标准、规范、准则_EPA Method 8032A Acrylamide by Gas Chromatography - Revision 1.pdfVIP

METHOD 8032A ACRYLAMIDE BY GAS CHROMATOGRAPHY 1.0 SCOPE AND APPLICATION 1.1 Method 8032 is used to determine trace amounts of acrylamide monomer (CAS No. 79- 06-1) in aqueous matrices. This method may be applicable to other matrices and to other similar analytes. 1.2 The method detection limit (MDL) in an aqueous matrix is 0.032 µg/L. 1.3 This method is restricted for use by, or under the supervision of, analysts experienced in the use of gas chromatographs and skilled in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results with this method. 2.0 SUMMARY OF METHOD 2.1 Method 8032 is based on bromination of the acrylamide double bond. The reaction product (2,3-dibromopropionamide) is extracted from the reaction mixture with ethyl acetate, after salting out with sodium sulfate. The extract is cleaned up using a Florisil column, and analyzed by gas chromatography with electron capture detection (GC/ECD). 2.2 Compound identification should be supported by at least one additional qualitative technique. Analysis using a second gas chromatographic column or gas chromatography/mass spectrometry may be used for compound confirmation. 3.0 INTERFERENCES 3.1 No interference is observed from seawater or in the presence of 8.0% of ammonium ions derived from ammonium bromide. 3.2 Impurities from potassium bromide are removed by the Florisil cleanup procedure. 4.0 APPARATUS AND MATERIALS 4.1 Gas chromatographic system 4.1.1 Gas chromatograph suitable for on-column injections with all required accessories, including detector, analytical columns, recorder, gases, and syringes. A data system for measuring peak heights and/or peak areas is recommended.