EPA-RCA: 8041A: Phenols by Gas Chromatography

Summary
Analytes
Revision
Data and Sites

Official Method Name

Phenols in Aqueous and Non-aqueous Samples by Capillary GC/FID or GC/ECD and Single or Dual Columns

Current Revision

Revision 1, November 2000

Media

VARIOUS

Instrumentation

Gas Chromatography with Flame Ionization Detection

Method Subcategory

Organic

Method Source

EPA-RCA

Citation

SW-846 Update IVB

Brief Method Summary

Samples are extracted and cleaned up (according to sample matrix) and the solvent appropriately exchanged. The phenols are then determined with or without derivatization. Underivatized phenols may be analyzed directly by gas chromatography, using either the single-column or dual-column approach. Alternatively, target phenols may be derivatized to form methylated phenols and pentafluorobenzylbromo ether derivatives which are then also analyzed using gas chromatography.

Scope and Application

This method determines the concentration of phenols in aqueous and non-aqueous samples by using open-tubular, capillary-column gas chromatography procedures while utilizing either single-column or dual column/dual-detector approaches.

Applicable Concentration Range

Not Available.

Interferences

(A) Memory Interferences: Carryover may occur whenever high and low concentration samples are analyzed in sequence. For prevention, rinse the sample syringe between samples with solvent. Also, unusually concentrated samples should be followed by the analysis of a solvent blank. Column blanks should be analyzed whenever a solvent blank indicates cross-contamination.
(B) Coeluting Compounds: Some compounds coelute on either one or both columns, in which case, they must be reported as coeluting. The samples may be reanalyzed by GC/MS. Some derivatized phenols are known to coelute and, therefore, may be analyzed in the underivatized form or by using a GC column which permits separation.
(C) Non-specific Interferences: May reduce sensitivity during the analysis of underivatized phenols. Also, sample extracts should be dry prior to methylation to avoid poor recoveries.

Quality Control Requirements

Refer to Chapter One and Methods 8000, 3500, and 3600 for specific QC procedures. Procedures include: validation of sample extraction and clean up, initial demonstration of capability, calibration verification, evaluation of retention times, analysis of method blanks, matrix spikes, duplicates, surrogates, and laboratory control samples.

Sample Handling

See SW-846 Chapter Four for information. Extracts to be methylated should undergo derivatization within 48 hours after extraction. The methylated extracts should then be analyzed immediately in order to avoid the possibility of additional reactions occurring.

Maximum Holding Time

See SW-846 Chapter Four for information.

Relative Cost

$201 to $400

Sample Preparation Methods

Methods 3500,3510,3520,3540,3550,3580

This method has 30 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
2,3,4,6-Tetrachlorophenol(58-90-2) 2,3,4,6-Tetrachlorophenol 2,4,5,6-Tetrachlorophenol Dowicide 6 Phenol, 2,3,4,6-tetrachloro-	N/A	146% Rec (SL)	3.30 % RSD (SL)	20.00 ug/g
2,3,5,6-Tetrachlorophenol(935-95-5) 2,3,5,6-Tetrachlorophenol Phenol, 2,3,5,6-tetrachloro-	N/A	236% Rec (SL)	3.50 % RSD (SL)	20.00 ug/g
2,3,5-Trichlorophenol(933-78-8) 2,3,5-Trichlorophenol Phenol, 2,3,5-trichloro-	N/A	136% Rec (SL)	4.10 % RSD (SL)	20.00 ug/g
2,3,6-Trichlorophenol(933-75-5) 2,3,6-Trichlorophenol Phenol, 2,3,6-trichloro-	N/A	125% Rec (SL)	2.60 % RSD (SL)	20.00 ug/g
2,3-Dimethylphenol(526-75-0) 2,3-Dimethylphenol 2,3-Xylenol Phenol, 2,3-dimethyl-	N/A	106% Rec (SL)	7.10 % RSD (SL)	20.00 ug/g
2,4,5-Trichlorophenol(95-95-4) 2,4,5-Trichlorophenol Dowicide 2 Phenol, 2,4,5-trichloro-	N/A	139% Rec (SL)	3.00 % RSD (SL)	20.00 ug/g
2,4,6-Trichlorophenol(88-06-2) 2,4,6-Trichlorophenol Dowicide 2S Phenachlor Phenol, 2,4,6-trichloro-	N/A	122% Rec (SL)	2.70 % RSD (SL)	20.00 ug/g
2,4-Dichlorophenol(120-83-2) 1,3-dichloro-4-Hydroxybenzene 2,4-Dichlorophenol DCP Dichlorophenol, 2,4- Phenol, 2,4-dichloro-	N/A	102% Rec (SL)	2.50 % RSD (SL)	20.00 ug/g
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-	N/A	93% Rec (SL)	11.50 % RSD (SL)	20.00 ug/g
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	N/A	157% Rec (SL)	7.30 % RSD (SL)	40.00 ug/g
2,5-Dimethylphenol(95-87-4) 1-Hydroxy-2,5-dimethylbenzene 2,5-Dimethylphenol 2,5-Xylenol 6-Methyl-m-cresol Phenol, 2,5-dimethyl- p-Xylenol	N/A	101% Rec (SL)	2.60 % RSD (SL)	20.00 ug/g
2,5-Dinitrophenol(329-71-5) 2,5-Dinitrophenol Phenol, 2,5-dinitro-	N/A	177% Rec (SL)	5.10 % RSD (SL)	40.00 ug/g
2,6-Dichlorophenol(87-65-0) 2,6-Dichlorophenol Phenol, 2,6-dichloro-	N/A	104% Rec (SL)	2.80 % RSD (SL)	20.00 ug/g
2,6-Dimethylphenol(576-26-1) 2,6-Dimethylphenol 2,6-Dmp 2,6-Xylenol Phenol, 2,6-dimethyl-	N/A	101% Rec (SL)	8.10 % RSD (SL)	20.00 ug/g
2-Chlorophenol(95-57-8) 2-Chlorophenol Phenol, 2-chloro- Phenol, o-chloro- o-Chlorophenol	N/A	93% Rec (SL)	11.60 % RSD (SL)	20.00 ug/g
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-	N/A	201% Rec (SL)	3.80 % RSD (SL)	40.00 ug/g
2-Nitrophenol(88-75-5) 2-Hydroxynitrobenzene 2-Nitrophenol Phenol, 2-nitro- Phenol, o-nitro- o-Hydroxynitrobenzene o-Nitrophenol	N/A	99% Rec (SL)	2.80 % RSD (SL)	20.00 ug/g
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	N/A	128% Rec (SL)	3.80 % RSD (SL)	20.00 ug/g
4-Nitrophenol(100-02-7) 1-hydroxy-4-Nitrobenzene 4-Hydroxynitrobenzene 4-Nitrophenol Phenol, 4-nitro- p-Hydroxynitrobenzene p-Nitrophenol	N/A	123% Rec (SL)	5.60 % RSD (SL)	20.00 ug/g
Dinoseb(88-85-7) 2,4-Dinitro-6-sec-butylphenol 2-sec-Butyl-4,6-dinitrophenol Butaphene Dinitrobutyl phenol Dinoseb Dinoseb (ANSI) Phenol, 2-(1-methylpropyl)-4,6-dinitro- Phenol,2-sec-butyl-4,6-dinitro-	N/A	210% Rec (SL)	4.90 % RSD (SL)	20.00 ug/g
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	N/A	168% Rec (SL)	5.00 % RSD (SL)	20.00 ug/g
Phenol(108-95-2) Benzene, hydroxy- Carbolic acid Hydroxybenzene Oxybenzene Phenic acid Phenol Phenyl hydrate Phenyl hydroxide	N/A	93% Rec (SL)	16.90 % RSD (SL)	20.00 ug/g
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A
m-Chlorophenol(108-43-0) 3-Chlorophenol Phenol, 3-chloro- Phenol, m-chloro- m-Chlorophenol	N/A	116% Rec (SL)	6.70 % RSD (SL)	20.00 ug/g
m-Cresol(108-39-4) 3-Cresol 3-Methylphenol Phenol, 3-methyl- m-Cresol m-Cresylic acid m-Hydroxytoluene m-Methylphenol m-Oxytoluene	N/A	98% Rec (SL)	10.30 % RSD (SL)	20.00 ug/g
m-Nitrophenol(554-84-7) 3-Nitrophenol Phenol, 3-nitro- m-Nitrophenol	N/A	124% Rec (SL)	4.00 % RSD (SL)	20.00 ug/g
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	N/A	95% Rec (SL)	13.60 % RSD (SL)	20.00 ug/g
p-Cresol(106-44-5) 1-Hydroxy-4-methylbenzene 4-Cresol 4-Hydroxytoluene 4-Methylphenol Phenol, 4-methyl- p-Cresol p-Cresylic acid p-Methylhydroxybenzene p-Oxytoluene p-Tolyl alcohol	N/A	96% Rec (SL)	3.40 % RSD (SL)	20.00 ug/g

Precision Descriptor Notes:	Precision and accuracy values are based on the analyses of five, 5 g aliquots of clean, sandy loam soil that were spiked separately and extracted using Method 3540 (Soxhlet) and methylene chloride as a solvent.
Detection Level Note:	None.

Revision	PDF/Link
Revision 1, November 2000

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EPA-RCA: 8041A: Phenols by Gas Chromatography

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