6420 PHENOLS*

6420 A. Introduction

1. Sources and Significance The methods presented in this section are intended for the
Phenols are found in many wastewaters and some raw source determination of individual phenolic compounds. For specific
waters in the United States. They generally are traceable to compounds covered, see each method. Method 6420B is a gas
industrial effluents or landfills. These compounds have a low chromatographic (GC) method using liquid-liquid extraction
taste threshold in potable waters and also may have a detrimental and either flame ionization detection (FID) or derivatization
effect on human health at higher levels. and electron capture detection (ECD) to determine a wide
variety of phenols at relatively low concentrations. In addi-
2. Selection of Method tion, 6420C, a liquid-liquid extraction gas chromatographic/
For methods of determining total phenols in water and waste- mass spectrometric (GC/MS) method, can be used to deter-
water, see Section 5530. mine the phenols at slightly higher concentrations.

* Approved by Standard Methods Committee, 2000.

6420 B. Liquid–Liquid Extraction Gas Chromatographic Method

This method is applicable to the determination of phenol and The basic sample wash (6420B.5a) may cause low recovery of
certain substituted phenols* in municipal and industrial dis- phenol and 2,4-dimethylphenol. Results obtained under these
charges. When analyzing unfamiliar samples for any or all of conditions are minimum concentrations.
these compounds, support the identifications by at least one c. Detection levels: The method detection level (MDL) is the
additional qualitative technique. Alternatively, use the derivati- minimum concentration of a substance that can be measured and
zation, cleanup, and electron capture detector gas chromatogra- reported with 99% confidence that the value is above zero. The
phy (ECD/GC) procedure to confirm measurements made by the MDL concentrations listed in Tables 6420:I and II were obtained
flame ionization detector gas chromatographic (FID/GC) proce- by using reagent water. Similar results were achieved with
dure. The method for base/neutrals and acids (Section 6410B) representative wastewaters. The MDL actually obtained in a
provides gas chromatograph/mass spectrometer (GC/MS) condi- given analysis will vary, depending on instrument sensitivity and
tions appropriate for qualitative and quantitative confirmation of matrix effects.
results using the extract produced. d. Safety: The toxicity or carcinogenicity of each reagent used
in this method has not been defined precisely. Take special care
1. General Discussion in handling pentafluorobenzyl bromide, which is a lachrymator,
and 18-crown-6-ether, which is highly toxic.
a. Principle: See Section 6010C.2 for discussion of gas chro-
matographic principles. A measured volume of sample is acidi- 2. Sampling and Storage
fied and extracted with methylene chloride. The extract is dried
and exchanged to 2-propanol during concentration. The extract is See Section 6410B.2.
separated by gas chromatography and phenols are measured with
a flame ionization detector. 3. Apparatus
The method provides for a derivatization and column chroma-
tography cleanup procedure to aid in the elimination of interfer- Use all the apparatus specified in Section 6410B.3a– g and i–
ences. Derivatives are analyzed by an electron capture k, and in addition:
detector. a. Chromatographic column, 100 mm long 10 mm ID, with
b. Interferences: TFE stopcock.
1) General precautions—See Section 6410B.1b1). b. Reaction flask, 15- to 25-mL round-bottom, with standard
2) Other countermeasures—The cleanup procedure in tapered joint, fitted with a water-cooled condenser and U-shaped
6420B.5c2) can be used to overcome many of these inteferences, drying tube containing granular calcium chloride.
but unique samples may require additional cleanup to achieve c. Gas chromatograph:† An analytical system complete with
the method detection levels. a temperature-programmable gas chromatograph suitable for on-

* 4-Chloro-3-methylphenol; 2-chlorophenol; 2,4-dichlorophenol; 2,4-dimethyl- † Gas chromatographic methods are extremely sensitive to the materials used.
phenol; 2,4-dinitrophenol; 2-methyl-4,6-dinitrophenol; 2-nitrophenol; 4-nitrophe- Mention of trade names by Standard Methods does not preclude the use of other
nol; pentachlorophenol; phenol; 2,4,6-trichlorophenol. existing or as-yet-undeveloped products that give demonstrably equivalent results.

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TABLE 6420:I. CHROMATOGRAPHIC CONDITIONS AND METHOD TABLE 6420:II. SILICA GEL FRACTIONATION AND ELECTRON CAPTURE GAS
DETECTION LEVELS CHROMATOGRAPHY OF PFBB DERIVATIVES
Method Method
Percent Recovery
Retention Detection Retention Detection
by Fraction*
Time Level Parent Time Level
Compound min g/L Compound 1 2 3 4 min g/L

2-Chlorophenol 1.70 0.31 2-Chlorophenol — 90 1 — 3.3 0.58

2-Nitrophenol 2.00 0.45 2-Nitrophenol — — 9 90 9.1 0.77
Phenol 3.01 0.14 Phenol — 90 10 — 1.8 2.2
2,4-Dimethylphenol 4.03 0.32 2,4-Dimethylphenol — 95 7 — 2.9 0.63
2,4-Dichlorophenol 4.30 0.39 2,4-Dichlorophenol — 95 1 — 5.8 0.68
2,4,6-Trichlorophenol 6.05 0.64 2,4,6-Trichlorophenol 50 50 — — 7.0 0.58
4-Chloro-3-methylphenol 7.50 0.36 4-Chloro-3-methylphenol — 84 14 — 4.8 1.8
2,4-Dinitrophenol 10.00 13.0 Pentachlorophenol 75 20 — — 28.8 0.59
2-Methyl-4,6-dinitrophenol 10.24 16.0 4-Nitrophenol — — 1 90 14.0 0.70
Pentachlorophenol 12.42 7.4
Column conditions: Chromosorb W-AW-DMCS (80/100 mesh) coated with
4-Nitrophenol 24.25 2.8 5% OV-17 packed in a 1.8-m-long 2.0-mm-ID glass column with 5% methane/
Column conditions: Supelcoport (80/100 mesh) coated with 1% SP-1240DA 95% argon carrier gas at 30-mL/min flow rate. Column temperature held isother-
packed in a 1.8-m-long 2-mm-ID glass column with nitrogen carrier gas at mal at 200°C. MDLs determined with an ECD.
30-mL/min flow rate. Column temperature was 80°C at injection, programmed * Eluent composition:
immediately at 8°C/min to 150°C final temperature. MDLs determined with an Fraction 1: 15% toluene in hexane.
FID. Fraction 2: 40% toluene in hexane.
Fraction 3: 75% toluene in hexane.
Fraction 4: 15% 2-propanol in toluene.

column injection and all required accessories including syringes,

analytical columns, gases, detector, and strip-chart recorder. dilute to volume with 2-propanol. Prepare fresh weekly. Prepare
Preferably use a data system for measuring peak areas. in a hood. Store at 4°C and protect from light.
1) Column for underivatized phenols—1.8 m long 2-mm ID g. Acetone, hexane, methanol, methylene chloride, 2-propa-
glass, packed with 1% SP1240DA on Supelcoport (80/100 mesh) nol, toluene, pesticide quality or equivalent.
or equivalent. The detection level and precision and bias data h. Silica gel, 100/200 mesh.‡ Activate at 130°C overnight and
presented herein were developed with this column. For guide- store in a desiccator.
lines for the use of alternate columns (e.g., capillary or mega- i. Stock standard solutions: Prepare from pure standard ma-
bore), see 6420B.5b1). terials or purchase as certified solutions. Prepare as directed in
2) Column for derivatized phenols—1.8 m long 2-mm ID, Section 6410B.4g, but dissolve material in 2-propanol.
glass, packed with 5% OV-17 on Chromosorb W-AW-DMCS j. Calibration standards: Prepare standards appropriate to
(80/100 mesh) or equivalent. This column was used to develop chosen means of calibration.
the detection limit and precision and bias data presented herein. 1) External standards—Prepare at a minimum of three con-
For guidelines for the use of alternate columns (e.g., capillary or centration levels for each compound by adding volumes of one
megabore), see 6420B.5b1). or more stock standards to a volumetric flask and diluting to
3) Detectors—flame ionization (FID) and electron capture volume with 2-propanol. Prepare one standard at a concentration
(ECD). Use the FID to determine parent phenols. Use the ECD near, but above, the MDL (see Table 6420:I or II) and the others
when determining derivatized phenols. For guidelines for use of to correspond to the expected range of sample concentrations or
alternative detectors, see 6420B.5b1). to define the working range of the detector.
2) Internal standards—Prepare at a minimum of three con-
4. Reagents centration levels for each compound by adding volumes of
one or more stock standards to a volumetric flask. To each
Use reagents listed in Section 6410B.4a–f, and in addition: calibration standard, add a known constant amount of one or
a. Sodium hydroxide solution (NaOH), 1N: Dissolve 4 g more internal standards, and dilute to volume with 2-propa-
NaOH in reagent water and dilute to 100 mL. nol. Prepare one standard at a concentration near, but above,
b. Sulfuric acid (H SO ), 1N: Slowly add 58 mL conc H SO the MDL and the others to correspond to the expected range
to 500 mL reagent water and dilute to 1 L. of sample concentrations or to define the working range of the
c. Potassium carbonate (K CO ), powdered. detector.
d. Pentafluorobenzyl bromide ( -bromopentafluorotoluene), k. Quality control (QC) check sample concentrate: Obtain a
97% minimum purity. (CAUTION: This chemical is a lachry- check sample concentrate containing each compound at a con-
mator.) centration of 100 g/mL in 2-propanol. If such a sample is not
e. 18-Crown-6-ether (1,4,7,10,13,16-hexaoxacyclooctadec- available from an external source, prepare using stock standards
ane), 98% minimum purity. (CAUTION: This chemical is highly prepared independently from those used for calibration.
toxic.)
f. Derivatization reagent: Add 1 mL pentafluorobenzyl bro-
mide and 1 g 18-crown-6-ether to a 50-mL volumetric flask and ‡ Davison grade 923, or equivalent.

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 PHENOLS (6420)/Liquid–Liquid Extraction GC Method

5. Procedure

a. Extraction: Mark water meniscus on side of sample bottle

for later determination of volume. Pour entire sample into a 2-L
separatory funnel. For samples high in organic content, solvent
wash sample at basic pH (as prescribed in next paragraph) to
remove potential interferences. During wash, avoid prolonged or
exhaustive contact with solvent, which may result in low recov-
ery of some phenols, notably phenol and 2,4-dimethylphenol.
For relatively clean samples, omit wash and extract directly.
To wash, adjust pH to 12.0 or greater with NaOH solution.
Add 60 mL methylene chloride and shake the funnel for 1 min
with periodic venting to release excess pressure. Discard solvent
layer. Repeat wash up to two additional times if significant color
is being removed.
Before extraction, adjust to pH of 1 to 2 with H SO . Extract
three times with methylene chloride as directed in Section
6410B.5a1). Assemble Kuderna–Danish apparatus, concentrate
extract to 1 mL, and remove, drain, and cool K–D apparatus as
directed in Section 6410B.5a1).
Increase temperature of hot water bath to 100°C. Remove
Snyder column and rinse flask and its lower joint into concen-
trator tube with 1 to 2 mL 2-propanol. Preferably use a 5-mL
syringe for this operation. Attach a two-ball micro-Snyder col-
umn to concentrator tube and prewet column by adding about
0.5 mL 2-propanol to the top. Place micro-K–D apparatus on
water bath so concentrator tube is partially immersed in hot
water. Adjust vertical position of apparatus and water tempera-
ture so as to complete concentration in 5 to 10 min. (CAUTION:
If temperature is raised too quickly, the sample may be
blown out of the K–D apparatus). At proper rate of distillation,
the column balls actively chatter but the chambers are not
flooded. When the apparent volume of liquid reaches 2.5 mL,
remove K–D apparatus and let drain and cool for at least 10 min.
Add 2 mL 2-propanol through top of micro-Snyder column and Figure 6420:1. Gas chromatogram of phenols. Column: 1% SP-1240DA
resume concentrating as before. When the apparent volume of on Supelcoport; program: 80°C at injection, immediate
8°C/min to 150°C; detector: flame ionization.
liquid reaches 0.5 mL, remove K–D apparatus and let drain and
cool for at least 10 min.
Remove micro-Snyder column and rinse lower joint into con-
centrator tube with a minimum amount of 2-propanol. Adjust alent to those given in Table 6420:I. Calibrate using the external
extract volume to 1.0 mL. Stopper concentrator tube and store at or the internal standard technique as follows:
4°C if further processing will not be done immediately. If extract a) External standard calibration procedure—Prepare standards
is to be stored 2 d, transfer to a TFE-sealed screw-cap vial. If as directed in 6420B.4j1) and follow the procedure of ¶ b3)
sample extract requires no further cleanup, proceed with chro- below. Tabulate data and obtain calibration curve or calibration
matographic analysis (¶ b below). If sample requires further factor as directed in Section 6200B.4c3).
cleanup, proceed to ¶ c below. b) Internal standard calibration procedure—Prepare samples
Determine original sample volume by refilling sample bottle as directed in 6420B.4j2) and follow the procedure of ¶ b3)
to mark and transferring liquid to a 1000-mL graduated cylinder. below. Tabulate data and calculate response factors as directed in
Record sample volume to nearest 5 mL. Section 6200B.4c2).
b. Flame ionization detector gas chromatography (FID/GC): Verify working calibration curve, calibration factor, or RF on
1) Operating conditions—Table 6420:I summarizes the rec- each working day by measuring one or more calibration stand-
ommended operating conditions for the gas chromatograph and ards. If the response for any compound varies from the predicted
gives retention times and MDLs that can be achieved under these response by more than 15%, prepare a new calibration curve
conditions. An example of the separations obtained with this for that compound.
column is shown in Figure 6420:1. Other packed or capillary 3) Sample analysis—If the internal standard calibration pro-
(open-tubular) columns, chromatographic conditions, or detec- cedure is used, add internal standard to sample extract and mix
tors may be used if the requirements of 6420B.7 are met. thoroughly immediately before injecting 2 to 5 L sample ex-
2) Calibration—To calibrate the system for underivatized phe- tract or standard into gas chromatograph using the solvent-flush
nols, establish gas chromatographic operating conditions equiv- technique. Smaller (1.0- L) volumes may be injected if auto-

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 PHENOLS (6420)/Liquid–Liquid Extraction GC Method

matic devices are used. Record volume injected to nearest

0.05 L and resulting peak size in area or peak height units.
Identify compounds in sample by comparing peak retention times
with peaks of standard chromatograms. Base width of retention time
window used to make identifications on measurements of actual
retention time variations of standards over the course of a day. To
calculate a suggested window size, use three times the standard
deviation of a retention time for a compound. Analyst’s experience
is important in interpreting chromatograms.
If the response for a peak exceeds the working range of the
system, dilute extract and re-analyze.
If peak response cannot be measured because of interferences,
use the alternative gas chromatographic procedure (¶ c below).
c. Derivatization and electron capture detector gas chroma-
tography (ECD/GC):
1) Derivatization—Pipet 1.0 mL of the 2-propanol solution of
standard or sample extract into a glass reaction vial. Add 1.0 mL
derivatizing reagent (6420B.4f); this is sufficient to derivatize a
solution having a total phenolic content not exceeding
0.3 mg/mL. Add about 3 mg K CO and shake gently. Cap
mixture and heat for 4 h at 80°C in a hot water bath. Remove
from hot water bath and let cool. Add 10 mL hexane and shake
vigorously for 1 min. Add 3.0 mL distilled, deionized water and
shake for 2 min. Decant a portion of the organic layer into a
concentrator tube and cap with a glass stopper.
2) Cleanup—Place 4.0 g silica gel in a chromatographic col-
umn. Tap column to settle silica gel and add about 2 g anhydrous
Na SO to the top. Pre-elute column with 6 mL hexane. Discard
eluate and just before exposing Na SO layer to air, pipet onto
the column 2.0 mL hexane solution [¶ c1) above] that contains
the derivatized sample or standard. Elute column with 10.0 mL Figure 6420:2. Gas chromatogram of PFB derivatives of phenols. Col-
hexane and discard eluate. Elute column, in order, with 10.0 mL umn: 5% OV-17 on Chromosorb W-AW-DMCS; tempera-
15% toluene in hexane (Fraction 1), 10.0 mL 40% toluene in ture: 200°C; detector: electron capture.
hexane (Fraction 2), 10.0 mL 75% toluene in hexane (Fraction
3), and 10.0 mL 15% 2-propanol in toluene (Fraction 4). Prepare
6. Calculation
all elution mixtures on a volume:volume basis. Elution patterns
for the phenolic derivatives are shown in Table 6420:II. Frac-
a. FID/GC analysis: Determine concentration of individual
tions may be combined as desired, depending on the specific
compounds. If the external standard calibration procedure is
phenols of interest or level of interferences.
used, calculate amount of material injected from peak response
3) Operating conditions—Table 6420:II summarizes the rec-
using calibration curve or calibration factor determined previ-
ommended operating conditions for the gas chromatograph and
ously. Calculate sample concentration from the equation:
gives retention times and MDLs that can be achieved under these
conditions. An example of the separations obtained with this
(A) (V )
column is shown in Figure 6420:2. Concentration, g/L
4) Calibration—Calibrate system daily by preparing a mini- (V ) (V )
mum of three 1-mL portions of calibration standards,
6420B.4j1), containing each of the phenols of interest and de- where:
rivatized as above. Analyze 2 to 5 L of each column eluate A amount of material injected, ng,
collected as in ¶ c5) below and tabulate peak height or area V volume of total extract, L,
responses against calculated equivalent mass of underivatized V volume of extract injected, L, and
phenol injected. Prepare a calibration curve for each compound. V volume of water extracted, mL.
Before using any cleanup procedure, process a series of cali-
bration standards through the procedure to validate elution pat- If the internal standard calibration procedure is used, calculate
terns and to assure absence of interferences from the reagents. concentration in sample using the response factor (RF) deter-
5) Sample analysis—Inject 2 to 5 L column fractions into the mined above and the equation:
gas chromatograph using the solvent-flush technique. Smaller
(1.0- L) volumes can be injected if automatic devices are used. (A ) (I )
Concentration, g/L
Record volume injected to nearest 0.05 L and resulting peak (A ) (RF) (V )
size in area or peak height units. If peak response exceeds linear
range of system, dilute extract and re-analyze. where:

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 PHENOLS (6420)/Liquid–Liquid Extraction GC Method

TABLE 6420:III. QC ACCEPTANCE CRITERIA*

Test Limit Range Range for
Conc. for s for X P, P
Compound g/L g/L g/L %

4-Chloro-3-methylphenol 100 16.6 56.7–113.4 49–122

2-Chlorophenol 100 27.0 54.1–110.2 38–126
2,4-Dichlorophenol 100 25.1 59.7–103.3 44–119
2,4-Dimethylphenol 100 33.3 50.4–100.0 24–118
2-Methyl-4,6-dinitrophenol 100 25.0 42.4–123.6 30–136
2,4-Dinitrophenol 100 36.0 31.7–125.1 12–145
2-Nitrophenol 100 22.5 56.6–103.8 43–117
4-Nitrophenol 100 19.0 22.7–100.0 13–110
Pentachlorophenol 100 32.4 56.7–113.5 36–134
Phenol 100 14.1 32.4–100.0 23–108
2,4,6-Trichlorophenol 100 16.6 60.8–110.4 53–119
* s standard deviation for four recovery measurements,
X average recovery for four recovery measurements, and
P, P percent recovery measured.
NOTE: These criteria are based directly on the method-performance data in Table 6420:IV. Where necessary, the recovery limits were broadened to ensure the limits’
applicability to concentrations below those used to develop Table 6420:IV.

A response for compound to be measured, Using a pipet, prepare QC check samples at a concentration of
I amount of internal standard added to each extract, g, 100 g/L by adding 1.00 mL of 100 g/mL QC check sample
A response for internal standard, and concentrate to each of four 1-L portions reagent water. Analyze
V volume of water extracted, L. check samples according to the method of 6420B.5 and proceed
with the check described in Sections 6200A.5a1) and 2). Use
b. Derivatization and ECD/GC analysis: To determine con- acceptance criteria given in Table 6420:III.
centration of individual compounds in the sample, use the equa- c. Analyses of laboratory-fortified samples: On an ongoing
tion: basis, make known additions to at least 10% of the samples from
each sample site being monitored. For laboratories analyzing one
(A) (V ) (B) (D) to ten samples per month, analyze at least one such sample with
Concentration, g/L a known addition per month. Use the procedure detailed in
(V ) (V ) (C) (E)
Sections 6200A.5c7) and 8), but use an addition of 100 g/L
rather than 20 g/L and compare percent recovery for each
where:
compound with the corresponding QC acceptance criteria found
A mass of underivatized phenol represented by area of peak in Table 6420:III. If the known addition was at a concentration
in sample chromatogram, determined from calibration curve 100 g/L, use either the QC acceptance criteria in Table
in 6420B.5c4), ng, 6420:III or optional QC acceptance criteria calculated for the
V total volume of column eluate or combined fractions from specific addition concentration based on the equations in Table
which V was taken, L, 6420:IV.
B total volume of hexane added in 6420B.5c1), mL, d. Quality-control check standard analysis: If analysis of any
D total volume of 2-propanol extract before derivatization, compound fails to meet the acceptance criteria for recovery,
mL, prepare and analyze a QC check standard containing each com-
V volume of eluate injected, L, pound that failed. NOTE: The frequency for the required analysis
V volume of water extracted in 6420B.5a, mL,
of a QC check standard will depend on the number of com-
C volume of hexane sample solution added to cleanup column
pounds being tested for simultaneously, the complexity of the
in 6420B.5c2), mL, and
E volume of 2-propanol extract carried through derivatization
sample matrix, and the performance of the laboratory.
in 6420B.5c1), mL. Prepare the QC check standard by adding 1.0 mL of QC check
sample concentrate to 1 L reagent water and proceed as in
Report results in g/L without correction for recovery. Report Section 6200A.5a3) using Table 6420:III.
QC data with sample results. e. Bias assessment and records: Assess method bias and
maintain records as directed in Section 6410B.7e.
7. Quality Control

a. Quality control program: See Section 6200A.5. 8. Precision and Bias

b. Initial quality control: To establish the ability to generate
data with acceptable bias and precision, perform the following This method was tested by 20 laboratories using reagent
operations: water, drinking water, surface water, and three industrial

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 PHENOLS (6420)/Liquid–Liquid Extraction GC/MS Method

TABLE 6420:IV. METHOD BIAS AND PRECISION AS FUNCTIONS OF CONCENTRATION*

Bias, as Single-Analyst Overall
Recovery, X Precision, s Precision, S
Compound g/L g/L g/L

4-Chloro-3-methylphenol 0.87C 1.97 0.11X 0.21 0.16X 1.41

2-Chlorophenol 0.83C 0.84 0.18X 0.20 0.21X 0.75
2,4-Dichlorophenol 0.81C 0.48 0.17X 0.02 0.18X 0.62
2,4-Dimethylphenol 0.62C 1.64 0.30X 0.89 0.25X 0.48
2-Methyl-4,6-dinitrophenol 0.84C 1.01 0.15X 1.25 0.19X 5.85
2,4-Dinitrophenol 0.80C 1.58 0.27X 1.15 0.29X 4.51
2-Nitrophenol 0.81C 0.76 0.15X 0.44 0.14X 3.84
4-Nitrophenol 0.46C 0.18 0.17X 2.43 0.19X 4.79
Pentachlorophenol 0.83C 2.07 0.22X 0.58 0.23X 0.57
Phenol 0.43C 0.11 0.20X 0.88 0.17X 0.77
2,4,6-Trichlorophenol 0.86C 0.40 0.10X 0.53 0.13X 2.40
*X expected recovery for one or more measurements of a sample containing a concentration of C,
s expected single-analyst standard deviation of measurements at an average concentration found of X,
S expected interlaboratory standard deviation of measurements at an average concentration found of X,
C true value for the concentration, and,
X average recovery found for measurements of samples containing a concentration of C.

wastewaters with known additions at six concentrations over 3. KAWAHARA, F.K. 1968. Microdetermination of derivatives of phenols
the range 12 to 450 g/L. Single-operator precision, overall and mercaptans by means of electron capture gas chromatography.
precision, and method bias were found to be related directly Anal. Chem. 40:100.
to compound concentration and essentially independent of 4. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1984. Definition and pro-
sample matrix. Linear equations describing these relation- cedure for the determination of the method detection limit. 40 CFR
ships for a flame ionization detector are presented in Table Part 136, Appendix B. Fed. Reg. 49, No. 209.
6420:IV. 5. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1984. Development of
detection limits, EPA Method 604, Phenols; Special letter report for
EPA Contract 68-03-2625. Environmental Monitoring and Support
9. References Lab., Cincinnati, Ohio.
6. BURKE, J.A. 1965. Gas chromatography for pesticide residue analysis;
1. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1984. Method 604: Phe- some practical aspects. J. Assoc. Offic. Anal. Chem. 48:1037.
nols. 40 CFR Part 136, 43290; Fed. Reg. 49, No. 209. 7. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1984. EPA Method Study
2. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1984. Determination of phenols 14, Method 604 —Phenols; EPA-600/4-84-044. National Technical
in industrial and municipal wastewaters; Final rep. EPA Contract 68-03- Information Serv., PB84-196211, Springfield, Va.
2625. Environmental Monitoring and Support Lab., Cincinnati, Ohio.

6420 C. Liquid–Liquid Extraction Gas Chromatographic/Mass Spectrometric Method

See Section 6410B.

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