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 Page 1 of 17 ------- 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 Page 2 of 17 ------- 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 Page 3 of 17 ------- 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. Page 4 of 17 ------- 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 Page 5 of 17 ------- 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 Page 6 of 17 ------- 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 Page 7 of 17 ------- 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 Page 8 of 17 ------- 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 Page 9 of 17 ------- 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 Page 10 of 17 ------- 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 Page 11 of 17 ------- 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. Page 12 of 17 ------- 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. Page 13 of 17 ------- School Air Toxics, Carbonyl Compounds SOP Rev. No. 6 June 12, 2009 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. Page 14 of 17 ------- 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 Page 15 of 17 ------- School Air Toxics, Carbonyl Compounds SOP Rev. No. 6 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. Page 16 of 17 ------- 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 Page 17 of 17 ------- |