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EPA Method 525.2:

Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry -Revision 2.0.

Summary:
Organic compound analytes, internal standards, and surrogates are extracted from a 1L sample by passing it through a disk or cartridge containing a solid matrix with a chemically bonded C18 organic phase [liquid-solid extraction (LSE)]. Organic compounds are extracted from the LSE with small quantities of ethyl acetate followed by methylene chloride with further evaporation of the solvent. Sample components are separated, measured, and identified by capillary column GC/MS.

Scope:
This method provides procedures for the determination of a wide range of organic compounds found in finished drinking water, source water, or drinking water in any treatment stage.

Citation:
Methods for the Determination of Organic Compounds in Drinking Water – Supplement III (EPA/600/R-95-131)

Interferences:
(A) Reagent contamination: Perform blank analyses.(B) Contamination from sample carryover: Rinsing apparatus replacing syringes and injection port liners as needed can minimize contamination.

QC Requirements:
Initial demonstration of laboratory capability followed by regular analyses of laboratory reagent blanks (LRBs), laboratory fortified blanks (LFBs), and laboratory fortified matrix samples. Initial demonstration of laboratory capability includes the analysis of four to seven replicates of a LFB containing each analyte of concern at a concentration in the range of 2 – 5 ug/L. Additional QC procedures are recommended. A method detection limit (MDL) must be determined for each analyte.

Maximum Holding Time:
Samples can be held for 14 days generally (see Sample Handling section of the method for exceptions). Extracts can be held up to 30 days.

Media:
WATER

Subcategory:
Organic

Concentration:
0.1 – 10 ug/L for most analytes.

Precision:
Precision and accuracy values were generated primarily from 8 replicate analyses of fortified reagent water using a liquid-solid C-18 extraction cartridges and a quadrapole mass spectrometer (see Table 3 of the Method). However data for all Aroclors/PCBs, pentachlorophenol, toxaphene, bis(2-ethylhexyl phthalate), and di-n-butyl phthalate were generated using C-18 liquid-solid extraction and an ion trap mass-spectrometer (see Table 6 of the Method). For these latter analytes 8 replicate reagent water samples were analyzed, except for PCB-1260 (6 replicates) and toxaphene (7 replicates), and except for bis(2-ethylhexyl) phthalate and di-n-butyl phthalate (for which 7 replicates of fortified tap water were analyzed). The method contains a large amount of additional information. NOTE: For chlordane data, see alpha- and gamma-chlordane, and for PCBs see specific Aroclors.

Detection:
MDLs were determined using the standard deviation of replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for (# of samples – 1) degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B.

Revision Number:
Revision 2.0, 1995

Test Description:
Organic compounds –

Instrument used for this test:
GCMS