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 DIETHYLENETRIAMINE, ETHYLENEDIAMINE, & TRIETHYLENETETRAMINE: METHOD 2540, Issue 2, dated 15 August 1994 - Page 3 of 4

11.

c. Desorb and analyze together with the working standards. d. Prepare a graph of DE vs. µg amine recovered. Analyze three quality control blind spikes and three analyst spikes to ensure that the calibration curve and DE graph are in control.

MEASUREMENT: 12. 13.

Set liquid chromatograph according to manufacturer's recommendations and conditions given on page 2540-1. Inject sample aliquot manually or with autosampler. Measure peak area. NOTE: If the peak response is above the range of the working standards, dilute the standards with DMF, reanalyze and apply the appropriate dilution factors in calculations.

CALCULATIONS: 14.

15.

Determine the mass, µg (corrected for DE) of each analyte found in the sample front sorbent (W f) and the sample back sorbent (W b) sections and in the average media blank front (B f) and back (B b) sections. Calculate concentration, C, of each analyte in the air volume sampled, (L):

EVALUATION OF METHOD: This method was developed by and subjected to the evaluation procedures of the OSHA Organics Methods Evaluation Branch [1]. NIOSH evaluated the method for recovery, storage stability, precision, and accuracy and found comparable results [2]. The detection limits obtained by OSHA [1] corresponded to air concentrations of 0.004 ppm, 0.15 ppm, and 0.004 ppm for DETA, EDA, and TETA respectively, for a 10-L air volume. The method was validated over the range of 0.8 to 80 µg/sample for DETA, 4.6 to 465 µg/sample for EDA, and 1.3 to 119 µg/sample for TETA [1]. Desorption efficiency studies as performed by OSHA [1] using 6 samples at 3 levels gave a recovery of 99.0% for DETA, 99.2% for EDA, and 99.8% for TETA. The recovery of DETA, EDA, and TETA from samples used in a 15-day storage study was 89, 94, and 91%, respectively. These samples were generated by spiking the amines onto a glass wool plug in front of a sampling tube and drawing approximately 10 liters of air at 80% relative humidity through them. A 30-day storage study conducted by NIOSH [2] showed similar recoveries. Collection efficiency studies were done [1] by drawing 10-L of air at 80% relative humidity through Teflon wool plugs positioned ahead of the samplers and spiked with the pure amine. No DETA or TETA was found on the back section with a loading of 57.2 µg of DETA or 32.5 µg of TETA. At a loading of 414 µg of EDA, the back section was found to contain 12.2 µg of EDA.

REFERENCES: [1]

[2] [3] [4]

Elskamp, Carl J. "OSHA Method #60, Ethylenediamine (EDA), Diethylenetriamine (DETA), Triethylenetetramine (TETA)." Organic Methods Evaluation Branch, OSHA Analytical Laboratory, Salt Lake City, Utah. September, 1986. Neumeister, Charles. NIOSH/MRSB In-House Evaluation of OSHA Method #60, (NIOSH, Unpublished, June 17, 1988). NIOSH Manual of Analytical Methods, 2nd. ed., V. 4, P&CAM 276, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 78-175 (1978). Anderson, K., Hallgren, C., Levin, J., and Nilsson, C. "Determination of Ethylenediamine in Air Using Reagent-Coated Adsorbent Tubes and High-Performance Liquid Chromatography on the NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94