Page:NIOSH Manual of Analytical Methods - 2552.pdf/3

 METHYL ACRYLATE: METHOD 2552, Issue 1, dated 1 5 March 2003 - page 3 of 3 c. Allow the tubes to air equilibrate for several minutes, then cap the ends of the tubes and allow to stand overnight. d. Desorb (steps 5-8) and analyze together with standards and blanks (steps 11 and 12). e. Prepare a graph o f DE vs. µg methyl acrylate recovered.

MEASUREMENT: 11. Set gas chromatograph according to manufacturer’s recommendations and to conditions given on page 2552-1. Inject a 1-µL sample aliquot manually using the solvent flush technique or with an auto sampler. NOTE: If peak area is above the linear range of the working standards, dilute with carbon disulfide solvent, reanalyze and apply the appropriate dilution factor in the calculations. 12. Measure peak areas.

CALCULATIONS: 13. Determine the mass, µg (corrected for DE), for m ethyl acrylate found in the sample front (W f) and back (W b) sorbent sections, and in the average media blank front (B f) and back (B b) sorbent section s. NO TE: If W b > W f/10, report breakthrough and possible sample loss. 14. Calculate concentration, C, of methyl acrylate in the air volume sampled, V (L):

NO TE : :g/L = m g/m 3

EVALUATION OF METHOD: This method development was a result of requests to update and improve problematic gas chromatography methods. After determining that Anasorb CMS sorbent tubes resulted in improved DE recoveries when compared to the results previously obtained using coconut shell charcoal tubes [1], the desorption efficiency was determined for m ethyl acrylate at 5 levels ranging from 19.2 µg to 172.3 µg. The average DE for methyl acrylate was determined to be 92.3% using Anasorb CMS sorbent tubes [1] while the previously determined DE for methyl acrylate using charcoal tubes was 81 % [4]. The LO D was determined to be 0.5 µg per sample. The precision, as determined from the pooled relative standard deviation (S r), was determined to be 0.007. Methyl acrylate storage stability @ 0.5xR EL was acceptable after 30 days (105 .3% ) [1].

REFERENCES: [1] Pendergrass S M [1 999 ]. Backup Data Report for Methyl Acrylate Method Development, NIOS H/MR SB, Cincinnati, OH., (unpublished, January). [2] NIOSH [1984]. Methyl Acrylate: Method 1459 (supplement issued 8/15/94). In: Eller PM, ed. NIOSH Manual of Analytical Methods. 3 rd rev. ed. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control, National Institute for Occupational Safety and Health, DHHS (N IOS H) Publication N o. 84-100. [3] NIO SH [1978]. Method S3 8 In: Taylor DG, e d. NIOS H Manual of Analytical Methods, 2 nd ed., Vol. 2. U.S. Department of Health, Education, and W elfare, Public Health Service, Centers for Disease Control, National Institute for Occupational Safety and Health. DHEW (NIOSH)Publ. No.77-157-B. [4] NIOSH [1977]. Docum entation of NIOSH Validation Tests, NIOSH Contract No. CDC-99-74-45.

METHOD WRITTEN BY:

Stephanie M. Pendergrass, NIOSH/DART

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition