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Manual300S ver.2.0

The SOFTA Corporation ELSD Manual provides operational guidelines and safety information for the Model 300S ELSD, emphasizing the importance of following proper procedures to avoid electrical, chemical, and physical hazards. It details the principles of operation, including nebulization, evaporation, and detection processes, as well as installation and maintenance instructions. The document also includes warnings about modifications, user responsibilities, and the necessity of using appropriate gases and connections during operation.

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0% found this document useful (0 votes)
23 views

Manual300S ver.2.0

The SOFTA Corporation ELSD Manual provides operational guidelines and safety information for the Model 300S ELSD, emphasizing the importance of following proper procedures to avoid electrical, chemical, and physical hazards. It details the principles of operation, including nebulization, evaporation, and detection processes, as well as installation and maintenance instructions. The document also includes warnings about modifications, user responsibilities, and the necessity of using appropriate gases and connections during operation.

Uploaded by

danilosmelo.blur
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 25

SOFTA CORPORATION

ELSD Manual
Model 300S

Version 2.0, August 2013

SofTA Corporation
11005 Dover Street Unit 300
Westminster, CO 80021
(303) 465-1106 Voice (626) 608-2785 Fax www.softacorporation.com
Notice
The information in this document is subject to change without notice and should not be constructed as
a commitment by SofTA Corporation. SofTA Corporation assumes no responsibility for any error
that may appear in this document. This document is believed to be complete and accurate at the time
of publication. In no event shall SofTA Corporation be liable for incidental or consequential damages
in connection with, or arising from, the use of this document.
2013 SofTA Corporation. Printed in the USA. All rights reserved. This document or parts may
not be reproduced in any form without the written permission of the publisher.
Intended Use
The SofTA ELS Detector manuals address their operation and performance without regard to the
nature of the material being analyzed or processed. They do not presume to inform, instruct or advise
users in the correct or safe execution of specific procedures. When you are using this instrument,
follow generally acceptable procedures for quality control and methods development.
Changes or modifications to this instrument not expressly approved by the party responsible for
compliance could void the user’s authority to operate the equipment.
CAUTION
This product complies with all applicable safety requirements. The user shall be made aware that if
this instrument is used in a manner not specified by the manufacturer, the protection provided by the
equipment may be impaired. The detector does not contain user-serviceable components. No routine
user maintenance is required.
Electrical Hazards
It is the user’s obligation to make certain that it is plugged in to an appropriate AC power outlet. To
avoid the possibility of electrical shock, do not open the detector cover. The cover protects from
potentially lethal voltages. Removing the cover will void your warranty. An instrument that has been
inappropriately serviced may be a shock hazard, even with the cover re-installed. Refer all service to
qualified personnel.

To avoid electrical shock, turn the power to the detector off and unplug the power cord from the rear
of the detector before you replace a fuse. To protect against fire hazard, replace fuse with those of the
same type and rating.
It is recommended that all components of the HPLC be connected to a common ground.
To avoid electrical shock, power off the detector before making any electrical connections.
Laser Safety
This ELSD is a Class I laser product with a Class IIIa (3R) embedded laser. The embedded laser
beam is less than 5 mW, 650 nm, and is collimated. There are no user adjustments for power,
alignment, or collimation. Under use conditions, the laser is never visible, and presents no special
safety considerations.

As required by regulation,
the back panel has the
following laser related
labels, in addition to a
serial number label.
Internal components may have the following label:

Never remove a component with this label. Doing so could expose a user to a potentially hazardous
laser beam. Always refer service to qualified personnel.

Chemical Hazards
When you handle solvents, change tubing, or operate the detector observe safe laboratory practices
when operating this detector to avoid chemical or electrical hazards.
Know the physical and chemical properties of the solvents and analytes you use. Refer to the
Material Safety Data sheets for any chemical you come in contact with.
Do not use gases that support combustion with combustible solvents. Always use inert gases.
To avoid inhaling harmful organic solvents and other materials, the detector exhaust should not be
allowed to enter the laboratory atmosphere.
Physical Hazards
To avoid burns, turn off the power at least 30 minutes before performing maintenance procedures.
Use caution when working with any polymer tubing under pressure:
Always wear eye protection when near pressurized tubing.
Extinguish all nearby flames
Do not use tubing that has been severely stressed, kinked or weaken by chemical attack.
Table of Contents
Notice ...................................................................... ii Drift Tube Page ..................................................... 13
Intended Use ........................................................... ii Control Page.......................................................... 14
CAUTION............................................................... ii Timer Page ............................................................ 14
Electrical Hazards ................................................... ii Filter Page ............................................................. 14
Laser Safety ............................................................ ii Load Method Page ................................................ 15
Chemical Hazards .................................................. iii Save Method Page................................................. 15
Physical Hazards .................................................... iii Calibration Page .................................................... 15
Detector Gain Page ............................................... 16
INTRODUCTION ............................................. 5 Full Scale Page ...................................................... 16
ELSD Principle of Operation ............................... 5 Error Condition Screen ......................................... 16
Introduction ............................................................. 5 Standby Countdown Screen .................................. 16
Operation................................................................. 5 Operating Conditions ......................................... 17
Nebulization ............................................................ 5 Start Up Procedure ................................................ 17
Evaporation ............................................................. 7 Shut Down Procedure ........................................... 17
Detection ................................................................. 7 Choosing Operating Conditions ............................ 18
Thermo-Split Spray Chamber Temperature.......... 18
Drift Tube Temperature ........................................ 19
UNPACKING AND INSTALLATION ............... 8 Mobile Phase Flowrate ......................................... 20
What you will need................................................ 8 Gradient Separations ............................................. 20
Unpacking .............................................................. 8 Suggested Operating Temperatures ...................... 20
Connections ........................................................... 8 Mobile Phase Considerations ................................ 21
Power connection .................................................... 8 Selecting a solvent ................................................ 21
Exhaust.................................................................... 9 Mobile Phase Flowrate and Composition ............. 21
Communication ....................................................... 9 Buffer Compatibility ............................................. 21
I/O Connections ...................................................... 9 Column Pre-Treatment.......................................... 21
Gas Connections ..................................................... 9 QC Test Conditions............................................... 21
Fluid Connections ................................................... 9
Nebulization Chamber Drain .................................. 9
MAINTENANCE & TROUBLESHOOTING ... 22
Routine Maintenance ............................................ 22
OPERATION ................................................. 10 Troubleshooting .................................................... 22
Instrument Controls ........................................... 10
Status Indicator Lights .......................................... 10
Status Alarm.......................................................... 10 APPENDIX .................................................... 23
MENU|POWER Key ............................................ 11 Accessories ........................................................... 23
Autozero Key ........................................................ 11 Specification ......................................................... 23
Display Screens ..................................................... 11 Warranty ............................................................... 24
Startup Screen ....................................................... 11 Shipments.............................................................. 24
Home Screen ......................................................... 12 Damaged Shipments ............................................. 24
RST/BLN Screen .................................................. 12 Filing of Claims .................................................... 25
Menu Screen ......................................................... 13 Returns .................................................................. 25
Spray Chamber Page ............................................. 13

4
1
Chapter

Introduction
ELSD Principle of Operation

Introduction
ELSDs are near universal detectors, primarily used in High Performance Liquid Chromatography
(HPLC) though they have been used successfully in other types of chromatography as well. Their
principal requirement is that the analyte be less volatile than the mobile phase. An ELSD cannot
detect highly volatile analytes. However, most analytes of interest are less volatile than the eluting
solvents.

Evaporative light scattering detectors are replacing ultraviolet (UV) detection because they
can detect most analytes, even those that do not absorb UV radiation, are stable during gradient
elutions, and respond to the relative mass of the analyte -an important feature that is useful when
detecting unknown materials. The ELSD is superior to the refractive index detector (RID), it can be
used with gradient chromatography, it is not susceptible to ambient temperature changes, and it does
not produce negative peaks, which can be difficult to quantify. The ELSD does not respond to the
mobile phase disruption seen as solvent front peaks in the void volume with UV and RI detectors, so
early eluting analytes can be easily quantified. Mass spectrometry (MS) detection is also a universal
detector, but its high cost and complexity have kept it from being widely used. In fact, the operation
requirements of MS closely match that of the ELSD. This allows the less expensive and complicated
ELSD to be used as a method development detector for methods to be used on the MS systems.
Operation
The SofTA ELSD employs a unique method of detection. The process involves the
nebulization of the column eluent, transforming it into an aerosol cloud. As this cloud travels through
a heated zone within the instrument, the more volatile mobile phase evaporates, leaving a smaller
cloud of analyte particles. These particles pass through a beam of light, scattering some of the light,
which is converted into an electronic signal.
Nebulization

Nebulization transforms the liquid phase leaving the column into an aerosol cloud of fine
droplets. The size and uniformity of the droplets are extremely important in achieving sensitivity and

5
reproducibility. The SofTA ELSD uses a special concentric flow nebulizer and a constant flow of an
inert gas to ensure a narrow droplet size distribution. Our nebulizer is constructed entirely from
Teflon®, which accumulates deposits less than either glass or stainless steel.
To handle flow rates and mobile phases
common in HPLC, all ELSDs need a way to divert part
of the aerosol cloud to waste. Softa uses a patent
pending Thermo-Split technology. Our Thermo-Split
chamber combines a gentle bend with temperature
controlled walls. When the aerosol exiting the nebulizer
encounters a cool environment, it partially condenses
into larger particles whose momentum carries them into
the wall and down the drain.

With cooling, the particles condense and


increase in size. They are carried into the
walls of the bend and exit via the drain.

With the Temperature control option installed,


the temperature of the Spray Chamber may be
elevated. As the aerosol traverses the chamber, it
partially evaporates, shifting the particle size
distribution low enough for essentially all the particles
to negotiate the bend. These operating conditions may
be useful for special applications. Under these
conditions a majority of the aerosol particles pass
through the chamber and are carried into the
evaporative zone.

With heat, the particles decrease in size and


all pass the bend in the Thermo-Split
chamber.

6
Evaporation

After passing through the nebulization chamber the


aerosol cloud is propelled through the heated evaporation tube
assisted by the carrier gas. In the evaporation tube the solvent
is volatilized to produce particles or droplets of pure analyte.
The temperature of the drift tube is set at the
temperature required to evaporate the solvent. The
temperature is kept as low as possible to avoid particle shape
distortion, evaporation of the analyte or when working with
thermally sensitive compounds.
Detection

The particles emerging from the evaporation tube


enter the optical cell, where the sample particles pass through
the light emitted by a low power laser. The particles scatter
the light, which is detected by a silicon photodiode located at
a 90° angle from the laser. A light trap is located opposite the
laser to collect the light not scattered by particles. The
quantity of light detected is proportional to the solute
concentration and solute particle size distribution. The
photodiode produces a signal, which is sent to the outputs for
collection.

7
2
Chapter

Unpacking and Installation


What you will need
In addition to the ELSD and its accompanying accessories you will need:

Gas Supply: Clean, dry, inert gas regulated to 65psi ± 5 psi is needed for nebulization. Either argon
or nitrogen is acceptable. Do not use gases that support combustion.

Exhaust Device: The carrier gas containing volatilized mobile phase and sample components will exit
the ELSD. You should provide a means of removing this from the laboratory. The ELSD should be
located close to a fume hood or other ventilation device.

Tubing, fittings and tools to connect your HPLC system to the ELSD.

Unpacking
The ELSD is shipped with the accessories listed in Appendix 1. Unpack carefully and confirm that all
the items are present. SofTA ELSDs come in a high quality shipping container, engineered to avoid
damage in transit. Save the shipping container and packaging for future shipments.

Connections
Power connection
The ELSD operates at either 120V or 240V, 50/60 Hz. Confirm that the SofTA ELSD is configured
for the correct voltage before plugging it into line voltage. If the power input module is set to the
wrong voltage, unplug the power cord form the module. Open the fuse compartment by gently prying
the cover from the module with a flat blade screwdriver. Remove the fuse block. Remove the voltage
configuration card from the module by gently pulling with pliers or tweezers. Rotate the plastic
voltage selector until the correct voltage appears on the side opposite the voltage selector. Replace the
card and fuse block. Confirm that the correct voltage is indicated through the cover before securing
the cover. Plug the modular power cord provided into the power input module on the back of the
detector.

8
Exhaust
The ELSD exhaust is a ½” O.D. stainless steel tube. Use ½” I.D. tubing to connect to a fume hood
during operation. Alternately, connect tubing and direct to a cooled collection vessel for later
disposal.

Communication
An output jack can be found on the back of the ELSD for connection to a chart recorder, computing
integrator or computerized data system. The maximum signal output is 5V.

I/O Connections
Pin 1 and Pin 2: A contact closure output. Pins are open when an error conditions exists.

Pin 3 and pin 4: A contact closure input to turn on/off gas remotely. Gas control toggles with
electrical continuity between these two pins. Maintain connectivity for a minimum of 500mS. A
subsequent toggle command within 2 seconds may be ignored.

Pin 5 and 6: A TTL output for instrument status. A logical high indicates the detector is in standby.

Pin 7 and pin 8: A contact closure input to reset baseline remotely. Maintain connectivity for a
minimum of 500mS. A subsequent toggle command within 2 seconds may be ignored.

Gas Connections
Connect a supply of clean, dry, inert gas regulated to 65psi ± 5 psi to the GAS INLET port on the back
of the unit. The internal gas regulator maintains the gas pressure at the factory set value displayed on
the front panel.

Fluid Connections
Connect the outlet from your column to the LIQUID INLET on the front of the unit. The length and
volume between the column outlet and the detector inlet should be kept as short as possible to avoid
unnecessary band broadening.

Nebulization Chamber Drain


The instrument’s internal “P” trap must be full during operation. Restricting the drain port with liquid
is very important to ensure detection sensitivity. Pump mobile phase at 1mL/min without gas flow for
10 minutes or until you see liquid coming out of the drain. Alternately, you may introduce 10 mL of
mobile phase into the drain using a squirt bottle or syringe.

Place the ¼” stainless steel drain adapter, provided in the accessory kit, on the drain port located on
the front of the instrument. Direct the outlet of the tube to a collection vessel. Watch the liquid level
in the vessel during operation and empty when full.

9
3
Chapter

Operation

Instrument Controls
The ELSD is controlled via four multi-function keys on the front panel labeled MENU|POWER,
▲, ▼ and AUTOZERO. The ELSD features a 2 line vacuum florescent display and a row of status
lights to aid in the operation of the detector.

Status Indicator Lights

The status lights below the display provide a visual indication of the conditions of the ELSD.
From left to right the function of the status lights are:
1. Spray Chamber Heater: The yellow light is illuminated when the heater is active, blinks when
the spray chamber is being controlled at the set temperature, and off when the spray chamber
is cooling to a lower temperature.
2. Drift Tube heater: The yellow light is illuminated when the heater is active, blinks when the
drift tube is being controlled at the set temperature, and off when the drift tube is cooling to a
lower temperature.
3. Optic Cell Heater: The yellow light is illuminated when the heater is active, blinks when the
optical cell is being controlled at the set temperature, and off when the optics cell is cooling to
a lower temperature.
4. Laser power: The green light is illuminated when the laser is on and stable and off when the
laser is off. The light blinks when laser power is low or unstable.
5. Gas Supply: The green light is on when the nebulizer gas pressure is within factory set limits,
and the gas valve is open. The green light will blink if a pressure error exists. The green light
will be off if the gas valve has been turned off.
6. Ready Condition: The green light is illuminated when all operating conditions are met and no
error conditions exist.

Status Alarm
The status alarm sounds when the detector status changes from not ready to ready or from ready to
not ready. The alarm is 10 short beeps repeated every 30 seconds. Pressing the AUTOZERO key resets
the alarm. The alarm can be disabled via the Control Page menu screen.

10
MENU|POWER Key
The MENU|POWER key is a multi-function key. An audible beep is heard when the key is activated.
When the instrument is off, press the MENU|POWER key to turn the ELSD on. Note that when the
power cord is plugged in the MENU|POWER key is dimly illuminated from behind with a blue light.
When the MENU|POWER key is used to turn on the ELSD, the backlighting expands to the other keys.
Once the ELSD is powered up the MENU|POWER key is used to view error conditions, cycle through
the menu, accept changes to set points, enter standby mode, and turn the power off.

Error condition exist when the ready light is not illuminated and when the * appears in the upper
right corner of the display. Press the MENU|POWER key and a description of the error is displayed in
the window. The display will cycle through all error conditions.

Pressing the MENU|POWER key once, when no error conditions exist, or twice times, if an error
condition exists, enters the menu screen.

Pressing the MENU|POWER key twice, when no error conditions exist, or three times, if an error
condition exists, enters the stand-by count down screen. Stand-by mode should be used when the
system is being shutdown. When the detector enters stand-by count down mode a timer is started.
After the time had expired the gas solenoid is closed, shutting off the flow of the nebulization gas, the
laser is turned off, and the heaters are disabled.

To turn the power off, press and hold the MENU|POWER key for 5 seconds. Wait at least 10
seconds before turning the instrument on, after it has been turned off.

Autozero Key
When the AUTOZERO key is depressed the ELS Detection signal will reset to about 20mV. An audible
beep is heard when the key is activated. When the detector is in the menu mode, the AUTOZERO
functions as an escape key, abolishing any changes made. The AUTOZERO key is also used to reset the
status alarm.

Display Screens
The ELSD uses one of 4 screens to aid in the operation of the detector.

Startup Screen

Program Loading
>>>>>>>>

The “>” moves from left to the right while the program is loaded. The process ends when “>” reaches
the far right.

After loading the program, the system begins running diagnostics. Pressing the MENU|POWER key
exits the start-up process without completing the diagnostics. If the MENU|POWER key is pressed
before the completion of the diagnostics, the ELSD enters a special diagnostic mode.
Running Diagnostics
Checking Laser Power

11
When the ELSD finishes the start-up process it enters the stand-by mode. Pressing the MENU|POWER
key to exit and enter the HOME Screen.

ELSD is in Standby Mode Push PWR to exit

Diagnostics Complete Laser Power OK

Home Screen

ELS Detection XX
20.000mV 20.0°C

Pushing ▲ or ▼ keys will circulate XX section to review operation condition. SC, DT, OC and ET
sections display their set points to the degree for 5 seconds when selected. Then they display the
actual temperatures to the tenth of a degree.
Pushing MENU|POWER key will bring up the Menu screen. If the key is pushed within 5 seconds after
an arrow key was pushed, the selection at XX will be displayed. Otherwise, the timer page will
always be the first menu page displayed.
If there is a “*” at the upper right corner, pushing MENU|POWER key will bring up a screen to explain
what’s wrong.

XX = SC, DT, OC, ET, RST, BLN, GAS, FLT or BFT, CL, GX, FS

SC = Spray Chamber (setpoint: 10°C to 70°C; readout range: -10.0°C to 120.0°C)


DT = Drift Tube (setpoint: 22°C to 120°C; readout range: -10.0°C to120.0°C)
OC = Optical Cell (setpoint: 22°C to 70°C; readout range: -10.0°C to 120.0°C)
ET = Exhaust Tube (setpoint: 22°C to 70°C; readout range: -10.0°C to 120.0°C)
RST= Reset baseline to about 20mV.
BLN = Baseline reading (5000.000 – 0.000mV)
GAS = Gas (0.0 to130.0psi)
FLT or BFT = Baseline Filter (OFF, weight 1 to 10, FLT or BFT)
CL = Calibration (20% to 200%)
GX = Gain (Normal or EDR)
FS = Full Scale (5V or 10mV)

RST/BLN Screen

ELS Detection RST ELS Detection BLN


20.000mV Baseline 20.000mV 221.22

When RST is selected from the menu screen, it will display “RST Baseline” for 5 seconds. Pushing
MENU|POWER key during this period will reset the ELS Detection signal to about 20mV. [Using the
AUTOZERO key can also reset the baseline.] After 5 seconds, the display changes to BLN and displays
the voltage offset by the autozero function. This value is important to note for each set of operating
conditions. If the value is high, greater than 500mV, the mobile phase is not being evaporated

12
completely and the temperature set points should be modified. Other contaminates in the system can
also affect this reading.

Menu Screen

<<MENU>>
[Spray Chamber Page]

Pressing the MENU|POWER key once, when no error conditions exist, or twice times, if an error
condition exists, enters the menu screen.
Push ▲ or ▼ keys to select the menus.
Push MENU|POWER twice to return to the Home screen.

Available Menus
[Spray Chamber Page] Sets Spray Chamber temperature.
[Drift Tube Page] Sets Drift Tube, optical cell and exhaust tube temperatures.
[Control Page] Sets Run/Standby mode, on/off Laser, on/off Alarm.
[Timer] Sets duration of the shut down time.
[Filter Page] Sets the type and weight of filter for noise filtration
[Load Method Page] Loads one of nine methods.
[Save Method Page] Saves a method
[Calibration Page] Attenuates or amplifies the detector output
[Detector Gain Page] Changes Gain
[Full Scale Page] Changes Full Scale

Spray Chamber Page

SPRAY CHAMBER SET


10.0°C 10°C

The reading under SPRAY CHAMBER is the current temperature. The reading under SET is the
setpoint.
Pushing ▲ or ▼ keys to change a setpoint at 1°C increment.
Pushing MENU|POWER key to accept the change and go back to Home screen.
Pushing AUTOZERO key to abolish the change and go back to Home screen.

Drift Tube Page

DRIFT TUBE SET


40.0°C 40°C

The reading under DRIFT TUBE is the current temperature. The reading under SET is the setpoint.
The temperatures of the optical cell and the exhaust tube are controlled at the same temperature as
that of DRIFT TUBE but their maximum temperature is limited.
Pushing ▲ or ▼ keys to change a set point at 1°C increment.
Pushing MENU|POWER key to accept the change and go back to Home screen.

13
Pushing AUTOZERO key to abolish the change and goes back to Home screen.

Control Page

Power Control:
[Run]

[Run], [Standby], [Laser Off] or [Laser On], [Turn off Sound] or [Turn on Sound]

Use ▲ or ▼ keys to select an action.


Push MENU|POWER key to take an action and go back Home screen.
Push AUTOZERO key to keep the current state and go back Home screen.

If the display reads Laser Off or Laser On, pushing MENU|POWER key will turn the laser off or on. The
laser may take up to 30 minutes to stabilize when it has been turned off, and on again.

If the display reads Turn off Sound or Turn on Sound, pushing MENU|POWER key will turn the status
alarm off or on. The status alarm sounds when the detector status changes from not ready to ready or
from ready to not ready. The alarm is 10 short beeps repeated every 30 seconds. Pressing the
AUTOZERO key resets the alarm.

Timer Page

STANDBY COUNTDOWN DEPRESS PWR button 5


Set: 05min 05:00 sec to turn of ELSD

1 min to 60 min

Use ▲ or ▼ keys to extend or reduce countdown interval.


Push MENU|POWER key to save the modified countdown interval but cancel countdown and return to
home screen.
Push AUTOZERO key to cancel the countdown, keep the previous interval and go back Home screen.

The timer default value is 5 minutes and is the recommended time. The time can be increased up to
60 minutes or decreased down to 1min.

Filter Page

Filter Weight:
1

OFF, 1 to 10, FLT or BFT

Use ▲ or ▼ keys to select an action.


Push MENU|POWER key to take an action and go back Home screen.
Push AUTOZERO key to keep the current state and go back Home screen.

14
There are two filter types to choose from FLT and BFT. The filter type is selected at the top of the
menu after weight 10. Select FLT or BFT and push the MENU|POWER KEY to enter. Then enter the
filter menu again and selected the appropriate filter weight. Filter weight is the level of baseline
noise filtration. OFF indicates no filtration. 10 is maximum filtration. In most cases, select BFT for
baseline filtering. The FLT setting applies a RC filter to the entire signal. For high-speed
chromatography, less than a 5 sec peak width, select BFT and turn the weight OFF. If the peak
widths are 5 to 30 seconds use the BFT filter with a weight of 1 to 10. For peak widths greater than
30 seconds, select the FLT setting with a weight of 1 to 10. When the baseline filter is on, a dramatic
operation condition change (e.g. turning on/off the HPLC pump), may upset the filter and cause
baseline drifting. The baseline will stabilize again in a few minutes.

Load Method Page

LOAD METHOD:

0 1 2 3 4 5 6 7 8 9

Method 0 is the current setup of the unit. It will be loaded upon power up. Use the ▲ or ▼ keys to
select a method number, pushing MENU|POWER key will apply the method and update the Method 0.
If the number selected has no method saved with, “Method not available” will be displayed. If the
non-volatile memory IC chip is damaged, the same message will be displayed.

Save Method Page

SAVE METHOD:
0 1 2 3 4 5 6 7 8 9

Up to 9 methods can be saved. Use the ▲ or ▼ keys to select a method number and the MENU|POWER
key to save the current conditions to the selected method number. A method includes Spray Chamber
Temperature Setpoint, Drift Tube Temperature Setpoint, Filter Weight, Calibration Factor, and
Detector Gain.

Calibration Page

Calibration:
100%

20% to 200% in 1% increments

Use ▲ or ▼ keys to select an action.


Push MENU|POWER key to take an action and go back Home screen.
Push AUTOZERO key to keep the current state and go back Home screen.

This feature scales the detector output. This feature is useful to match individual detectors to each
other for standardization within a lab, or set the full scale output to a value other than 5V or 10mV. At
100%, the signal is neither amplified nor attenuated.

15
Detector Gain Page

AMPLIFIER GAIN:
Normal

Normal, EDR

Use ▲ or ▼ keys to select an action.


Push MENU|POWER key to take an action and go back Home screen.
Push AUTOZERO key to keep the current state and go back Home screen.

There are two gain settings: Norm and EDR. Use Normal setting for all analytical scale analysis.
Analyte quantities from 10ng to 10,000ng can be quantified on Normal. “EDR” or Extended
Dynamic Range provides a greater dynamic range than the Normal setting. Analyte quantities from
20ng to 200,000ng can be quantified in this gain level.

Full Scale Page

FULL SCALE:
10mV

Another selection is 5V. Use whichever setting is appropriate for your data collection system. Using
the Calibration parameter can also modify the full scale. See Calibration page section for details.

Error Condition Screen


If any of the detector parameters are not met, the Ready status indicator will not illuminate and the *
will appear in the upper right corner of the home screen. Press the MENU|POWER key for more
information about the affected parameter.

Standby Countdown Screen

STANDBY COUNTDOWN DEPRESS PWR button 5


Set: 05min 05:00 sec to turn of ELSD

Pressing the MENU|POWER key twice, when no error conditions exist, or three times, if an error
condition exists, enters the standby countdown screen. Press MENU|POWER and hold for 5 seconds if
you wish to turn off the detector immediately. It is recommended that the standby mode be activated
when shutting down the detector. The timer allows enough time for the vapor to be expelled from the
detector before the gas is turned off eliminating the possibility of condensation in the optics cell. After
the time had expired the gas solenoid is closed, shutting off the flow of the nebulization gas, the laser
is turned off, and the heaters are disabled. If there are no leaks between the gas source and the
detector, the user will not need to return to the system after the standby sequence has started. The
system runs the diagnostic tests, then enters standby mode. Press MENU|POWER to exit standby and
begin running the detector.

16
Operating Conditions
Start Up Procedure
If this is the first time you have operated the detector, please refer to the Quick Start Guide. It is
very important that you reproduce the QC tests found in the Quick Start Guide before beginning your
analysis.

1. Make all connections; gas, liquid, power, communications, exhaust, and drain as described
in Chapter 2.

2. Turn on the power to the ELSD. Allow the system to run through the start-up sequence
and then push the MENU|POWER key to exit standby and enter the Home screen.

3. Allow the Drift Tube and Spray Chamber temperatures to reach thermal equilibrium as
indicated by the blinking of the corresponding status lights.

4. While waiting for the temperatures to reach the setpoints, start the HPLC Pump to deliver
the mobile phase to the detector. Don’t turn on the gas yet. Monitor the Thermo-Split drain
on the front of the unit. It may take up to 10 minutes (flowrate=1.0ml/min) to see liquid
coming out of the drain tube. Stop the pump

5. When temperatures reach setpoints, turn on the regulated gas flow and gradually increase
the gas pressure to 65psi ± 5 psi. If you use an on-off valve to turn on the gas, make sure
the upstream gas pressure is below 70psi before you turn on the valve. Gas pressure higher
than 70psi may permanently damage the detector. Re-start the pump.

6. A “*” may be blinking at the upper right corner indicating the detector is not ready yet.
You can depress MENU|POWER key to check what is not ready.

7. When the detector is ready, begin data collection system and monitor the baseline.

8. Press the AUTOZERO key to rest the baseline to approx. 20mV. Repeated autozeros may be
necessary until the baseline stabilizes.

9. When the baseline is stable (variation is less than 1.0mV when FS is set as 5V) and the “*”
has disappeared the Ready status light will be illuminated.

10. Inject your standard or sample and begin analysis.

Shut Down Procedure


1. Depress the MENU|POWER key to enter the standby countdown screen. Stop the flow of
mobile phase to the system.

2. Allow the detector to count down with the 5-minute timer.

3. If there are no leaks between your gas source and the ELSD, you do not have to turn the
gas off at the source.

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Choosing Operating Conditions
The drift tube temperature and the Thermo-Split spray chamber temperature are selected to provide
the maximum detector response with minimum baseline noise. The temperatures are selected based
on the solvent volatility and mobile phase flowrate. Some experimentation will be required to
optimize the Model 300S ELSD.

When setting the ELSD temperatures for a new method, select 25°C for spray chamber temperature
and 55°C for drift tube temperature. These temperatures should then be adjusted for the best signal to
noise ratio during method optimization. For the best performance, a mobile phase that is highly
organic and volatile requires an ambient or elevated spray chamber temperature and moderately high
drift tube temperature. When highly aqueous or high boiling point organic mobile phases with the
detector, the best performance will at sub-ambient spray chamber temperatures and moderate drift
tube temperatures.

Thermo-Split Spray Chamber Temperature


The Thermo-Split Spray Chamber can operate from 10°C to 70°C. The Spray Chamber temperature
controls the vapor phase split ratio. For an easily evaporated mobile phase, the split ratio can be set
low. To achieve this, the Thermo-Split chamber is heated. As the aerosol traverses the chamber, it
partially evaporates, shifting the particle size distribution low enough for essentially all the particles
to negotiate the bend. So, when highly organic mobile phases are used, the Thermo-Split chamber is
used at ambient or elevated temperatures. Under these conditions a majority of the aerosol particles
pass through the chamber and are carried into the evaporative zone.

For difficult to evaporate mobile phases, or high flow rates the split ratio needs be high so the
Thermo-Split chamber is cooled. When the aerosol exiting the nebulizer encounters a cooled
environment, it partially condenses into larger particles whose momentum carries them into the wall
and down the drain. By making the walls suitably cold, 99+% of an aqueous stream can be diverted
away from the evaporative zone.

As an example, the following data was collected with 90% water and 10% methanol at 1ml/min, a
more difficult to evaporate mobile phase. The recommended conditions for this mobile phase are
15°C Spray Chamber and 45°C Drift Tube. Figure 3.1 shows the effect of Spray Chamber
temperature on the resulting peaks when the drift tube temperature is held constant.

Figure 3.1: Spray Chamber Temperature Effects – Sub-ambient

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As the Spray Chamber temperature increases from 0° to 15°C, more of the vapor phase goes to Drift
Tube and not to the drain and the signal becomes larger. When the Spray Chamber is heated from
15°C to 25°C the signal decreases because the vapor is partially evaporated in the spray chamber.
When the SC temperature is higher than 30°C, more of the vapor is sent to the Drift Tube. A Drift
Tube temperature of 45°C is not sufficient to evaporate the larger volume of vapor and results in more
baseline noise.

When the mobile phase is changed to 90% Methanol and 10% water at 1 mL/min the recommended
conditions are Spray Chamber 50°C and Drift Tube 70°C. In Figure 3.2, the drift tube was held
content at 70°C and the spray chamber was lowered. The signal height decreased as the spray
chamber temperature decreased because more of the vapor was diverted from the Drift Tube and sent
to the drain.

Figure 3.2: Spray Chamber Temperature Effects – Elevated

Drift Tube Temperature


The drift tube temperature can be set from ambient to 120°C. The drift tube temperature is set at a
temperature high enough to evaporate the mobile phase and not vaporize the analyte. A higher drift
tube temperature may give result in a quieter baseline but smaller peak. The drift tube temperature
should always be higher than the spray chamber temperature but only as high as needed to achieve a
quite baseline.
In this example the mobile phase was 90% water and 10% methanol at 1ml/min and the spray
chamber was held constant at 10°C. Figure 3.3 shows the effect of drift tube temperature on the
signal.

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Figure 3.3: Drift Tube Temperature Effects

The effect of temperature on signal between 45°C and 50°C is small, but as the drift tube temperature
increased above 60°C the signal height decreased.

A drift tube temperature setting that is too high could vaporize the analyte and cause a loss of
sensitivity. If the analyte is thermally labile, use a lower temperature to improve sensitivity.
However, there will be a point where the temperature is not high enough to evaporate the mobile
phase and the increase in noise will negate the increase in signal. Optimize for the best signal to noise
ratio.

Mobile Phase Flowrate


Mobile phase flowrate will also affect the optimum temperature set point. The higher the flowrate of
an aqueous mobile phase, the lower the spray chamber temperature will need to be. High flowrates of
volatile mobile phases may require a higher drift tube temperature. The Model 300S ELSD may
perform best at sub-ambient spray chamber temperatures if the flowrate is extremely high, even for
volatile mobile phases.

Gradient Separations
For gradient separations, select the system temperatures required for the least volatile segment of the
gradient program.

Suggested Operating Temperatures


Solvent @ 1.0mL/min Drift Tube Temperature, °C Spray Chamber Temperature, °C
90/10 Water/METHANOL 45 15
90/10 Methanol/WATER 65 50
50/50 Methanol/Water 60 30
Acetonitrile 60 50
Methanol 60 50
Water 45 10

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Mobile Phase Considerations

Selecting a solvent
High purity mobile phase solvents with low boiling points are recommended for use with the ELSD.
Solvents should be spectral or HPLC grade. Dirty or contaminated solvents will cause baseline noise
and drift, blocked fluid paths, and a build up in the detector. All solvents used should have less than
1ppm of residue after evaporation and filtered to less than 0.45µm. Solvents can be evaluated by
pumping them directly into the detector, and comparing the noise to other known solvents. We have
found that not all HPLC grade solvents are acceptable for use with an ELSD. Preservatives commonly
used in Tetrahydrofuran (THF), will increase the noise level. If unstabilized THF is used, ensure that
it is fresh. THF can contain peroxides that can increase noise and are potentially explosive if taken to
dryness.

Mobile Phase Flowrate and Composition


The recommended flowrate for the ELSD is 0.25mL/min to 3mL/min. The mobile phase flowrate will
affect baseline noise. In general, more baseline noise will be generated by higher flowrate of a mobile
phase.

The ELSD will operate with common HPLC solvents that are volatile enough to form a vapor under
the operating conditions. This includes common HPLC solvents such as water, methanol, acetonitrile,
acetone, isopropyl alcohol, and THF. Normal phase solvents such as dichloromethane and hexane
may also be used. Note that solvents with higher boiling points will generally result in more baseline
noise. These should be used in limited percentages or at a lower flowrates.

Buffer Compatibility
The ELSD is not compatible with mobile phase modifiers that are not volatile, such as salts. Some
modifiers are volatile and can be used. These include but are not limited to acetic acid, trifluoroacetic
aid (TFA), formic acid, triethylamine, and ammonia. The concentration of buffer in the mobile phase
should be as low as possible.

Column Pre-Treatment
Chromatographic columns may introduce particles into the mobile phase, which may lead to increased
noise and blocked fluid paths. It is recommended that the chromatographic column be flushed with at
least 10 column volumes before it is connected to the ELSD.

QC Test Conditions
Please refer to the QC report shipped with your ELSD for the exact conditions used to test your
ELSD. The general conditions are:

1.0 ml/min of 50/50 Water/Methanol


Spray Chamber 30°C
Drift Tube 60°C
Filter 5
Injected Standard: 1000ng Sodium Benzoate in water

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4
Chapter

Maintenance & Troubleshooting


Routine Maintenance
The ELSD does not require regular user maintenance. There are no user serviceable components
inside the ELSD. Opening the case will void your warranty. Please call SofTA Corporation before
attempting any service.

The ELSD should be cleaned and calibrated once a year by a SofTA qualified technician.

Troubleshooting
Please check the SofTA Corporation website, www.softacorporation.com, for troubleshooting
assistance and helpful advice for the operation of your ELSD. Or you may contact us for assistance.

22
5
Chapter

Appendix
Accessories
Part No.
Recorder Cable 100/300-001
Fuses, 3AG 6A, or 3A 100/300-002
Operating Manual 100-003
Power cord 100/300-005

Specification
Dimensions 9.8” W x 18” D x 11.5” H
Weight 25 lbs
Display 2 Line x 20 Character per line VFD
User Interface Four multi-function keys
Evaporative Zone Temperature Ambient to 120°C
Thermo-Split™ Chamber
10°C to 70°C
Temperature
Liquid Flow Rate 0.2mL/min to 5mL/min
Gas Requirements 65psi ± 5 psi Nitrogen or other inert gas
Gas Consumption ~ 2.5 SLPM
Intended for indoor use only, 60°F to 85°F and <90% R.H.
Operating Conditions
non condensing
Nominal 120 VAC, 50/60 Hz or Nominal 240 VAC, 50/60
Electrical Requirements
Hz; 600 watts
Wetted Materials Stainless steel, glass, anodized aluminum, Teflon™
Light Source 670 nm Laser Diode, <5mW
Detector Hermetically sealed photo-diode/operational amplifier
Output Signal 0 - 5 VDC
Interface RS232, Contact Closure

23
Warranty
SofTA Inc. warrants its products against defects in workmanship or material under normal use or
service for one year. All obligations or liabilities under this warranty are limited to repair or
replacement, at SofTA Inc.’s option, F.O.B. Thornton, CO, of parts that are returned, freight prepaid
and which are accepted as being defective upon inspection of SofTA Inc..

Components that are subject to normal wear and/or are scheduled for routine replacement within the
warranty period, and/or parts that are subjected to effects of corrosion or deterioration by chemical or
other action are excluded from the above warranty. Repair or replacement will not be made under
warranty for malfunction because of inadequate facilities, operating conditions or utilities.

Equipment and components must be returned with SofTA Inc.’s prior approval and contain a SofTA
Inc. Return Authorization Number. Call SofTA Inc. (303-465-1106).

Guarantees/Warranties on accessories and equipment included by SofTA Inc. from other


manufacturers are limited to the guarantees given on such equipment by the respective manufacturers.

Any modifications made to equipment covered by this warranty, without written permission from
SofTA Inc. will void the warranty. SofTA Inc. reserves the right not to honor this warranty if the
products are obviously mishandled by the user.

SofTA Inc. assumes no responsibility for consequential, economic, incidental damages of any nature,
or on-site re-installation costs arising out of future alleged failure of any of its products or their
accessories.

This warranty supersedes any and all previous warranties unless otherwise agreed upon at the time of
sale, such as for customized equipment.

Shipments
All shipments are made F.O.B. Broomfield, CO. Instruments and major components will be packed
and shipped via surface, unless otherwise requested. Supplies and/or replacement parts are packed
and shipped via UPS ground, UPS Blue, air parcel post, or parcel post, unless otherwise requested.

Damaged Shipments
The Interstate Commerce Commission has held that carriers are as responsible for concealed damage
as for visible damage in transit. Unpack shipment promptly after receipt, as there may be concealed
damage even though no evidence of it is apparent. When concealed damage is discovered, cease
further unpacking of the unit involved and request immediate inspection by the local agent or carrier
and secure a written report of the findings to support a claim. This request must be made within 15
days of receipt. Otherwise, the carrier will not honor the claim. Do not return damaged goods to the
factory without first securing an inspection report and contacting SofTA Inc. for a return authorization
number.

24
Filing of Claims
After a damage inspection report has been secured, SofTA Inc. will cooperate in supplying
replacements and handling a claim that may be initiated by either party.

Returns
No returns may be made without prior notification and authorization. If for any reason, it is necessary
to return material to us, please contact our customer service department for a return authorization
number and forwarding instructions.

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