ASTM D1783-01(2007)
(Test Method)Standard Test Methods for Phenolic Compounds in Water
Standard Test Methods for Phenolic Compounds in Water
SIGNIFICANCE AND USE
Phenolic compounds are sometimes found in surface waters from natural and industrial sources. Their presence in streams and other waterways frequently will cause off flavor in fish tissue and other aquatic food.
Chlorination of waters containing phenols may produce chlorophenols that are odoriferous and objectionable tasting.
SCOPE
1.1 These test methods cover the preparation of the sample and the determination of the concentration of phenolic compounds in water. They are based on the color reaction of phenol (C6H5OH) with 4-aminoantipyrine and any color produced by the reaction of other phenolic compounds is reported as phenol. The concentration of phenol measured represents the minimum concentration of phenolic compounds present in the sample.
1.2 Phenolic compounds with a substituent in the para position may not quantitatively produce color with 4-aminoantipyrine. However, para substituents of phenol such as carboxyl, halogen, hydroxyl, methoxyl, or sulfonic acid groups do produce color with 4-aminoantipyrine.
1.3 These test methods address specific applications as follows:
RangeSections Test Method A—Chloroform Extraction
Test Method B—Direct Photometric0 to 100 μg/L
>0.1 mg/L
(100 μg/L)11 to 17
18 to 24
1.4 It is the users' responsibility to assure the validity of the standard test method for use in their particular matrix of interest.
1.5 This standard does not purport to address all the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements see 6.3.2 and 8.6.
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Designation: D1783 − 01(Reapproved 2007)
Standard Test Methods for
Phenolic Compounds in Water
This standard is issued under the fixed designation D1783; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D1192 Guide for Equipment for Sampling Water and Steam
in Closed Conduits (Withdrawn 2003)
1.1 These test methods cover the preparation of the sample
D1193 Specification for Reagent Water
and the determination of the concentration of phenolic com-
D1293 Test Methods for pH of Water
poundsinwater.Theyarebasedonthecolorreactionofphenol
D2777 Practice for Determination of Precision and Bias of
(C H OH) with 4-aminoantipyrine and any color produced by
6 5
Applicable Test Methods of Committee D19 on Water
thereactionofotherphenoliccompoundsisreportedasphenol.
D3370 Practices for Sampling Water from Closed Conduits
Theconcentrationofphenolmeasuredrepresentstheminimum
D5789 Practice for Writing Quality Control Specifications
concentration of phenolic compounds present in the sample.
for Standard Test Methods for Organic Constituents
1.2 Phenolic compounds with a substituent in the para
(Withdrawn 2002)
position may not quantitatively produce color with
D5810 Guide for Spiking into Aqueous Samples
4-aminoantipyrine. However, para substituents of phenol such
D5847 Practice for Writing Quality Control Specifications
as carboxyl, halogen, hydroxyl, methoxyl, or sulfonic acid
for Standard Test Methods for Water Analysis
groups do produce color with 4-aminoantipyrine.
3. Terminology
1.3 These test methods address specific applications as
follows:
3.1 Definitions—For definitions of terms used in these test
Range Sections methods, refer to Terminology D1129.
Test Method A—Chloroform Extraction 0 to 100 µg/L 11 to 17
3.2 Definitions of Terms Specific to This Standard:
Test Method B—Direct Photometric >0.1 mg/L 18 to 24
(100 µg/L)
3.2.1 phenolic compounds—hydroxy derivatives of benzene
and its condensed nuclei.
1.4 It is the users’ responsibility to assure the validity of the
standard test method for use in their particular matrix of
4. Summary of Test Methods
interest.
4.1 Test Method A and Test Method B are photometric
1.5 This standard does not purport to address all the safety
procedures based on the reaction of steam-distillable phenolic
concerns, if any, associated with its use. It is the responsibility
compounds with 4-aminoantipyrine.
of the user of this standard to establish appropriate safety and
health practices and determine the applicability of regulatory
4.2 Test Method A differs from Test Method B mainly in
limitations prior to use. For specific hazard statements see
thatthesampleisextractedwithchloroform,therebyproviding
6.3.2 and 8.6.
20-fold greater sensitivity.
4.3 Both procedures involve first separating the phenolic
2. Referenced Documents
compounds from the background matrix by distillation. Due to
2.1 ASTM Standards:
the differing solubilities and boiling points of the various
D1129 Terminology Relating to Water
phenolic compounds, each phenolic comes over in the distil-
lation at a different rate. Some phenolics will be substantially
transferred near the beginning of the distillation and some will
ThesetestmethodsareunderthejurisdictionofD19onWaterandarethedirect
not start to distill until near the end. For this reason some
responsibility of Subcommittee D19.06 on Methods for Analysis for Organic
phenolics may not have been quantitatively transferred to the
Substances in Water.
Current edition approved Dec. 1, 2007. Published January 2008. Originally
receiving flask when the specified volume of distillate has been
approved in 1960. Last previous edition approved in 2001 as D1783 – 01. DOI:
collected.
10.1520/D1783-01R07.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1783 − 01 (2007)
5. Significance and Use carbon tetrachloride (CCl ). Discard the oil- or tar-containing
layer. Remove any CCl remaining in the aqueous portion of
5.1 Phenolic compounds are sometimes found in surface
the sample by gentle heating.
waters from natural and industrial sources. Their presence in
streams and other waterways frequently will cause off flavor in
NOTE 1—The presence of CuSO is detrimental since it is converted to
cupric hydroxide (Cu(OH) ) by the NaOH. The Cu(OH) acts as an
fish tissue and other aquatic food.
2 2
oxidizing agent on phenols.
5.2 Chlorination of waters containing phenols may produce
chlorophenols that are odoriferous and objectionable tasting.
7. Apparatus
7.1 Buchner-Type Funnel with Coarse Fritted Disk—At
6. Interferences
least three funnels are needed for determination of phenolic
6.1 Common interferences that may occur in waters are compounds by Test Method A. Alternatively, standard glass
phenol-decomposing bacteria, reducing substances, and funnels and pre-fluted filter paper may be used. The funnel
strongly alkaline conditions of the sample. Provisions incorpo- paper must be large enough to hold5gof sodium sulfate.
rated in these test methods will minimize the effects of such These funnels are not used in Test Method B.
interferences.
7.2 Photometer—A spectrophotometer or filter photometer,
suitable for use at 460 nm (Test MethodA) or at 510 nm (Test
6.2 Treatment procedures required prior to the analysis for
removal of interfering compounds may result in the unavoid- Method B), and accommodating a cell that gives a light path of
1.0to10cmshallbeused.Thesizeofthecellusedwilldepend
able elimination or loss of certain types of phenolic com-
pounds.Itisbeyondthescopeofthesetestmethodstodescribe on the absorbance of the colored solutions being measured and
the characteristics of the photometer. In general, if the absor-
proceduresforovercomingallofthepossibleinterferencesthat
may be encountered in the test methods, particularly with bances are greater than 1.0 with a larger cell, the next smaller
size cell should be used.
highly contaminated water and industrial waste water. The
procedures used must be revised to meet the specific require-
7.3 Distillation Apparatus—A 1-L, heat-resistant, distilling
ments.
flaskattachedtoaGrahamcondenserbymeansofaglassjoint.
6.3 A few methods for eliminating certain interferences are
7.4 pH Meter—This apparatus shall conform to the require-
suggested. (See Section 8 for descriptions of reagents re-
ments in Test Methods D1293.
quired.)
6.3.1 Oxidizing Agents—If the sample smells of chlorine, or 8. Reagents
if iodine is liberated from potassium iodide on acidification of
8.1 Purity of Reagents—Reagent grade chemicals shall be
the sample, remove the oxidizing agents so indicated immedi-
used in all tests. Unless otherwise indicated, it is intended that
ately after sampling. The presence of oxidizing agents in the
all reagents shall conform to the specifications of the Commit-
sample may oxidize some or all of the phenols in a short time.
tee onAnalytical Reagents of theAmerican Chemical Society,
Ferrous sulfate or sodium arsenite solution may be added to 4
where such specifications are available. Other grades may be
destroy all of the oxidizing substances. Excess ferrous sulfate
used, provided it is first ascertained that the reagent is of
or sodium arsenite do not interfere since they are removed in
sufficiently high purity to permit its use without lessening the
the distillation procedure.
accuracy of the determination.
6.3.2 Sulfur Compounds—Compounds that liberate hydro-
8.2 Purity of Water—Unless otherwise indicated, references
gen sulfide (H S) or sulfur dioxide (SO ) on acidification may
2 2
to water shall be understood to mean water conforming to
interfere with the phenol determination. Treatment of the
Specification D1193Types I, II, III, or IV.Water used for these
acidified sample with copper sulfate usually eliminates such
test methods shall be free of phenolic compounds, residual
interferences.Acidify the sample with sulfuric acid (H SO )or
2 4
chlorine, and substances that interfere with the test. Water
hydrochloric acid (HCl) until just acid to methyl orange. Then
sufficiently free of phenolics can be generated by boiling the
add a sufficient quantity of copper sulfate (CuSO ) solution to
water for 20 min.
give a light blue color to the sample or until no more copper
sulfide (CuS) precipitate is formed. Excessive amounts of H S
8.3 Aminoantipyrine Solution (20 g/L)—Dissolve 2.0 g of
or SO may be removed from the acidified sample by a brief
4-aminoantipyrine in water and dilute to 100 mL. Prepare this
aeration treatment or stirring before the addition of the CuSO
reagent fresh as used.
solution or both. Warning: Acidification of certain samples
NOTE2—Themeltingpointofasatisfactorygradeof4-aminoantipyrine
mayproducevigorousevolutionofcarbondioxide(CO ),SO ,
2 2
ranges from 108.0 to 109.5°C.
H S, or other gases. Therefore, perform the acidification
8.4 Ammonium Chloride Solution (20 g/L)—Dissolve 20 g
cautiously and stir the samples during the process. Complete
of ammonium chloride (NH Cl) in water and dilute to 1 L.
the evolution of gases before the sample is stoppered.
6.3.3 Oils and Tars—If the sample contains oil or tar, some
phenolic compounds may be dissolved in these materials. An
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
alkaline extraction, in the absence of CuSO (Note 1), may be
listed by the American Chemical Society, see Analar Standards for Laboratory
used to eliminate the tar and oil. Adjust the pH of the sample
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
between 12 and 12.5 with sodium hydroxide (NaOH) pellets to
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
avoid extraction of the phenols. Extract the mixture with MD.
D1783 − 01 (2007)
8.5 Ammonium Hydroxide (NH OH) (sp gr 0.90)— TEST METHOD A—CHLOROFORM EXTRACTION
Concentrated ammonium hydroxide (NH OH).
11. Scope
8.6 Carbon Tetrachloride (CCl ). Warning: Phenol, carbon
11.1 This test method is generally applicable to water that
tetrachloride, and chloroform are potentially hazardous to
containslessthan100µg/L(0.1mg/L)ofphenoliccompounds.
human health. Avoid inhalation and direct contact. Use in a
Lower levels may be achieved with different instruments and
well-ventilated hood.
larger cells. Higher levels can be achieved by dilution.
8.7 Chloroform (CHCl ).
11.2 The lowest levels of analyte detection or accurate
8.8 Hydrochloric Acid (HCl) (sp gr 1.19)—Concentrated
quantitation are laboratory and sample matrix dependent and it
hydrochloric acid (HCl).
is up to the users of the test method to determine these levels
in their own situation.
8.9 Phenol Solution, Stock (1 mL = 10 mg phenol)—
Dissolve 1.00 g of phenol (C H OH) in freshly boiled and
11.3 This test method was tested on municipal wastewater
6 5
cooled water. Dilute to 1 000 mL with freshly boiled cooled
treatment plant influent and effluent, lake water, river water,
water. Prepare a fresh stock solution within 30 days of use.
and industrial treatment plant effluent. It is the user’s respon-
sibility to insure the validity of this test method for waters of
8.10 Phenol Solution, Intermediate (C H OH) (1 mL = 10
6 5
untested matrices.
µg phenol)—Dilute 10.0 mLof the stock solution to 1 000 mL
with freshly boiled and cooled water. Prepare this solution
12. Summary of Test Method
fresh on the day it is used.
12.1 This is a photometric test method, based on the
8.11 Phenol Solution, Standard (C H OH) (1 mL = 1.0 µg
6 5
reaction of steam-distillable phenolic compounds with
phenol)—Dilute 50 mLof the intermediate solution to 500 mL
4-aminoantipyrine at a pH of 10.0 6 0.2 in the presence of
with freshly boiled and cooled water. Prepare this solution
K Fe(CN) . The antipyrine dye formed is extracted from the
fresh within2hof use.
aqueous solution with chloroform and the absorbance is
measured at 460 nm. The concentration of phenolic com-
8.12 Potassium Ferricyanide Solution(K Fe(CN) ) (80
3 6
pounds in the sample is expressed in terms of micrograms per
g/L)—Dissolve8.0gof(K Fe(CN) )inwateranddiluteto100
3 6
litre of phenol C H OH.
mL. Filter if necessary. Prepare fresh weekly.
6 5
8.13 Sodium Bisulfate (NaHSO ).
13. Calibration
8.14 Sodium Sulfate (Na SO ), anhydrous and granular.
13.1 Prepare a series of 500-mL C H OH standards in
2 4
6 5
freshly boiled and cooled water containing 0, 5, 10, 20, 30, 40,
8.15 Sulfuric Acid (H SO ) (sp gr 1.84)—Concentrated
2 4
and 50 mL of standard C H OH solution (1 mL = 1.0 µg
6 5
sulfuric acid (H SO ).
2 4
C H OH). Use all solutions at room temperature.
6 5
8.16 Sulfuric Acid Solution (H SO ) (1+9)—Cautiously add
2 4
13.2 Developcolorintheseriesofstandardsandpreparethe
one volume of concentrated H SO to nine volumes of water
2 4
chloroform extracts in accordance with the procedures pre-
with continuous cooling and mixing. Solution will become hot.
scribed in Section 14 and 15.
9. Sampling 13.3 Measure the absorbance of each standard at 460 nm
against the reagent method blank (blank) as zero absorbance.
9.1 Collect the sample in accordance with Specification
Plot the absorbances against the corresponding weights in
D1192 and Practices D3370.
micrograms of phenol.
9.2 When samples are composited, chill the samples or the
NOTE 3—Make a separate calibration curve for each spectrophotometer
composite sample immediately and keep at a temperature of
or photoelectric colorimeter. Check each curve periodically to ensure
not more than 4°C during the compositing period. The collec-
reproducibility.
tion time for a single composite sample shall not exceed 4 h. If
14. Distillation Procedure
longer sampling periods are necessary, collect a series of
composite samples. Then preserve such composite samples in
14.1 Measure 500 mL of the sample into a beaker. Adjust
accordance with Section 10 until analyzed.
the pH of the sample to between pH 0.5 and 4 with H SO
2 4
solution (1+9). Use methyl orange indicator solution or a pH
10. Pr
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D 1783–91(Reapproved 1995) Designation:D1783–01 (Reapproved 2007)
Standard Test Methods for
Phenolic Compounds in Water
This standard is issued under the fixed designation D 1783; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
1.1 These test methods cover the preparation of the sample and the determination of the concentration of phenolic compounds
inwater.Theyarebasedonthecolorreactionofphenol(C H OH)with4-aminoantipyrineandanycolorproducedbythereaction
6 5
of other phenolic compounds is reported as phenol. The concentration of phenol measured represents the minimum concentration
of phenolic compounds present in the sample.
1.2 Phenolic compounds with a substituent in the para position may not quantitatively produce color with 4-aminoantipyrine.
However,parasubstituentsofphenolsuchascarboxyl,halogen,hydroxyl,methoxyl,orsulfonicacidgroupsdoproducecolorwith
4-aminoantipyrine.
1.3 These test methods address specific applications as follows:
Range Sections
Test Method A—Chloroform Extraction 0 to 100 µg/L 11 to 17
Test Method B—Direct Photometric >0.1 mg/L 18 to 24
(100 µg/L)
1.4 It is the users’ responsibility to assure the validity of the standard test method for use in their particular matrix of interest.
1.5 This standard does not purport to address all the safety concerns, if any, associated with its use. It is the responsibility of
the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements see Note 1 and Note 3For specific hazard statements see 6.3.2 and 8.6.
2. Referenced Documents
2.1 ASTM Standards:
D 1129 Terminology Relating to Water Water
D 1192Specification Guide for Equipment for Sampling Water and Steam in Closed Conduits Conduits
D 1193 Specification for Reagent Water Water
D 1293 Test Methods for pH of Water Water
D 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D–19D19 on Water Water
D 3370Practices for Sampling Water from Closed Conduits Practices for Sampling Water from Closed Conduits
D 5789 Practice for Writing Quality Control Specifications for Standard Test Methods for Organic Constituents
D 5810 Guide for Spiking into Aqueous Samples
D 5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions—For definitions of terms used in these test methods, refer to Terminology D 1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 phenolic compounds—hydroxy derivatives of benzene and its condensed nuclei.
4. Summary of Test Methods
4.1 Test MethodsMethod A and Test Method B are photometric procedures based on the reaction of steam-distillable phenolic
compounds with 4-aminoantipyrine.
These test methods are under the jurisdiction of D-19D19 on Water and are the direct responsibility of Subcommittee D19.06 on Methods for Analysis for Organic
Substances in Water.
Current edition approved Sept. 15, 1991.Dec. 1, 2007. Published December 1991.January 2008. Originally published as D1783–60T.approved in 1960. Last previous
edition D1783–87.approved in 2001 as D 1783 – 01.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1783–01 (2007)
4.2 TestMethodAdiffersfromTestMethodBmainlyinthatthesampleisextractedwithchloroform,therebyproviding20-fold
greater sensitivity.
4.3 Both procedures involve first separating the phenolic compounds from the background matrix by distillation. Due to the
differing solubilities and boiling points of the various phenolic compounds, each phenolic comes over in the distillation at a
differentrate.Somephenolicswillbesubstantiallytransferrednearthebeginningofthedistillationandsomewillnotstarttodistill
until near the end. For this reason some phenolics may not have been quantitatively transferred to the receiving flask when the
specified volume of distillate has been collected.
5. Significance and Use
5.1 Phenolic compounds are sometimes found in surface waters from natural and industrial sources. Their presence in streams
and other waterways frequently will cause off flavor in fish tissue and other aquatic food.
5.2 Chlorination of waters containing phenols may produce chlorophenols that are odoriferous and objectionable tasting.
6. Interferences
6.1 Common interferences that may occur in waters are phenol-decomposing bacteria, reducing substances, and strongly
alkaline conditions of the sample. Provisions incorporated in these test methods will minimize the effects of such interferences.
6.2 Treatment procedures required prior to the analysis for removal of interfering compounds may result in the unavoidable
elimination or loss of certain types of phenolic compounds. It is beyond the scope of these test methods to describe procedures
for overcoming all of the possible interferences that may be encountered in the test methods, particularly with highly contaminated
water and industrial waste water. The procedures used must be revised to meet the specific requirements.
6.3 A few methods for eliminating certain interferences are suggested. (See Section 8 for descriptions of reagents required.)
6.3.1 Oxidizing Agents— If the sample smells of chlorine, or if iodine is liberated from potassium iodide on acidification of the
sample, remove the oxidizing agents so indicated immediately after sampling.The presence of oxidizing agents in the sample may
oxidize some or all of the phenols in a short time. Ferrous sulfate or sodium arsenite solution may be added to destroy all of the
oxidizingsubstances.Excessferroussulfateorsodiumarsenitedonotinterferesincetheyareremovedinthedistillationprocedure.
6.3.2 Sulfur Compounds— Compounds that liberate hydrogen sulfide (H S) or sulfur dioxide (SO ) on acidification may
2 2
interfere with the phenol determination. Treatment of the acidified sample with copper sulfate usually eliminates such
interferences.Acidify the sample with sulfuric acid (H SO ) or hydrochloric acid (HCl) until just acid to methyl orange.Then add
2 4
a sufficient quantity of copper sulfate (CuSO ) solution to give a light blue color to the sample or until no more copper sulfide
(CuS) precipitate is formed. Excessive amounts of HSorSO may be removed from the acidified sample by a brief aeration
2 2
treatment or stirring before the addition of the CuSO solution or both.
NOTE1—Warning:solution or both. Warning: Acidification of certain samples may produce vigorous evolution of carbon dioxide (CO ), SO,H S,
2 2 2
or other gases. Therefore, perform the acidification cautiously and stir the samples during the process. Complete the evolution of gases before the sample
is stoppered.
6.3.3 Oils and Tars— If the sample contains oil or tar, some phenolic compounds may be dissolved in these materials. An
alkaline extraction, in the absence of CuSO (Note 1 (Note ), may be used to eliminate the tar and oil.Adjust the pH of the sample
between 12 and 12.5 with sodium hydroxide (NaOH) pellets to avoid extraction of the phenols. Extract the mixture with carbon
tetrachloride (CCl ). Discard the oil- or tar-containing layer. Remove any CCl remaining in the aqueous portion of the sample
4 4
by gentle heating.
NOTE2—The 1—The presence of CuSO is detrimental since it is converted to cupric hydroxide (Cu(OH) ) by the NaOH. The Cu(OH) acts as an
4 2 2
oxidizing agent on phenols.
7. Apparatus
7.1 Buchner-Type Funnel with Coarse Fritted Disk—Atleastthreefunnelsareneededfordeterminationofphenoliccompounds
by Test Method A. Alternatively, standard glass funnels and pre-fluted filter paper may be used. The funnel paper must be large
enough to hold5gof sodium sulfate. These funnels are not used in Test Method B.
7.2 Photometer—A spectrophotometer or filter photometer, suitable for use at 460 nm (Test Method A) or at 510 nm (Test
Method B), and accommodating a cell that gives a light path of 1.0 to 10 cm shall be used. The size of the cell used will depend
on the absorbance of the colored solutions being measured and the characteristics of the photometer. In general, if the absorbances
are greater than 1.0 with a larger cell, the next smaller size cell should be used.
7.3 Distillation Apparatus—A 1-L, heat-resistant, distilling flask attached to a Graham condenser by means of a glass joint.
7.4 pH Meter—This apparatus shall conform to the requirements in Test Methods D 1293.
8. Reagents Note3—Warning:Phenol, carbon tetrachloride, and chloroform are potentially hazardous to human health.
Caution—Avoid inhalation and direct contact. Use in a well-ventilated hood.
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
D1783–01 (2007)
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
8.2 Purity of Water— Unless otherwise indicated, references to water shall be understood to mean water conforming to
Specification D 1193 Types I, II, III, or IV. Water used for these test methods shall be free of phenolic compounds, residual
chlorine, and substances that interfere with the test. Water sufficiently free of phenolics can be generated by boiling the water for
20 minutes. min.
8.3 Aminoantipyrine Solution (20 g/L)—Dissolve2.0gof4-aminoantipyrineinwateranddiluteto100mL.Preparethisreagent
fresh as used.
NOTE4—The 2—The melting point of a satisfactory grade of 4-aminoantipyrine ranges from 108.0 to 109.5°C.
8.4 Ammonium Chloride Solution (20 g/L)—Dissolve 20 g of ammonium chloride (NH Cl) in water and dilute to 1 L.
8.5 Ammonium Hydroxide (NH OH) (sp gr 0.90)—Concentrated ammonium hydroxide (NH OH).
4 4
8.6 CarbonTetrachloride (CCl ).).Warning:Phenol,carbontetrachloride,andchloroformarepotentiallyhazardoustohuman
health. Avoid inhalation and direct contact. Use in a well-ventilated hood.
8.7 Chloroform (CHCl ).
8.8 Hydrochloric Acid (HCl) (sp gr 1.19)—Concentrated hydrochloric acid (HCl).
8.9 Phenol Solution, Stock (1 mL = 10 mg phenol)—Dissolve 1.00 g of phenol (C H OH) in freshly boiled and cooled water.
6 5
Dilute to 1 000 mL with freshly boiled cooled water. Prepare a fresh stock solution within 30 days of use.
8.10 Phenol Solution, Intermediate (C—(C H OH) (1 mL = 10 µg phenol)—Dilute 10.0 mLof the stock solution to 1 000 mL
6 5
with freshly boiled and cooled water. Prepare this solution fresh on the day it is used.
8.11 Phenol Solution, Standard (C—(C H OH) (1 mL = 1.0 µg phenol)—Dilute 50 mLof the intermediate solution to 500 mL
6 5
with freshly boiled and cooled water. Prepare this solution fresh within2hof use.
8.12 Potassium Ferricyanide Solution (K Fe(CN) ) (80 g/L)— Dissolve 8.0 g of (K Fe(CN) ) in water and dilute to 100 mL.
3 6 3 6
Filter if necessary. Prepare fresh weekly.
8.13 Sodium Bisulfate (NaHSO ).
8.14 Sodium Sulfate (Na SO ), anhydrous and granular.
2 4
8.15 Sulfuric Acid (H SO ) (sp gr 1.84)—Concentrated sulfuric acid (H SO ).
2 4 2 4
8.16 Sulfuric Acid Solution (H SO ) (1+9)—Cautiously add one volume of concentrated H SO to nine volumes of water with
2 4 2 4
continuous cooling and mixing. Solution will become hot.
9. Sampling
9.1 Collect the sample in accordance with Specification D 1192 and Practices D 3370.
9.2 When samples are composited, chill the samples or the composite sample immediately and keep at a temperature of not
more than 4°C during the compositing period. The collection time for a single composite sample shall not exceed 4 h. If longer
sampling periods are necessary, collect a series of composite samples. Then preserve such composite samples in accordance with
Section 10 until analyzed.
10. Preservation of Samples
10.1 Phenolic compounds in water are subject to both chemical and biochemical oxidation. Preserve samples within 4 h of
collection. Acidify the samples to a pH between 0.5 and 2.0 with H PO , HCl, H SO , or NaHSO .
3 4 2 4 4
10.2To10.2 To further minimize any changes in the phenolic content of the sample, keep it cold, preferably between 2°C and
4°C until analysis. The preserved samples should be in glass, not plastic bottles, and preferably analyzed within 28 days after
collection.
TEST METHODA—CHLOROFORM EXTRACTION
11. Scope
11.1 This test method is generally applicable to water that contains less than 100 µg/L (0.1 mg/L) of phenolic compounds.
Lower levels may be achieved with different instruments and larger cells. Higher levels can be achieved by dilution.
11.2 The lowest levels of analyte detection or accurate quantitation are laboratory and sample matrix dependent and it is up to
the users of the test method to determine these levels in their own situation.
11.3 This test method was tested on municipal wastewater treatment plant influent and effluent, lake water, river water, and
industrial treatment plant effluent. It is the user’s responsibility to insure the validity of this test method for waters of untested
matrices.
Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.
D1783–01 (2007)
12. Summary of Test Method
12.1 This is a photometric test method, based on the reaction of steam-distillable phenolic compounds with 4-aminoantipyrine
at a pH of 10.0 6 0.2 in the
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