ASTM D3634-99(2005)
(Test Method)Standard Test Method for Trace Chloride Ion in Engine Coolants
Standard Test Method for Trace Chloride Ion in Engine Coolants
SCOPE
1.1 This test method covers the determination of chloride ion in engine coolants in the range from 5 to 200 ppm in the presence of up to 0.6 weight % mercaptobenzothiazole.
1.2 Other materials that react with silver ion will interfere.
1.3 Chloride in engine coolants containing an aryltriazole instead of mercaptobenzothiazole can be determined directly by this test method without pretreatment with hydrogen peroxide.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
This standard does not purport to address all of 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. Specific hazards statements are given in Section .
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3634–99 (Reapproved 2005)
Standard Test Method for
Trace Chloride Ion in Engine Coolants
This standard is issued under the fixed designation D 3634; 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 3. Summary of Test Method
1.1 This test method covers the determination of chloride 3.1 The sample is first treated at a pH of 12 to 13 with
ion in engine coolants in the range from 5 to 200 ppm in the aqueous hydrogen peroxide to oxidize the mercaptobenzothia-
presence of up to 0.6 weight % mercaptobenzothiazole. zole to soluble, noninterfering sulfonate. The treated sample is
1.2 Other materials that react with silver ion will interfere. dissolved in glacial acetic acid and titrated potentiometrically
1.3 Chloride in engine coolants containing an aryltriazole with dilute standard silver nitrate solution. Since the solubility
instead of mercaptobenzothiazole can be determined directly of silver chloride in this system is sufficient to prevent
by this test method without pretreatment with hydrogen per- obtaining a suitable inflection at the very low limit of the test
oxide. method, some chloride is deliberately added to the glacial
1.4 The values stated in SI units are to be regarded as acetic acid solvent and then corrected for by a blank titration.
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 This test method permits the determination of very low
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the levels of chloride ion in engine coolants containing the
commoncorrosioninhibitor,mercaptobenzothiazole,orrelated
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- mercaptans, which would normally interfere with the titration
by also forming insoluble silver salts with silver nitrate.
bility of regulatory limitations prior to use. Specific hazards
statements are given in Section 7.
5. Apparatus
2. Referenced Documents
5.1 Manual Titrations:
5.1.1 pH Meter—AnexpandedscalepHmeterwhichcanbe
2.1 ASTM Standards:
D 1176 Practice for Sampling and Preparing Aqueous So- read to 1 or 2 mV is desirable but not required. A silver billet
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indicator electrode and glass reference electrode are used for
lutions of Engine Coolants or Antirusts for Testing Pur-
poses the chloride titration. The silver electrode should be polished
occasionally with fine steel wool or scouring powder and
D 1193 Specification for Reagent Water
E 200 Practice for Preparation, Standardization, and Stor- thoroughly rinsed.
5.1.2 Buret, 10-mL, micro, Class A, calibrated in 0.02-mL
age of Standard and Reagent Solutions for Chemical
Analysis divisions.
5.1.3 Beakers, electrolytic, 250-mL tall form.
2.2 Manufacturing Chemists Association Document:
MCA Chemical Safety Data Sheet SD-53 5.2 Automatic Titrators are satisfactory for this test method,
provided they exhibit resolution and accuracy equivalent to
that specified for manual titrations.
This test method is under the jurisidiction ofASTM Committee D15 on Engine
Coolants and is the direct responsibility of Subcommittee D15.04 on Chemical ThesolesourceofsupplyoftheSilverBilletElectrodeknowntothecommittee
Properties. atthistimeisFisherScientific(www.fishersci.com,CatalogNo.13-620-122).Ifyou
Current edition approved Oct. 1, 2005. Published November 2005. Originally are aware of alternative suppliers, please provide this information to ASTM
e1
approved in 1977. Last previous edition approved in 1999 as D 3634 – 99 . International Headquarters. Your comments will receive careful consideration at a
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or meeting of the responsible technical committee, which you may attend.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM The sole source of supply of the reference electrode known to the committee at
Standards volume information, refer to the standard’s Document Summary page on this time is Fisher Scientific (www.fishersci.com, Catalog No. 13-620-216). If you
the ASTM website. are aware of alternative suppliers, please provide this information to ASTM
Available from the Manufacturing Chemists Association, 1825 Connecticut International Headquarters. Your comments will receive careful consideration at a
Ave., Washington, DC 20009. meeting of the responsible technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3634–99 (2005)
5.3 Pipets, 10, 20, and 100-mL, Class A. 7.2 Acetone—Extremely flammable; harmful if swallowed
5.4 Flask, Erlenmeyer,250mL,witha24/40standardtaper, or inhaled; causes irritation.
female ground glass joint. 7.3 Acetic Acid, Glacial—Poison, causes severe burns;
5.5 Condenser—The condenser shall be of the water- combustible; harmful if swallowed or inhaled.
cooled, reflux, glass-tube type, having a condenser jacket 7.4 Hydrogen Peroxide Solution—Strong oxidizer; contact
approximately 200 mm in length. The bottom end of the withothermaterialmaycausefire;causessevereburns.Donot
condenser shall have a 24/40 male ground glass joint to match tightlystoppercontainers.Forfurtherdetails,seeMCAChemi-
the Erlenmeyer flask. cal Safety Data Sheet SD-53.
5.6 Flask, volumetric, 200 mL, Class A. 7.5 Silver Nitrate—May be fatal if swallowed; causes se-
vere burns.
NOTE 1—All glassware should be thoroughly cleaned and reserved for
7.6 Sodium Hydroxide Solution—Causes severe burns to
use in this test method. Great care must be exercised to avoid contami-
skin and eyes.
nation. Glassware should be cleaned with chromic acid (Warning—See
7.1.) cleaning solution, then thoroughly rinsed with water, then with
8. Sampling
acetone (Warning—See 7.2.), and dried.
8.1 Sampling of engine coolant should be carried out in
6. Reagents and Materials
accordance with Practice D 1176.
6.1 Purity of Reagents—Reagent grade
...
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