Supelco ATIS User manual

ATIS™ OPERATION MANUAL
Adsorbent Tube Injector System
T702019A
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Introduction
The Adsorbent Tube Injector System (ATIS) is a sample preparation device that provides a quick
and efficient way to transfer calibration standards or samples onto an adsorbent tube. The ATIS
employs the technique of flash vaporization to vaporize the sample in a continuous flow of inert
gas. The inert gas carries the sample to the tube. After enough time has elapsed, typically less
than 5 minutes, the tube is removed from the ATIS and analyzed using the appropriate technique
for that adsorbent tube.
The ATIS performs these tasks:
• Injects calibration standards onto adsorbent tubes to calibrate your analytical system.
• Injects surrogates and system monitoring compounds onto an adsorbent tube before or after
sampling.
• Removes moisture from the tube prior to analysis (dry purging).
• Vaporizes neat compounds into a gas-sampling bag to create a calibration standard.
The ATIS can be expanded:
• Thermally extract solid samples and collect the volatiles onto an adsorbent tube. The
temperature range is adjustable from ambient to 150°C. Extraction glassware is available
(ordered separately) that will accommodate solid samples up to 76mm (3”) length, and
13mm (1/2”) in diameter.
• Purge volatiles from an aqueous sample onto an adsorbent tube at ambient temperatures. A
purge & trap / humidifier module is available (ordered separately) that interfaces with the
ATIS. This module can also be used to generate a dynamic humidified stream of an inert
gas for spiking calibration standards. The purge & trap module includes purge and trap
glassware, and a separate flow controller that allows the user to set a separate purge (wet)
flow rate independently of the (dry) flow rate.
How the ATIS Works
The ATIS is comprised of the following major components:
• Injection Glassware
• Adsorbent Injector Heating Block
• Carrier Gas Flow Control
Injection Glassware
The sample pathway of the ATIS is constructed of glass and stainless steel. The calibration
standard is injected by a syringe through a replaceable septum in the center of the injection
glassware. The injection glassware has an internal volume of 10 milliliters. This provides
adequate volume for the vaporized liquid to expand.
Injector Heater Block
The injector heater block transfers heat produced by the block heater to the injection glassware.
The heated glassware vaporizes the sample. A thermometer port is located in the top of the
injector block to monitor the temperature during use.
Carrier Gas Flow Control
A supply of clean gas (nitrogen, helium, or air) is required to flow through the injection glassware
during sample introduction. The gas carries the calibration standards / sample to the adsorbent
tube during sample preparation.
The ATIS includes an adjustable flow controller and an on/off control valve. The flow controller
will maintain a constant flow of gas, regardless of changing downstream pressures i.e., an
adsorbent tube. The flow range is adjustable from 0 to 110mL/min. This flow controller provides
better accuracy and control of the flow rate than a rotameter or needle valve. The on/off valve
allows the gas supply to be turned off when the unit is not in use. A gas purifier is included that
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will remove trace levels of hydrocarbon contaminants from your gas stream. However, additional
purification may be required if your gas supply has high contamination levels.
Safety Information
The TALBOYS®Dry Block Heater included with this product is the heat source for the ATIS. This
product operates at temperatures high enough to cause serious burns to the skin. A heat shield
is provided to reduce the risk of getting burned while the ATIS is in use. The temperature of the
heat shield will be approximately half of the set block temperature.
Danger: Do not use the ATIS in the presence of flammable or combustible materials or explosive
gases. Fire or explosion may result, causing death or injury. This device contains electrical
components that may ignite such materials.
Danger: Do not connect the ATIS to any flammable gases i.e., hydrogen. This will create a fire
and/or explosion hazard.
Warning: The ATIS should be placed in a fume hood or have its own ventilation duct when in
use.
Warning: Be careful when working around the ATIS when the block heater temperature is turned
on.
Warning: Do not block the exit port of the pressure relief valve. Doing so could cause pressure
to build in the system that may cause the septum to blow out of the septum holder, or worse
case, cause the glassware to explode. The pressure relief valve will open to relieve the gas
pressure if it exceeds 6psig.
Warning: Before performing any maintenance, turn off the block heater, unplug the electrical
cord, and allow sufficient time to let the block heater to cool down.
In addition to reading this manual, please read the operating manual included with the TALBOYS
Dry Block Heater (follow the instructions for the Standard Dry Block Heater) before using the
ATIS.
Specifications
Dimensions
Requires a 61mm x 61mm (2’ x 2’) space to house the assembled unit.
Power Requirements for the TALBOYS Block Heater
Cat# 28520-U ATIS 120 VAC +/-10% 50/60 Hz, 110 Watts, 0.9 Amps
Cat# 28521-U ATIS 240 VAC +/-10% 50/60 Hz, 110 Watts, 0.5 Amps
Certifications for the TALBOYS Block Heaters
Safety Standards:
IEC 61010-1 Safety requirements for electrical equipment for measurement, control and
laboratory use. Part I: General Requirements.
IEC 61010-2-010 Part II: Particular requirements for laboratory equipment for the heating of
materials.
UL Std.No. 61010-1
EMC standards: EN6100-3-2 EN61000-3-3, EN61000-4-5 FCC-B, EN61000-4-4 EN55022-A,
EN61000-4-2, EN61000-4-3, EN61000-4-11, EN61000-4-6, EN45501
Associated EU guidelines:
EMC directive 89/336/EEC, LVD directive 73/23/EEC
Temperature Range with all the ATIS parts attached:
Slightly above ambient to 150°C (302°F)
Pneumatic Specifications:
Maximum operating pressure 60psig (Suggested operating pressure 25-30psig)
Gas Flow Range:
0-110 mL/min at 25-30 psig
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The ATIS Components
• Operation Manual
1. Block Heater
2. Injector Heater Block
3. Gas Purifier
4. Copper Tubing 1/8” OD
5. Flow Controller and On/Off Valve & Pressure Relief
6. Polypropylene Tubing 1/8” OD
7. 1/4” to 1/8” Reducing Union
8. Injection Glassware
9. 1/4” Union with Thumbwheel
10. Heat Shield
11. Thermometer
12. Luer/Hose-Barb Adapter
Spare Parts
SP1. 6mm Ferrules “Black”
SP2. 1/4” Ferrules “Orange”
SP3. Half-Hole Septa
SP4. Spare Relief Valve and 3/16” Ferrules
SP5. 1/4” PTFE Ferrules “White”
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Installation
Site Preparation
Place the ATIS in a fume hood and away from any combustibles. The ATIS requires a regulated
supply (25–30psig) of nitrogen, helium, or air. Nitrogen is your best choice because it’s dry,
clean, and relatively inexpensive. The ATIS also requires an electrical supply 120 VAC or 240
VAC (depending on the unit you purchased). The Block Heater must be plugged into a grounded
outlet. See the operation manual included with TALBOYS Dry Block Heater for additional
information.
Tools Required for Assembly (not included)
• Small tubing cutter
• Knife or scissors
• 7/16” open-end wrench
• 1/2” open-end wrench
• 9/16” open-end wrench
• Flow meter (to set the gas flow rate)
Assembling the ATIS
To assemble the ATIS requires you to cut the supplied tubing to fit your workspace and to attach
the tubing to the appropriate fittings. We have installed the appropriate ferrules in each of the
fittings for your convenience. The fittings that connect to the ATIS glassware include a VESPEL®
ferrule. Use caution when tightening the fittings to the glassware – very little force is needed to
create a seal to the glassware. PTFE ferrules are also included if you prefer to use them instead
of the “orange” VESPEL type ferrules.
For additional help in plumbing the ATIS see the pneumatic diagram in Appendix 1 of this
manual.
The picture to the right illustrates what the
ATIS should look like AFTER you have
assembled it.
Place the injector heater block (with the
open slot facing to your right) in the
opening of the dry block heater.
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Using a tubing cutter, cut a piece of
copper tubing to connect the gas
purifier to a regulated gas supply (user
supplied) of nitrogen, helium, or
compressed air. Pressure should be set
to 25 to 30psig after installation is
complete.
Using a wrench, tighten the nut 3/4 of a
turn, past fingertight.
Cut a second piece of copper tubing to
connect the outlet of the gas purifier to
the inlet of the on/off valve connected to
the flow controller.
Using a wrench, tighten both of these nuts
3/4 of a turn, past fingertight.
NOTE: Position the flow controller so you
have access to it during use.
Connect the 1/4” to 1/8” reducing union
to the injection glassware. The
SUPELCO Logo on the glassware should
face you.
Using a wrench, gently tighten the larger
nut 1/8 of a turn, past fingertight.
NOTE: Over-tightening will cause the
glassware to break.
Cut a piece of the white polypropylene
tubing to connect the outlet of the flow
controller to the union you attached to the
Injection Glassware.
Allow extra slack in the tubing so the tubing will absorb
the shock if the tubing is accidentally bumped. This helps
to prevent the glassware from breaking during use.
Using a wrench, tighten both of these nuts
3/4 of a turn, past fingertight.
Danger: Do not plumb the ATIS to an
y
flammable gases i.e., hydrogen. This wil
l
create a fire and/or explosion hazard.
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Slide the injection glassware into the
injector heater block until the stem of the
injection glassware protrudes through the
recess of the injector block.
Install the thumbwheel to the 1/4” union.
See the next section to choose the correct size
ferrule for the adsorbent tube you plan to use.
Install the 1/4” union over the stem of the
glassware that protrudes through the recess.
Using a wrench, tighten the CENTER hex
portion of the union 1/8 of a turn while holding
the injection glassware by the septum holder.
The recess secures the union so you can attach your adsorbent tube by using only the thumbwheel. The
recess also promotes heat to transfer to the union. This prevents the calibration standard/sample from
condensing inside the union.
Place the heat shield over the injector
heater block so the septum holder
protrudes through the hole of the heat
shield. The base of the heat shield will
rest on the gray cover of the dry block
heater.
Insert the thermometer through the hole
of the heat shield. Note: The thermometer
port is dual tapered and will accept both a
normal thermometer, or a smaller diameter
digital thermometer.
The ATIS is now completely assembled.
Your set-up should look like the picture to
the right.
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How to Attach your Adsorbent Tubes
The thumbwheel will accept tubes with either 6mm or 1/4” by placing the appropriate ferrule in the
thumbwheel. For odd size tubes use the Luer/Hose-Barb Adapter included. The pictures below
illustrate some examples.
NOTE: While using the ATIS, the temperature of the adsorbent tube will be close to the ambient
temperature of your lab. However if the adsorbent tube is attached to the thumbwheel for a long
period, the heat from the injector block will transfer to the attached adsorbent tube. The rate at
which this occurs is dependent on both the block heater temperature and whether the adsorbent
tube is made of glass or stainless steel. The transfer of heat will be greater with stainless steel
than glass tubes.
Installing Thermal Desorption Tubes
For 6mm OD tubes, install a 6mm ferrule
“black” in the thumbwheel.
For 1/4” OD tubes, install a 1/4” ferrule
“orange” in the thumbwheel.
Installing Solvent Desorption Tube
Use the Luer/Hose-Barb Adapter and a
piece of flexible tubing (not supplied) to
connect odd size adsorbent tubes. To
attach the Adapter, install a 1/4” ferrule
“orange” in the thumbwheel. The smooth
section of the adapter goes into the
thumbwheel.
Caution: Make sure the flexible tubing you
choose will withstand the temperatures
you plan on using. The wrong tubing
could melt or off-gas by-products if left
attached for a long period of time.
Installing Adsorbent Tubes with Male
Luer fittings
The inner diameter of the Luer/Hose Barb
Adapter will accept adsorbent tubes that
have a male luer fitting.
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Installing Gas-Sampling Bags
Gas-sampling bags can be attached using
the Luer/Hose-Barb Adapter and a piece
of flexible tubing. If the stem of the bag is
3/16” in diameter you can use 3/16”
ferrule (included SP4) in the thumbwheel
in place of the adapter.
Setting the ATIS Parameters
There are two parameters you need set; one is the flow rate, the other is the block temperature.
Setting the Flow Rate (Carrier Gas)
Insert the type of adsorbent tube you plan to use in the thumbwheel of the ATIS, and gently tighten
the thumbwheel. With the gas supply on, attach a flow meter to the opposite end of the adsorbent
tube. Turn the on/off valve attached to the flow controller to the ON position. (The arrow on the
knob should be pointing towards the flow controller when it is ON.) Adjust the gas flow rate using
the black knob of the flow controller.
• To increase the flow rate -- turn the knob counter-clockwise.
• To decrease the flow rate -- turn the knob clockwise.
The flow controller has a 13-turn adjustment knob; each complete turn of the knob is
approximately 8 to 10mL/min change in the flow rate. The flow range of the flow controller is 0 to
110mL/min at 25-30psig.
Caution: Do not over-tighten the flow controller knob in either direction, or you could damage the
flow controller.
Setting the Temperature
The power switch is located on the right side of the block heater. When the switch is in the center
position, the unit is OFF. Depressing the switch to the left engages the Low Heat range control.
Depressing the switch to the right engages the High Heat range control.
The temperature range of the block heater with all the ATIS components attached:
• Low Heat Range is slightly above ambient to approx. 100°C (212°F)High Heat Range is approx. 75°C
to 150°C (167°F to 302°F)
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Maintenance
Suggested maintenance for the ATIS includes the following:
• Check the temperature setting daily.
• Check the flow rate daily.
• Replace the septum after 25 injections.
• Replace the injection glassware after the first sign of any deposits.
• Replace the gas purifier annually.
Replacing the Pressure Relief Valve
In the event that you need to replace the pressure relief valve, a spare valve is included with the
ATIS.
To replace the valve:
1) Remove the nut that holds the relief valve.
Note: You may have to break the old relief valve to remove it from the nut.
2) Place a new 3/16” ferrule in the fitting.
3) Start the nut on the threads of the fitting.
4) Insert the relief valve through the nut and into the ferrule.
5) Gently push the relief valve so it is flush with nut.
6) Tighten the nut 1/8 to 1/4 of a turn. Do not over-tighten.
Guidelines for Using the ATIS
To accurately quantify the concentration of a sample acquired with an adsorbent tube, the
analytical system must first be calibrated. The ATIS simplifies this task. Below are a few starting
parameters, some experimentation may be needed to optimize the conditions for your application.
Allow enough time for the block heater to equilibrate to the desired temperature before injecting
your standards. You will also want to make sure you have gas flowing through your adsorbent
tube, prior to injecting your standard so the compounds will be carried to the tube.
Injecting Gas Phase Standards
Gas phase standards are available in compressed gas cylinders, made up in gas sampling bags,
or gas sampling bulbs.
• Set the block temperature between 60° to 75°C.
• Set the flow rate of the carrier gas to 50mL/min.
• Allow the adsorbent tube to remain attached for 2 to 5 minutes after injecting the gas mix with
the carrier gas on.
• The delivery rate of the gas syringe should be less than 10mL/min.
Large syringe volumes of gas standards can be injected through the septum of the injection
glassware, but the injection rate of the syringe plunger must be slow. The rate that you inject the
gas mix will have an affect on the total flow rate passing through the adsorbent tube. For
example: If you injected a 100mL syringe volume of a gas mix into the injection glassware, and it
takes you 10 seconds to inject the entire 100mL volume, the flow rate going through the adsorbent
tube for those 10 seconds is 600mL/min. That is too fast. There is a good chance that the
compounds in the gas mix could breakthrough the adsorbent and not be retained. In general, the
delivery rate of the syringe should be less than 10mL/min.
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