ASTM D3634-99(2009)
(Test Method)Standard Test Method for Trace Chloride Ion in Engine Coolants
Standard Test Method for Trace Chloride Ion in Engine Coolants
SIGNIFICANCE AND USE
This test method permits the determination of very low levels of chloride ion in engine coolants containing the common corrosion inhibitor, mercaptobenzothiazole, or related mercaptans, which would normally interfere with the titration by also forming insoluble silver salts with silver nitrate.
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 standard. No other units of measurement are included in this standard.
1.5 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 7.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D3634 − 99(Reapproved 2009)
Standard Test Method for
Trace Chloride Ion in Engine Coolants
This standard is issued under the fixed designation D3634; 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 3. Summary of Test Method
3.1 The sample is first treated at a pH of 12 to 13 with
1.1 This test method covers the determination of chloride
aqueous hydrogen peroxide to oxidize the mercaptobenzothi-
ion in engine coolants in the range from 5 to 200 ppm in the
azoletosoluble,noninterferingsulfonate.Thetreatedsampleis
presence of up to 0.6 weight % mercaptobenzothiazole.
dissolved in glacial acetic acid and titrated potentiometrically
1.2 Other materials that react with silver ion will interfere.
with dilute standard silver nitrate solution. Since the solubility
1.3 Chloride in engine coolants containing an aryltriazole of silver chloride in this system is sufficient to prevent
instead of mercaptobenzothiazole can be determined directly obtaining a suitable inflection at the very low limit of the test
by this test method without pretreatment with hydrogen per- method, some chloride is deliberately added to the glacial
oxide. acetic acid solvent and then corrected for by a blank titration.
1.4 The values stated in SI units are to be regarded as
4. Significance and Use
standard. No other units of measurement are included in this
4.1 This test method permits the determination of very low
standard.
levels of chloride ion in engine coolants containing the
1.5 This standard does not purport to address all of the
commoncorrosioninhibitor,mercaptobenzothiazole,orrelated
safety concerns, if any, associated with its use. It is the
mercaptans, which would normally interfere with the titration
responsibility of the user of this standard to establish appro-
by also forming insoluble silver salts with silver nitrate.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazards
5. Apparatus
statements are given in Section 7.
5.1 Manual Titrations:
5.1.1 pH Meter—An expanded scale pH meter which can be
2. Referenced Documents
read to 1 or 2 mV is desirable but not required. A silver billet
4 5
2.1 ASTM Standards:
indicator electrode and glass reference electrode are used for
D1176 Practice for Sampling and Preparing Aqueous Solu-
the chloride titration. The silver electrode should be polished
tions of Engine Coolants orAntirusts forTesting Purposes
occasionally with fine steel wool or scouring powder and
D1193 Specification for Reagent Water
thoroughly rinsed.
E200 Practice for Preparation, Standardization, and Storage
5.1.2 Buret, 10-mL, micro, Class A, calibrated in 0.02-mL
of Standard and Reagent Solutions for ChemicalAnalysis
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 Related Fluids and is the direct responsibility of Subcommittee
D15.04 on Chemical Properties. ThesolesourceofsupplyoftheSilverBilletElectrodeknowntothecommittee
Current edition approved Nov. 1, 2009. Published December 2009. Originally atthistimeisFisherScientific(www.fishersci.com,CatalogNo.13-620-122).Ifyou
´1
approved in 1977. Last previous edition approved in 2005 as D3634 – 99(2005) . are aware of alternative suppliers, please provide this information to ASTM
DOI: 10.1520/D3634-99R09. International Headquarters. Your comments will receive careful consideration at a
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 (2009)
5.3 Pipets, 10, 20, and 100-mL, Class A. 7. Hazards
5.4 Flask, Erlenmeyer, 250 mL, with a 24/40 standard taper, 7.1 Chromic Acid—Highly toxic; cancer suspect agent;
corrosive; avoid skin contact.
female ground glass joint.
5.5 Condenser—Thecondensershallbeofthewater-cooled, 7.2 Acetone—Extremely flammable; harmful if swallowed
or inhaled; causes irritation.
reflux, glass-tube type, having a condenser jacket approxi-
mately 200 mm in length. The bottom end of the condenser
7.3 Acetic Acid, Glacial—Poison,causessevereburns;com-
shall have a 24/40 male ground glass joint to match the
bustible; harmful if swallowed or inhaled.
Erlenmeyer flask.
7.4 Hydrogen Peroxide Solution—Strong oxidizer; contact
5.6 Flask, volumetric, 200 mL, Class A.
withothermaterialmaycausefire;causessevereburns.Donot
tightlystoppercontainers.Forfurtherdetails,seeMCAChemi-
NOTE 1—All glassware should be thoroughly cleaned and reserved for
cal Safety Data Sheet SD-53.
use in this test method. Great care must be exercised to avoid contami-
nation. Glassware should be cleaned with chromic acid (Warning —See
7.5 Silver Nitrate—Maybefatalifswallowed;causessevere
7.1.) cleaning solution, then thoroughly rinsed with water, then with
burns.
acetone (Warning—See 7.2.), and dried.
7.6 Sodium Hydroxide Solution—Causes severe burns to
6. Reagents and Materials
skin and eyes.
6.1 Purity of Reagents—Reagent grade chemicals shall be
8. Sampling
used in all tests. U
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