ASTM D4458-94(1999)

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An American National Standard
Designation:D 4458–94 (Reapproved 1999)
Standard Test Method for
Chloride Ions in Brackish Water, Seawater, and Brines
This standard is issued under the fixed designation D 4458; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope chromate precipitate. The end point is the appearance of the
first permanent orange color.
1.1 This test method is applicable to the measurement of
4.2 This test method is suitable for analyzing solutions with
chloride in highly mineralized waters such as oil field brines,
a pH between 6.0 and 8.5.
seawater, and brackish water. The test method is based upon
the titration of chloride with silver nitrate, using a visual
5. Significance and Use
indicator.
5.1 Chloride is present in virtually all oil field brines,
1.2 Samples containing from 10 to 150 mg of chloride can
seawaters, and many waste waters. Identification of the origin
be analyzed by this test method. These levels are achieved by
of the water and selection of its disposal method may be based
dilution as described in the test method.
upon the chloride content. The chloride content is also used to
1.3 Itistheuser’sresponsibilitytoassurethevalidityofthe
estimate the resistivity of formation waters and to differentiate
method for untested types of water.
between subsurface formations.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
6. Interferences
responsibility of the user of this standard to establish appro-
6.1 Sulfide, bromide, iodide, thiocyanate, cyanide, phos-
priate safety and health practices and determine the applica-
phate, sulfite, carbonate, hydroxide, and iron interfere in this
bility of regulatory limitations prior to use.
test method. Sulfide, sulfite, and thiosulfate can be removed
with a peroxide treatment, but usually no attempt is made to
2. Referenced Documents
removebromideandiodidebecausetheyareusuallypresentin
2.1 ASTM Standards:
3 insignificant quantities compared to chloride. If necessary, the
D 1129 Terminology Relating to Water
pH can be raised and the hydroxides of several metals,
D 1193 Specification for Reagent Water
including iron, can be filtered off. Iron, barium, lead, and
D 2777 Practice for Determination of Precision and Bias of
bismuth precipitate with the chromate indicator.
Applicable Methods of Committee D-19 on Water
D 3370 Practices for Sampling Water from Closed Con-
7. Apparatus
duits
7.1 Laboratory Glassware.
3. Terminology 7.2 Buret, 25-mL capacity.
7.3 Hotplate.
3.1 Definitions—For definitions of terms used in this test
7.4 Magnetic Stirrer and TFE-fluorocarbon-Coated Stirring
method, refer to Terminology D1129.
Bars.
4. Summary of Test Method
8. Reagents
4.1 This test method is based upon the Mohr procedure for
8.1 Purity of Reagents—Reagent grade chemicals shall be
determiningchlorideionwithsilvernitrate.Thechloridereacts
used in all tests. Unless otherwise indicated, it is intended that
withthesilverionbeforeanysilverchromateforms,duetothe
allreagentsshallconformtothespecificationoftheCommittee
lower solubility of silver chloride. The potassium chromate
on Analytical Reagents of the American Chemical Society,
indicator reacts with excess silver ion to form a red silver
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
This test method is under the jurisdiction ofASTM Committee D-19 on Water
andisthedirectresponsibilityofSubcommiteeD19.05onInorganicConstituentsin
Water. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved Sept. 15, 1994. Published November 1994. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D4458–85. Last previous edition D4458–85 (1989). listed by the American Chemical Society, see Analar Standards for Laboratory
Hillebrand, W. F., Lundell, G. E. F., Bright, H.A., and Hoffman, J. I., Applied Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Inorganic Analysis, 2nd Ed., 732, John Wiley& Sons, Inc., New York, NY, 1953. and National Formulary,U.S.PharmaceuticalConvention,Inc.(USPC),Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4458–94 (1999)
TABLE 1 Aliquot Size for Chloride Determination
sufficiently high purity to permit its use without lessening the
accuracy of the determination. Specific Gravity Sample Dilution Equivalent Aliquot, mL
8.2 Purity of Water—Unlessotherwiseindicated,references
1.000 to 1.010 None—Take 50 mL for 50
analysis
towatershallbeunderstoodtomeanreagentwaterconforming
1.010 to 1.025 None—Take 25 mL for 25
to Specification D1193, Type III.
analysis
8.3 Silver Nitrate Solution, Standard (equivalent to 5 mg
1.025 to 1.050 Dilute 25 mL to 100 mL, 12.5
−
take 50 mL
Cl /mL)—Dissolve23.9582gofAgNO inapproximately700
1.025 to 1.090 Dilute 25 mL to 100 mL, 6.25
mL of water.Add 1 drop concentrated nitric acid (HNO ) and
take 25 mL
dilute to 1 L in a volumetric flask. The HNO will eliminate
1.090 to 1.120 Dilute 25 mL to 500 mL, 1.25
take 25 mL
any precipitation of silver hydroxide which would change the
1.120 to 1.150 Dilute 25 mL to 1000 0.625
concentration. Standardize against sodium chloride (NaCl) by
mL, take 25 mL
the procedure described in 8.4. Store in an amber-brown bottle
to protect the solutio
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