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Method Summary

Method Source U.S. EPA Engineering and Analysis Division
Method Number603
Revision Information40 CFR Part 136, Appendix A (Current Edition)
Method NameDescriptive Name: Acrolein and Acrylonitrile Purge and Trap via GC with Flame Ionization Detector (FID)

Official Name: Acrolein and Acrylonitrile

MediaMedia: WATER
SubcategoryOrganic
Citation EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)
Method Download Adobe Acrobat (pdf) icon Download full method now (PDF file)
Summary of MethodA 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 ApplicationThis method determines target compounds of Acrolein and Acrylonitrile potentially found in municipal and industrial discharges.
Applicable Concentration RangeMDL 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.
QC RequirementsInitial 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 HandlingSample 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.
Max Holding Time14 days without preservation. Samples for Acrolein with no pH adjustment is 3 days.
Relative Cost/Effort$201 to $400
Sample Prep Method(s)None.
 

Method Acrolein and Acrylonitrile Purge and Trap via GC with Flame Ionization Detector (FID) has 4 analytes associated with it.

Analyte


Detection
Level


Bias Precision Pct False
Positive
Herbicides
(E-12839)
N/AN/AN/A 
Volatile organic compounds
(E-12419)
N/AN/AN/A 
Acrylonitrile
(107-13-1)
.5 ug/L84 % Rec (SL)5 % RSD (SL)5 ug/L
Acrolein
(107-02-8)
.7 ug/L104 % Rec (SL)4 % RSD (SL)5 ug/L
export_analytes
Precision Descriptor NotesPrecision and accuracy values are from a single laboratory study using reagent water, municipal wastewater, and industrial wastewater spiked at four concentrations over the range of 5.0 to 100 mg/L with seven replicates per matrix.
Detection Level NoteMDL procedure is equivalent to the procedure at 40 CFR part 136, Appendix B. MDLs were determined using the standard deviation of 7 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for 6 degrees of freedom at the 99% confidence level (3.14). Detailed instructions for how MDLs are determined are found in Section 12.1 of the Method.
 
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