EPA-EAD: 603:  Acrolein and Acrylonitrile Purge and Trap via GC with Flame Ionization Detector (FID)

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Acrolein and Acrylonitrile
Current Revision
40 CFR Part 136, Appendix A (Current Edition)
Media
WATER
Instrumentation
Gas Chromatography with Flame Ionization Detection
Method Subcategory
Organic
Method Source
  EPA-EAD
Citation
  EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)
Brief Method Summary
A sample is purged with an inert gas transforming the Acrolein and Acrylonitrile to the vapor phase where it is collected on an absorbent trap at ambient temperature. After the sample is purged, the trap is then heated, backflushed, and desorbed with the inert gas onto an chromatographic column. The gas chromatograph is temperature programmed to separate the Acrolein and Acrylonitrile, which are then detected by a flame ionization detector (FID).
Scope and Application
This method determines target compounds of Acrolein and Acrylonitrile potentially found in municipal and industrial discharges.
Applicable Concentration Range
MDL to 1000xMDL (ug/L).
Interferences
(A) Impurities in gas and plumbing: Impurities in the inert gas and organic plumbing system of the purge and trap concentrator tend to be the main cause of interference in the analytical system. The use of non-Teflon tubing and fittings should be avoided.
(B) Contamination during collection: Samples can become contaminated by diffusion of volatile organic compounds across the septum seal during collection and storage. Use Field Blanks to verify possible contamination.
(C) Carryover: Contamination by carry-over in the analytical system can occur, especially in samples that are extremely concentrated. Frequent bakeout and cleaning of the purging system can help prevent carry-over.
Quality Control Requirements
Initial demonstration of laboratory capability and the periodic analysis of laboratory reagent blanks, fortified blanks, and other laboratory solutions as a continuing check on performance.
Sample Handling
Sample should be placed in a 25 mL or larger glass; screw cap with a hole in the center for a Teflon-faced silicone septum. The sample should not have a headspace and should be kept refrigerated until analysis. If the sample is believed to contain free or combined chlorine, add 10mg/40mL of sodium thiosulfate upon collection and shave vigorously for one minute. Adjust the pH of the sample to that of about 4-5 with (1+1) HCl or NaOH.
Maximum Holding Time
14 days without preservation. Samples for Acrolein with no pH adjustment is 3 days.
Relative Cost
$201 to $400
Sample Preparation Methods
None.