EPA Method 1653

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EPA Method 1653:
Chlorinated Phenolics associated with the pulp and paper industry wastewater by GCMS. Official Name: Chlorinated Phenolics in Wastewater by In Situ Acetylation and GCMS

A 1-L sample is spiked with stable isotopically labeled analogs of the compounds of interest and an internal standard. The solution is adjusted to a neutral pH and a potassium carbonate buffer is added and then raised to 9-11.5. The chlorophenolics are converted in situ to acetates by the addition of acetic anhydride. The solution is extracted with hexane. The extracted is concentrated to a final volume of 0.5 mL and an instrument internal standard is added to the extract. The extract is then analyzed by a GCMS. The labeled compounds and internal standard serve to correct the variability of the analytical technique.

This is a GC-MS method that determines the quantity of chlorinated phenolics (chlorinated phenols, guaiacols, catechols, vanillins, syringalehydes) and other compounds associated with CWA, RCRA, and CERCLA, which are amenable to in situ acetylation, extraction, and analysis by GC-MS. The target analytes of interest are specifically associated with the pulp and paper industry. This method is designed to meet the survey and monitoring requirements of the EPA.

EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)

(A) Contamination of glassware: Glassware should be scrupulously cleaned, solvent rinsed and baked at 450oC for a minimum of one hour.(B) Co-extraction: High levels of non-chlorinated phenols may cause poor recovery of the compounds of interest, particularly in samples collected in the vicinity of a source of creosote.(C) Degradation: Catechols are susceptible to degradation by active sites on injection port liners and columns, and are subject to oxidation to the corresponding chloro-o-benzoquinones. A small amount of ascorbic acid may be added to samples to prevent auto-oxidation. The addition for pulp and paper industry samples applies to effluent samples only. The internal standard, 3,4,5-trichlorophenol, has been reported to be an anaerobic degradation product of 2,3,4,5-tetrachlorophenol and/or pentachlorophenol. If an interference occurs, labeled pentachlorophenol or another labeled compound may be used as an alternative internal standard; otherwise all standards and reference compounds must be used as specified in this method.(D)Blank Contamination: Blank contamination by pentachlorophenol has been reported to be traceable to potassium carbonate. Potential contamination may be removed by baking overnight at 400 to 500oC.

QC Requirements:
Initial demonstration of laboratory capability, analysis of samples spiked with labeled compounds to evaluate and document data quality and the periodic analysis of laboratory reagent blanks, fortified blanks, and other laboratory solutions as a continuing check on performance.

Maximum Holding Time:
Extract and acetylate within 30 days of collection Analyze within 30 days of acetylation.



MDL to 1000 ug/L (depending on interferences).

Sample Prep:


MDL 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 14.1 of the Method.

Revision Number:
Revision A, August 1997