Attachment 08 - NIH Amine in Air.1714658465138.docx

Attachment 08: NIH Amine in Air Objective of the Analysis: This protocol is based on OSHA standard method for amine measurement in air, PV2016. The concentration of amine in indoor air can be measured using this technique.

Procedure of Sample Collection and Storage:

NIH shall collect the air samples, and the Contractor shall pick up the samples from NIH Bethesda, Building 11. The Contractor shall provide NIH with sampling kits for collecting each sample.

Air samples shall be collected by drawing a known volume of air through a 10% phosphoric acid coated XAD-7 tube at an air flow rate of 0.1L/min for 4 to 8 hours.

The Contractor’s personnel assigned to pick up the samples shall be trained in sampling procedures, such as wearing gloves and eye protection when collecting samples. Adsorbed air samples shall be placed on the lab-provided chiller and reach the Laboratory within the prescribed time as determined by the lab.

Sample Preservation and Storage After collection of samples in the lab-provided cartridges, they shall be preserved either in a cooler. ice box, or refrigerator at a temperature of 4 °C.

Method of Shipping and Duration and Receiving The Contractor shall place the sample into a cooler with ice for immediate delivery or shipment to the laboratory. The sample shall be received with a chain of custody (COC). The COC shall have the name of the sample collector, date and time of sample collection, signature or initial of the sample collector, location of the sample and type of sample to be analyzed.

Procedure Samples shall be collected by drawing a known volume of air through a 10% phosphoric acid coated XAD-7 tube. Samples are desorbed with 1 mL of 1:1 solution of methanol:deionized water for one-half hour with shaking, then 0.5 mL of the sample is removed and added to 0.5 mL of 1:4 solution of 1.0 N NaOH:methanol and analyzed by gas chromatography using a flame ionization detector (GC-FID). An alternate desorbing solvent is 1 mL of 0.888 N NH4OH in methanol on a shaker for 30 minutes, then analysis by GC-FID.

Samples shall be collected using a personal, calibrated sampling pump, with the sampling device attached to within ±5% of the recommended flow rate. Samples are to be collected on 10% phosphoric acid coated XAD-7 tubes, lot 540, containing 80 mg adsorbing section with a 40 mg backup section separated by a 2-mm portion of urethane foam, with a silanized glass wool plug before the adsorbing section, and a 3- mm plug of urethane foam at the back of the backup section. The ends are to be flame sealed and the glass tube containing the adsorbent shall be 7-cm x 6-mm o.d., SKC tubes, or equivalent. Immediately before sampling, break off the ends of the sampling tube. All tubes shall be from the same lot. Attach the sampling tube to the pump with flexible tubing. It is desirable to utilize sampling tube holders which have a protective cover to shield the employee from the sharp, jagged end of the sampling tube. Position the tube so that sampled air passes through the reference, larger, section of the tube first. Air being sampled shall not pass through any hose or tubing before entering the sampling tube.

Attach the sampler vertically with the reference (larger section) pointing downward, in the worker's breathing zone, and positioned so it does not impede work performance or safety. After sampling for the appropriate time, remove the sample and seal the tube with plastic end caps. Wrap each sample end-to-end with a Form OSHA-21 seal. Submit at least one blank sample with each set of samples. Handle the blank sampler in the same manner as the other samples except draw no air through it. Record sample time, flow rate, and air volumes (in liters of air) for each sample, along with any potential interference. Ship any bulk samples separate from the air samples. Submit the samples to the laboratory for analysis as soon as possible after sampling. If delay is unavoidable, store the samples in a refrigerator.

Maintenance Plan for the Instrument The Contractor shall perform maintenance on their equipment as outlined per the manufacturer’s instructions.

The maintenance protocol shall be available and be delivered to NIH upon request.

Calibration Procedure The lab shall provide the calibration protocol of their GC/FID instrument to NIH upon request.

Quality Assurance and Quality Control Quality assurance and quality control shall conform to OSHA PV2016 method.

Data Acquisition The data shall be collected according to the OSHA PV2016 method.

References M. E. Eide, Occupational Safety and Health Administration, Cyclohexylamine, Method PV2016, February, 1994. https://www.osha.gov/sites/default/files/methods/OSHA%20PV2016.pdf SGS Galson, AIR SAMPLING PUMPS/ACCESSORIES, https://www.sgsgalson.com/equipment-category/13/