ASTM D1783-01(2012)e1
(Test Method)Standard Test Methods for Phenolic Compounds in Water
Standard Test Methods for Phenolic Compounds in Water
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.
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:
Range
Sections
Test Method A—Chloroform Extraction
Test Method B—Direct Photometric
0 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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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´1
Designation: D1783 − 01 (Reapproved 2012)
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 U.S. Department of Defense.
ε NOTE—Editorial corrections were made throughout in January 2015.
1. Scope 2. Referenced Documents
1.1 These test methods cover the preparation of the sample 2.1 ASTM Standards:
and the determination of the concentration of phenolic com- D1129 Terminology Relating to Water
poundsinwater.Theyarebasedonthecolorreactionofphenol D1192 Guide for Equipment for Sampling Water and Steam
(C H OH) with 4-aminoantipyrine and any color produced by in Closed Conduits (Withdrawn 2003)
6 5
thereactionofotherphenoliccompoundsisreportedasphenol. D1193 Specification for Reagent Water
Theconcentrationofphenolmeasuredrepresentstheminimum D1293 Test Methods for pH of Water
concentration of phenolic compounds present in the sample. D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.2 Phenolic compounds with a substituent in the para
D3370 Practices for Sampling Water from Closed Conduits
position may not quantitatively produce color with
D5789 Practice for Writing Quality Control Specifications
4-aminoantipyrine. However, para substituents of phenol such
for Standard Test Methods for Organic Constituents
as carboxyl, halogen, hydroxyl, methoxyl, or sulfonic acid
(Withdrawn 2002)
groups do produce color with 4-aminoantipyrine.
D5810 Guide for Spiking into Aqueous Samples
1.3 These test methods address specific applications as
D5847 Practice for Writing Quality Control Specifications
follows:
for Standard Test Methods for Water Analysis
Range Sections
Test Method A—Chloroform Extraction 0 to 100 µg/L 11 to 17
3. Terminology
Test Method B—Direct Photometric >0.1 mg/L 18 to 24
(100 µg/L)
3.1 Definitions—For definitions of terms used in these test
methods, refer to Terminology D1129.
1.4 It is the users’ responsibility to assure the validity of the
3.2 Definitions of Terms Specific to This Standard:
standard test method for use in their particular matrix of
3.2.1 phenolic compounds—hydroxy derivatives of benzene
interest.
and its condensed nuclei.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Methods
responsibility of the user of this standard to establish appro-
4.1 Test Method A and Test Method B are photometric
priate safety, health, and environmental practices and deter-
procedures based on the reaction of steam-distillable phenolic
mine the applicability of regulatory limitations prior to use.
compounds with 4-aminoantipyrine.
For specific hazard statements see 6.3.2 and 8.6.
1.6 This international standard was developed in accor-
4.2 Test Method A differs from Test Method B mainly in
dance with internationally recognized principles on standard-
thatthesampleisextractedwithchloroform,therebyproviding
ization established in the Decision on Principles for the
20-fold greater sensitivity.
Development of International Standards, Guides and Recom-
4.3 Both procedures involve first separating the phenolic
mendations issued by the World Trade Organization Technical
compounds from the background matrix by distillation. Due to
Barriers to Trade (TBT) Committee.
1 2
ThesetestmethodsareunderthejurisdictionofD19onWaterandarethedirect For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibility of Subcommittee D19.06 on Methods for Analysis for Organic contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Substances in Water. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 15, 2012. Published August 2012. Originally the ASTM website.
approved in 1960. Last previous edition approved in 2007 as D1783 – 01R07. DOI: The last approved version of this historical standard is referenced on
10.1520/D1783-01R12E01. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D1783 − 01 (2012)
the differing solubilities and boiling points of the various cautiously and stir the samples during the process. Complete
phenolic compounds, each phenolic comes over in the distil- the evolution of gases before the sample is stoppered.)
lation at a different rate. Some phenolics will be substantially 6.3.3 Oils and Tars—If the sample contains oil or tar, some
transferred near the beginning of the distillation and some will phenolic compounds may be dissolved in these materials. An
not start to distill until near the end. For this reason some alkaline extraction, in the absence of CuSO , may be used to
phenolics may not have been quantitatively transferred to the eliminate the tar and oil.Adjust the pH of the sample between
receivingflaskwhenthespecifiedvolumeofdistillatehasbeen 12 and 12.5 with sodium hydroxide (NaOH) pellets to avoid
collected. extraction of the phenols. Extract the mixture with carbon
tetrachloride (CCl ). Discard the oil- or tar-containing layer.
5. Significance and Use
Remove any CCl remaining in the aqueous portion of the
5.1 Phenolic compounds are sometimes found in surface
sample by gentle heating.
waters from natural and industrial sources. Their presence in
NOTE 1—The presence of CuSO is detrimental since it is converted to
streams and other waterways frequently will cause off flavor in
cupric hydroxide (Cu(OH) ) by the NaOH. The Cu(OH) acts as an
2 2
fish tissue and other aquatic food.
oxidizing agent on phenols.
5.2 Chlorination of waters containing phenols may produce
7. Apparatus
chlorophenols that are odoriferous and objectionable tasting.
7.1 Buchner-Type Funnel with Coarse Fritted Disk—At
6. Interferences
least three funnels are needed for determination of phenolic
compounds by Test Method A. Alternatively, standard glass
6.1 Common interferences that may occur in waters are
funnels and pre-fluted filter paper may be used. The funnel
phenol-decomposing bacteria, reducing substances, and
paper must be large enough to hold5gof sodium sulfate.
strongly alkaline conditions of the sample. Provisions incorpo-
These funnels are not used in Test Method B.
rated in these test methods will minimize the effects of such
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
Method B), and accommodating a cell that gives a light path of
removal of interfering compounds may result in the unavoid-
1.0to10cmshallbeused.Thesizeofthecellusedwilldepend
able elimination or loss of certain types of phenolic com-
on the absorbance of the colored solutions being measured and
pounds.Itisbeyondthescopeofthesetestmethodstodescribe
the characteristics of the photometer. In general, if the absor-
proceduresforovercomingallofthepossibleinterferencesthat
bances are greater than 1.0 with a larger cell, the next smaller
may be encountered in the test methods, particularly with
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.)
8. Reagents
6.3.1 Oxidizing Agents—If the sample smells of chlorine, or
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
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
or SO may be removed from the acidified sample by a brief
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
aeration treatment or stirring before the addition of the CuSO
listed by the American Chemical Society, see Analar Standards for Laboratory
solution or both. (Warning—Acidification of certain samples
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
mayproducevigorousevolutionofcarbondioxide(CO ),SO ,
2 2 and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
H S, or other gases. Therefore, perform the acidification MD.
´1
D1783 − 01 (2012)
8.3 Aminoantipyrine Solution (20 g/L)—Dissolve 2.0 g of 4 h of collection.Acidify the samples to a pH between 0.5 and
4-aminoantipyrine in water and dilute to 100 mL. Prepare this 2.0 with H PO , HCl, H SO , or NaHSO .
3 4 2 4 4
reagent fresh as used.
10.2 To further minimize any changes in the phenolic
contentofthesample,keepitcold,preferablybetween2°Cand
NOTE2—Themeltingpointofasatisfactorygradeof4-aminoantipyrine
ranges from 108.0 to 109.5°C.
4°C until analysis. The preserved samples should be in glass,
notplasticbottles,andpreferablyanalyzedwithin28daysafter
8.4 Ammonium Chloride Solution (20 g/L)—Dissolve 20 g
collection.
of ammonium chloride (NH Cl) in water and dilute to 1 L.
8.5 Ammonium Hydroxide (NH OH) (sp gr 0.90)—
4 TEST METHOD A—CHLOROFORM EXTRACTION
Concentrated ammonium hydroxide (NH OH).
11. Scope
8.6 Carbon Tetrachloride (CCl ). Warning—Phenol, car-
11.1 This test method is generally applicable to water that
bon 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
8.9 Phenol Solution, Stock (1 mL = 1.0 mg phenol)—
in their own situation.
Dissolve 1.00 g of phenol (C H OH) in freshly boiled and
6 5
11.3 This test method was tested on municipal wastewater
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-
8.10 Phenol Solution, Intermediate (C H OH) (1 mL = 10
6 5 sibility to insure the validity of this test method for waters of
µg phenol)—Dilute 10.0 mLof the stock solution to 1 000 mL
untested matrices.
with freshly boiled and cooled water. Prepare this solution
fresh on the day it is used. 12. Summary of Test Method
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
phenol)—Dilute 50 mLof the intermediate solution to 500 mL reaction of steam-distillable phenolic compounds with
4-aminoantipyrine at a pH of 10.0 6 0.2 in the presence of
with freshly boiled and cooled water. Prepare this solution
fresh within2hof use. K Fe(CN) . The antipyrine dye formed is extracted from the
3 6
aqueous solution with chloroform and the absorbance is
8.12 Potassium Ferricyanide Solution(K Fe(CN) ) (80
3 6
measured at 460 nm. The concentration of phenolic com-
g/L)—Dissolve8.0gof(K Fe(CN) )inwateranddiluteto100
3 6
pounds in the sample is expressed in terms of micrograms per
mL. Filter if necessary. Prepare fresh weekly.
litre of phenol C H OH.
6 5
8.13 Sodium Bisulfate (NaHSO ).
13. Calibration
8.14 Sodium Sulfate (Na SO ), anhydrous and granular.
2 4
13.1 Prepare a series of 500-mL C H OH standards in
6 5
8.15 Sulfuric Acid (H SO ) (sp gr 1.84)—Concentrated
2 4
freshly boiled and cooled water containing 0, 5, 10, 20, 30, 40,
sulfuric acid (H SO ).
2 4
and 50 mL of standard C H OH solution (1 mL = 1.0 µg
6 5
8.16 Sulfuric Acid Solution (H SO ) (1+9)—Cautiously add
2 4
C H OH). Use all solutions at room temperature.
6 5
one volume of concentrated H SO to nine volumes of water
2 4
13.2 Developcolorintheseriesofstandardsandpreparethe
with continuous cooling and mixing. Solution will become hot.
chloroform extracts in accordance with the procedures pre-
scribed in Section 14 and 15.
9. Sampling
13.3 Measure the absorbance of each standard at 460 nm
9.1 Collect the sample in accordance with Specification
against the reagent method blank (blank) as zero absorbance.
D1192 and Practices D3370.
Plot the absorbances against the corresponding weights in
9.2 When sampl
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D1783 − 01 (Reapproved 2012) D1783 − 01 (Reapproved 2012)
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 U.S. Department of Defense.
ε NOTE—Editorial corrections were made throughout in January 2015.
1. 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 (C H OH) with 4-aminoantipyrine and any color produced by the reaction
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, 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:
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 6.3.2 and 8.6.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1192 Guide for Equipment for Sampling Water and Steam in Closed Conduits (Withdrawn 2003)
D1193 Specification for Reagent Water
D1293 Test Methods for pH of Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D5789 Practice for Writing Quality Control Specifications for Standard Test Methods for Organic Constituents (Withdrawn
2002)
D5810 Guide for Spiking into Aqueous Samples
D5847 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 D1129.
3.2 Definitions of Terms Specific to This Standard:
These test methods are under the jurisdiction of D19 on Water and are the direct responsibility of Subcommittee D19.06 on Methods for Analysis for Organic Substances
in Water.
Current edition approved June 15, 2012. Published August 2012. Originally approved in 1960. Last previous edition approved in 2007 as D1783 – 01R07. DOI:
10.1520/D1783-01R12.10.1520/D1783-01R12E01.
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 ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D1783 − 01 (2012)
3.2.1 phenolic compounds—hydroxy derivatives of benzene and its condensed nuclei.
4. Summary of Test Methods
4.1 Test Method A and Test Method B are photometric procedures based on the reaction of steam-distillable phenolic
compounds with 4-aminoantipyrine.
4.2 Test Method A differs from Test Method B mainly in that the sample is extracted with chloroform, thereby providing 20-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
different rate. Some phenolics will be substantially transferred near the beginning of the distillation and some will not start to distill
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
oxidizing substances. Excess ferrous sulfate or sodium arsenite do not interfere since they are removed in the distillation procedure.
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 H S or SO 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. Warning:(Warning—Acidification of certain samples may
produce vigorous evolution of carbon dioxide (CO ), SO , H S, or other gases. Therefore, perform the acidification cautiously and
2 2 2
stir the samples during the process. Complete the evolution of gases before the sample is stoppered. Acidification of certain
samples may produce vigorous evolution of carbon dioxide (CO) ), SO , H S, or other gases. Therefore, perform the acidification
2 2 2
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 , 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 by gentle heating.
4 4
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 oxidizing
4 2 2
agent on phenols.
7. Apparatus
7.1 Buchner-Type Funnel with Coarse Fritted Disk—At least three funnels are needed for determination of phenolic compounds
by Test Method A. Alternatively, standard glass funnels and pre-fluted filter paper may be used. The funnel paper must be large
enough to hold 5 g of 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.
´1
D1783 − 01 (2012)
7.4 pH Meter—This apparatus shall conform to the requirements in Test Methods D1293.
8. Reagents
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
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 D1193 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 min.
8.3 Aminoantipyrine Solution (20 g/L)—Dissolve 2.0 g of 4-aminoantipyrine in water and dilute to 100 mL. Prepare this reagent
fresh as used.
NOTE 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 Carbon Tetrachloride (CCl ). Warning—Phenol, carbon tetrachloride, and chloroform are potentially hazardous to human
health. Avoid inhalation and direct contact. Use in a well-ventilated hood.Warning: Phenol, carbon tetrachloride, and chloroform
are potentially hazardous to human 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 = 10mL = 1.0 mg phenol)—Dissolve 1.00 g of phenol (C H OH) in freshly boiled and cooled
6 5
water. 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 H OH) (1 mL = 10 μg phenol)—Dilute 10.0 mL of the stock solution to 1 000 mL with
6 5
freshly boiled and cooled water. Prepare this solution fresh on the day it is used.
8.11 Phenol Solution, Standard (C H OH) (1 mL = 1.0 μg phenol)—Dilute 50 mL of the intermediate solution to 500 mL with
6 5
freshly boiled and cooled water. Prepare this solution fresh within 2 h of 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 D1192 and Practices D3370.
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
10.2 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.
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.
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D1783 − 01 (2012)
TEST METHOD A—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 wate
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