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Ascarite II Performance As a Carbon Dioxide Scrubber: Use with the Fumiscope Fumigant Monitoring Instrument

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Ascarite II Performance As a Carbon Dioxide Scrubber: Use with the Fumiscope Fumigant Monitoring Instrument Ascarite II Performance as a Carbon Dioxide Scrubber: Use with the Fumiscope Fumigant Monitoring Instrument. April 20-30, 2009 Project Principal Co-investigators: Alan V. Barak, Ph. D. Lisa K. Mosser, B. Sc. Entomologist/Commodity Treatment Sr. Analytical Chemist USDA, CPHST, Otis Laboratory USDA, APHIS, CPHST, NRMAL 1398 West Truck Road 3505 25th Ave. Buzzards Bay, MA 02542 Gulfport, MS 35901 Ph. 508.563.9303 Ph. 228-822-3111 [email protected] [email protected] Woodward Bailey, Ph. D. Treatment Program Manager USDA, APHIS, CPHST, TQAU 1730 Varsity Drive, Suite 400 Raleigh, NC 27606-5202 Ph. 919-855-7502 [email protected] Background During the course of Methyl Bromide (MeBr) fumigation, certain commodities (green wood, produce) evolve varying and significant amounts of Carbon dioxide (CO2). This CO2 registers as MeBr on fumigant monitors that use non-discriminatory thermal conductivity technology. The product Ascarite II (Sodium hydroxide based) can remove CO2 from the sample stream. However, its longevity and performance in conjunction with the Fumiscope and at several CO2 concentrations has not been verified or well- documented. Page 1 of 24 Brief Project Outline The initial objectives were to 1.) Document and quantify possible blow-by of CO2 through Ascarite. By that, we mean the amount of CO2 that may pass the Ascarite tube without being scrubbed. 2.) Determine how long and how efficiently tubes of Ascarite II will perform to our specifications when CO2 of concentrations from 0.5 up to 5% are present under conditions of use during typical fumigation monitoring. These experiments were conducted at the USDA, APHIS, CPHST, NRMAL facility in Gulfport, MS. Project supported under Project 94181-C9Q51. Initial Calibration Tests. The Qubit S-157 CO2 Analyzer (the Qubit) was calibrated at 0-2000 ppm CO2 as follows. Clean cylinder air was passed through a Drierite tube (#26930, 10-20 mesh), then through a polycarbonate Ascarite II tube (made from an empty Drierite 26930 tube) to clean all CO2. Using factory calibration, this produced a reading of 0 ppm CO2 on the Qubit. The flow was adjusted to an index of 75 on the Gilmont indexed flow gauge (the Gauge). Tables from Gilmont indicated that this would supply about 475 ml/min air flow. T he Qubit was then calibrated at 0 ppm CO2. Then, the Ascarite tube was removed and the Qubit was calibrated at 2000 ppm CO2 by preparing a 3-L gas bag with 2000 ppm CO2, and then allowing the gas to flow through the Qubit. Lastly, air flow was produced by connecting an Air Cadet vacuum pump in-line, after the Qubit. The equipment set-up for calibration is shown in Figure 1. below. Following this, a calibration check was performed by passing 2000 ppm CO2, applying the Ascarite tube after about 2.5 minutes, and then removing the Ascarite tube after about 6.5 minutes. The resultant evidence of accurate calibration is presented below in Figure 2. Page 2 of 24 Figure 1. Set-up of the Qubit CO2 for calibration, with (r-l) sample supply bag, Drierite tube, Ascarite (in Drierite tube), Gilmont gauge, Qubit S-157 CO2 analyzer, and Air Cadet vacuum source. 2500 Qubit Calibration 0-2000 PPM CO2 2000 2 1500 PPM CO2 1000 Qubit PPM COPPM Qubit 500 0 0 2 4 6 8 10 12 Elapsed Time in Minutes Figure 2. Verification of zero and 2000 ppm CO2 span of the Qubit analyzer. Page 3 of 24 Initial tests for blow-by of CO2. A Fumiscope tube was prepared with 10 g 20-30 mesh Ascarite. A supply of 5% CO2 in a 100-L gas bag was connected so as to pass through a Drierite tube, the Ascarite, the flow gauge, and then the Qubit. PPM CO2 was logged every 10 seconds, and the and air flow was recorded every 5 minutes or when a significant change was noted. The experiment was continued until CO2 was detected passing through the Ascarite. The result is shown below in Figure 3. 600 5% Blowby with Fumiscope Tube 100 90 500 PPM CO2 80 Flow Gauge 70 FlowIndex Gauge 400 60 300 50 40 200 PPM CO2 PPM 30 20 100 10 0 0 0 10 20 30 40 50 60 70 Elapsed Time in Minutes Figure 3. After connection of the Ascarite tube, CO2 remained at trace levels (ca. 10 ppm). After about 63.5 minutes, an attempt was made to bring air flow back to about 75 on the gauge. This was not successful. It was apparent that, although we were able to scrub CO2 from the sample stream, this was only done with a decrease in air flow caused by plugging of the Ascarite and therefore much greater vacuum needed to pull the sample through the tube. The condition of the Ascarite tube is shown in Figure 4. Page 4 of 24 Figure 4. Glass Ascarite tube after tube became plugged. With sufficient vacuum applied, we could continue to force the scrubbing of 5% CO2. Only a small proportion of the Ascarite tube was consumed, before complete stoppage required ending the test. An alternative Ascarite tube arrangement was tested. A piece of Tygon tube (10 mm OD, 6 mm ID) was fitted made to hold 10.0 g Ascarite. The flexible tube allowed us to manipulate the tube to break up plugging, thus allowing air flow and CO2 to run to completion, thus consuming the entire tube. It was our theory that as long as air flowed, the Ascarite would scrub CO2 without significant blow-by. The system was run continually, and each time air flow appeared to decrease, the tube was flexed, thus breaking up any stoppage and allowing the reaction front to move through the tube. The result is shown in Figure 5, below. As long as a small amount of Ascarite is available for the scrubbing reaction, the procedure is effective. However, this is not a practical procedure. But, it does clearly show blow-by is not an issue as long as air flow can be continued. This raises questions of pump performance, which will be discussed later. Page 5 of 24 100 5% Blowby - Flexible Tygon Tube 100 90 80 90 PPM CO2 LEFT 70 Flow Gauge RIGHT FlowIndex Gauge 60 80 2 50 40 70 PPM COPPM 30 20 60 10 0 50 0 10 20 30 40 50 60 70 80 90 100 110 120 Elapsed Time in Minutes Figure 5. Performance of 10 g Ascarite in a flexible 6 mm ID Tygon tube with a constant supply of 5% CO2. By breaking up flow stoppage due to the Ascarite/CO2 reaction front, we were able to continue to scrub CO2 until the tube was almost completely used up. Evidence of this is shown in Figure 6. The failure of an Ascarite tube to function over time with high CO2 is the result of plugging, not blow-by. Page 6 of 24 Tests with Variable CO2 Concentrations and 20-30 Mesh Ascarite II. The following tests were conducted using the Fumiscope, a standard glass Ascarite tube filled with 10 g of 20-30 mesh Ascarite II. Air movement was provided by the Fumiscope pump, and measured using the integral flow gauge. In addition, a precision digital manometer was placed in-line with a T connector to monitor the pressure drop (vacuum) created when the system needed to overcome tube plugging. Concentrations of 0.5, 1.0, 2.0, 3.0, 4.0, and 5.0 % CO2 were used. The experimental set- up is shown below in Figure 7. The order of flow was: gas bag, Drierite, Ascarite, T- offset manometer, Fumiscope. Fumiscope flow was adjusted back to 1.0 SCFH if sample flow dropped to less than 0.9 SCFH (ca. 472 ml/min). The Fumiscope was zeroed with cylinder air, and re-zeroed after the first minute, to compensate for any pressure effects on the zero point. The results of all tests are presented graphically, showing Fumiscope flow rate, g/m3, and vacuum in mm Hg. Tests were discontinued after Ascarite was used up, or g/m3 or pressure readings indicated plugging was complete. Figure 7. Experimental set-up of 100-L gas-bag CO2 supply, Fumiscope with digital manometer, Drierite tube, and glass Ascarite tube. Page 7 of 24 Figure 8. Tests with 0.5% CO2, 20-30 mesh Ascarite II. The tube was practically used up after 3.5 hours, and vacuum draw remained low, indicting good sample air flow. However, Fumiscope flow was adverse at about 175 minutes. 2.0 10 0.5% CO2 with Fumiscope 9 Fumiscope Flow LEFT 8 1.5 Hg mm Vacuum(-) As MeBr g/m3 LEFT 7 mm Hg Vacuum RIGHT 6 1.0 5 4 3 SCFHg/m3 / 0.5 2 1 0.0 0 0 25 50 75 100 125 150 175 200 225 Elapsed Time in Minutes Figure 9. Tests with 1.0% CO2 and 20-30 mesh Ascarite II. A vacuum increase coincided with increase in Fumiscope g/m3 as MeBr and after flow could no longer be kept at 1.0 SCFH due to pump overload. Failure estimated to be after about 95minutes. 4.5 90 1% CO2 & with Fumiscope 4.0 80 Fumiscope Flow LEFT 3.5 70 As MeBr g/m3 LEFT Vacuum (-) mm Hg mm Vacuum(-) 3.0 mm Hg Vacuum RIGHT 60 2.5 50 2.0 40 1.5 30 SCFHg/m3 / 1.0 20 0.5 10 0.0 0 0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 Elapsed Time in Minutes Page 8 of 24 Figure 10.
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