EPA-NERL: 528: Phenols in Water by GC/MS

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Phenols in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS)

Current Revision

Revision 1.0, April 2000

Media

WATER

Instrumentation

Gas Chromatography with Mass Spectrometry Detection

Method Subcategory

Organic

Method Source

EPA-NERL

Citation

Methods for the Determination of Organic and Inorganic Compounds in Drinking Water, Volume 1 (EPA/815-R-00-014)

Brief Method Summary

A 1-L sample is extracted using a solid phase extraction (SPE) cartridge. Phenols trapped by the SPE cartridge are eluted with methylene chloride. The concentrations of phenols in the extract are determined using a gas chromatography (GC) system equipped with a mass spectrometer (MS) detector.

Scope and Application

This method determines phenols in finished drinking water.

Applicable Concentration Range

0.1-15 ug/L for most analytes; 1-15 ug/L for others.

Interferences

(A) Contamination: Solid Phase Extraction (SPE) devices and reagents can introduce contaminants. Also, the suggested internal standard may contain phenolic contaminants; if suspected chose another standard.

(B) Silicone: Methylene chloride may leach silicone compounds; these will usually not interfere.

Quality Control Requirements

Initial demonstration of laboratory capability followed by regular analyses of continuing calibration checks, laboratory performance check standards, laboratory reagent blanks, laboratory fortified blanks, and laboratory fortified matrix samples. A method detection limit (MDL) must be determined for each analyte of interest.

Sample Handling

Sampling equipment, including automatic samplers, must be free of plastic tubing, gaskets, and other parts that may leach interfering analytes into the sample. Dechlorinate samples with 40-50 mg of sodium sulfite. After sodium sulfite is dissolved, acidify samples to less than pH 2 with 6 N hydrochloric acid. Samples must not exceed 10^oC during the first 48 hours after collection. Samples stored in the lab must be held at or below 6^oC until extraction, but should not be frozen. Extracts should be kept at 0^oC or less.

Maximum Holding Time

14 days; 30 days after extraction.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 15 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
2,4,6-Trichlorophenol(88-06-2) 2,4,6-Trichlorophenol Dowicide 2S Phenachlor Phenol, 2,4,6-trichloro-	0.046 ug/L	93% Rec (SL)	11.00 % RSD (SL)	1.00 ug/L
2,4-Dichlorophenol(120-83-2) 1,3-dichloro-4-Hydroxybenzene 2,4-Dichlorophenol DCP Dichlorophenol, 2,4- Phenol, 2,4-dichloro-	0.027 ug/L	88% Rec (SL)	4.80 % RSD (SL)	1.00 ug/L
2,4-Dimethylphenol(105-67-9) 2,4-Cimethylphenol 2,4-Dimethylphenol 2,4-Xylenol 4,6-Dimethylbenzene Bacticin Dimethylbenzene,1-hydroxy-2,4- Dimethylbenzene,4-hydroxy-1,3- Dimethylphenol, 2,4- Phenol, 2,4-dimethyl-	0.026 ug/L	76% Rec (SL)	8.00 % RSD (SL)	1.00 ug/L
2,4-Dinitrophenol(51-28-5) .alpha.-Dinitrophenol 2,4-Dinitrophenol 2,4-Dnp Aldifen Dinitrobenzene,1-hydroxy-2,4- Fenoxyl carbon n Phenol, 2,4-dinitro	0.310 ug/L	62% Rec (SL)	16.00 % RSD (SL)	1.00 ug/L
2-Chlorophenol(95-57-8) 2-Chlorophenol Phenol, 2-chloro- Phenol, o-chloro- o-Chlorophenol	0.020 ug/L	90% Rec (SL)	7.90 % RSD (SL)	1.00 ug/L
2-Methyl-4,6-dinitrophenol(534-52-1) 2,4-Dinitro-6-methyl-phenol 2,4-Dinitro-o-cresol 2-Methyl-4,6-dinitrophenol 4,6-Dinitro-o-cresol DNOC Dinitrocresol Methyl-4,6-dinitrophenol,2- Phenol, 2-methyl-4,6-dinitro-	0.260 ug/L	92% Rec (SL)	8.90 % RSD (SL)	1.00 ug/L
2-Nitrophenol(88-75-5) 2-Hydroxynitrobenzene 2-Nitrophenol Phenol, 2-nitro- Phenol, o-nitro- o-Hydroxynitrobenzene o-Nitrophenol	0.026 ug/L	75% Rec (SL)	11.00 % RSD (SL)	1.00 ug/L
4-Chloro-3-methylphenol(59-50-7) 3-Methyl-4-chlorophenol 4-Chloro-1-hydroxy-3-methylbenzene 4-Chloro-3-cresol 4-Chloro-3-hydroxytoluene 4-Chloro-3-methylphenol 4-Chloro-m-cresol Chlorophenol, 4-, methyl, 3- Parachlorometacresol Phenol, 4-chloro-3-methyl- p-Chloro-m-cresol	0.036 ug/L	91% Rec (SL)	8.40 % RSD (SL)	1.00 ug/L
4-Nitrophenol(100-02-7) 1-hydroxy-4-Nitrobenzene 4-Hydroxynitrobenzene 4-Nitrophenol Phenol, 4-nitro- p-Hydroxynitrobenzene p-Nitrophenol	0.420 ug/L	96% Rec (SL)	14.00 % RSD (SL)	1.00 ug/L
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
Organochlorine pesticides(E-12851) Organochlorine pesticides Pesticides, organochlorine	N/A	N/A	N/A
Pentachlorophenol(87-86-5) PCP Penchlorol Penta Pentachlorophenol Phenol, pentachloro- Santophen I	0.250 ug/L	103% Rec (SL)	7.60 % RSD (SL)	1.00 ug/L
Phenol(108-95-2) Benzene, hydroxy- Carbolic acid Hydroxybenzene Oxybenzene Phenic acid Phenol Phenyl hydrate Phenyl hydroxide	0.580 ug/L	91% Rec (SL)	20.00 % RSD (SL)	1.00 ug/L
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A
o-Cresol(95-48-7) 1-Hydroxy-2-methylbenzene 2-Cresol 2-Hydroxytoluene 2-Methylphenol Phenol, 2-methyl- o-Cresol o-Cresylic acid o-Hydroxytoluene o-Methylphenol o-Oxytoluene	0.026 ug/L	85% Rec (SL)	7.30 % RSD (SL)	1.00 ug/L

Precision Descriptor Notes:	Precision and accuracy values were determined using data from seven replicate analyses of fortified reagent water samples. Samples were analyzed using a hot splitless injection protocol. Additional precision and accuracy values are available in the method.
Detection Level Note:	MDLs represent performance on the primary column. Secondary columns used in validation of the method allowed for much lower MDLs for some analytes. Consult the method for more information. MDLs were determined using the standard deviation of 7 or 8 replicate analyses of a analyte-fortified reagent water (over a 3-day span) multiplied by the t-value for 6 or 7 degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B and Section 9.2.4 of the method.

Precision Descriptor Notes:

Precision and accuracy values were determined using data from seven replicate analyses of fortified reagent water samples. Samples were analyzed using a hot splitless injection protocol. Additional precision and accuracy values are available in the method.

Detection Level Note:

MDLs represent performance on the primary column. Secondary columns used in validation of the method allowed for much lower MDLs for some analytes. Consult the method for more information.
MDLs were determined using the standard deviation of 7 or 8 replicate analyses of a analyte-fortified reagent water (over a 3-day span) multiplied by the t-value for 6 or 7 degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B and Section 9.2.4 of the method.

Revision	PDF/Link
Revision 1.0, April 2000

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EPA-NERL: 528: Phenols in Water by GC/MS

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