Page:NIOSH Manual of Analytical Methods - 2561.pdf/3
AM INO E TH ANO L CO MP OU ND S: ME TH OD 2561, Issue 1, dated 1 5 Ma rch 2003 - Page 3 of 4 10. Analyze three quality control blind spikes and three analyst spikes to ensure that the calibration graph and D E graph are in control.
MEASUREMENT: 11. Set gas chromatograph according to manufacturer’s recomm endations and to conditions given on page 2561-1. Inject sample aliquot with autosampler, or manually using solvent flush technique. NOTE: If peak area is above the linear range of the working standards, dilute with eluent, reanalyze, and apply the appropriate dilution factor in calculations. 12. Mea sure peak area. Divide the peak area of an alyte by the peak area of internal standard on the sam e chromatogram.
CALCULATIONS: 13. Dete rm ine the m ass , :g (corrected for D E), of analyte found in the sam ple front (W f) and back (W b) sorbent sec tions, and in the average m edia blank front (B f) and back (B b) sorben t. NOTE: If W b > W f/10, report breakthrough and possible sample loss. 14. Calculate conce ntration, C, of analyte in the air volume sam pled, V (L):
EVALUATION OF METHOD: Current Validation This method was developed in response to a request for a method to use in a field study. The m ethod for dimethylethanolamine and dim ethylisopropanolamine was validated using analytes fortified on XAD-7 sorbent tubes (SKC, Inc. #226-94, Lot 1994). Desorption efficiency (DE) and precision are listed in Table 2. Storage stability studies were done at approximately 100 µg each analyte/sample. The sam ples were stored for up to 5 weeks in the freezer (-4°C). The recovery for dimethylethanolamine (110.9 :g/sample) was 98.4% and for dimethylisopropanolamine (104.6 :g/sample) w as 100.2% .
REFERENCES: [1] Grote AA[2002]. NIOSH Backup Data Report for NIOSH m ethod 2561. Nationa l Institute for Occupational Safety and He alth, DART /CEM B, Cincinnati, OH. (unpublished repo rt). [2] NIOSH [2002]. Evaluation of Visual Disturbances Related to Amine Exposure. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 200101444-2867. [3] DataChem Laboratories [2001]. NIOSH Analytical Reports for NIOSH Sequence 9675-CA through -CH. Cincinnati, OH: National Institute for Occupational Safety and Health, DAR T/CE MB . (unpublished, May). [4] NIOSH [1994]. Aminoethanol Compounds l: Method 2007. In: Eller PM, Cassinelli ME, eds. NIOSH Manual of Analytical Methods, 4 nd ed. C incinn ati, OH : U.S. Departm ent of He alth and Human Services, Pu blic Health Service, Centers for Disease Control and Prevention, National Istitute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 94-113.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition