School Air Toxics, Diisocyanates SOP
September 8, 2009
STANDARD OPERATING PROCEDURE
FOR
MEASUREMENT OF DIISOCYANATES
USING THE BUCK ELITE-5
SAMPLING PUMP
U.S. Environmental Protection Agency
Region 4, Science and Ecosystem Support Division
Athens, Georgia, 30605
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School Air Toxics, Diisocyanates SOP
September 8, 2009
Acknowledgement
This Standard Operating Procedure (SOP) was developed by EPA Region 4,
Science and Ecosystem Support Division. This SOP is based on the
Commonwealth of Kentucky's ambient monitoring SOP template. Special thanks
to ERG for operational content and illustrations.
For questions or comments please contact:
Greg Noah, EPA, Region 4, SESD at noah.area@epa.gov or 706-355-8635
Mike Jones, EPA-OAQPS-AQAD at iones.mike@epa.gov or 919-541 -0528
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School Air Toxics, Diisocyanates SOP
September 8, 2009
Table of Contents
I. Introduction 4
II. Installation 5
A. Sampler Siting 5
B. Sampler Installation 5
III. Operating Procedure 8
A. Equipment and Supplies 8
B. Initial Receipt Activities 8
C. Installing the Piperazine Preloaded Filter Cassette 8
D. Configuring the Buck Elite Pumps 12
E. Setting the Flow Rate 14
F. Pump Calibration 14
G. Conducting the Sampling Event 15
Retrieving Piperazine Filter Cassettes 17
Field Data Recovery 18
Sample Shipping 18
IV. Data Forms 18
A. RTI Chain of Custody Form 19
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INTRODUCTION
School Air Toxics, Diisocyanates SOP
September 8, 2009
This procedure is designed to provide instruction on collecting ambient
diisocyanate compounds using the Buck Elite personal air sampling pump.
The procedure follows the tenets/specifications presented in the Occupational
Safety and Health Administration's (OSHA) OSHA No. 42.
Samples are collected by drawing a known volume of air through glass fiber
filters coated with 0.1 mg of 1 -(2-pyridyl) piperazine (1-2PP) which are
contained in open-face cassettes. Samples are extracted with 90/10 (v/v)
acetonitrile/dimethyl sulfoxide (ACN/DMSO) and analyzed by high
performance liquid chromatography (HPLC) using an ultraviolet or
fluorescence detector.
The Buck Elite is a battery-powered, data logging personal air sampler that is
capable of programmed start/stop and duration sampling. The Buck Elite has
a data logging feature that can store seven days of flow data in its internal
memory if data is logged every minute. Four sequential samples over a 24
hour period (detailed on page 17 of this SOP) will be collected for this study.
The Buck Elite was designed to operate from 0.8 standard liter per minute
(800 cc per minute) to 6.0 standard liters per minute. The flow rate accuracy
is guaranteed to + 5% of the calibration set point.
This SOP is designed to be a step by step method for operating the sampler
to be used in conjunction with the manufacturer's operators manual.
Laboratory Analysis Methodology may be referenced by contacting the
Eastern Research Group (ERG) directly at 919-468-7800 or by email
Julie.Swift@erg.com. Maintenance and troubleshooting should be conducted
using the operator's manual.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
FIGURE 1. Buck Elite Sampling Pump
Photograph courtesy of A. P. Buck Iric,
II. INSTALLATION
A. Sampler Siting
Check the areas for safety. Ensure there will be enough room for the
operator to move freely while working, and ensure physical conditions of
the location will allow the operator to work safely.
The sampling system should be set in a location unobstructed from any
side. No tree limbs or other hanging obstructions should be above the
sampler. It is suggested that the horizontal distance from the sampler to
the closest vertical obstruction higher than the sampler be at least twice
the height of the vertical obstruction.
Locate the sampling system on a reasonably level structure with the
probe inlet positioned at a height between two (2) and fifteen (15) meters
above ground level.
B. Sampler Installation
The inlet of the probe must be at least 2 meters above ground level and
the probe inlet line length can be no more than 2 feet long. Also, the
sampling pump and collection media (i.e., 03 scrubber and DNPH
Cartridge) must be placed inside an enclosure/storage container to shield
it from weather. The inlet of the probe must be at least 2 meters above
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School Air Toxics, Diisocyanates SOP
September 8, 2009
ground level and the probe inlet line length can be no more than 2 feet
long.
ERG has supplied an enclosure to meet the above requirements and is
described below. The enclosure and collection components constitute a
complete diisocyanates sampling system with the exception of the four
sample pump and the system stand. The enclosure is a weather-tight
NEMA 4 rated non-metallic unit. Figure 2 presents a view of the outside
of the enclosure with four sample collection filter cassettes attached.
FIGURE 2. Diisocyanate Sampling System Enclosure
Photograph courtesy of Dave Dayton, ERG
The recommended approach to constructing a stand and field mounting
the enclosure is as follows:
1. Using the mounting tabs provided at each outside corner on the
back panel of the main enclosure chassis; attach the enclosure so
that the top of the chassis is between 1.5 and 2 meters above
ground level. If the enclosure is to be attached to wooden stand
material, 4 lag bolts and washers have been supplied for use. If the
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School Air Toxics, Diisocyanates SOP
September 8, 2009
stand material is not compatible for attaching with lag bolts,
hardware for attaching the enclosure will be the responsibility of the
monitoring agency.
2. The sample inlets will now be at the required height specification of
at least 2 meters above grade.
3. Each enclosure is outfitted with a hasp and a small padlock to
provide some security. To open the enclosure, ensure that the
hasp tongue is not over the hasp loop. Turn the screw fasteners
located at the top and bottom of the front of the enclosure door
counter-clockwise until they release. To close and seal the
enclosure, fasten the hasp and turn the screw fasteners clock-wise
until they set.
4. Everything required to conduct diisocyanates samples collection is
included inside the enclosure. Figure 3 presents a view of the
inside of the enclosure with one of the four EPA supplied pumps
installed.
FIGURE 3. Diisocyanate Sampling System Enclosure
5. Locate the self-adhering Velcro strips inside the enclosure. The
loop sides of the strips have been securely adhered to the rear
panel of the enclosure. Carefully remove the white plastic material
on the hook side of the Velcro strips to expose its associated
adhesive. Position a sampling pump in front of each Velcro strip
such that the strip runs down the center of the back side of the
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School Air Toxics, Diisocyanates SOP
September 8, 2009
pump vertically. Press the pump in against the exposed Velcro strip
adhesive to attach it to the back side of the pump. The attached
Velcro will help ensure that the pump remains upright during
sampling, but will still allow the pump to be easily removed from the
enclosure if required.
6. With the enclosure assembled and attached to the stand, level and
secure the stand at the site. Sandbags or lag bolts may also be
used to secure the sampler.
III. OPERATING PROCEDURE
A. Equipment and Supplies
Buck Elite pump (with back pressure substitute device)
Sampling system enclosure
Tripod or stand
Platinum grade silicone tubing (received from ERG)
Flow meter (calibrated by and received from ERG)
Piperazine preloaded filter cassette
Logbook
Powderfree gloves
ERG sample paperwork
Cooler with ice substitute
B. Initial Receipt Activities
1. Plug sampler into AC power and charge the internal battery for at
least 24 hours.
2. Check parts and components against the packing list.
3. After charging, ensure sampler will power up and that the main
screen is operational.
C. Installing the Piperazine Preloaded Filter Cassette
The steps presented below should be followed when loading the
piperazine preloaded filter cassette shown in Figure 4 in preparation for a
sampling episode.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
FIGURE 4. 1 -(2-pyridyl) Piperazine Preloaded Filter Cassette
m
1. Remove the protective cap from the collection head.
2. Pull down to completely extend each of the four lengths of platinum
grade silicon tubing (silicon tubing) with the syringe tips inserted.
3. Remove the plug from the outlet port of the filter cassette. The
outlet plug is blue in color, as shown in Figure 5.
Figure 5. Outlet port of filter cassette
Photograph courtesy of Dave Dayton, ERG
4, Insert the syringe tip into the outlet port of the filter cassette.
Ensure that it fits snugly to produce a leak-free connection as
shown in Figure 6.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
Figure 6. Filter cassette attached to silicon tubing with syringe tip inserted
Photograph courtesy of Dave Dayton, ERG
Press the filter cassette upward into the cassette holder, as shown
in Figure 7. Repeat steps 4 and 5 for each of the four collection
channels. (Caution: Press only hard enough to ensure that the
cassette is securely held. This does not take a large volume of
force. Do not press so hard that the cassette cannot be easily
removed by simply pulling downward.)
Figure 7, Filter cassette secured in cassette holder
Photograph courtesy of Dave Dayton, ERG
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School Air Toxics, Diisocyanates SOP
September 8, 2009
6. Although riot a requirement, it would be prudent to be able to look
down into each of the cassette holders from above to visually
inspect each of the four connections to ensure that they are
appropriate, as shown in Figure 8.
Figure 8. Visual inspection of tubing to cassette outlet port
Photograph courtesy of Dave Dayton, ERG
7. Arrange tubing as shown in Figure 9, to ensure that it will not
become crimped when the protective cover is reinstalled.
Figure 9. Tubing arranged to avoid crimping
Photograph courtesy of Dave Daytori, ERG
8. Reinstall protective cover.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
9. Remove the plug from the inlet port of the filter cassette. The inlet
plug is red in color, as shown in Figure 10.
Figure 10. Inlet port of filter cassette
Photograph courtesy of Dave Dayton, ERG
The system is now ready to measure initial flow rates. To accomplish
these measurements, the silicon tubing on the calibrated flow meter is
attached to the inlet port of each channel, each pump is actuated, and
each measurement is read directly from the scale presented on the flow
meter. After collection is completed, post collection flow rates must be
measured and the outlet port plug (blue) and inlet port plug (red) on each
cassette must be reinserted.
D. Configuring the Buck Elite Pumps
The Buck Elite pumps require a specific minimum volume of back
pressure to function properly. The filter cassettes used to collect
Diisocyanate samples are zero back pressure media. Accordingly, the
pumps must be configured using a back pressure substitute device as
supplied by Buck. The back pressure substitute device is a small orifice
assembly with a piece of connecting Tygon tubing (see Figure 11-A) that
is attached directly to the inlet of each Buck Elite pump (see Figure 11-B).
The length of platinum grade silicon tubing that runs to each filter channel
is then attached to the inlet of the back pressure substitute device. The
back pressure substitute device was provided with each Buck Elite pump
supplied by US EPA. It is contained in a plastic bag In the box that the
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School Air Toxics, Diisocyanates SOP
September 8, 2009
pump was received in and can be identified by the label "DP Adaptor"
and part number MK-30229. After attaching the back pressure substitute
device to each pump, proceed to setting the flow rate and calibrating the
pump per the steps below.
Figure 11-A. Back Pressure Substitute Device (DP Adaptor MK-30229)
Photograph courtesy of Dave Daytori, ERG
Figure 11-B. Installed Back Pressure Substitute Device
Silicon Tubing to each collection channel
Back Pressure Substitute Device
Pump Inlet
1
I
Photograph courtesy of Dave Daytori, ERG
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September 8, 2009
E. Setting the Flow Rate
1. Connect the flow meter to the filter cassette by inserting the syringe
tip connected to the flow meter into each inlet port.
2. Press the Menu key (Down arrow) to the Flow adjust menu.
3. Press and hold the SET key and use arrows to get desired flow (this
clears all previous data). The design flow rate for diisocyanate
sampling for the study is 900cc/min.
COLLECTION Target = 0.9 LPM (900 cc/min)
4. Releasing the SET key will store the flow rate.
5. Press the ON/OFF key to return to the Main Display.
6. Repeat for the remaining 3 channels.
F. Pump Calibration
To CALIBRATE pump flow:
1. To measure the flow rate connect the flow meter to the inlet port of
each channel.
2. Press the Main Display down arrow to the Calibration Mode.
3. Press the SET key and release, pump begins to flow at preset flow
rate from the steps above in C. Setting the Flow Rate.
4. Observe the flow on the flow meter. Read the center of the ball in
the flow meter at "eye level" for the best accuracy. It should match
within +/- 4% of the 900cc/min collection flow rate. Press and hold
the SET key and adjust the Up or Down arrow to change the Factor
for the pump speed to match the desired collection flow rate.
CALIBRATION Target = 0.9 LPM (900 cc/min)
5. Press ON/OFF to return to Main Display.
6. Record the data from the calibration in the field logbook.
7. Repeat for the remaining 3 channels.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
Conducting the Sampling Event
1. Record activities / maintenance in logbook.
2. Prepare sample paperwork. On the RTI Chain of Custody Record
complete the top four lines of information and list all four sample ID
numbers in the table. Record any pertinent observations on the
"Comments" line on the right side of the table.
3. Make sure the flow rate is set and pump calibrated according to
the instructions in Section D. Setting the Flow Rate and E. Pump
Calibration.
4. Put on a clean pair of powder-free gloves.
5. Inspect the piperazine filter cassette to verify that end caps are in
place and have not fallen off through shipping. If end caps are not
in place, use a new cassette.
NOTE: If running a field blank, follow steps 3 and 4 above, then
remove the end caps from the piperazine filter cassette, count to
ten, replace the end caps, and place it back into the antistatic bag.
Label the bag to designate the filter cassette as a field blank. Log
the filter ID as field blank in the comments section of the RTI Chain
of Custody Form.
6. Carefully install new piperazine filter cassettes on all 4 channels
according to Section C. Ensure all connections are secure. Install
the flow meter at the inlet port of the cassette.
7. Press the down arrow key under the "EXIT" command. The
"RUN/MENU" screen should now be displayed.
8. Turn the pump on using the up arrow key below the "RUN"
command.
9. Record the flow meter flow rate in the field logbook. Read the
center of the ball in the flow meter at "eye level" for the best
accuracy.
10. To turn pump off, press and hold the power button until the
countdown ceases.
11. Press the down arrow key under the "EXIT" command to return to
the "RUN/MENU" screen.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
12. Remove flow meter from the inlet probe.
13. Press the Menu key (Down arrow) to scroll down to reset mode. If
previous sampling data needs to be erased then press and hold
SET key and press Up arrow. Press Yes to clear all data. If
previous sampling data does not need to be erased then use
Down arrow to scroll down to Timing Routine menu.
14. Activate Timing Routine - press and hold SET key and press Up
arrow twice to get to Start/Stop screen.
15. To Set a Start Time press and hold SET key and push Down
arrow, the top line displays the current time in the pump clock.
Bottom line displays the start time for sampling. Set up a time of
midnight for the given sample date for the pump to turn on
unattended and start sampling.
16. Press and hold SET key to activate time change sequence and
use Up or Down arrows to make changes for the parameter that is
flashing. To advance to next parameter and make changes press
and hold SET key to advance and use Up and Down arrows to
make changes. To back up, press the ON key.
17. After Start time is set, press Down arrow to scroll to 5min/hr Cycle
where pump can be setup up for 5 min ON and 5 min OFF cycle
within one hour block. By default all 5 minute segments are set to
Y=ON. To change to N=OFF Press and Hold SET key and press
UP or DOWN arrow. To advance to next segment Press and Hold
SET key and use UP and DOWN arrow to make changes. If no
changes are required press only the DOWN arrow to scroll to
STOP Time set up screen. Enter the desired time for pump to stop
sampling and shut down. If no Stop time is set pump will run until
battery gets low.
NOTE: Four sequential samples must be programmed! Each
sampler will have a different start and stop time as follows:
Pumpl: 00:01 to 05:01
Pump 2: 06:01 to 11:01
Pump 3: 12:01 to 17:01
Pump 4: 18:01 to 23:01
Sample time programming is critical! ALL SAMPLES MUST
SUCCESSFULLY RUN FOR A COMPLETE SAMPLING EVENT.
18. Press only the Down arrow to scroll through all menus to activate
other parameters like key lock, Log sample rate, Log Download or
Clear, set time clock and back to the main screen where user can
start sampling.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
19. Press RUN key to start sampling. Pump will display Delayed Start
Time, then it will shut down within 30 seconds and go into hold
mode.
NOTE: If pump is turned on while it is in hold mode, user input will
be required either to Cancel or Resume delayed Start Sampling. If
clock time goes past programmed Start time, then pump will not
turn on at programmed time. Delayed Start time run needs to be
manually cancelled and start time needs to be setup again.
Retrieving Piperazine Filter Cassettes
NOTE: Gloves must be changed for each sample, i.e. between
retrieving a sample and preparing a new run, gloves MUST be
changed to prevent cross contamination.
1. Add flow meter to sample inlet.
2. Press the power button to activate the pump's display.
3. Press the down arrow key to exit the data screen.
4. Press the up arrow key (should be the button under the "RUN"
command) to turn on the pump.
5. Record the flow meter flow rate in the field logbook. Read the
center of the ball in the flow meter at "eye level" for the best
accuracy.
6. Calculate an average flow from the pre and post flow checks.
Record the result in the field logbook. Multiply the average flow rate
by the sample time to determine a total volume. Record the date
sampled, time sampled, and total volume on the RTI Chain of
Custody form. Check the "Air" box, provide a sample description,
indicate one container, and designate "Diisocyanate" for the
analytical parameter on the RTI Chain of Custody form.
7. Remove the filter cassette and immediately cap at each end.
Place the capped cassette in a polypropylene bag. The bag must
be placed in a cooler cooled to sub-ambient temperature (~4 °C)
with ice substitutes and return to RTI for analysis.
8. Repeat for all sampling channels.
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Field Data Recovery
School Air Toxics, Diisocyanates SOP
September 8, 2009
1. On the RTI Chain of Custody Form ensure all aforementioned
blanks are filled for ALL channels, and the first line of "Relinquished
By:" is filled out by the sampler.
2. Data may be downloaded to a laptop using the Buck PC link cable.
RTI does not require this data, but direction can be found on pages
15 and 16 in the Buck Elite Instruction Manual document.
NOTE: The data logging feature must be enabled prior to the
sampling event.
Sample Shipping
The samples should be a in a polypropylene bag along with the
paperwork and packed in a small box/cooler. The samples are required
to be shipped cold and at 4 °C. Use the pre-filled out FedEx label
provided by RTI, and fill out the "Sender" section with the sampling
agency's address and phone number. Send priority overnight to RTI.
If the shipping form is lost, use the address below for shipping to
RTI, and contact them directly for the FedEx accounting.
Address: RTI Laboratories, Inc.
31628 Glendale Street
Livonia, Ml 48150-1827
(734) 422-8000
DATA FORMS
All sample related run data forms will be supplied by ERG/RTI. Check the data
sheets for completion after every setup or retrieval event. The operator is
expected to keep a logbook to document all site activities, quality assurance
activities, and sampling activities. The RTI Chain of Custody Form is attached
below.
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School Air Toxics, Diisocyanates SOP
September 8, 2009
RTI Chain of Custody Form
CD
RTI LABORATORIES, INC.
CHAIN OF CUSTODY RECORD
j PAGE: j i
A2LA Ceit *1570.01.'02 NELAC Cert ACD0973 M3E Ceit A!R-B150-2-42
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