EPA-EAD: 604: Phenols in Water Using GCECD/FID

Summary
Analytes
Revision
Data and Sites

Official Method Name

Phenols

Current Revision

40 CFR Part 136, Appendix A (Current Edition)

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

EPA-EAD

Citation

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

Brief Method Summary

A 1-L sample is acidified and extracted with methylene chloride using a separatory funnel. The methylene chloride extract is dried and exchanged to 2-propanol during concentration to a volume of 10-mL or less. The concentrations of phenols in the extract are measured using a gas chromatography (GC) system equipped with a flame ionization detector (FID). The method also provides for a derivatization and column chromatography cleanup procedure to aid in the elimination of interferences. Using this approach, the concentrations of phenols in the extract are measured by detecting derivatives using a GC system with an Electron Capture Detector (ECD).

Scope and Application

This method covers the determination of phenol and certain substituted phenols in wastewater and other waters.

Applicable Concentration Range

Ranges differ for each analyte depending on matrix and interferences.

Interferences

(A) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse.

(B) Reagent contamination: Use high purity reagents.

(C) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by performing the derivitization cleanup procedure in the method.

(D) Basic-sample wash: The wash can significantly reduce recovery of phenol and 2,4-dimethylphenol.

Quality Control Requirements

Each laboratory that uses this method is required to operate a formal quality control program. The minimum requirements of this program consist of an initial demonstration of laboratory capability and an ongoing analysis of spiked samples to evaluate and document data quality. The laboratory must maintain records to document the quality of data that is generated. Ongoing data quality checks are compared with established performance criteria to determine if the results of analyses meet the performance characteristics of the method. When results of sample spikes indicate atypical method performance, a quality control check standard must be analyzed to confirm that the measurements were performed in an in-control mode of operation.

Sample Handling

Grab samples must be collected in glass containers. [Note: Do NOT pre-rinse bottles]. Composite samples should be collected in refrigerated glass containers in accordance with the requirements of the program. Automatic sampling equipment must be as free as possible of Tygon tubing and other potential sources of contamination.

All samples must be iced or refrigerated at 4⁰C from the time of collection until extraction. Fill the sample bottles and, if residual chlorine is present, add 80 mg of sodium thiosulfate per liter of sample and mix well. EPA Methods 330.4 and 330.5 may be used for measurement of residual chlorine. Field test kits are available for this purpose.

Maximum Holding Time

Extract w/in 7 days; Analyze extracts w/in 40 days.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 14 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-	0.640 ug/L	84% Rec (ML)	27.00 % RSD (ML)	20.00 ug/L
2,4-Dichlorophenol(120-83-2) 1,3-dichloro-4-Hydroxybenzene 2,4-Dichlorophenol DCP Dichlorophenol, 2,4- Phenol, 2,4-dichloro-	0.390 ug/L	83% Rec (ML)	22.00 % RSD (ML)	20.00 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-	0.320 ug/L	54% Rec (ML)	29.00 % RSD (ML)	20.00 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	13.000 ug/L	77% Rec (ML)	41.00 % RSD (ML)	50.00 ug/L
2-Chlorophenol(95-57-8) 2-Chlorophenol Phenol, 2-chloro- Phenol, o-chloro- o-Chlorophenol	0.310 ug/L	79% Rec (ML)	26.00 % RSD (ML)	20.00 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-	16.000 ug/L	82% Rec (ML)	33.00 % RSD (ML)	50.00 ug/L
2-Nitrophenol(88-75-5) 2-Hydroxynitrobenzene 2-Nitrophenol Phenol, 2-nitro- Phenol, o-nitro- o-Hydroxynitrobenzene o-Nitrophenol	0.450 ug/L	77% Rec (ML)	39.00 % RSD (ML)	20.00 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	0.360 ug/L	77% Rec (ML)	25.00 % RSD (ML)	20.00 ug/L
4-Nitrophenol(100-02-7) 1-hydroxy-4-Nitrobenzene 4-Hydroxynitrobenzene 4-Nitrophenol Phenol, 4-nitro- p-Hydroxynitrobenzene p-Nitrophenol	2.800 ug/L	46% Rec (ML)	40.00 % RSD (ML)	50.00 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	7.400 ug/L	93% Rec (ML)	26.00 % RSD (ML)	20.00 ug/L
Phenol(108-95-2) Benzene, hydroxy- Carbolic acid Hydroxybenzene Oxybenzene Phenic acid Phenol Phenyl hydrate Phenyl hydroxide	0.140 ug/L	44% Rec (ML)	26.00 % RSD (ML)	20.00 ug/L
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A

Precision Descriptor Notes:	The precision and accuracy values were determined using regression equations derived from a 20 laboratory validation study. The study determined analytes at six concentrations in the range of 12 to 450 ug/L in multiple matrix types (including reagent water, drinking water, surface water, and three industrial wastewaters).
Detection Level Note:	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	PDF/Link
40 CFR Part 136, Appendix A (Current Edition)

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EPA-EAD: 604: Phenols in Water Using GCECD/FID

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