
5. Power OFF the Pump Control.
6. Open the transparent sliding door to the analysis compartment.
7. Loosen the cell mounting screw and remove the cell from the retaining bracket.

A. Flexible analysis cell tubing

8. Carefully remove the flexible tubing from the two ports on the cell.

9. Connect the flexible tubing to the ports on the new analysis cell
10. Insert the cell in the retaining bracket and tighten the cell mounting screw.
11. Power ON the Pump Control.

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9 Maintenance and Troubleshooting

Replace the Analysis Cell Tubing


1. Drain the system. See Drain the System on page 9 - 22.
2. Place the Pump Control switch on the analyzer front panel in the OFF position
3. Open the transparent sliding door to the analysis compartment.

A. Flexible analysis cell tubing


B. Back connector (for back cell port tubing)
C. Front connector (for front cell port tubing)

4. Remove the flexible analysis cell tubing from the rigid tubing connector in the analysis com-
partment.
5. Loosen the cell mounting screw and remove the cell from the retaining bracket as shown
below.

A. Flexible analysis cell tubing

6. Remove the flexible analysis cell tubing from the two ports on the cell.
7. Connect the new flexible analysis cell tubing to the ports on the new analysis cell and to the
rigid tubing connector. The tubing for the front port of the cell connects to the front rigid
tubing connector and the tubing for back port of the cell connects to the back rigid tubing
connector.

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Analysis Cell Assembly

8. Insert the cell in the retaining bracket and tighten the cell mounting screw.
9. Close the analysis compartment door.
10. Power ON the Pump Control.
Clean the Analysis Cell Assembly
The analysis cell should be removed periodically and cleaned to remove any residue.

1. Go to Unit [n] > Drain and Load.


2. Select Leave mixing chamber empty.
3. Click Continue.
4. When prompted to load the sample, click Cancel.
5. Place the Pump Control switch on the analyzer front panel in the OFF position.
6. Open the transparent sliding door to the analysis compartment. Loosen the cell mounting
screw and remove the cell from the retaining bracket.

A. Flexible analysis cell tubing

7. Carefully remove the flexible tubing from the rigid tubing connector which is mounted along
the right side of the analysis compartment.
8. Carefully remove the flexible tubing from the two ports on the cell.

9. Disassemble the cell by removing the ten screws in the cell window retaining plates.

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9 Maintenance and Troubleshooting

Do not use cloth made of a coarse material or abrasive cleansers when cleaning the
cell windows. Particles may lodge in scratches, which could alter X-ray pulse rates
and cause invalid analysis results.

10. Use either IPA or a mild detergent to clean the cell windows. Use an air blower to remove
any debris from the cell body, window retaining plates, and ports.

11. Assemble the cell by placing a cell window and a cell window retaining plate on each side of
the cell body. The cell window retaining plate must be positioned so that the sloped part
matches that of the cell body and other plate.

Ensure the sloped portions of the cell body and retaining


plates are aligned.

12. Insert the ten screws removed in step 8 into the window retaining plates, but do not tighten.

When assembling the cell, alternate the tightening of screws. Failure to do so could
result in air entering the cell, causing bubble elimination problems.

13. Using a screwdriver, tighten the screws around the cell by tightening one screw and then
tightening the screw diagonally opposite that screw. See the following illustration for the
tightening sequence. This sequence helps to ensure uniform closure around the cell.

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Analysis Cell Assembly

14. Connect the flexible tubing to the ports on the analysis cell and to the rigid tubing connector.
The tubing for the front port of the cell connects to the front rigid tubing connector. The
tubing for the back port of the cell connects to the back rigid tubing connector.
15. Insert the cell in the retaining bracket and tighten the cell mounting screw.
16. Place the Pump Control switch in the ON position.
17. Go to Unit [n] > Rinse > SediGraph.

18. Select Autorinse then click Continue to rinse the analysis cell.

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9 Maintenance and Troubleshooting

CLEAN THE COLLIMATOR SLITS


Replace the Analysis Cell Assembly on page 9 - 9

The collimator slits may become blocked by dust or debris which accumulates in the analysis
compartment over a period of time, causing inaccurate results.

1. Power OFF the analyzer.


2. Remove the retaining screws from the top of the analyzer; then remove the top panel.
3. Remove the analysis cell. See Replace the Analysis Cell Assembly on page 9 - 9 for
removal instructions.
4. Remove the two foam plugs in the top of the analysis module.
5. Use a hex driver with an extension to remove the collimator retaining screws.
6. Reach through the door of the analysis compartment to lift the top collimator out of the
analysis module.

A. Foam plugs
B. Collimator retaining screws

7. Use a lint-free cloth to clean the shiny area near the center of the collimator removed and
the corresponding area of the collimator remaining in the analysis module.

Do not use cloth made of a coarse material or abrasive cleansers when cleaning the
collimating slits.

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Clean the Collimator Slits

8. Replace the top collimator and the retaining screws.

Tighten the collimator retaining screws only enough to securely hold the collimator in
place. Over-tightening the screws can close the collimating slits, reducing the intensity
of (or completely blocking) the X-rays.

9. Tighten the retaining screws for the top collimator.


10. Replace the two foam plugs in the top of the analysis module.
11. Replace the analysis cell and the top panel.
12. Power ON the analyzer.

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9 Maintenance and Troubleshooting

CLEAN THE AIR FILTER


The air filter on the analyzer should be cleaned every 30 days (more often in environments with
increased levels of dust) and replaced once a year.

1. Slide out the drip tray on the front of the analyzer.

A. Air filter
B. Drip tray

2. Remove the air filter from drip tray by squeezing the filter while pulling it away from the drip
tray.
3. Rinse the filter thoroughly and shake out the excess water. Place it aside and allow it to dry.
4. Install a new filter or after the filter has dried, replace it.
5. Check to see that the analyzer is level.

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Clean the Instrument

CLEAN THE INSTRUMENT


The exterior casing of the instrument may be cleaned using a clean, lint-free cloth dampened with
isopropyl alcohol (IPA), a mild detergent, or a 3% hydrogen peroxide solution. Do not use any type
of abrasive cleaner. It is not necessary to remove knobs, screws, etc. while cleaning. If a
MasterTech is installed, clean it in the same manner.

n Do not allow liquid to penetrate the casing of the analyzer. Doing so could result in
damage to the unit.
n Use only a mild detergent in water to clean safety shields. The use of isopropyl
alcohol can damage the shield surface.

CLEAN THE MIXING CHAMBER AND BEZEL


The mixing chamber bezel should be cleaned periodically to prevent contaminants from entering
the mixing chamber. To clean the bezel:

n Remove the bezel and clean using a mild detergent. Rinse, then dry thoroughly before
replacing it on the mixing chamber.

The mixing chamber should be removed and cleaned periodically to remove any residue.

When cleaning the mixing chamber, avoid getting the electrical connections wet. Do
not immerse the chamber in liquid. Doing so could damage the system.

1. Drain the mixing chamber.

a. Go to Unit [n] > Drain and Load.


b. Select Leave mixing chamber empty.
c. Click Continue.
d. When prompted to load the sample, click Cancel.

2. Disconnect the flexible tubing from the mixing chamber, exercising caution to prevent dam-
age to the tubing.
3. Disconnect the electrical cable.

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9 Maintenance and Troubleshooting

A. Flexible tubing
B. Flexible tubing
C. Flexible tubing
D. Flexible tubing
E. Flexible tubing
F. Electrical cable

4. Clean the chamber using IPA or a mild detergent. Rinse thoroughly. All ports should be
cleaned using an air blower.
5. Reconnect the tubing to the mixing chamber.
6. To reconnect the mixing chamber, ensure the tubing is securely fastened at each port.
7. Reconnect the electrical cable.

REPLACE THE FLEXIBLE TUBING


Drain and Load Operation on page 5 - 2

The analyzer includes a complete plumbing system for circulation of sedimentation liquid and
particle suspension between the cell, the mixing chamber, an external rinse container, and an
external waste container. In order for the system to operate properly, damaged or deteriorated
tubing must be replaced.Tubing from the mixing pump, the cell pump, and the analysis cell can be
replaced independently.

Use the tube installation tool to help install the tubing. It is included in the tool
accessories kit.

When replacing tubing, always drain the system first.

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Check the Mixing Pump Operation

CHECK THE MIXING PUMP OPERATION


The mixing pump should be checked every 30 days (or every 160 runs, whichever comes first) to
see if it is operating correctly.

1. Go to Unit [n] > Enable Manual Control to display the instrument schematic.
2. Right-click the Mixing Pump icon, then select Turn on from the pop-up menu.

A. MasterTech pump
B. Mixing pump
C. Mixing chamber
D. Cell pump
E. Analysis cell
F. MasterTech arm
G. MasterTech stirrer
H. MasterTech Beaker
Items in the red box show only if
MasterTech is installed

3. If the pump fails to start, refer to the Reset the Mixing Pump and Cell Pump on page 9 -
21.
4. Right-click on the Mixing Pump icon.
5. Select Turn off from the pop-up. If the pump fails to stop, the fluid control board may need
replacing. Contact your service representative.

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9 Maintenance and Troubleshooting

CHECK THE CELL PUMP OPERATION


Reset the Mixing Pump and Cell Pump on the facing page

The cell pump should be checked every 30 days (or every 160 runs, whichever comes first) to see
if it is operating correctly.

1. Go to Unit [n] > Enable Manual Control to display the instrument schematic.
2. Right-click the Cell Pump icon, then select Turn on from the pop-up.

A. MasterTech pump
B. Mixing pump
C. Mixing chamber
D. Cell pump
E. Analysis cell
F. MasterTech arm
G. MasterTech stirrer
H. MasterTech Beaker
Items in the red box show only if
MasterTech is installed

3. Perform the following steps. If any of these steps fail, seeReset the Mixing Pump and Cell
Pump on the facing page .

For each of the following steps, right-click the Cell Pump icon, then select the item listed:

n Increase speed
n Decrease speed
n Flow up in cell
n Flow down in cell
n Increase speed
n Decrease speed

4. Right-click the Cell Pump icon, then select Turn off. If the pump fails to stop, the fluid
control board may need replacing. Contact a service representative.

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Reset the Mixing Pump and Cell Pump

RESET THE MIXING PUMP AND CELL PUMP


If an electrical overload occurs with the mixing pump or the cell pump, the pumps should be rest.

1. Power OFF the Pump Control.


2. Allow the internal varistor to cool down (approximately two to three minutes).
3. Check the tubing to verify that it is routed properly.
4. Place the Pump Control switch in the AUTO position.
5. Check the pump operation.

Contact your Micromeritics service representative if the problem continues.

REPLACE THE CELL WINDOWS


Clean the Analysis Cell Assembly on page 9 - 11

X-ray photons from the X-ray source pass through the cell windows to the X-ray detector on the
other side of the cell. If cell windows become scratched or damaged, settling particles may
become entrapped. This could alter X-ray pulses, resulting in invalid analyses. The analysis cell
windows should be replaced when necessary.

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9 Maintenance and Troubleshooting

DRAIN THE SYSTEM


Unit [n] > Drain and Load
Drain and Load Operation on page 5 - 2

Ensure that the outlet tube is in the waste reservoir and the rinse tube is in the rinse liquid
reservoir.

1. Select Leave mixing chamber empty.


2. Click Continue. A progress message displays.
3. Click Cancel.

CHECK THE LEVEL OF THE ANALYZER


An unlevel analyzer may cause inaccurate analyses. Check every 30 days to see if the analyzer is
level.

1. Open the analysis compartment door and locate the level indicator.
2. Look straight down at the indicator. The analyzer is level when the bubble is centered inside
the black circle on the level indicator.

Level indicator

3. If the analyzer is not level, lift the corner of the analyzer then turn the appropriate foot
counterclockwise to raise the unit or clockwise to lower the unit.

4. Set the analyzer down and observe the indicator. The bubble should be centered inside the
black circle on the level indicator.

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Replace the X-ray Indicator Lamps

REPLACE THE X-RAY INDICATOR LAMPS


The X-RAY STANDBY indicator and the X-RAY ON indicator on the front panel of the analyzer
contain an internal lamp.

If the X-RAY ON indicator lamp is burned out or installed incorrectly, the instrument
will be inoperative.

Disconnect the analyzer power cord from the AC power source before attempting to
replace the lamp. Failure to do so could result in electrical shock or damage to the
instrument.

1. Remove the cover lens from the analyzer by prying with a flat object.

2. Using a flat object, pull the lever which raises the lamp socket out of the lamp compartment.

3. Remove the lamp by pulling it away from the socket.

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9 Maintenance and Troubleshooting

4. Push lamp socket lever toward the analyzer and insert replacement lamp into socket.

5. Replace the indicator cover lens.


6. Connect the analyzer power cord to an AC power source.
7. Power ON the analyzer.
8. Place the keyswitch in the appropriate position.
9. Verify that the lamp is working.

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Replace the Mixing Pump Tubing

REPLACE THE MIXING PUMP TUBING


1. Place the analyzer on the edge of a table or flat surface.
2. Remove the pump chassis cover.
3. Drain the system. See Drain the System on page 9 - 22.
4. Power OFF the Pump Control.
5. Rotate the mixing pump lever to the left (the mixing pump is the pump on the right) to place
the mixing pump housing in the open position.

A. Mixing pump lever (open position)


B. Mixing pump tubing

6. Remove the mixing pump flexible tubing from the rigid tubing connectors on both sides of
the pump. Discard the used tubing.
7. Using the tube installation tool supplied in the accessories kit, attach one end of the new
flexible mixing pump tubing to the rigid tubing connector on the right.
8. Thread the tubing through the pump as shown below.

9. Attach the other end of the tubing to the rigid connector on the left.
10. Rotate the mixing pump lever to the right to place the mixing pump housing in the closed
position.
11. Replace the pump chassis cover.
12. Power ON the Pump Control.

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9 Maintenance and Troubleshooting

PERFORM A REFERENCE MATERIAL ANALYSIS


It is a good practice to perform a reference material analysis every week to ensure that the
analyzer is operating within specifications. Reference material kits, including instructions for
performing the reference material analysis, are available from Micromeritics.

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Cause of Bubbles

CAUSE OF BUBBLES
If bubble problems continue to exist, perform the following steps to determine their source.

1. Install a clean, cell assembly in the cell holder and ensure it is free of bubbles.
2. Go to Unit [n] > Baseline and perform the steps for collecting baseline data.

If the analyzer is successful in obtaining a baseline, the cell proceeds to a parked position,
indicating that bubbles are caused by:

n improper tubing routing,


n a failed valve,
n window misalignment, or
n a loose inlet / outlet port on the cell assembly.

If the analyzer is unable to obtain a baseline, an error message appears in the lower status
window. This indicates X-ray detection and / or generation problems may be present.
Contact your Micromeritics service representative for corrective action.

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9 Maintenance and Troubleshooting

POWER INSTRUMENT ON AND OFF

DO NOT connect or disconnect cables when the instrument is powered ON.

Power ON the equipment in the following order:

1. Computer, monitor, and printer.


2. Place the Pump Control switch (located on the front panel) in the AUTO position.
3. Analyzer.
4. Insert the X-ray key into the X-ray keyswitch then turn the switch to the X-RAY ON position.
5. Wait 30 minutes for the analyzer to warm up before performing an analysis.

It is recommended that the analyzer remain on unless it is going to be idle for a period
of more than 24 hours. Leaving the analyzer on helps prolong the life of its major com-
ponents.

Power OFF the equipment in the following order:

Always exit the analysis program before turning off the computer. Failure to do so
could result in loss of data.

1. Exit the analysis program. If an analysis is in progress when closing the application, the fol-
lowing message is displayed:
Instrument is busy. Continue program exit?

Select Yes and the analysis program closes. The analysis continues and data
continue to be collected. Queued reports under the printer will print. If a
power failure occurs and an uninterruptible power supply (UPS) is not
attached to the analyzer, the data collected after exiting the analysis program
are lost.

Select No to continue the analysis. Select Yes to close the application.


2. Computer, monitor, printer.
3. Analyzer.

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Recover from a Power Failure

RECOVER FROM A POWER FAILURE


The analyzer saves entered and collected data in case of power failure. File parameters and any
other data entered will still be present when power is restored. If an analysis was in progress when
the power failure occurred, it will be canceled when the analyzer restarts. Any data collected
during the analysis will still be present, but the analysis should be restarted in order to produce
complete results.

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9 Maintenance and Troubleshooting

MASTERTECH TROUBLESHOOTING AND MAINTENANCE


Power failure

Cause A: Power cable not connected or switch not in ON position.


Action A: Make sure power cable is plugged into the power source and the power
ON/OFF switch is in the ON position.
Cause B: Input power fuse blown.
Action B: Replace the fuse. See Replace the MasterTech Input Power Fuse on the
facing page.

Stirrer will not work.

Cause: Stirrer is improperly connected.


Action: Check the stirrer’s electrical connection.

Turntable will not move.

Cause: Arm is in the LOAD position.


Action: Press the AUTO/LOAD switch on the front panel to lower the arm.

MasterTech pump will not run.

Cause: Pump switch on the front panel may be in the OFF position.
Action: Press the pump AUTO/ OFF switch on the front panel.

Ultrasonic probe will not work.

Cause: Probe improperly connected to the MasterTech.


Action: Check the MasterTech connector cable.

Ultrasonic agitation diminished.

Cause: The ultrasonic probe tip may need replacing.


Action: See Replace the MasterTech Ultrasonic Probe Tip on the facing page.

MasterTech will not initiate commands from the computer.

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Replace the MasterTech Ultrasonic Probe Tip

Cause: The cable may be connected improperly from the MasterTech to the computer.
Action: Check the cable connections.

Pump leaks or is not operating efficiently.

Cause: Tubing is leaking or clogged.


Action: See Replace the Flexible Tubing on page 9 - 18.

REPLACE THE MASTERTECH ULTRASONIC PROBE TIP


Parts and accessories can be found online at www.Micromeritics.com.

After extended periods of use, the tip of the ultrasonic probe on the MasterTech may become
pitted, causing diminished agitation.

1. Remove the damaged tip from the probe using the wrenches provided.
2. Attach the new probe tip to the probe body. Use the wrenches to tighten securely.

Never hold the probe by the tip. Doing so may cause damage to the probe.

REPLACE THE MASTERTECH INPUT POWER FUSE

A. Power switch
B. Power connector
C. Fuse cover

n The power cord should be disconnected from the instrument before removing the
cover from the input power connector. Failure to disconnect the power cord could
result in electrical shock.
n The input power connector can be used with either a single-fuse arrangement
(100/120VAC) or a double-fuse arrangement (220/240VAC). Use the
appropriate fuse(s) for the input power source. The fuses must be identical in type
and rating to that specified. Use of other fuses could result in electrical shock
and/or damage to the instrument.

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9 Maintenance and Troubleshooting

Fuses may be obtained from Micromeritics or a vendor of your choice as long as they
meet the requirements specified in this section.

Power Source Required Fuses


100/120VAC Single fuse, 3AG (Slo-Blo) 250V, 2.5A, 6.35mm x 31.75mm. Single
pole input.
220/240VAC Double fuse, Time-lag (Slo-Blo), 250V, 1.25A, 5mm x 20mm. Double
pole input.

1. Ensure the instrument is powered OFF and the power cord is disconnected.
2. Open the cover to the right of the power entrance and remove the fuse block by inserting the
tip of a small pocket screwdriver (or pointed object) in the left side of the power module then
gently prying the cover open.

Do not to pry in the middle of the cover near the hinges. Doing so may break the
hinge.

A. Fuse cover closed


B. Fuse cover opened (swing to
the left)
C. Fuse block removed

3. Gently lift until the cover opens approximately 1/4 inch, then swing the hinged cover to the
left.
4. Remove the fuse block. If necessary, use needle-nose pliers to grasp the block.
5. Insert the appropriate fuse(s) for the input power source.

6. Position the fuse block so that the side containing the fuse(s) is facing the power module
and insert it into the connector. Do not close the cover.
7. Fuse the power line according to local safety practices.

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Replace the MasterTech Input Power Fuse

n If the single-fuse arrangement is used, the fuse block is positioned so that the side with the
single-fuse slot and the jumper bar is away from the cover.

n If the double-fuse arrangement is used, the fuse block is positioned so that the side with
the double-fuse slots is away from the cover (insert just opposite of single-fuse
arrangement).

8. Snap the fuse block and cover assembly back into the input power connector. If the fuse
block does not seat properly:

a. Remove the fuse block retaining screw.


b. Lift the fuse block from the cover.
c. Rotate the fuse block.
d. Mount the fuse block to the cover.
e. Replace the retaining screw.

Once the fuse block and cover assembly are in place, the position of the indicator pin shows the
input power selected.

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A Advanced Reports - Python Module

A ADVANCED REPORTS - PYTHON MODULE


The mic Python module is automatically imported when running a user supplied script. The
module provides access to particle size data, and provides support for summary, tabular, and
graphical reports.

n Summary reports. Consist of summary sections, each containing a two-column table of label
and value pairs. Summary reports are created with the mic.summary call.
n Tabular reports. Consist of one or more tables each containing one or more labeled columns
of data. Tabular reports are created with the mic.table call.
n Graphical reports. Consist of a single graph with one or more curves on one or two y-axes.
Graphical reports are created with the mic.graph call.
Calls for accessing the sample file data can be found in the Mic Module Python Calls section of
this appendix. More advanced example python scripts are included in the analyzer software.

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A Advanced Reports - Python Module

ADVANCED REPORT OPTIONS


Up to five Advanced reports, each with up to 10 summary reports, 10 tabular reports, and 10
graphical reports can be created. To use this feature, a file containing a Python script that imports
a "mic" Python module must be created. See MicModule Python Calls on page A - 30 for an
example of a Python script and functions for the "mic" Python module.

1. Create the Python script and save it in the Scripts directory.


2. Open a sample file with a Complete status.
3. Select Advanced in the view selector drop-down list at the bottom of the window to return to
the tabbed view.
4. On the Report Options tab, select Advanced in the Selected Reports list box, then click
Edit.
5. On the Advanced Report Options window, click Add in the Available Scripts group box to
locate and select the Python script. Repeat for each script to be added.

6. In the Selected Reports group box, click the drop-down arrows to select up to five Python
scripts previously added in the Available Scripts box.
7. On the Report Options tab, click Preview. The Python Reports will be included on the tabs
across the top portion of the Reports window.

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Advanced Report Options

Advanced Reports
Selections Description
Advanced Report 1 Use the drop-down lists to select currently-defined functions used to
through 5 define the report calculations and output.
[drop-down box]
Available Scripts Lists the available reports and provides the option to add, replace,
[group box] edit, or remove reports.

For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.

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A Advanced Reports - Python Module

SCRIPTS

Run a Script
1. Open a sample file with a Complete file status.
2. Select Advanced in the view selector drop-down list at the bottom of the window.
3. Select the Report Options tab.
4. Highlight Advanced in the Selected Reports list box, then click Edit.
5. On the Advanced Report Options window, click Add.
6. Locate and select one or more python scripts then click Select. The selected scripts
become a part of the drop-down list in the Available Scripts section of the Advanced Report
Options window.
7. In the Select Reports section, select up to five Advanced reports in the drop-down lists.
8. Click OK.
9. Click Preview on the Report Options tab to view all reports selected in the previous window.
Remove a Script
Select the script in the Available Scripts box then click Remove. The script is removed from the
application however, the original .py text file is not affected.

Edit a Script

Selections Description
Add [button] Adds one or more scripts to the Available Scripts box. The added
scripts then become available as options in the Selected Reports
section.
Edit [button] Edits the script stored within the application but does not affect the
original .py text file.
Remove [button] Removes the script from the Available Scripts box but does not affect
original .py text file.
Replace [button] Replaces the contents of the selected script however, the script
name remains the same.

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Python Reports

PYTHON REPORTS

Graphic Report
This script is an example of the mic module producing a graph with two curves:

1 import mic
2 import numpy as np
3
4 mic.graph( 'My Graph', 'X', 'F(X)' )
5 myx = np.array( [0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0 ] )
6 mic.graph.add( 'X2', myx, myx*myx, marker='o' )
7 mic.graph.add( 'sin(X)', myx, np.sin(myx), marker='^' )

The results are:

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A Advanced Reports - Python Module

Summary Report
This script produces a summary report with two summaries:

1 import mic
2 import numpy as np
3
4 mic.summary( "My Summaries" )
5 mic.summary.add( "Summary A",
6 ["Label 1:", "Label 2:", "Label 3:"],
7 ["val1", "val2", "val3"] )
8 mic.summary.add( "Summary B",
9 ["Label 4:", "Label 5:", "Label 6:"],
10 ["val4", "val5", "val6"] )

The result is:

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Python Reports

Tabular Report
If more than one column is required, the call mic.table is employed. This script produces a tabular
report consisting of two tables.

This script uses the Python package numpy and c-style formatting of the numerical
values.

11 import mic
12 import numpy as np
13
14 mic.table( "My Tables" )
15 mic.table.addtable( "My Set A" )
16 mic.table.addcolumn( "X", ["1.0", "2.0", "3.0"] )
17 mic.table.addcolumn( "Y", ["0.5", "1.0", "1.5"] )
18 x1 = 0.2
19 x2 = 0.5
20 x3 = 3.14159/2
21 mic.table.addtable( "My Set B" )
22 mic.table.addcolumn( "X", ['{:8.3f}'.format(x1),
23 '{:8.3f}'.format(x2),
24 '{:8.3f}'.format(x3)] )
25 mic.table.addcolumn( "sin(X)", ['{:8.3f}'.format(np.sin(x1)),
26 '{:8.3f}'.format(np.sin(x2)),
27 '{:8.3f}'.format(np.sin(x3))] )
28 mic.table.addcolumn( "cos(X)", ['{:8.3f}'.format(np.cos(x1)),
29 '{:8.3f}'.format(np.cos(x2)),
30 '{:8.3f}'.format(np.cos(x3))] )

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A Advanced Reports - Python Module

The result is:

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Acquire Basic Information

ACQUIRE BASIC INFORMATION


The following script generates a report that lists sample information, material properties, analysis
options, and collected sedimentation data. See Get Particle Sizing Sample on page A - 18 for
API information.

1 from math import log


2 import numpy as np
3 import mic
4
5 sample_data = mic.particle_sizing_sample()
6 coarser_data = mic.particle_sizing_coarser()
7 finer_data = mic.particle_sizing_finer()
8 reference_data = mic.particle_sizing_reference()
9 overlays_data = mic.particle_sizing_overlay(0)
10
11 sample_information = sample_data["SampleInfo"]
12 mat_props = sample_data["MaterialProperties"]
13 anl_opts = sample_data["AnalysisOptions"]
14 collected_data = sample_data["CollectedData"]
15
16 # Sample information
17 mic.summary(title="Summary Report")
18 params = sample_information["params"]
19 params_summary = []
20 sampleinfo_summary = [
21 ['Description:', sample_information["sample description"]],
22 ] + [["Parameter {} - {}:".format(i + 1, params[i]['name']),
23 "{}".format(params[i]['value'])]
24 for i in range(len(sample_information["params"]))]
25 mic.summary.add('Sample Information',
26 [desc for desc, value in sampleinfo_summary],
27 [value for desc, value in sampleinfo_summary])

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A Advanced Reports - Python Module

28
29 # Material properties
30 interp_tbl = mat_props["interpolation table"]
31 matprops_summary = [
32 ['Analysis type:', mat_props["analysis type"]],
33 ['Starting size:', "{} µm diameter".format(mat_props["starting
size"])],
34 ['Ending size:', "{} µm diameter".format(mat_props["ending
size"])],
35 ['Sample ID:', mat_props["sample ID"]],
36 ['Sample density:', "{} g/cm³".format(mat_props["sample
density"])],
37 ['Liquid ID:', mat_props["liquid ID"]],
38 ['Liquid fixed density:', "{} g/cm³".format(mat_props["liquid fixed
density"])],
39 ['Liquid fixed viscosity:', "{} mPa*s".format(mat_props["liquid fixed
viscosity"])],
40 ['X-ray intensity:', mat_props["xray intensity"]],
41 ] + [["Interpolation table row {}:".format(i + 1),
42 "Cell temperature: {} °C, Density: {} g/cm³, Viscosity: {} mPa*s"
43 .format(interp_tbl[i]["cell temperature"],
44 interp_tbl[i]["density"],
45 interp_tbl[i]["viscosity"])]
46 for i in range(len(interp_tbl))]
47 mic.summary.add('Material Properties',
48 [desc for desc, value in matprops_summary],
49 [value for desc, value in matprops_summary])
50
51 # Analysis options
52 anlopts_summary = [
53 ['MasterTech stir time:', "{} sec".format(anl_opts['mt stir time'])],
54 ['MasterTech stir speed:', anl_opts['mt stir speed']],
55 ['MasterTech probe time:', "{} sec".format(anl_opts['mt probe time'])],
56 ['Stop at mass percent:', anl_opts['stop at mass percent']],

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Acquire Basic Information

57 ['Ending percent:', "{}%".format(anl_opts['ending percent'])],


58 ['Number of tests:', anl_opts['number of tests']],
59 ['Leave pump on:', 'yes' if anl_opts['leave pump on'] else 'no'],
60 ['Wait for temperature stabilization:',
61 'yes' if anl_opts['wait for temp stabilization'] else 'no'],
62 ['Mixing stir speed:', anl_opts['mix stir speed']],
63 ['Full scale pump speed:', anl_opts['full scale pump speed']],
64 ['Bubble detection:', anl_opts['bubble detection']],
65 ['Rinse after analysis:', anl_opts['rinse after analysis']],
66 ['Auto rinse:', anl_opts['is auto rinse']],
67 ['Rinse cycles:', anl_opts['rinse cycles']],
68 ['Rinse pump speed:', anl_opts['rinse pump speed']],
69 ]
70 mic.summary.add('Analysis Options',
71 [desc for desc, value in anlopts_summary],
72 [value for desc, value in anlopts_summary])
73
74 # Collected data
75 colldata_summary = [
76 ["Mean base/Full:", '{:.4f} kCnts/s'.format(collected_data["mean base/-
full"])],
77 ["Base/Full scale:", '{:.4f} kCnts/s'.format(collected_data["base/full
scale"])],
78 ]
79 mic.summary.add('Collected Data',
80 [desc for desc, value in colldata_summary],
81 [value for desc, value in colldata_summary])
82
83 # Cumulative mass graph
84 test = 'avg'
85 dist = 'mass'
86 mic.graph(title='Cumulative Mass Test Average',
87 xlabel='Particle size (µm diameter)', ylabel='Cumulative')

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A Advanced Reports - Python Module

88 xs = collected_data['low diameter'][test][dist]
89 ys = collected_data['cumulative'][test][dist]
90 mic.graph.add("Cumulative", xs, ys)
91
92 # Sedimentation data table
93 test = '1' # First test
94 sedtimes = collected_data['unsmoothed']['sedimentation times'][test]
95 sedheights = collected_data['unsmoothed']['sedimentation heights'][test]
96 sedperiods = collected_data['unsmoothed']['sedimentation periods'][test]
97 mic.table(title="Sedimentation Data for Test {}".format(test))
98 mic.table.addtable('Sedimentation Data')
99 mic.table.addcolumn('Sedimentation time (sec)', [sedtime/100.0 for sedtime
in sedtimes])
100 mic.table.addcolumn('Sedimentation height (cm)', ['{:.4f}'.format(height)
for height in sedheights])
101 mic.table.addcolumn('Sedimentation period (µs)', ['{:.4f}'.format(period)
for period in sedperiods])

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Acquire Report Results

ACQUIRE REPORT RESULTS


The Advanced Reports provide a way to access Log Probability, Rosin Rammler, Baseline, and
Fullscale data.

1 import mic
2 import numpy as np
3
4 # Returns slope, intercept, r² information.
5 def get_linear_fit(xs, ys):
6 slope, intercept = np.polyfit(xs, ys, 1)
7 correlation_matrix = np.corrcoef(xs, ys)
8 correlation_xy = correlation_matrix[0,1]
9 r_squared = correlation_xy ** 2
10 return slope, intercept, r_squared
11
12 sample_data = mic.particle_sizing_sample()
13 collected_data = sample_data["CollectedData"]
14
15 # Log probability graph
16 test = 'avg'
17 dist = 'mass'
18 mic.graph(title='Log Probability for {} using {} Distribution'.format(test,
dist),
19 xlabel='Particle size (µm)', ylabel='Logprob')
20 logprob = collected_data['logprob'][test][dist]
21 slope, intercept, r_squared = get_linear_fit(logprob['X'], logprob['Y'])
22 mic.graph.add("Logprob: slope={:.4f}, intercept={:.4f}, r²={:.4f}"
23 .format(slope, intercept, r_squared),
24 logprob['X'], logprob['Y'])
25
26 # Rosin Rammler graph
27 test = '1' # First test
28 dist = 'mass'

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A Advanced Reports - Python Module

29 mic.graph(title='Rosin Rammler for Test {} using {} Distribution'.format


(test, dist),
30 xlabel='Particle size (µm)', ylabel='RR')
31 rosinrammler = collected_data['rosinrammler'][test][dist]
32 slope, intercept, r_squared = get_linear_fit(rosinrammler['X'], rosinrammler
['Y'])
33 mic.graph.add("RR: slope={:.4f}, intercept={:.4f}, r²={:.4f}"
34 .format(slope, intercept, r_squared),
35 rosinrammler['X'], rosinrammler['Y'])
36
37 # Baseline graphs
38 mic.graph(title='Raw Baseline', xlabel='Cell position (cm)', ylabel='Intens-
ity (µs)')
39 xs = collected_data['baseline']['heights']
40 ys = collected_data['baseline']['periods']
41 mic.graph.add("Baseline", xs, ys)
42 mic.graph(title='Reported Baseline', xlabel='Cell position (cm)',
ylabel='Intensity (1000/µs)')
43 reported_xs = [0.01 if x < 1.0e-6 else x for x in xs]
44 reported_ys = [1.0e3 / y if y > 1.0e-6 else 0.0 for y in ys]
45 mic.graph.add("Baseline", reported_xs, reported_ys)
46
47 # Fullscale graphs
48 mic.graph(title="Raw Fullscale for Test {}".format(test),
49 xlabel='Cell position (cm)', ylabel='Intensity (µs)')
50 xs = collected_data['fullscale'][test]['heights']
51 ys = collected_data['fullscale'][test]['periods']
52 mic.graph.add('Fullscale raw', xs, ys)
53 mic.graph(title="Reported Fullscale for Test {}".format(test),
54 xlabel='Cell position (cm)', ylabel='Intensity (1000/µs)')
55 reported_xs = [0.01 if x < 1.0e-6 else x for x in xs]
56 reported_ys = [1.0e3 / y if y > 1.0e-6 else 0.0 for y in ys]
57 mic.graph.add("Fullscale", reported_xs, reported_ys)
58

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Acquire Overlay Sample Data

ACQUIRE OVERLAY SAMPLE DATA


There are four functions that can be used to get overlay information. The Report Options must
have:

n Reference (corresponds to particle_sizing_reference),


n Specification (corresponds to def particle_sizing_coarser() and def particle_sizing_finer()),
n Overlays (corresponds to def particle_sizing_overlays(number)) selection

1 Acquire Overlay Sample Data


2 def particle_sizing_coarser():
3 '''Get particle_sizing sample information, material properties, analysis
options,
4 and collected data of the coarser reference file.
5
6 Usage:
7
8 coarser = particle_sizing_coarser()
9
10 The returned dict has the same layout as the structure returned by
11 particle_sizing_sample()
12 '''
13
14 def particle_sizing_finer():
15 '''Get particle_sizing sample information, material properties, analysis
options,
16 and collected data of the finer reference file.
17
18 Usage:
19
20 finer = particle_sizing_finer()
21
22 The returned dict has the same layout as the structure returned by
23 particle_sizing_sample()

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24 '''
25
26 def particle_sizing_reference():
27 '''Get particle_sizing sample information, material properties, analysis
options,
28 and collected data of the reference reference file.
29
30 Usage:
31
32 reference = particle_sizing_reference()
33
34 The returned dict has the same layout as the structure returned by
35 particle_sizing_sample()
36 '''
37
38 def particle_sizing_overlay(sample_number):
39 '''Get particle sizing sample information, material properties, analysis
options,
40 and collected data of the sample_number overlay reference files.
41
42 Usage:
43
44 first_overlay = particle_sizing_overlay(0)
45
46 The returned dict has the same layout as the structure returned by
47 particle_sizing_sample()
48 '''
49
50 This is an example code block that makes use of it:
51 import mic
52
53 sample_data = mic.particle_sizing_sample()
54 collected_data = sample_data["CollectedData"]

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55 finer_data = mic.particle_sizing_finer()
56 reference_data = mic.particle_sizing_reference()
57 coarser_data = mic.particle_sizing_coarser()
58 first_overlay = mic.particle_sizing_overlay(0)
59
60
61 # Cumulative mass graph
62 test = 'avg'
63 dist = 'mass'
64 mic.graph(title='Cumulative Mass Test Average',
65 xlabel='Particle size (µm diameter)', ylabel='Cumulative')
66 xs = sample_data['CollectedData']['low diameter'][test][dist]
67 ys = sample_data['CollectedData']['cumulative'][test][dist]
68 mic.graph.add("Sample", xs, ys)
69 xs = finer_data['CollectedData']['low diameter'][test][dist]
70 ys = finer_data['CollectedData']['cumulative'][test][dist]
71 mic.graph.add("finer", xs, ys)
72 xs = coarser_data['CollectedData']['low diameter'][test][dist]
73 ys = coarser_data['CollectedData']['cumulative'][test][dist]
74 mic.graph.add("finer", xs, ys)
75 xs = reference_data['CollectedData']['low diameter'][test][dist]
76 ys = reference_data['CollectedData']['cumulative'][test][dist]
77 mic.graph.add("finer", xs, ys)
78
79
80

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A Advanced Reports - Python Module

GET PARTICLE SIZING SAMPLE

1 def particle_sizing_sample():
2 '''Get particle_sizing sample information, material properties, analysis
options,
3 and collected data.
4
5 Usage:
6
7 sample = particle_sizing_sample()
8
9 The returned dict has the following layout.
10
11 sample = {
12 'SampleInfo' : {
13 'sample description': str,
14 'params' : list( {'name': str, 'value': float } )
15 },
16 'MaterialProperties' : {
17 'analysis type': str,
18 'starting size': float,
19 'ending size': float,
20 'sample ID': str,
21 'sample density': float,
22 'liquid ID': str,
23 'liquid fixed density': float,
24 'liquid fixed viscosity': float,
25 'xray intensity': str,
26 'interpolation table': {
27 'cell temperature': double,
28 'density': double,
29 'viscosity': double,

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30 },
31 },
32 'AnalysisOptions' : {
33 'mt stir time': float,
34 'mt stir speed': float,
35 'mt probe time': double,
36 'stop at mass percent': bool,
37 'ending percent': double,
38 'number of tests': int,
39 'leave pump on': bool,
40 'wait for temp stabilization': bool,
41 'mix stir speed': double,
42 'full scale pump speed': double,
43 'bubble detection': str,
44 'rinse after analysis': bool,
45 'is auto rinse': bool,
46 'rinse cycles': double,
47 'rinse pump speed': double,
48 },
49 'CollectedData': {
50 'analysis times': dict( {'0': str,
51 '2': str,
52 ...,
53 '7': str } ),
54 'unsmoothed': dict( { 'sedimentation heights': dict( { '0':
list(float),
55 '1':
list(float),
56 ...
57 '7':
list(float) } ),
58 'sedimentation times' : dict( { '0':
list(float),
59 '1':

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list(float),
60 ...
61 '7':
list(float) } ),
62 'sedimentation periods' : dict( { '0':
list(float),
63 '1':
list(float),
64 ...
65 '7':
list(float) } ),
66 'masses' : dict( { '0': list(float),
67 '1': list(float),
68 ...
69 '7': list(float) } ),
70 'sizes' : dict( { '0': list(float),
71 '1': list(float),
72 ...
73 '7': list(float) } ),
74 } )
75 'smoothed': dict( { 'masses' : dict( { '0': list(float),
76 '1': list(float),
77 ...
78 '7': list(float) } ),
79 'sizes' : dict( { '0': list(float),
80 '1': list(float),
81 ...
82 '7': list(float) } ) }
),
83 'mean base/full' : float,
84 'base/full scale' : float,
85 'low diameter' : dict( { '0' : dict( {
86 'mass': list(float)
87 'area': list(float)

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88 'volume': list(float)
89 'number': list(float)
90 } ),
91 '1' : dict( { ... } ),
92 ...
93 '7' : dict( {... } ),
94 'avg' : dict( {... } ) } )
95 'high diameter': dict( { '0' : dict( {
96 'mass': list(float)
97 'area': list(float)
98 'volume': list(float)
99 'number': list(float)
100 } ),
101 '1' : dict( { ... } ),
102 ...
103 '7' : dict( {... } ),
104 'avg' : dict( {... } ) } ),
105 'average diameter': dict( { '0' : dict( {
106 'mass': list(float)
107 'area': list(float)
108 'volume': list
(float)
109 'number': list
(float)
110 } ),
111 '1' : dict( { ... } ),
112 ...
113 '7' : dict( {... } ),
114 'avg' : dict( {... } ) } ),
115 'cumulative': dict( { '0' : dict( {
116 'mass': list(float)
117 'area': list(float)
118 'volume': list(float)

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119 'number': list(float)


120 } ),
121 '1' : dict( { ... } ),
122 ...
123 '7' : dict( {... } ),
124 'avg' : dict( {... } ) } ),
125 'frequency': dict( { '0' : dict( {
126 'mass': list(float)
127 'area': list(float)
128 'volume': list(float)
129 'number': list(float)
130 } ),
131 '1' : dict( { ... } ),
132 ...
133 '7' : dict( {... } ),
134 'avg' : dict( {... } ) } ),
135 'rosin rammler': dict( { '0' : dict( {
136 'mass': list(float)
137 'area': list(float)
138 'volume': list(float)
139 'number': list(float)
140 } ),
141 '1' : dict( { ... } ),
142 ...
143 '7' : dict( {... } ) } ),
144 'specific area': dict( { '0' : dict( {
145 'mass': list(float)
146 'area': list(float)
147 'volume': list(float)
148 'number': list(float)
149 } ),
150 '1' : dict( { ... } ),

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151 ...
152 '7' : dict( {... } ),
153 'avg' : dict( {... } ) } ),
154 'area in interval': dict( { '0' : dict( {
155 'mass': list(float)
156 'area': list(float)
157 'volume': list
(float)
158 'number': list
(float)
159 } ),
160 '1' : dict( { ... } ),
161 ...
162 '7' : dict( {... } ),
163 'avg' : dict( {... } ) } ),
164 'specific number': dict( { '0' : dict( {
165 'mass': list(float)
166 'area': list(float)
167 'volume': list
(float)
168 'number': list
(float)
169 } ),
170 '1' : dict( { ... } ),
171 ...
172 '7' : dict( {... } ),
173 'avg' : dict( {... } ) } ),
174 'number in interval': dict( { '0' : dict( {
175 'mass': list
(float)
176 'area': list
(float)
177 'volume': list
(float)
178 'number': list

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(float)
179 } ),
180 '1' : dict( { ... } ),
181 ...
182 '7' : dict( {... } ),
183 'avg' : dict( {... } ) } ),
184 'log probability': dict( { '0' : dict( {
185 'mass': list(float)
186 'area': list(float)
187 'volume': list
(float)
188 'number': list
(float)
189 } ),
190 '1' : dict( { ... } ),
191 ...
192 '7' : dict( {... } ),
193 'avg' : dict( {... } ) } ),
194 'phi size': dict( { '0' : dict( {
195 'mass': list(float)
196 'area': list(float)
197 'volume': list(float)
198 'number': list(float)
199 } ),
200 '1' : dict( { ... } ),
201 ...
202 '7' : dict( {... } ),
203 'avg' : dict( {... } ) } ),
204 'settling velocity': dict( { '0' : dict( {
205 'mass': list
(float)
206 'area': list
(float)
207 'volume': list

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(float)
208 'number': list
(float)
209 } ),
210 '1' : dict( { ... } ),
211 ...
212 '7' : dict( {... } ),
213 'avg' : dict( {... } ) } ),
214 'phi size low': dict( { '0' : dict( {
215 'mass': list(float)
216 'area': list(float)
217 'volume': list(float)
218 'number': list(float)
219 } ),
220 '1' : dict( { ... } ),
221 ...
222 '7' : dict( {... } ),
223 'avg' : dict( {... } ) } ),
224 'settling velocity low': dict( { '0' : dict( {
225 'mass': list
(float)
226 'area': list
(float)
227 'volume': list
(float)
228 'number': list
(float)
229 } ),
230 '1' : dict( { ... } ),
231 ...
232 '7' : dict( {... } ),
233 'avg' : dict( {... } ) } ),
234
235 'baseline' : dict( { 'heights' : list(float), 'periods' : list

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(float) } ),
236 'fullscale' : dict( { '0' : dict( { 'heights' : list(float),
'periods' : list(float) } ),
237 '1' : dict( { ... } ),
238 ...
239 '7' : dict( { ... } ),
240 'avg' : dict( {... } ) } ),
241 'logprob' : dict( {'0': {'mass': { 'X' : list(float),
242 'Y' : list(float) }
243 'area': { ... },
244 'number': { ... },
245 'volume': { ... },
246 },
247 '1': {...},
248 ...
249 '7': {...},
250 'avg': {...},
251 } )
252 'rosinrammler': dict( {'0': {'mass': { 'X' : list(float),
253 'Y' : list(float), }
254 'area': { ... },
255 'number': { ... },
256 'volume': { ... },
257 },
258 '1': {...},
259 ...
260 '7': {...},
261 'avg': {...},
262 } )
263 }
264 }
265 '''
266

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267 def particle_sizing_coarser():


268 '''Get particle_sizing sample information, material properties, analysis
options,
269 and collected data of the coarser reference file.
270
271 Usage:
272
273 coarser = particle_sizing_coarser()
274
275 The returned dict has the same layout as the structure returned by
276 particle_sizing_sample()
277 '''
278
279 def particle_sizing_finer():
280 '''Get particle_sizing sample information, material properties, analysis
options,
281 and collected data of the finer reference file.
282
283 Usage:
284
285 finer = particle_sizing_finer()
286
287 The returned dict has the same layout as the structure returned by
288 particle_sizing_sample()
289 '''
290
291 def particle_sizing_reference():
292 '''Get particle_sizing sample information, material properties, analysis
options,
293 and collected data of the reference reference file.
294
295 Usage:
296

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297 reference = particle_sizing_reference()


298
299 The returned dict has the same layout as the structure returned by
300 particle_sizing_sample()
301 '''
302
303 def particle_sizing_overlay(sample_number):
304 '''Get particle sizing sample information, material properties, analysis
options,
305 and collected data of the sample_number overlay reference files.
306
307 Usage:
308
309 first_overlay = particle_sizing_overlay(0)
310
311 The returned dict has the same layout as the structure returned by
312 particle_sizing_sample()
313 '''
314

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Enable the Use of Overlay Data

ENABLE THE USE OF OVERLAY DATA


1. On the Report Options tab, click Overlays.
2. On the Plot Overlay Sample Selection window, to move a file from the Available Files list
box to the Selected Files list box, either double-click a file name in the Available Files list
box or click one or more files in the Available Files list box then click Add.

3. Click OK.
4. On the Report Options tab, highlight Advanced in the Selected Reports list box.
5. On the Advanced Report Options window, click Add in the Available Scripts group box and
select a Python script.
6. In the Select Reports group box, select the drop-down arrow to select a report to be used in
the overlay.
7. Click OK.
8. Run the script using the instructions found in Scripts on page A - 4.

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A Advanced Reports - Python Module

MICMODULE PYTHON CALLS

Tables
Available Mic Python calls for tables:

n Create a new tabular report


n Add a column
n Add a table

Add a Table
This script adds a table to the last created tabular report:

1 mic.table.addtable( name )
2
3 Keyword arguments:
4
5 name --- the table name

Add a Column
This script adds a column to the last created table:

1 mic.table.addcolumn(header, values, align='r'):


2
3 Keyword arguments:
4
5 header --- column header; must be a string (or convertible)
6 values --- column values; must be a list of strings (or convertible)
7 align --- column alignment; 'r', 'l', 'c' for right, left, and center jus-
tified

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MicModule Python Calls

Create a New Tabular Report

1 mic.table( title='User Table' )


2
3 Keyword arguments:
4
5 title --- the tabular report title (default = 'User Table')

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A Advanced Reports - Python Module

Summary Reports

Add a Summary Section


This script adds a summary section to the last created summary report:

1 mic.summary.add(name, labels, values):


2
3 Keyword arguments:
4
5 name --- summary section name
6 labels --- column of labels; must be a list of strings
7 (or convertible) and the same length as values
8 values --- column of values; must be a list of strings
9 (or convertible) and the same length as labels

Create a New Summary Report

1 mic.summary( title='User Summary' )


2
3 Keyword arguments:
4
5 title --- the summary title

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MicModule Python Calls

Graphic Reports

Add a Curve
This script adds a curve to the last created graphical report:

1 mic.graph.add(name, x, y, yyaxis=False, color=None, linestyle='-',


2 marker='a', graphtype='both', interpolation='akima'):
3
4 Keyword arguments:
5
6 name --- the curve name
7 x --- list of x values; must be a list of floats
8 (or convertible) and the same length as y
9 y --- list of y values; must be a list of floats
10 (or convertible) and the same length as x
11 yyaxis --- place this curve on the yy-axis if True
12 otherwise place on the y-axis (default = False)
13 color --- RGB color as an HTML hex string (e.g., '#4169e1')
14 or a three-element list or tuple (e.g., [65,105,225]);
15 if None, color is automatically selected (default = None)
16 linestyle --- line style; (default = '-')
17 '-' : solid
18 '--' : dash
19 '.' : dot
20 '-.' : dash dot
21 '-..' : dash dot dot
22 marker --- marker shape; (default = 'a')
23 '+' : plus
24 'o' or '0' : circle
25 'x' : cross
26 '^' : up triangle
27 'v' : down triangle
28 's' : square

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A Advanced Reports - Python Module

29 'd' : diamond
30 '8' : hourglass
31 '~' : horizontal hourglass
32 '' or None : no marker
33 'a' : automatically selected
34 graphtype --- graph type; (default = 'both')
35 'curve' or 'c' : curve
36 'points' or 'p' : points
37 'both' or 'b' : curve-and-points
38 'hist' or 'h' : histogram
39 interpolation -- linear or akima spline interpolation (default='akima')
40 'akima' use akima spline
41 'linear' use linear interpolation

Add a Curve Using the Second Y-Axis


This script adds a curve to the last created graphical report using the second y-axis:

1 mic.graph.addyy(name, xx, yy):


2
3 Add a curve to the last created graphical report using the second
4 y-axis. The arguments to this call are the same as to mic.graph.add.

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MicModule Python Calls

Create a New Graphical Report

1 mic.graph(title='User Graph', xlabel='X axis', ylabel='Y axis',


2 yylabel='YY axis',
3 xlinear=True, ylinear=True, yylinear=True,
4 xinvert=False, yinvert=False, yyinvert=False,
5 xrange=None, yrange=None, yyrange=None, xbars_id=''):
6
7 Keyword arguments:
8
9 title --- the graphical report title (default = 'User Graph')
10 xlabel --- x-axis label (default = 'X axis')
11 ylabel --- y-axis label (default = 'Y axis')
12 yylabel --- yy-axis label (default = 'YY axis')
13 xlinear --- x-axis linear scale; if false, use log scale
14 (default = True)
15 ylinear --- y-axis linear scale; if false, use log scale
16 (default = True)
17 yylinear --- yy-axis linear scale; if false, use log scale
18 (default = True)
19 xinvert --- Invert x-axis if true (default = False)
20 yinvert --- Invert y-axis if true (default = False)
21 yyinvert --- Invert yy-axis if true (default = False)
22 xrange --- None, or two values giving the min and max
23 range of the axis.
24 yrange --- None, or two values giving the min and max
25 range of the axis.
26 yyrange --- None, or two values giving the min and max
27 range of the axis.
28 xbars_id --- None, or the id of an xbar control created
29 via the mic.control() object

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A Advanced Reports - Python Module

Get Sample Information Item

1 mic.sample_information( item, sample_number = 0 ):


2
3 Keyword arguments:
4
5 item --- string identifying the item to be returned.
6 For example; 'sample mass', or 'sample description'
7 The default is an empty string for which the return
8 value is a list of all available keywords
9
10 sample_number --- Sample to retrieve
11 0 : current sample file (default)
12 1 through 8 : corresponding overlay sample file
13
14 Usage:
15
16 all_keywords = sample_information()
17 mass = sample_information('sample mass')
18 mass = sample_information('sample mass',0)

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B Chemical Aids for Particle Dispersion

B CHEMICAL AIDS FOR PARTICLE DISPERSION


Name Type Active Ingredient
Aerosol 22 Anionic Tetrasodium N-(1,2-dicarboxyet hyl)-Noct-
adecysulfosuccinanate, 35%
Aerosol OT Anionic Dioctyl ester of sodium sulfosuccinic acid, 70%
Atlas G-3300 Anionic Amine salt of alkylaryl sulfonate
Calcium Chloride Cationic CaCl2
Calgon Anionic Sodium hexametaphosphate, unadjusted
Calgon T Anionic Part of sodium replaced by other cations, predominantly zinc
Cobaltous Chloride Cationic CoCl2
Cobalt Citrate Anionic Co3(C6H5O7)2
Daxad 23 Anionic Sodium salt of polymerized carboxylic acid, 25%
Daxad 30 Anionic Sodium salt of polymerized carboxylic acid, 25%
FC-134 Cationic Fluorochemical surfactant
FC-161 Anionic Fluorochemical surfactant
FC-170 Nonionic Fluorochemical surfactant
Igepal CO-530 Nonionic Nonylphenoxypoly (ethyleneoxy) ethanol, 100%
Oleic Acid Anionic CH3(CH2)7CH=CH(CH2)7COOH
Renex 648 Nonionic Ethoxylated nonylphenol, 100%
Sodium Silicate Anionic Na2SiO3
Triton X-100 Nonionic Octyl phenoxy polyethoxy ethanol, 100%
Tamol SN Anionic Sodium salt of condensed naphthalene sulfonic acid, 100%
TSPOP Anionic Tetrasodiumpyrophosphate, Na4P2O7
Twitchell Base 8240 Anionic Sodium salt of low molecular weight, sulfonated oil, parafin
oil, water, and diethylene glycol
Tween 20 Nonionic Polyoxyethylene Sorbitan monolaureate (polysorbate 20),
100%
Zonyl S-13 Anionic Fluoroalkyl phosphate
Zonyl A Nonionic Ethylene oxide-ester condensate

Data extracted from McCutcheon’s Detergents and Emulsifiers, McCutcheon Division, MC


Publishing Co., Glen Rock, NJ, 1980.

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C Data Reduction

C DATA REDUCTION

DATA ACQUISITION
The basic data acquired are in the form of cumulative mass percent finer vs. diameter. An
explanation of the method for acquiring the data are provided below.

DIAMETER
Diameter for a given set of sedimentation conditions is given by Stokes equation as follows:

where

D = diameter (cm, multiply by 10000 for micrometers)


η = liquid viscosity (poise, multiply by 0.01 for cp)
h = sedimentation height (cm)
ρ = sample density (g/cm3)
ρo = liquid density (g/cm3)
g = acceleration due to gravity (981 cm/s/s)
t = sedimentation time (sec)

All data are acquired at one of 220 predetermined sedimentation heights, ranging from 2.54 cm to
0.0079375 cm.

Sample density is user-entered. Liquid viscosity and density are user-entered, or they are
calculated using the sedimentation cell temperature and interpolating from the user-selected
Liquid Properties Set (see Liquid Properties Interpolation).

Target diameters for data collection are determined as follows:

Up to 250 target diameters are selected, evenly spaced on a log diameter basis, between the user
selected starting diameter and ending diameter. Note that this gives the operator some choice in
the resolution of the data relative to the log diameter axis: selecting a narrower range of analysis
provides more data points in a given range of diameters. Maximum resolution is obtained by
selecting starting and ending diameters spanning only one decade (factor of 10), providing 250
data points per decade resolution.

Target sedimentation heights and times are selected based on run type (high speed, standard, or
high resolution) and Stokes’ equation.

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C Data Reduction

During analysis, mass % data will be taken at these target heights, and as close to these target
times as possible, allowing for cell movement, data acquisition delay time, and sequential
collection of data points. The actual time of data collection will be recorded for each point, so that
actual diameter may be calculated later.

Height, time, density, and viscosity data are stored separately, so that corrections to density and
viscosity can be made after the analysis and diameters are recalculated.

LIQUID PROPERTIES INTERPOLATION


The density and viscosity of the sedimentation liquid at the time of analysis are interpolated as
follows, using a liquid properties table of three points of density and viscosity versus temperature,
and the cell temperature reading at the start of analysis.

DENSITY

t1, t2, t3 = temperatures from liquid properties table (degrees C)


d1, d2, d3 = densities at t1, t2, t3 respectively (g/cm3)
A = first order coefficient
β = second order coefficient
tc = cell temperature reading at start of analysis (degrees C)
ρo = liquid density at analysis temperature (g/cc)

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C Data Reduction

VISCOSITY

t1, t2, t3 = 1/(t + 273.15) for t = each of the 3 temperatures in the liquid properties
table (t in degrees C)
ʋ1, ʋ2, ʋ3 = ln(ʋ) for ʋ = each of the 3 viscosities (cp)
A, B, C = 0th, 1st, and 2nd order coefficients, respectively
tk = cell temperature at start of analysis (K, i.e., 273.15 + degrees C)
η = viscosity at analysis temperature (cp)

MASS PERCENT
The mass percent of sample present at a given sedimentation height after a given time is
determined by relating the x-ray transmission intensity at that point to the intensity with no sample
present (baseline), and the intensity with all of the sample present (full scale):

Im = intensity at data point (mass % being determined)


Ib = intensity at baseline (mass % = 0)
If = intensity at full scale (mass % = 100)

The Ib and If values are average values to minimize random variations in the X-ray intensity. The
average of these values is used to compute the mass percent.

One set of baseline data may be used for scaling multiple analyses until another set of baseline
data are collected.

After the sample is loaded while the cell pump is still on and the sample fully suspended and
evenly distributed throughout the cell, bubble elimination data are collected at between 110 and
220 predetermined analysis heights, based on the type of bubble elimination selected. In addition,
a single average full-scale value is computed at the starting analysis height.

Mass percent data appearing on the ‘Analysis Results’ screen has been smoothed with an 11-
point evenly weighted running average.

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When data are saved permanently after all analyses on a sample are completed, the mass
percent values are smoothed before storage in the sample file as follows:

The mass percent values are smoothed with an 11-point running average, just as for the ‘Analysis
Results’ screen. From these data, a set of mass percent values are interpolated at 250 evenly
spaced intervals on a log diameter basis, using linear interpolation between the two adjacent
collected points to get each evenly spaced point. This is done because the next smoothing step
requires evenly spaced data points, and the collected data can vary from even log diameter
spacing due to limitations on time of collection, as noted above.

The evenly spaced mass percent values are smoothed using a digital filter which removes high-
frequency variations from the data. The final, stored mass percent values are obtained by
interpolating to a standard size table with 40 logarithmicly, evenly-spaced sizes per decade.

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REDUCTION OF COLLECTED DATA


MASS DATA
In order to obtain cumulative mass percent data, the smoothed mass percent data scaled to the
specified full scale value:

For each of the total number of points collected:

Cumulative mass percent coarser data are simply the difference of scaled mass percent
finer data from 100:

For each of the total number of points collected:

These cumulative mass data (finer and coarser) are represented directly in tabular form and as y-
axis data in the CUMULATIVE MASS FINER VS. DIAMETER and CUMULATIVE MASS
COARSER VS. DIAMETER plots (cumulative mass distribution curve). Also, cumulative mass
data are used to derive mass frequency and log probability data.

MASS FREQUENCY DATA


The mass frequency of a particle size interval is the difference between the cumulative mass
percent interpolated at the end points of the interval. The interpolation is performed using a spline
fit to the cumulative mass data.

CUMULATIVE DATA
Any cumulative quantity can be expressed as Coarser or Finer (Retained or Passed on the
Tabular Report by Sieve Size).

For data defined by the standard class sizes (Summary, Tabular Defined by Size Class, and
Graphs):

CumFracCoarseri = ∑FreqFrack for all classes k such that AvgDiamk > AvgDiami

CumFracFineri = ∑FreqFrack for all classes k such that AvgDiamk > AvgDiami

CumFracRetaini = ∑FreqFrack for all classes k such that AvgDiamk > AvgDiami

CumFracPassi = ∑FreqFrack for all classes k such that AvgDiamk < AveDiami

      or equivalently,

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CumFracFineri = 1.0 - CumFracCoarseri-1

CumFracRetaini = CumFracCoarseri-1

CumFracPassi = 1.0 - CumFracCoarseri-1

For Tabular Defined by SizeTable or by Sieve Sizes:

CumFrac (Coarser or Finer, Retained or Passed) is calculated for the standard size
classes as defined above. CumFrac is then interpolated from CumFrac vs. Particle
Size at each particle size in the Size table or aperture size in the Sieve table.

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PEAK REPORT DATA


Peak report data are calculated as:

Starting at the small particle size end of the frequency distribution:

1. Scan DiffFreqFraci for a local maximum, i.e.,

DiffFreqFrack > DiffFreqFrack+1, and


DiffFreqFrack > DiffFreqFrack-1
AvgDiamk is the mode of the candidate peak.
2. Scan DiffFreqFraci from class k toward smaller particle sizes to find a local minimum, i.e.,

DiffFreqFracm = 0, or
DiffFreqFracm < DiffFreqFracm+1 and DiffFreqFracm < DiffFreqFracm-1
LowDiamm is the low diameter of the candidate peak.
3. Scan DiffFreqFraci from class k toward larger particle sizes to find a local minimum, i.e.,

DiffFreqFracn = 0, or
DiffFreqFracn < DiffFreqFracn+1 and DiffFreqFracn < DiffFreqFracn-1
HighDiamn is the high diameter of the candidate peak.
4. Sum values of FreqFraci from i=m to i=n.

If the sum is greater than or equal to the Minimum Fraction to Report, the candidate peak is
qualified and the sum is the Fraction of Distribution. Other peak quantities are calculated
using the same formulas as for the entire distribution, except the only range from class m to
class n is used.
Otherwise, the candidate peak is disqualified.
In either case, peak identification repeats from step 1, starting with class n. When the end of the
distribution is reached by scanning in either step 1 or step 3, peak identification is complete.

In step 1 if the end of the distribution is reached on an increasing frequency slope, i.e.,
DiffFreqFrack > DiffFreqFrack-1, then class k is treated as the mode of a candidate peak and as
the high size end of the candidate peak.

If the beginning or end of the distribution is reached while scanning for a local minimum in step 2
or 3, the beginning or ending class is treated as the local minimum.

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For calculating Standard Deviation for N tests, peaks from the various tests are simply matched by
their order, i.e., peak 1 from test 1 is matched with peak 1 from test 2, etc. If all tests do not have
the same number of peaks, Standard Deviation for N tests is reported as N/A (not available). If the
peak numbers are not the same and the user chose average of n tests, a single row is filled in with
all N/A (including the peak number).

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NUMBER FREQUENCY DATA


The number frequency is computed from the mass frequency distribution as defined by the
standard size classes.

For each class:

where

NumFreqN = NumberfFrequency for class N


MassFreqN = Mass frequency for class N
AvgDiam = Average diameter for class N

The cumulative number percent for a class is computed as the summation of the non-negative
frequencies for all smaller classes.

SURFACE AREA FREQUENCY DATA


The surface area frequency is computed from the mass frequency distribution as defined by the
standard size classes.

For each class:

where

AreaFreqN = NumberfFrequency for class N


MassFreqN = Mass frequency for class N
AvgDiam = Average diameter for class N

The cumulative number percent for a class is computed as the summation of the non-negative
frequencies for all smaller classes.

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SIZE STATISTICS
STANDARD DEVIATION OF QUANTITY FOR N TESTS
For quantity, substitute the variable name for which the standard deviation is being determined.
The subscript k refers to the test number.

If NumTests < = 1, StdDevTestQuantity = 0.

Otherwise,

MODE
In order to do a mode calculation, the definition of the standard classes is extended over the range
of input for all the data; frequencies are calculated for these classes. It is this frequency data that
is used in determining the peak quantities so that all the classes are of the same width.

ModeDiam = AvgDiami such that DiffFreqFraci is the maximum DiffFreqFrac

MEDIAN
MedianDiam = Diameter interpolated from HighDiam vs. CumFracCoarser at CumFracCoarser =
0.5.

If the calculation is being performed on a peak, the interpolation point is at


CumFracCoarser = (Cum-FracCoarserm + CumFracCoarsern)/2.

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ARITHMETIC CALCULATIONS
MEAN

STANDARD DEVIATION (OF THE DISTRIBUTION)

COEFFICIENT OF VARIATION

SKEWNESS

KURTOSIS

+Xẟ

where x is a user-selected number.

-Xẟ

where x is a user-selected number.

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GEOMETRIC CALCULATIONS
MEAN

GeoMeanDiam = 10

STANDARD DEVIATION (OF THE DISTRIBUTION)

STANDARD DEVIATION OF LOG

SKEWNESS OF LOG

KURTOSIS OF LOG

+Xẟ

-Xẟ

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SPECIFICATION / REFERENCE QUANTITIES


OUT OF SPEC
SampCumFraci = cumulative fraction coarser/finer/passed/retained for class i from sample
distribution.

CoarseSpecCumFraci = cumulative fraction coarser/finer/passed/retained for class i from Coarse


Specification distribution interpolated if the bins are of different size. This is always the average of
all tests in the named sample file.

FineSpecCumFraci = cumulative fraction coarser/finer/passed/retained for class i from


FineSpecification distribution interpolated if the bins are of different size. This is always the
average of all the tests in the named sample file.

If {SampCumFracCoarseri-1 > CoarseSpecCumFracCoarseri-1}

OutSpecFracCoarseri = SampCumFracCoarseri-1 - CoarseSpecCumFrac


Coarseri-1

If {SampCumFracCoarseri-1 < FineSpecCumFracCoarseri-1}

OutspecFracCoarseri = SampCumFracCoarser - FineSpecCumFrac

Coarseri-1

or,

OutSpecFracFineri = -OutSpecFracCoarseri-1

OutSpecFracRetaini = OutSpecFracCoarseri-1

OutSpecFracPassi = OutSpecFracCoarseri-1

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DIFFERENCE FROM REFERENCE


SampCumFraci = cumulative fraction coarser/finer/passed/retained for class i from sample
distribution.

RefSpecCumFraci = cumulative fraction coarser/finer/passed/retained for class i from Reference


Specification distribution interpolated if the bins are of different size. This is always the average of
all the tests in the named sample file.

DiffRefCoarseri = SampCumFraci - RefCumFraci

or,

DiffRefFineri = DiffRefCoarseri-1

DiffRefRetaini = DiffRefCoarseri-1

DiffRefPassi = DiffRefCoarseri-1

MAXIMUM OUT OF SPEC


MaxOutSpecFrac = maximum (abs value (OutSpecFraci))

PASS / FAIL BY SPECIFICATION


If MaxOutSpecFrac = 0, PassFail = Passed by Specification

Otherwise, PassFail = FAILED by Specification

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SPC REPORT VARIABLES


REGRESSION CHART VARIABLES
The line of best fit for the Regression Chart is calculated by the usual least squares method. 1 ) If
there is only a single point or all N points have the same x-value, there can be no line of best fit in
the standard form.

The coefficient of correlation for this line is also calculated in the usual way. 2 )

CONTROL CHART VARIABLES

1 ) BASIC Scientific Subroutines Vol II, by F.R. Ruckdeschel, Copyright 1981 BYTE
Publications/McGraw Hill, p. 16.
2 ) Mathematical Handbook for Scientists and Engineers, G.A. Korn and T.M. Korn, McGraw Hill,
Sec. 18.4. (1968)

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REYNOLDS NUMBER
The Reynolds Number is calculated as follows:

where

D = specified starting diameter


ρo = liquid density
ρ = sample density
η = liquid viscosity
g = acceleration due to gravity
K = Stokes’ constant = 18

The Reynolds Number is displayed on the tabular report.

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LOG PROBABILITY
Log probability data are a transformation of cumulative mass finer data as a means of determining
how well cumulative and differential mass data represent statistical normal distributions. Since
cumulative mass finer data are essentially data indicating the probabilities of finding particles of
mass finer at given diameters, log normal probability data are a fit of the cumulative mass data to
the defined, symmetrical probabilities tabulated for a normal distribution.

The log probability table used is a subset of 99 points, ranging from (-2.88, 0.2%) to (0.0, 50.0%)
to (+2.88, 99.8%), from a standard normal distribution table (see log probability interpolation
table). The x-axis and y-axis data which are plotted on a log probability graph are calculated as
follows:

1. X-axis boundaries are determined by the spline interpolation at 0.2% and 99.8% from
cumulative mass finer vs. log diameter. This gives Xprob_beg and Xprob_end, respectively.

2. For each of the number of points collected,

If Diameter value is between Xprob_beg and Xprob_end and

if CumMassFiner value is between 0.2% and 99.8%, then

Xprob value = Diameter value

Yprob value = Spline interpolation at CumMassFiner values of the x vs. y log probability
table values

Log Probability Interpolation Table


X(%) Y X(%) Y X(%) Y
0.20 -2.88 33.00 -0.44 68.08 0.47
0.99 -2.33 34.83 -0.39 69.15 0.50
2.02 -2.05 35.94 -0.36 69.85 0.52
3.01 -1.88 37.07 -0.33 70.88 0.55
4.01 -1.75 37.83 -0.31 71.90 0.58
4.95 -1.65 38.97 -0.28 72.91 0.61
5.94 -1.56 40.13 -0.25 73.89 0.64
6.94 -1.48 40.90 -0.23 74.86 0.67
7.93 -1.41 42.07 -0.20 76.11 0.71
9.01 -1.34 42.86 -0.18 77.04 0.74
10.03 -1.28 44.04 -0.15 77.94 0.77

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Log Probability Interpolation Table (continued)


X(%) Y X(%) Y X(%) Y
10.93 -1.23 44.83 -0.13 79.10 0.81
11.90 -1.18 46.02 -0.10 79.95 0.84
12.92 -1.13 46.81 -0.08 81.06 0.88
14.01 -1.08 48.01 -0.05 82.12 0.92
14.92 -1.04 48.80 -0.03 82.89 0.95
16.11 -.099 50.00 0.00 83.89 0.99
17.11 -0.95 51.20 0.03 85.08 1.04
17.88 -0.92 51.99 0.05 85.99 1.08
18.94 -0.88 53.19 0.08 87.08 1.13
20.05 -0.84 53.98 0.10 88.10 1.18
20.90 -0.81 55.17 0.13 89.07 1.23
22.06 -0.77 35.96 0.15 89.97 1.28
22.96 -0.74 57.14 0.18 90.99 1.34
23.89 -0.71 57.93 0.20 92.07 1.41
25.14 -0.67 59.10 0.23 93.06 1.48
26.11 -0.64 59.87 0.25 94.06 1.56
27.09 -0.61 61.03 0.28 95.05 1.65
28.10 -0.58 62.17 0.31 95.99 1.75
29.12 -0.55 62.93 0.33 96.99 1.88
30.15 -0.52 64.06 0.36 97.98 2.05
30.85 -0.50 65.17 0.39 99.01 2.33
31.92 -0.47 67.00 0.44 99.80 2.88

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Standard Report Tables


Standard Diameter Standard Mass %
300 95
250 90
200 85
150 80
100 75
80 70
60 65
50 60
40 55
30 50
25 45
20 40
15 35
10 30
8 25
6 20
5 15
4 10
3 5
1.5
1
0.8
0.6
0.5
0.4
0.3
0.2
0.1

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D Exported Data Example

D EXPORTED DATA EXAMPLE


This exported data has been truncated for this manual.

Sample Information File

Sample Information

Sample: MPSRM
Operator: AWT
Submitter: Micromeritics
Parameter 1 0.000
Parameter 2 0.000
Parameter 3 0.000
Type of data: Automatically collected

Analysis Conditions

Parameter set name: Garnet Medium Particle Size Reference

Sample Properties

Particle description: Garnet


Density: 3.880 g/cm³

Liquid Properties

Parameter set name: Water


Classification: Interpolated

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D Exported Data Example

Table of User Entered Densities and Viscosities

Temperature Viscosity Density


(°C) (mPa·s) (g/cm³)
---
26.0 0.8737 0.9968
32.0 0.7679 0.9951
38.0 0.6814 0.9930

Analysis Control Parameters

Starting diameter: 50.00 µm


Ending diameter: 0.18 µm
Analysis type: High Speed

Analysis Options

MasterTech stir time: 30 s


MasterTech stirrer speed: Low
MasterTech probe time: 15 s
Stop at selected mass percent: No
Ending percent finer: 0.0
Number of tests: 1
Leave pump on during analysis: No
Wait for temperature stabilization: Yes
Mixing chamber stirrer speed: 6
Full scale pump speed: 3
Bubble detection method: Medium
Rinse after analysis: Yes
Rinse method: Fixed Cycles
Rinse cycles: 3

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D Exported Data Example

Rinse pump speed: 4

Report Options

Report ID: Garnet Medium Particle Size Reference

Distribution Type: Mass


Selected Test: Last

Reference Sample:

1) C:\Users\Public\Documents\Micromeritics\SediGraph III
Plus\data\example\MPSRMCEN.SMP

Specification Samples:

1) C:\Users\Public\Documents\Micromeritics\SediGraph III
Plus\data\example\MPSRMCRS.SMP
2) C:\Users\Public\Documents\Micromeritics\SediGraph III
Plus\data\example\MPSRMFIN.SMP

Overlay Samples:

1) C:\Users\Public\Documents\Micromeritics\SediGraph III
Plus\data\example\MPSRMCEN.SMP
2) C:\Users\Public\Documents\Micromeritics\SediGraph III
Plus\data\example\MPSRMCRS.SMP
3) C:\Users\Public\Documents\Micromeritics\SediGraph III
Plus\data\example\MPSRMFIN.SMP

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D Exported Data Example

Peak selection type: Automatic


Minimum percent of dist. to report: 5.0 %
Minimum valley depth to separate peaks: 0.00

Reports

Combined Report Yes


Standard Class Size Table No
Standard Sieve Table No
Particle Size Table No
Cumulative Fraction Table No
Cumulative Graph Yes
Frequency Graph Yes
Difference from Ref Graph Yes
Out of Spec Graph Yes
Rosin Rammler No
Summary Report No
Baseline Yes
Surface Area No
Surface Area Population No
Number No
Number Population No
Log Probability No
Advanced Reports No
Sample Log No

Combined Report

Standard Class Size Table No


Standard Sieve Table No
Particle Size Table Yes
Cumulative Fraction Table Yes

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D Exported Data Example

Cumulative Graph Yes


Frequency Graph No
Difference from Ref Graph No
Out of Spec Graph No
Rosin Rammler No
Summary Report Yes
Baseline No
Surface Area No
Surface Area Population No
Number No
Number Population No
Log Probability No
Advanced Reports No
Sample Log No

Cumulative Finer Mass Fraction vs. Diameter

Plot Type: Curve


Overlay: Samples
Autoscale x-axis: Yes
Autoscale y-axis: Yes
X axis range: 0.0090 to 125,000.0000 µm
Y axis range: -0.100 to 1.100

Mass Frequency vs. Diameter

Plot Type: Curve


Overlay: Tests
Autoscale x-axis: Yes
Autoscale y-axis: Yes
X axis range: 0.0090 to 125,000.0000 µm
Y axis range: -0.100 to 1.100

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D Exported Data Example

Cumulative Finer Mass Fraction Difference From Reference Graph

Plot Type: Curve


Overlay: Tests
Autoscale x-axis: No
Autoscale y-axis: Yes
X axis range: 1.0000 to 7.0000 µm
Y axis range: -1.0000 to 1.1000

Cumulative Finer Mass Fraction Out of Specification Graph

Plot Type: Curve


Overlay: Tests
Autoscale x-axis: Yes
Autoscale y-axis: Yes
X axis range: 0.0090 to 125,000.0000 µm
Y axis range: -1.0000 to 1.1000

Collected Data

Sample recorded at first analysis: Garnet


Liquid recorded at first analysis: Water
Use auxiliary baseline: No
Mean baseline value: 135 kCnts/s

Test Summary:

Mean
Cell Liquid Full
Test Temperature Density Viscosity Scale
Number (°C) (g/cm³) (mPa·s) (kCnts)

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D Exported Data Example

-----
1 35.0 0.9941 0.7226 84
2 35.0 0.9941 0.7227 84
3 35.0 0.9941 0.7227 84
4 35.0 0.9941 0.7227 84
5 35.0 0.9941 0.7227 84
6 35.0 0.9941 0.7227 84
7 35.0 0.9941 0.7227 84
8 35.0 0.9941 0.7227 84

Instrument name: 0003


Serial number: 0003

Test 1

Cumulative Cumulative Cumul-


ative
Particle Mass Particle Mass Particle Ma-
ss
Diameter Finer Diameter Finer Diameter Fin-
er
(µm) (Fraction) (µm) (Fraction) (µm)
(Fraction)
------
51.5822 0.997 7.7179 0.958 1.1548 0.0-
99
48.6968 0.997 7.2862 0.943 1.0902 0.0-
91
45.9727 0.997 6.8786 0.924 1.0292 0.0-
84
43.4010 0.996 6.4938 0.900 0.9716 0.0-
77
40.9732 0.996 6.1306 0.871 0.9173 0.0-

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D Exported Data Example

70
38.6812 0.995 5.7876 0.837 0.8660 0.0-
64
36.5174 0.995 5.4639 0.799 0.8175 0.0-
58
34.4747 0.995 5.1582 0.756 0.7718 0.0-
52
32.5462 0.995 4.8697 0.711 0.7286 0.0-
46
30.7256 0.995 4.5973 0.663 0.6879 0.0-
41
29.0068 0.995 4.3401 0.615 0.6494 0.0-
37
27.3842 0.994 4.0973 0.568 0.6131 0.0-
33
25.8523 0.994 3.8681 0.522 0.5788 0.0-
30
24.4062 0.993 3.6517 0.478 0.5464 0.0-
27
23.0409 0.993 3.4475 0.437 0.5158 0.0-
24
21.7520 0.993 3.2546 0.400 0.4870 0.0-
22
20.5353 0.994 3.0726 0.366 0.4597 0.0-
20
19.3865 0.994 2.9007 0.335 0.4340 0.0-
18
18.3021 0.996 2.7384 0.307 0.4097 0.0-
15
17.2783 0.997 2.5852 0.283 0.3868 0.0-
13
16.3117 0.998 2.4406 0.261 0.3652 0.0-
11
15.3993 0.998 2.3041 0.242 0.3447 0.0-
08
14.5378 0.998 2.1752 0.224 0.3255 0.0-
06
13.7246 0.998 2.0535 0.209 0.3073 0.0-

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D Exported Data Example

03
12.9569 0.997 1.9387 0.194 0.2901 0.0-
01
12.2321 0.996 1.8302 0.181 0.2738 -
0.002
11.5478 0.994 1.7278 0.168 0.2585 -
0.004
10.9018 0.992 1.6312 0.156 0.2441 -
0.005
10.2920 0.990 1.5399 0.145 0.2304 -
0.006
9.7163 0.987 1.4538 0.135 0.2175 -
0.006
9.1728 0.983 1.3725 0.125 0.2054 -
0.005
8.6596 0.977 1.2957 0.116 0.1939 -
0.003
8.1752 0.969 1.2232 0.107 0.1830 -
0.001

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E Sample Dispersion

E SAMPLE DISPERSION
Use of the SediGraph requires that each powder be well dispersed in a liquid of known density
and viscosity and that the difference between the powder and liquid densities be accurately
known. Viscosity and density data for some common liquids are given in Sources of Dispersing
Aids on page I - 1. Handbook values for other liquids are usually sufficiently accurate, so the
latter requirement means that only the powder density must be determined if it is unknown and if
composition information does not permit calculation from handbook values. For this, one of
Micromeritics’ pycnometers is recommended. For materials likely to have dead-end pores into
which liquid may not completely penetrate, the effective density1 ) may need to be determined
using the sedimentation liquid to be employed and a gas pycnometer.

The liquid should be one in which the powder can be completely dispersed (separated into
unattached particles) for accurate size results to be obtained. Obviously, the liquid should be
nontoxic, readily available, and one in which the sample is insoluble. Complete insolubility may be
difficult to achieve in some instances. Solubility problems may be minimized by allowing the liquid
to stand in contact with the particle material prior to using the liquid for the test sample. This
cannot completely eliminate problems, however, because particle solubility is a function of particle
size. Small particles are more soluble than large ones. In a dispersion of different sizes, the
smallest particles tend to go into solution while precipitation occurs on the larger particles. In
making a particle size distribution analysis, particle solubility is indicated if the recorded
distribution consistently fails to attain zero percent even long after the analysis is complete.

There are no established rules or laws by which complete particle dispersion can be assured.
Only guidelines can be offered. Some powders disperse easily in any of several liquids and
remain so while others require careful attention to conditions in order to achieve dispersion and
are prone to reagglomerate if conditions shift a small amount. A few can be dispersed only after
extended treatments.

Agitation, resulting in the application of strong shear forces, aids dispersion. The more violent the
agitation — perhaps carried out in a high-speed blender, homogenizer, or an ultrasonic device —
the better generally is the dispersion. Stirring a suspension while subjecting it to ultrasonic
dispersion generally achieves the best dispersion because this ensures that all portions of the mix
are brought into the zones of greatest energy.

For a few friable materials such agitation can result in comminution of the particles for which
measurements are preferred. This is not likely to be the case with solid particles, particularly when
the particles are under 50 to 100 μm in diameter.

1 ) The procedure for determining the effective density is discussed in Application Note #94.
Contact your local sales representative or the Micromeritics sales office to request a copy.

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Air bubbles cause misleading results if trapped in the liquid during agitation. Care should be taken
to avoid bubble entrapment, especially when the liquid is highly viscous. The SediGraph performs
bubble elimination routines and checks to verify their effectiveness, but the best agitation
procedure is one that does not introduce them in the first place.The magnetic stirrer built into the
instrument is a convenient means for maintaining a homogeneous particle dispersion but will
cause flocculation in certain magnetically susceptible materials. With such particles, stirring can
be accomplished by using the ultrasonic dispersion accessory or the MasterTech.

Chemical wetting or dispersing agents also generally aid dispersion. A great variety of such
products are marketed. Chemical Aids for Particle Dispersion on page B - 1 and Sources of
Dispersing Aids on page I - 1 list some of the more useful dispersing aids, as well as sources for
some of these materials. These agents have been found useful for particle dispersion in
Micromeritics’ Materials Analysis Laboratory but are not the only agents available. It is to be noted
that liquid density and viscosity values may need slight adjustment if more than about 0.1% by
weight (based on the dry weight of the sample) of dispersing agent is added and precise
measurements are needed.

Some commercial surfactants are intended for use in specific pH ranges and in particular
nonaqueous solutions. Slight solution composition differences may alter the effectiveness of any
agent. The chemical supplier should be contacted about this type of problem. Sometimes merely
shifting the pH of an aqueous dispersion will yield great improvements in the degree of dispersion.
Metal oxides and metals that are likely to have oxide layers on their surface ordinarily are most
easily dispersed in mildly alkaline media. Metal powders with any likelihood of grease on them
should always be degreased prior to a dispersion attempt. Noble metal powders usually need a
wetting agent for good dispersion. Dispersions involving hydrocarbon liquids that are immiscible
with water are often difficult to make unless the powder is quite dry. Sometimes moisture picked
up from the air is more than enough to cause difficulties.

Micromeritics offers Sedisperse liquids in three series for dispersing particles at low solids
concentrations. A- and P-series are stable, balanced formulations containing highly purified,
saturated aliphatic hydrocarbons and added surfactants. A-series Sedisperse liquids are colorless
while the P-series are pale yellow. These liquids produce nearly universal dispersion of powder-
liquid systems with solids concentrations below three weight percent generally, and as much as
five weight percent in some cases. Sedisperse liquids solubilize adsorbed moisture.

W-series Sedisperse liquids are slightly anionic, non-foaming, aqueous formulations. They also
produce nearly universal dispersion of systems with concentrations generally below three weight
percent. Sedisperse liquids contain built-in surfactants and dispersants so that nothing else needs
to be added for the dispersion of particles except mechanical and / or ultrasonic energy. These
liquids are available over a range of densities and viscosities, thus making them applicable to
particles of widely varying properties. Sedisperse liquids are designed to be used without dilution
or the addition of surfactants, and exhibit good shelf life and stability. A data sheet is supplied with
each liquid giving handling details, density, and viscosity data over a temperature range of 24 to
45 °C.

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The A-series Sedisperse liquids are the most widely useful and will disperse most powders,
including metals, oxides, silicates, pigments, Portland cements, propellants, and many other
powders. Those few materials not dispersing well in the A-series liquids can usually be dispersed
in the P-series Sedisperse liquids. These are special formulations, slightly cationic, developed to
disperse difficult metal and pigmented resin powders. The W-series Sedisperse liquids should be
used to disperse those materials which are soluble in the organic Sedisperse liquids. See
Sedisperse Particle Dispersion Liquids on page H - 1.

Some powders flocculate upon standing a few moments after having been dispersed. Such
flocculation is quite readily detected with the SediGraph. The indicated size distribution as plotted
by the instrument during a test will proceed normally until flocculation starts. The first evidence of
flocculation will likely be an increase in the indicated particle concentration and this will then be
followed by a precipitous drop in the plotted percentage. Flocculation, of course, prevents
accurate particle size analysis, and better dispersion and stabilization techniques must be sought.

As a general guide, the best dispersing technique (includes agent and procedure) is the one
producing consistently the finest distribution of sizes by SediGraph analysis. We make this
assertion because of the high reproducibility of the SediGraph when presented identical samples.
If the sample preparation technique is deficient in freeing particles one from another or if, though
unlikely, is producing particle fracture, this will be evidenced by an inconsistency of results.

The rheological behavior of high concentrations of fine powder in a liquid gives a good preliminary
indication of the suitability of both the liquid medium and the dispersing agent. Some powders
containing as much as 50 percent liquid act as if they were almost a solid mass, but a few tenths of
a percent of wetting agent can cause the mass to take on the consistency of soup. This reaction is
indicative of a very good agent. The effect will not often be so dramatic, but working the mass with
a spatula will give a good indication of the efficacy of an agent.

A test for the optimum quantity of a dispersing agent is conducted by measuring the sediment
volume from a slurry of about 5 weight percent concentration. The slurry and agent must be mixed
and allowed to stand in a sedimentation tube undisturbed by either mechanical vibrations or
thermal currents. The minimum sediment volume indicates the best agent concentration level. If
several dispersing agents are compared at the same time, the minimum sediment volume is also
a measure of the best dispersing agent.

No particular sample concentration is required in using the SediGraph as long as the dispersed
sample reduces the radiation beam intensity by 13 to 70 percent. The recommended procedure
for initial testing is to prepare a dispersion of approximately 5 volume percent concentration.
Portions of this preparation are added to pure suspending liquid until an adequate concentration
for analysis is achieved. The advantage of this procedure is that less concentrated dispersions
can generally be produced without fear of flocculation once the initial preparation is made.

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F SediGraph Results Relative to Other Methods

F SEDIGRAPH RESULTS RELATIVE TO OTHER METHODS


The SediGraph 5100 Analyzer, sieve analysis, and hydrometer measurements yield particle size
distributions on a mass (weight) basis. Microscopic measurements result in size data as a function
of the number of particles. Measurements that involve light scattering, transmission, or diffraction
relate size most appropriately to particle cross sectional area. Particle counting systems, electric
zone sensing, gives size in terms of particle volume.

Mass-based measurements can be expected to be in agreement with respect to their reliability


and the applicability to the size range involved, provided the particles are spherical and solid.
When the particles are irregular, close agreement should not necessarily be anticipated. Sieve
analysis, for example, must be very carefully performed with fine particles to ensure complete
separation according to size without damaging the sieves. Even so, the size determined is not
necessarily the same as that measured by the SediGraph. The SediGraph determines the size of
all particles in terms of the E.S.D. (equivalent spherical diameter). Since sieve openings are
usually square, elongated particles sometimes pass a given sieve in one orientation and at other
times are retained. These differences obviously lead to differences in results.

Light-based instruments incorporate various means for tuning, calibrating, and data reduction,
which can make them agree satisfactorily for some materials with most any one of the other
techniques. Any setting is dependent to a degree on the refractive index of the measured
particles; however, so agreement cannot be general or over all particle size ranges. The shape of
the particles also influences all results.

Mass and volume measurements are equivalent numerically. Therefore, analyses with the
SediGraph and the electric sensing zone can be expected to agree if the particles are spherical,
solid, and if their size range is sufficiently narrow for all of them to be accurately detected by the
electric sensing zone.

Again, precise agreement is not to be expected with irregular particles, for the electric sensing
zone measures something closely akin to the diameter an irregular particle would assume were it
melted into a sphere. This is not necessarily the equivalent spherical diameter.

Microscopic measurements yield particle diameters that, for spheres, are essentially E.S.D. As
before, measured sizes will deviate from E.S.D. when the particles are irregular— the greater the
irregularity, the greater the deviation. The numbers will not correspond even approximately
because, as noted above, the measurements are on a different basis. However, number-based
measurements are readily converted into mass-based (or volume-based) results by applying the
relationship to incremental sizes.

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where Y is the mass percent of particles having the diameter D and n the number of particles of
that diameter. The denominator, therefore, represents the entire spectrum of sizes. The following
tabulation presents number-based data and calculations leading to the number-based and mass-
based diameter distributions.

D n Percent nD3
Largest Number of by Percent by
Particle
Number Mass
Diameter Diameter Particles
Less than Less
Range Within Within
Diameter Than
(μm) Range Range Diameter
(μm)
5.4 - 5.0 5.4 10 100.0 1575 0.0481 0.0481
100.0
4.9 - 4.5 4.9 51 99.2 6000 0.1833 95.2
4.4 - 4.0 4.4 65 95.3 5537 0.1692 76.9
3.9 - 3.5 3.9 70 90.3 4152 0.1269 59.9
3.4 - 3.0 3.4 133 84.9 5227 0.1597 47.3
2.9 - 2.5 2.9 160 74.6 3902 0.1192 31.3
2.4 - 2.0 2.4 288 62.3 3981 0.1216 19.4
1.9 - 1.5 1.0 271 40.1 1859 0.0568 7.2
1.4 - 1.0 1.4 162 19.2 445 0.0136 1.5
0.9 - 0.5 0.9 72 6.7 52 0.0016 0.2
0.4 - 0 0.4 14 1.1 1 0.0000 0.0
1296 = ∑n 32731 = ∑nD3

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G Sedimentation Theory

G SEDIMENTATION THEORY

CALCULATIONS
Sedimentation size analysis is based upon the fact that the measured equilibrium velocity of a
particle through a viscous medium, resulting from the action of the gravitational force, can be
related to the size of the particle by Stokes’ law. For spherical particles, Stokes’ law is expressed
by:

(1)

where

(2)

and D is the diameter of the spherical particle, v its equilibrium sedimentation velocity, and ρ its
density. The fluid medium is characterized by viscosity η and density ρo ; g is the acceleration of
gravity. These equations apply rigorously as long as the particle Reynolds number, Dvρo/η, is less
than 0.3 and they apply up to a Reynolds number of 0.5, with about 3% error.1 )

In practice, truly spherical particles are seldom encountered, and Stokes’ law is not exact for any
other shape. Since irregular shapes cannot in any case be described by a single linear dimension,
it is accepted practice to specify the size of non-spherical particles in terms of the diameter of a
sphere of the same material that would have the same sedimentation velocity. Thus, for non-
spherical particles, the terms “Stokes’ diameter” or “equivalent spherical diameter” are universally
understood. The term “equivalent spherical diameter” (E.S.D.) is sometimes used in a different
context to mean the diameter of a sphere of the same material that would have the same mass as
the particle in question; that is, the results of measurements of particle dimensions from electron
micrographs are frequently reduced to size distribution curves in terms of mass E.S.D. In general,
the relationship between these two measures of size is given by the inequality.

(3)

The ratio expressed in equation (3) is usually close to unity.

Data on the sedimentation velocity of suspended particles may be obtained in two ways: (a) by
measuring the concentration of particles remaining in suspension as a function of time, or (b) by
measuring the quantity of sediment produced as a function of time. The latter approach is less
desirable mathematically because of the graphical differentiation required to reduce the data to a
size distribution curve.

1 ) Lapple, C.E., et al, Fluid and Particle Mechanics, University of Delaware, Newark, 1956.

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Tests based on the first approach are traditionally performed in the following way. A dilute,
dispersion of the fine particle material is stirred to render it homogeneous and then allowed to
stand undisturbed while undergoing sedimentation. Time is measured from the beginning of the
settling period. By Stokes’ law, a particle of diameter D will settle a distance h in time t according to
the expression:

(4)

where K is given by equation (2). Consequently, after a given time ti all particles larger than the
corresponding diameter Di will have fallen below a given distance h from the surface of the
suspension. If the initial (uniform) concentration of material is Co g/cm3 and the concentration
after time ti at distance h is Ci g/cm3, then Pi, the weight percent of material finer than Di, is given
by:

(5)

By obtaining values of Ci after various times, the corresponding values of Pi and Di may be
calculated, which when plotted yield an integral, or cumulative distribution of particle size in terms
of Stokes’ E.S.D.

The SediGraph uses a finely collimated X-ray beam to measure particle concentration in terms of
the transmitted intensity of the X-ray beam through the suspension relative to the clear or particle-
free suspending fluid. This transmittance is a function of the weight concentration of the
suspended solid at the depth of measurement. Since the X-ray beam can be made extremely
small and because it does not disturb the suspension, it constitutes an ideal measuring technique.

If a sample container or cell of rectangular cross section is irradiated from a direction


perpendicular to one of its sides by a collimated X-ray beam, the fraction of the incident radiation
transmitted by the cell when filled with the suspension under study is given by:

(6)

where I and Io are the transmitted and incident intensities; a1, as, and ac the X-ray absorption
coefficients of the liquid, the particulate solids, and the cell walls, respectively; ɸ1 and ɸs the
weight fractions of liquid and solid present in the suspension; L1 the internal cell thickness in the
direction of irradiation; L2 the total thickness of the cell walls. By using the relation ɸ1=1-ɸs and by
defining a transmittance T as the ratio of the transmission of the cell when filled with a sample
dispersion to its transmission when filled with pure suspending liquid, there is obtained:

(7)

or

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(8)

where A is a constant for the particular apparatus and suspension components.

By collimating the X-ray beam through horizontal slits with a vertical dimension small compared to
the sedimentation depth, h, the measured values of T can be used in calculating the particle size
distribution; that is:

(9)

where To refers to the transmittance of the initial suspension.

METHOD OF ANALYSIS
Generally, the sedimentation method derives its results from the rates that different size particles
fall in a liquid due to the force of gravity. Rate, as used here, is the distance that a particle falls in a
certain period of time. The scientific law which describes the rate that particles fall in a liquid is
called Stokes’ Law. Large particles fall at a faster rate than smaller particles, as shown in the
following illustration.

A. Lowest Falling Rate


B. Highest Falling Rate

In order to determine particle diameters accurately using the falling rates of particles, the density
and viscosity of the liquid used must be known as well as the density of the particles. Density is the
mass of a material that it takes to fill a unit of space. Viscosity may be thought of as the resistance
of the liquid applied to falling particles. For example, a particle falls much slower in syrup than in
water because syrup has a higher viscosity. It should also be noted that temperature affects both
the density and viscosity of liquids; therefore, the temperature of the liquid must be known for
particle size determinations to be accurate.

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The falling rates for various particle sizes are computed before analysis using Stokes’ Law. A
vertical distance and an elapsed time are selected for each falling rate such that a particle falling
at a certain rate will fall a certain distance in a selected time. Relative particle concentration is then
measured at the selected distance and time.

Initially, a completely mixed (homogeneous) suspension of particles is established in a container


by rapidly circulating the mixture. The circulation is stopped, and the relative concentrations of
particles are measured at the selected vertical distances from the top of the container and at the
selected elapsed times after circulation is stopped.

The particle size associated with each concentration measurement is the size of the largest
particle present at the height and time of the measurement. All particles larger than that size have
higher falling rates, and have fallen to a lower point in the container. Smaller particles are still
present at equal concentrations just above and below the specified point. Thus, the concentration
measured at the specified point is the concentration of particles smaller than or equal to that size.

This series of relative concentrations of particles smaller than various sizes is the particle size
distribution.

% Maximum Concentration at Typical Specified Points

Since different particles usually have different shapes, the standard measure used to report
particle size is Equivalent Spherical Diameter. This is the diameter of a sphere (or perfectly
rounded mass) of the same material with the same falling rate.

SYSTEM OPERATION
The sedimentation method is used for particle size analysis in the SediGraph. The rates of particle
fall due to gravity are calculated and X-ray absorption (concentration) of particles at different
heights and points in time are determined, and the results of those determinations are provided as
graphs and tabular reports. Sedimentation analysis takes place in the analyzer. Data are sent to
the computer which provides the graphs and tabular reports.

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The material to be analyzed is dispersed in a liquid, according to the type of analysis to be


performed. (For more information concerning the relationship of dispersion to the type of analysis,
see appendices B and C.) At the appropriate time, the dispersed mixture is poured into the mixing
chamber on the front of the analyzer.

A magnetic stirrer located under the mixing chamber keeps the particles suspended (that is,
keeps the particles from sedimenting) until it is time for the analysis. The stirring speed can be
adjusted as required to properly suspend the particles. If the particles to be analyzed are attracted
to the magnetic stirrer, the magnetic stirrer can be replaced with a mechanical stirrer. If the
dispersion energy required to keep the particles in a dispersed state in the mixing chamber is
more than can be provided by the stirrer used, an ultrasonic probe can be inserted into the mixing
chamber.

Sedimentation takes place inside an analysis cell as shown in the following illustration. At the
appropriate time, the particle mixture is transferred by the analyzer from the mixing chamber to the
analysis cell. Particle circulation is stopped, and the particles are allowed to sediment (or fall)
inside the analysis cell under the influence of gravity. The SediGraph then determines the particle
size distribution.

A. Lowest Falling Rate


B. Highest Falling Rate

An X-ray beam (made up of a number of fine parallel rays) is provided from a source inside the
analyzer. A unit which detects X-rays is placed directly across from the X-ray source. The analysis
cell is placed in the path of the X-ray beam, between the X-ray source and the detector. The cell
contains a window on each side so that the X-rays can pass through the cell to the detector.
Sedimenting particles (particles falling under the influence of gravity) inside the cell cross the path
of the X-ray beam. The particles in the path of the beam absorb X-rays (that is, the particles keep
some X-rays from reaching the detector). The amount of X-ray absorption at the point in the cell
where the beam is located is determined as a percentage of the X-ray absorption with the highest
particle concentration for that sample. Based upon particle falling rates, this percentage is related
to the maximum particle size above that point in the cell.

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A. X-Rays
B. X-Ray Source
C. Sample Cell
D. Particle
E. X-Ray Detector

The SediGraph system uses both particle falling rates and the amount of X-ray absorption for
particle size analysis. Particle falling rates (according to Stokes’ Law) are used to determine the
points in the cell beyond which certain size particles have fallen. X-ray absorption is used to
determine the percentage of total particle mass at different points in the cell. The resulting particle
size distribution data are processed by the system computer and used to provide graphs and
tabular reports which provide details of the analysis.

PARTICLE FALLING RATES


Particle falling rates are very significant in the determination of particle size distribution. However,
there are several important considerations in the accurate determination of particle falling rates.
There must be a reference point for measuring particle falling distances. The SediGraph uses an
automatic beam-split feature for establishing a reference point. Small particles have a low falling
rate, which could require considerable amounts of time for analysis. The SediGraph uses cell
movement during analysis to shorten analysis times by measuring small particle concentration at
very short sedimentation distances. Cell movement does not affect particle falling rates within the
cell. Particle dispersion also affects falling rates; therefore, proper particle dispersion is required
when using the SediGraph.

Beam-Split

A. X-Ray Source
B. 100% Beam
C. 50% Beam
D. Detector
E. Inside Top of Cell

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Since the top of the cell is used as the reference point for measuring particle falling rates, the
exact position of the cell (relative to the X-ray beam) must be known in order for particle falling
rates to be correct. The SediGraph determines the position of the cell by moving the cell to the
point where the top edge of the cell splits the X-ray beam (exactly in half), and by storing this
beam-split data in the system computer so that this position can be located for the next analysis.
Beam-split is done automatically by the system at the start of any automatic scanning operation;
no message is displayed on the monitor unless beam-split cannot be performed for some reason.

Cell Movement

A. Cell is Moved Down

The cell is attached to an elevator assembly which moves the cell down during analysis to speed
the data collection process. The system computer performs the calculations associated with
particle falling rates as the distances and times are changed according to the movement of the
cell. For example, as shown in the cell movement illustration, it might take 30 minutes for the
particle shown to fall the distance from the top of the cell to the X-ray beam; however, by moving
the cell down, the particle reaches the beam in, perhaps, three minutes. The system computer
uses this time and distance in determining the particle falling rate.

Particle Dispersion
The particle falling rates also depend upon how well the particles in the cell are dispersed (or
separated). Joined particles behave as a single particle with a greater falling rate than if the joined
particles were separate (as shown in the following illustration).

A. Joined Particles Have Higher Falling Rate

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X-RAY ABSORPTION
In addition to particle falling rates, the SediGraph uses the relative amount of X-ray absorption as
part of the analysis process. As falling particles in the cell cross the path of the X-ray beam, they
absorb X-rays. In order for X-ray absorption to be used for measuring the distribution of particle
masses in the cell: (1) the minimum and maximum X-ray absorption must be determined for each
X-ray absorption measurement point in the cell; (2) any bubbles in the cell must be detected and
eliminated; and (3) the particles must be properly dispersed, as explained in Appendices B and C.

Baseline (Minimum) Absorption


In order for the X-Ray absorption values to be accurate, a reference (or baseline) must be used
with each value. This baseline is the amount of X-ray absorption with no particle mass present.
However, since the sedimentation liquid also absorbs X-rays, the amount of X-ray absorption for
the liquid must be included in the baseline. The shape of the cell, or cell profile, affects the
accuracy of baseline X-ray absorption values. The SediGraph automatically determines the
baseline and makes baseline corrections for any changes in the shape of the cell. This feature is
called baseline correction. Let’s look at how it works.

When instructed, the SediGraph performs an X-ray scan of the cell filled only with the selected
sedimentation liquid. The reason for this scan is to determine the amount of X-ray absorption of
the cell and liquid alone before any particles are introduced. The scan progresses from the bottom
of the cell toward the top in exactly the same manner as will be done when sample particles are
present.

As the cell is scanned, X-ray absorption reference values (referred to as baseline values) are
determined at many points along the cell. The baseline value is the amount of X-ray absorption at
that point in the cell. The baseline value is for 0% concentration since the cell contains only the
sedimentation liquid and no particles.

A. X-Rays
B. X-Ray Source
C. Sample Cell
D. X-Ray Detector
E. Clear Liquid in Cell

Slight differences in the cell thickness at the measurement points (up to 250) along the cell
change the amount of X-ray absorption for those points. The amount of X-ray absorption at each
point is stored in the system computer and recalled during the analysis to adjust the baseline at
those same points in the cell.

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The baseline values do not change unless the sedimentation liquid changes, the shape of the cell
changes, or the X-ray intensity changes. It is, however, recommended that you obtain a baseline
measurement at the beginning of each shift or whenever a different dispersant (or a new batch) is
to be used. This assures accurate analysis results. The baseline operation is selected from the
Unit [n] menu.

Full-Scale (Maximum) Absorption


Before each analysis, the SediGraph examines the cell filled with particles suspended in liquid
(particles not allowed to sediment). As the cell is being examined, a full-scale X-ray absorption
value (or maximum absorption) is determined for each point along the cell as shown in the
following illustration. This full-scale absorption value is for 100% concentration, since the cell
contains suspended particles, which represents the highest particle concentration for that
analysis. The full-scale absorption values change with each analysis since a different number and
composition of particles is used.

A. X-Rays
B. X-Ray Source
C. Sample Cell
D. Particle
E. X-Ray Detector

The X-ray absorption is measured at up to 250 positions in the cell. This may be reported on the
Baseline / Full scale report. The full scale scan used in the analysis is computed as the average of
10 readings measured at a fixed position.

The full-scale absorption profile operation is performed automatically by the system. Since
baseline absorption and full-scale absorption are known for each analysis point in the cell before
the analysis, the absorption during the analysis is a percentage somewhere between baseline and
full-scale. Using particle falling rate determinations, the system determines the size of the
particles which have fallen beyond the specific analysis point in the cell. Therefore, the absorption
percentage at each specific analysis point in the cell indicates the percentage of particles that are
below a certain particle size. When this is done for a number of points in the cell, the particle size
distribution can be determined.

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Bubble Detection / Elimination


If air bubbles are formed in the cell during analysis, the amount of X-ray absorption at those points
will be detected as a sharp, discrete change. This would make the analysis results invalid. In order
to prevent this, the SediGraph has a built-in bubble detection and elimination feature. This feature
automatically detects and removes bubbles from the cell. A message is displayed on the screen
indicating this operation is in process.

A. Bubbles
B. Cell Tilted for Bubble Discharge

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H Sedisperse Particle Dispersion Liquids

H SEDISPERSE PARTICLE DISPERSION LIQUIDS


Sedisperse A-series and P-series liquids are stable, balanced formulations for dispersing
insoluble particles. These liquids are primarily saturated aliphatic hydrocarbons. Sedisperse A-
series liquids are colorless while P-series liquids are pale yellow. These liquids produce nearly
universal dispersions of powder-liquid systems with solids concentrations below three weight
percent and to as much as five weight percent in some cases. Sedisperse liquids solubilize
adsorbed moisture.

Sedisperse W-series liquids are slightly anionic, non-foaming, aqueous formulations for
dispersing insoluble particles. They also produce nearly universal dispersions of systems with
solids concentrations generally below three weight percent.

Sedisperse liquids are non-irritating, non-toxic, non-carcinogenic, and non-explosive. The organic
Sedisperse liquids will burn, but will not support combustion at room temperature.

STORAGE REQUIREMENTS
Keep containers closed. Keep containers from freezing. If a container develops a leak during
storage, transfer it to another clean container. Spillage may be cleaned using detergent and
water. Sometimes particles may crystallize and settle out of Sedisperse liquids during storage.
This is usually a result of exposure to cold temperatures. It is corrected by warming the
Sedisperse to 40-50 °C and then vigorously shaking the liquid in a closed container to re-dissolve
the particulates. Micro-organisms may also begin to grow in Sedisperse W-series liquids. These
can usually be removed by filtering and the liquid is again usable for particle dispersion.

TECHNICAL DATA
Recommended techniques for using these liquids:

1. Disperse particles using energy from an ultrasonic bath or probe accompanied by


continuous, moderate mechanical agitation to force particles through the nodes of the
standing ultrasound waves.

2. For sedimentation particle size analysis, first disperse the powder in Sedisperse and
estimate the size of the largest particles using a microscope. Next, calculate the liquid
viscosity needed by using the relationship.

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H Sedisperse Particle Dispersion Liquids

where

η = minimum viscosity permitted in mPa•s (or cp)


Dmax = equivalent spherical diameter of the largest particles in μm
ρ = density of the particles in g/cm3

MATERIAL PROPERTIES
A Material Safety Data Sheet (MSDS) is supplied with each purchase. It should be consulted for
the following information:

n Oral toxicity
n Local effect on eyes
n Local effect on skin
n Shock sensitivity
n Decomposition characteristics
n Heat generation characteristics
n Recommended extinguishing agents
n Hazard by inhalation

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H Sedisperse Particle Dispersion Liquids

FIRST AID TREATMENT


The Material Safety Data Sheet (MSDS) supplied with each liquid should be consulted for the
following first aid information:

n Skin contact
n Eye contact
n Inhalation
n Antidote in case of swallowing

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I Sources of Dispersing Aids

I SOURCES OF DISPERSING AIDS


Dispersant Source
Aerosol OT American Cyanamid Company, Process Chemicals Department,
Aerosol 22 One-T Cyanamid Plaza, Wayne, NJ 07470
Calcium Chloride Can be purchased at most laboratory supply houses.
Calgon Calgon Corporation, Water Management Division, Calgon Center, P.
Calgon T O. Box 1346, Pittsburgh, PA 15230
Cobalt Citrate Shepherd Chemical Company, Cincinnati, OH 45212
Cobaltous Chloride Can be purchased at most laboratory supply houses.
Daxad 23, 30 Hampshire Chemical Corporation, 55 Hayden Avenue, Lexington,
MA 02173
Dispex 40 Allied Colloids, 2301 Wilroy Road, Suffolk, VA 23434
FC-134, -161 and -170 3M Company, Chemical Division, St. Paul, MN 55141
Igepal CO-530 GAF Corporation, 1361-T Alps Road, Wayne, NJ 07470
Lomar D Henkel, 300 Brookside Avenue, Ambler, PA 19002
Oleic Acid Can be purchased at most laboratory supply houses.
Renex 648 ICI Americas, Inc., Chemical Division, New Concordville Pike, Wilm-
Tween 20 ington, DE 19897
Atlas G-3300
Triton X-100 Rohm and Haas Company, Independence Mall West, Philadelphia,
Tamol SN PA 19105
Sodium Silicate N Brand Philadelphia Quartz Company, 1301-T E. Fort Avenue, Baltimore,
MD 21230
Pyrophosphate (TSPP) Can be purchased at most laboratory supply houses.
Zonyl A, S-13 E. I. DuPont de Nemours and Company, Dyes and Chemical Divi-
sion, 1000-T Market Street, Wilmington, DE 19898

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J Stokes' Law

J STOKES' LAW
A particle falling due to gravity in a viscous liquid is acted upon by three forces: a gravitational
force acting downward, a buoyant force acting upward, and a drag force acting upward. The
descriptive equation of this motion is

(1)

where m is the mass of the particle, mo the mass of a volume of liquid equal to the volume of the
particle, g the acceleration of gravity, FD the drag force, v the particle velocity, and t the time.

Small particles reach a stable, or terminal, velocity very rapidly; hence, dv/dt quickly becomes
zero. The equation of motion for a sphere of diameter D and density ρ falling in a liquid of density
ρo then becomes

(2)

Dimensional analysis reveals that stable particle motion through a liquid is governed by two
dimensionless groups: the particle Reynolds number Re

(3)

where η is the liquid viscosity, and a drag coefficient CD expressed by

(4)
*

The relationship between Re and CD for laminar (not turbulent) flow conditions is well established
experimentally for low values of the Reynolds number to be

(5)

Combining equations (2) through (5) yields

which has come to be identified as the Stokes law equation1 ) .

1 ) Stokes, G.G., Mathematical and Physical Paper III, Cambridge University Press, 1891.

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Index

INDEX configuration
unit 2 - 11
contact us iii
corporate profile ii
A cumulative finer mass percent vs diameter
report example 6 - 14
about this manual iv cumulative graph options report 7 - 7
air filter, clean 9 - 16 cumulative table report 7 - 6
analysis
perform 5 - 1
prepare for 5 - 1 D
quick start 5 - 11
analysis cell data reduction C - 1
replace 9 - 9 data, manually enter 3 - 4
replace tubing 9 - 10 diagnostics 8 - 1
analysis cell assembly 9 - 9 save files for problem diagnosis 8 - 1
analysis cell, clean 9 - 11 dispersing aids, sources I - 1
Analysis options 4 - 7 drain and load operation 5 - 2
analyzer drain system 9 - 22
components 1 - 1
configure 2 - 11
schematic 2 - 20 E
show status 2 - 23
software 2 - 1 EFUP vii
autorinse 2 - 15 environmentally friendly use period vii
equipment options and upgrades 1 - 3
B export files 2 - 24
exported data example D - 1
exterior
baseline measurement 5 - 4 clean 9 - 17
baseline options report 7 - 4
baseline report 6 - 2
baseline report example 6 - 12 F
bezel, clean 9 - 17
bubbles, cause of 9 - 27 fields and buttons, common 2 - 2
file status 2 - 5
C files
export 2 - 24
list 2 - 25
calculations open a sample file 3 - 3
SPC report variables C - 15 flexible tubing, replace 9 - 18
cell pump operation, check 9 - 20
cell windows, replace 9 - 21
chemical aids for particle dispersion B - 1 G
collimator slits, clean 9 - 14
combined report 7 - 5 general safety v
combined report, example 6 - 13

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Index

ultrasonic probe tip, replace 9 - 31


I MasterTech 052 components 1 - 9
MasterTech Automatic 5 - 6
initialize MasterTech 5 - 15 MasterTech input power fuse, replace 9 - 31
input power fuse. MasterTech, replace 9 - 31 MasterTech Schedule 5 - 8
instrument, status 2 - 19 material properties 4 - 2
intended use vi menu structure 2 - 1
interactive reports 6 - 4 merge data 3 - 7
invert size axis 2 - 16 methods, about 2 - 10
MicroActive reports 6 - 3
mixing chamber, clean 9 - 17
L mixing pump tubing, replace 9 - 25
mixing pump, check operation 9 - 19
level analyzer 9 - 22
libraries 2 - 9
liquid properties 4 - 10 O
list files 2 - 25
log option presentation 2 - 7
show instrument 2 - 19 options
log probability report 7 - 8 sieve table 2 - 14
overlays
sample file 6 - 10
M
maintenance 9 - 1 P
analysis cell clean 9 - 11
analysis cell replace tubing 9 - 10 parameter files
analysis cell, replace 9 - 9 about 4 - 1
bezel, clean 9 - 17 file name extensions 4 - 1
bubbles, cause of 9 - 27 report options 4 - 12
cell windows, replace 9 - 21 particle dispersion, chemical aids for B - 1
clean instrument exterior 9 - 17 particle size table report 7 - 9
collimator slits clean 9 - 14 parts and accessories 9 - 5
flexible tubing, replace 9 - 18 power 9 - 6
MasterTech input power fuse, replace 9 - power analyzer on and off 9 - 28
31 power failure, recover from 9 - 29
MasterTech ultrasonic probe tip, preventive maintenance 9 - 8
replace 9 - 31 pump, reset mixing pump and cell pump 9 -
mixing chamber, clean 9 - 17 21
X-ray indicator lamps, replace 9 - 23 Python
manual control get particle sizing sample A - 18
enable 9 - 7 Python module 7 - 1, A - 1
manual, about this iv acquire basic information A - 9
mass frequency vs diameter report acquire overlay sample data A - 15
example 6 - 15 acquire report results A - 13
MasterTech advanced reports 7 - 1, A - 1
initialize 5 - 15 get sample information item A - 36

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Index

graphic report A - 33 log probability 7 - 8


MicModule Python calls A - 30 mass frequency vs diameter report
overlay data A - 29 example 6 - 15
reports A - 5 MicroActive 6 - 3
scripts A - 4 options 4 - 12
summary report A - 32 particle size table 7 - 9
tables A - 30 Rosin Rammler 7 - 10
sample log 7 - 10
SPC report options 6 - 3
Q standard class size table report 7 - 11
start 6 - 1
quick start analysis 5 - 11 summary report options 7 - 13
reports, Python module A - 5
Reynolds number options 2 - 14
R rinse 5 - 16
Rosin Rammler report 7 - 10
reference material analysis
perform 5 - 21
reference material analysis, perform 9 - 26 S
report
standard sieve table 7 - 12 safe servicing 9 - 5
report examples safety 1 - 4
baseline report 6 - 12 sample analysis
combined report 6 - 13 perform 5 - 13
cumulative finer mass percent vs dia- sample dispersion E - 1
meter 6 - 14 sample file 3 - 2, 5 - 1
mass frequency vs diameter report about 3 - 1
example 6 - 15 open 3 - 3
report options overlays 6 - 10
selected 7 - 1 sample log
Report Style 2 - 17 report 7 - 10
reports schematic
about 6 - 1 instrument 2 - 20
advanced, Python module 7 - 1, A - 1 SediGraph results F - 1
baseline 6 - 2 sedimentation theory G - 1
baseline options 7 - 4 Sedisperse particle dispersion liquids H - 1
combined report example 6 - 13 selected reports
cumulative finer mass percent vs dia- baseline options 7 - 4
meter report example 6 - 14 combined report 7 - 5
cumulative graph options 7 - 7 cumulative graph options 7 - 7
cumulative percent table 7 - 6 cumulative table 7 - 6
examples 6 - 12 log probability 7 - 8
baseline report 6 - 12 particle size table 7 - 9
features and shortcuts 6 - 5 Rosin Rammler 7 - 10
reports 6 - 5 standard class size table report 7 - 11
generate sample file overlays 6 - 10 standard sieve table 7 - 12
interactive 6 - 4 summary report options 7 - 13

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Index

shortcuts, application 2 - 6
show instrument log 2 - 19
X
show instrument schematic 2 - 20
sieve table 2 - 14 x-ray certification 1 - 6
software X-ray indicator lamp, replace 9 - 23
about 2 - 1
setup 2 - 25
updates 2 - 26
software uninstall 2 - 26
SPC report 6 - 3
calculations C - 15
specifications
MasterTech 1 - 12
SediGraph III Plus 1 - 7
standard class size table report 7 - 11
standard sieve table report 7 - 12
status
analyzer 2 - 23
instrument 2 - 19
Stokes' Law J - 1
summary report options 7 - 13

T
troubleshooting 9 - 1
analysis cell, replace 9 - 9
analysis cell, replace tubing 9 - 10
and maintenance
manual control, enable 9 - 7
power failure, recover from 9 - 29
preventive maintenance 9 - 8
troubleshooting, analysis cell, clean 9 - 11

U
unit configuration 2 - 11
unit selection 2 - 16

W
warranty i

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