School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
STANDARD OPERATING PROCEDURE
FOR
MEASUREMENT OF CARBONYL COMPOUNDS
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, Carbonyl Compounds SOP
Rev. No. 6
June 12, 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.greg@epa.gov or 706-355-8635
Adam Eisele, EPA, Region 8, OPRA at eisele.adam(S)epa.gov or 303-312-6838
Mike Jones, EPA-OAQPS-AQAD at iones.michael@epa.gov or 919-541-0528
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
Table of Contents
I. Introduction 4
II. Installation 6
A. Sampler Siting 6
B. Sampler Installation 6
III. Operating Procedure 11
A. Equipment and Supplies 11
B. Initial Receipt Activities 11
C. Setting the Flow Rate 11
D. Pump Calibration 12
E. Conducting the Sampling Event 12
Site Arrival Daily Activities 12
Preparing Sampler for a Sampling Event 12
Retrieving DNPH Cartridges 14
Field Data Recovery 15
Sample Shipping 15
IV. Data Forms 16
A. ERG Carbonyl Compounds Sample Data 17
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
INTRODUCTION
This procedure is designed to provide instruction on collecting ambient
carbonyl compounds (aldehydes and ketones) using the Buck Elite-5 personal
air sampling pump. The procedure follows the tenets/specifications presented
in EPA's Compendium Method TO-11 A. Carbonyl compounds are adsorbed
and converted into stable hydrazones using dinitrophenylhydrazine (DNPH)
cartridges.
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 sampling data in its
internal memory if data is logged every minute. The sampling time should
always be 24 hours for the Toxics in Schools 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(S)erg.com. Maintenance and troubleshooting should be conducted
using the operator's manual.
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
FIGURE 1. Buck Elite-5 Sampling Pump
Photograph courtesy of A. P. Buck Inc.
INSTALLATION
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
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 sampler 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 sampler on a reasonably level structure with the probe inlet
positioned at a height between two (2) and fifteen (15) meters above the
ground.
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
ground level and the probe inlet line length can be no more than 2 feet
long. Also, the sampling pump must be placed inside an
enclosure/storage container to shield it from weather. To keep the
contents inside the container cool, the container should be opaque and
light in color.
To accomplish this, the sampling pump container must be attached to a
tripod or stand or placed on a table to meet this probe inlet height
requirement, while using an inlet probe no longer than 2 feet. A hole
should be cut in the bottom of the container to allow for pass through of
the sampling probe. Note the shape of the supplied sampling probe in
Figure 6 and where the best position will be for the inlet before drilling.
Try to keep the stainless steel tubing close to the side of the container to
secure it if necessary.
Attach the inlet probe to the bottom of the container by unscrewing and
removing the top nut where the inside sample line will attach and the top
nut on the bulkhead fitting. From the bottom of the container, insert the
top of the bulkhead fitting up into the container and replace the bulkhead
nut and sample line nut. Ensure the bulkhead nut is tight, but do not over
tighten. To provide stability to the probe, holes may be drilled into the
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
sides of the container and cable ties or equivalent may be used to secure
the probe to the outside of the container.
To attach the plastic container to the tripod, two holes may be cut in the
side of the plastic container, and cable ties or rope may be used to create
a loop through the container. Hang the loop that is through the container
over a structure (tension knob, clamp, etc...) on the tripod. Other
methods of hanging the sampling system and media enclosure may be
acceptable. Ensure the sampling system enclosure is secured to the
tripod.
The inlet probe attached to the bottom of the container is attached to the
inlet of the collection media and the outlet of the sampling media is
attached to the sampling pump using Platinum Grade silicone tubing.
The silicone tubing to facilitate these connections is be supplied by ERG.
With the protective enclosure attached, place and level the tripod at the
site. Sandbags may be used to secure the sampler.
Assemble the ozone scrubber and the DNPH cartridge, and connect
them to the sampling probe and pump according to Figure 5.
Note the both the 03 scrubber and DNPH cartridge have 2 different sized
ports for the inlet and the outlet. The smaller diameter port is the inlet
and the larger diameter port is the outlet. Slide the outlet port (larger
diameter opening)of the 03 scrubber over the inlet port (smaller opening)
of the DNPH cartridge. Press the together firmly to ensure a secure leak-
free connection. Slide the silicone tubing from the sampling pump over
the outlet of the DNPH tube. Slide the silicone tubing from the sampling
probe over the inlet of the 03 scrubber (see Figure 5).
If collocated samplers will be located at the site, the two samplers must
be within four (4) meters of each other, but outside of two (2) meters.
The inlet heights must be within one (1) meter vertically.
FIGURE 2. Carbonyl Sampling Assembly
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
Rain Shield
Probe Inlet
Air Flow
t
Ozone
Scrubber
2,4-DNPH
Cartridge
Buck Elite
Pump
FIGURE 3. Flow Check Assembly
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
Rotameter
I
Air Flow
o
t
Ozone
Scrubber
2,4-DNPH
Cartridge
Buck Elite Pump
FIGURE 4. Waters DNPH Filter Cartridge
Cartridge Inlet
FIGURE 5. Ozone scrubber and DNPH cartridge
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
(sample probe must be attached to the inlet of the ozone scrubber with the gold ring)
FIGURE 6. Carbonyl Inlet Probe
OPERATING PROCEDURE
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
A. Equipment and Supplies
Buck Elite pump
Enclosure (plastic storage container)
Tripod or stand
Platinum grade silicone tubing (received from ERG)
Rotameter (calibrated by and received from ERG)
Ozone scrubber (received from ERG)
Capped DNPH cartridge (received from ERG)
Logbook
Powderfree gloves
ERG sample paperwork
Cooler with ice substitute
Paper shipping sleeves for sampled cartridges
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. Setting the Flow Rate
1. Securely connect the rotameter to the collection media using the
silicone tubing provided with the rotameter as shown in Figure 3.
NOTE: The small diameter port on the Waters O3 scrubber and
DNPH cartridges are the inlets
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 carbonyl
sampling for the study is 800cc/min.
4. Releasing the SET key will store the flow rate.
5. Press the ON/OFF key to return to the Main Display.
D. Pump Calibration
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
To CALIBRATE pump flow:
1. To measure the flow rate have the ozone scrubber, DNPH
cartridge, and rotameter connected in the flow check assembly as
shown in Figure 3.
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 rotameter. Read the center of the ball in
the rotameter at "eye level" for the best accuracy. It should match
within +/- 4% of the 800cc/min design 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 flow rate. ERG has
previously checked the rotameter and notes that they are accurate
to approximately 20cc/min. This bias is acceptable.
CALIBRATE Target=0.8 Lpm (800 cc/min)
5. Press ON/OFF to return to Main Display
6. Record the data from the calibration in the field logbook.
E. Conducting the Sampling Event
Site Arrival Daily Activities
Record activities and/or maintenance activities in logbook
Preparing Sampler for a Sampling Event
1. Prepare sample paperwork. On the ERG Carbonyl Compounds
Data Sheet, complete the "Lab Pre-Samp." and "Field Setup"
sections. In the top part of the PAMS table, record the number
under "Cartridge Lot #" and "Sample ID". Record any pertinent
observations in the "Comments" section at the bottom of the form.
2. Make sure the flow rate is set and pump calibrated according to the
instructions in C. Setting the Flow Rate and D. Pump Calibration.
3. Put on a clean pair of powderfree gloves.
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
4. Inspect the ozone scrubber and DNPH cartridge to verify that end
caps are in place and have not fallen off through shipping. If end
caps were not in place, use a new cartridge.
5. Carefully assemble ozone scrubber and DNPH according to Figure
2, making sure all connections are secure. Install the rotameter
before the collection media as shown in Figure 3.
6. Turn the pump on and record the rotameter flow rate in the "Pre-
Sampling Rotameter Reading" field on the ERG Carbonyl
Compounds Data Sheet "Field Setup" section. Read the center of
the ball in the rotameter at "eye level" for the best accuracy. ERG
has previously calibrated the rotameter and will determine the
corrected flow from the rotameter's calibration curve upon receipt.
7. Turn pump off.
8. Remove Rotameter from the sample line and reconnect ozone
scrubber and DNPH cartridge according to Figure 2. Store
rotameter in clean Ziploc bag or equivalent.
9. 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.
10. By default Timing Routine is deactivated. To activate press and
hold SET key and press Up arrow twice to get to Start/Stop screen.
11. 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.
12. 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.
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School Air Toxics, Carbonyl Compounds SOP
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13. After Start time is set, press Down arrow to scroll to 5min/hr Cycle
where pump can be setup up for 5min 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.
14. 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.
15. Press RUN key to start sampling, Pump will display Delayed Start
Time. Then it will shut down within 30 sees 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 DNPH Cartridges
1. Put on a clean pair of powderfree gloves.
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.
2. Add rotameter to sampling line according to Figure 3.
3. Turn the pump on and record the rotameter flow rate in the "Post
Sampling Rotameter Reading" field on the ERG Carbonyl
Compounds Data Sheet "Field Recovery" section. Read the center of the
ball in the rotameter at "eye level" for the best accuracy. ERG has
previously calibrated the rotameter and will determine the corrected
flow from the rotameter's calibration curve upon receipt.
4. Turn pump off.
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
5. Remove the DNPH cartridge and immediately cap at each end.
6. Place the capped cartridge in the paper shipping sleeves, and write
the sample day and the site ID on the sleeve. Place the cartridges
in a polypropylene bag. The bag must be placed in a cooler cooled
to subambient temperature (~4 °C) with ice substitutes and return to
ERG for analysis.
Field Data Recovery
1. On the ERG Carbonyl Compounds Sample Data Sheet, fill in the
"Elapsed Time" field in the "Field Recovery" section. Be sure the
"Post Sampling Rotameter Reading" field on the ERG Carbonyl
Compounds Data Sheet "Field Recovery" section is completed.
Review the ERG Carbonyl Compounds Sample Data Sheet and
make sure all blanks are filled.
2. Data may be downloaded to a laptop using the Buck PC link cable.
ERG 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 ERG, and fill out the "Sender" section with the sampling
agency's address and phone number. Send priority overnight to ERG.
If the shipping form is lost, use the address below for shipping to
ERG, and contact them directly for the FedEx accounting.
Address: ERG
601 Keystone Park Drive
Suite 700
Morrisville, NC 27560
919-468-7924
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School Air Toxics, Carbonyl Compounds SOP
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June 12, 2009
IV. DATA FORMS
All sample related run data forms will be supplied by ERG. 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 ERG Carbonyl Compounds Sample
Data Sheet is attached below.
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School Air Toxics, Carbonyl Compounds SOP
Rev. No. 6
June 12, 2009
ERG Carbonyl Compounds Sample Data Sheet
fcERG
CARBONYL COMP
d.
-9 <§
3 <9
i
it
u. £
Field
Reeoveiy
Lab
Recovery
Site Code:
City/State:
AQS Code:
ERG Lab ID #
OUNDS DATA SHEET
Collection Date:
Cartridge Lot #:
Duplicate Event (Y'/N):
Set-Up Date: Operator: Sys. #:
Pre-Sampl.ng Rotarreter Reading (cc/min):
Recover/ Date:
Elapsed Timer Reset (Y/N):
Post Samp ing Rotameter Reading (ec/min):
Cartridges Capped (WN):
Rece-ved by: Date:
Status: Valid Void (Circle one;
If void, why:
San'p-e Vo-ume (total Liters):
Sample Duration
Elapsed Time:
Status: Valid
Refrigerator No:
Temperature:
(3 or 2* hr):
Void (Circle one)
(0
2
Sample Date
Sample
Time
Sample
Duration
Sample
Volume
Cartridge
Lot*
Sample ID
Lab ID
Wh1e: Sample raveler
Canary: Lab Copy
Pirk: Fielc Copy
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