SediGraph III Plus Operator Manual Rev A Aug 2021
SediGraph III Plus Operator Manual Rev A Aug 2021
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.
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____________________________________________________________________________
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.
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.
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
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.
GENERAL SAFETY
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 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.
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 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.
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.
Warranty i
Corporate Profile ii
Contact Us iii
General Safety v
8 Diagnostics 8-1
Save Files for Problem Diagnosis 8-1
Index Index - 1
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.
A. Ethernet
port
B. Aux RS-232
C. MasterTech
RS-232
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.
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.
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.
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).
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
Frequency 50/60Hz
Overvoltage category II
Physical
Environment
Indoor only
Indoor or outdoor use Altitude: 2000 m max
Pollution degree of the intended environment: 2
Computer Requirements
Drives USB port
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.
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
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.
After using the probe, press the switch again to place the probe in
automatic mode. Then replace it in its holder.
REAR COMPONENTS
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.
Electrical
Frequency 50/60 Hz
1.25 A (100/120VAC)
Current
0.75 A (220/240VAC)
Environment
Indoor only
Indoor or outdoor use Altitude: 2000 m max
Pollution degree of the intended environment: 2
Physical
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.
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.
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.
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.
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.
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.
LIBRARIES
Options > Manage Libraries
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.
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 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.
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.
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.
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.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
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.
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.
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.
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.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
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.
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
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.
Schematic (continued)
Component Description
Turn On / Off. Turn the MasterTech pump on and off.
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.
SHOW STATUS
Unit [n] > Show Status
Use to show the current status for each port.
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.
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.
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.
SOFTWARE SETUP
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.
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:
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.
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.
When working with an existing sample file, consider copying the sample file to
maintain the original configuration options.
n Copy and paste onto the graph area of the interactive window.
n Import data into the interactive window.
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.
6. Ensure that all parameter fields are set appropriately, then click Paste.
Example:
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.
MERGE DATA
Use to merge data collected from an external source.
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.
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.
Properties. Click to edit the properties of the analysis liquid. See Liquid
Properties on page 4 - 10.
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.
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.
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.
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.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
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.
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.
If only small particles are present in the sample (less than 1 mm),
select Fine bubble detection.
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]
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.
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.
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.
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.
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.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
REPORT OPTIONS
File > Open > [.RPO File]
Or, click the Report Options tab when in Advanced option presentation.
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.
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.
5 PERFORM AN ANALYSIS
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.
Before collecting baseline data or performing an analysis, the cell and mixing chamber must be
drained and the sample (or baseline liquid) loaded.
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.
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.
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:
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.
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.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
MASTERTECH AUTOMATIC
Unit[n] > MasterTech Automatic
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.
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.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
MASTERTECH SCHEDULE
Unit [n] > MasterTech Schedule
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.
Sample analysis. Click Browse, then choose the sample file or use
with the sample in this beaker position.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
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.
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.
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.
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.
INITIALIZE MASTERTECH
Unit [n] > Initialize MasterTech
When the MasterTech is initialized, the tray is aligned so that beaker #1 is in the start position.
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.
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.
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.
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.
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.
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.
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.
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
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
REPORT EXAMPLES
BASELINE REPORT
COMBINED REPORT
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.
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.
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.
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.
BASELINE OPTIONS REPORT
The Baseline report shows a baseline measurement of the x-ray intensity as a function of cell
elevator position.
COMBINED REPORT
The Combined report combines a selection of any SediGraph report onto a single page.
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.
GRAPH OPTIONS
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.
ROSIN RAMMLER
This report shows the sample's particle distribution using a graph of the Rosin Rammler
parameter as a function of the particle diameter.
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.
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.
For fields and buttons not listed in this table, see Common Fields and But-
tons on page 2 - 2.
Do not modify this instrument without the authorization of a Micromeritics service per-
sonnel.
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.
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.
X-RAY ON indicator is turned on, but the computer display shows 0 kilocounts.
X-RAY STANDBY indicator was turned on, but when keyswitch is placed in X-RAY
ON position, XRAY ON indicator does not turn on.
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:
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
The collimator slits may become blocked by dust or debris which accumulates in the analysis
compartment over a period of time, causing inaccurate results.
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.
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.
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.
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.
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.
2. Disconnect the flexible tubing from the mixing chamber, exercising caution to prevent dam-
age to the tubing.
3. Disconnect the electrical cable.
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.
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.
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.
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.
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.
Ensure that the outlet tube is in the waste reservoir and the rinse tube is in the rinse liquid
reservoir.
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.
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.
4. Push lamp socket lever toward the analyzer and insert replacement lamp into socket.
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.
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:
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.
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.
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.
Cause: Pump switch on the front panel may be in the OFF position.
Action: Press the pump AUTO/ OFF switch on the front panel.
Cause: The cable may be connected improperly from the MasterTech to the computer.
Action: Check the cable connections.
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.
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.
Fuses may be obtained from Micromeritics or a vendor of your choice as long as they
meet the requirements specified in this section.
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.
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.
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:
Once the fuse block and cover assembly are in place, the position of the indicator pin shows the
input power selected.
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.
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.
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.
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.
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='^' )
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"] )
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))] )
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']],
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])
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'
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"]
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
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,
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':
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)
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)
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
(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
(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
(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
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.
Tables
Available Mic Python calls for tables:
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:
Summary Reports
Graphic Reports
Add a Curve
This script adds a curve to the last created graphical report:
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
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
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).
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.
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.
DENSITY
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):
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.
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.
Cumulative mass percent coarser data are simply the difference of scaled mass percent
finer data from 100:
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.
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,
CumFracRetaini = CumFracCoarseri-1
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.
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.
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).
where
The cumulative number percent for a class is computed as the summation of the non-negative
frequencies for all smaller classes.
where
The cumulative number percent for a class is computed as the summation of the non-negative
frequencies for all smaller classes.
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.
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.
MEDIAN
MedianDiam = Diameter interpolated from HighDiam vs. CumFracCoarser at CumFracCoarser =
0.5.
ARITHMETIC CALCULATIONS
MEAN
COEFFICIENT OF VARIATION
SKEWNESS
KURTOSIS
+Xẟ
-Xẟ
GEOMETRIC CALCULATIONS
MEAN
GeoMeanDiam = 10
SKEWNESS OF LOG
KURTOSIS OF LOG
+Xẟ
-Xẟ
Coarseri-1
or,
OutSpecFracFineri = -OutSpecFracCoarseri-1
OutSpecFracRetaini = OutSpecFracCoarseri-1
OutSpecFracPassi = OutSpecFracCoarseri-1
or,
DiffRefFineri = DiffRefCoarseri-1
DiffRefRetaini = DiffRefCoarseri-1
DiffRefPassi = DiffRefCoarseri-1
The coefficient of correlation for this line is also calculated in the usual way. 2 )
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)
REYNOLDS NUMBER
The Reynolds Number is calculated as follows:
where
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.
Yprob value = Spline interpolation at CumMassFiner values of the x vs. y log probability
table values
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
Sample Properties
Liquid Properties
Analysis Options
Report Options
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
Reports
Combined Report
Collected Data
Test Summary:
Mean
Cell Liquid Full
Test Temperature Density Viscosity Scale
Number (°C) (g/cm³) (mPa·s) (kCnts)
-----
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
Test 1
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-
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
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.
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.
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.
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.
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
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)
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.
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.
(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
(8)
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)
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.
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.
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.
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.
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.
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.
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.
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.
Beam-Split
A. X-Ray Source
B. 100% Beam
C. 50% Beam
D. Detector
E. Inside Top of Cell
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
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).
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.
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.
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.
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.
A. Bubbles
B. Cell Tilted for Bubble Discharge
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:
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.
where
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
n Skin contact
n Eye contact
n Inhalation
n Antidote in case of swallowing
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)
(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)
1 ) Stokes, G.G., Mathematical and Physical Paper III, Cambridge University Press, 1891.
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
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