ASTM D3634-99e1

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 of 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.
1.5 This standard does not purport to address all of the safety problems, 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

• Status: Historical
• Publication Date: 09-May-1999
• ICS: 71.100.45 - Refrigerants and antifreezes
• Technical Committee: D15 - Engine Coolants and Related Fluids
• Drafting Committee: D15.04 - Chemical Properties

Relations

• Replaced By: ASTM D3634-99(2005) - Standard Test Method for Trace Chloride Ion in Engine Coolants
• Effective Date: 01-Oct-2005
• Referred By: ASTM D7518-20 - Standard Specification for 1,3 Propanediol (PDO) Base Engine Coolant for Automobile and Light-Duty Service
• Effective Date: 10-May-1999
• Referred By: ASTM E1177-23 - Standard Specification for Engine Coolant Grade Glycol
• Effective Date: 10-May-1999
• Referred By: ASTM D7388-23 - Standard Specification for Engine Coolant Grade 1,3-Propanediol (PDO)
• Effective Date: 10-May-1999
• Referred By: ASTM D8085-17 - Standard Specification for Non-Aqueous Engine Coolant for Automobile and Light-Duty Service
• Effective Date: 10-May-1999
• Referred By: ASTM D3585-08(2020) - Standard Specification for ASTM Reference Fluid for Coolant Tests
• Effective Date: 10-May-1999
• Referred By: ASTM D7714-11(2021) - Standard Specification for Glycerin Base Engine Coolant for Automobile and Light-Duty Service
• Effective Date: 10-May-1999
• Referred By: ASTM D4985-10(2023) - Standard Specification for Low Silicate Ethylene Glycol Base Engine Coolant for Heavy Duty Engines Requiring a Pre-Charge of Supplemental Coolant Additive (SCA)
• Effective Date: 10-May-1999
• Referred By: ASTM D7640-16(2021) - Standard Specification for Engine Coolant Grade Glycerin
• Effective Date: 10-May-1999
• Referred By: ASTM D3306-21 - Standard Specification for Glycol Base Engine Coolant for Automobile and Light-Duty Service
• Effective Date: 10-May-1999
• Referred By: ASTM D5752-10(2017) - Standard Specification for Supplemental Coolant Additives (SCAs) for Use in Precharging Coolants for Heavy-Duty Engines
• Effective Date: 10-May-1999
• Referred By: ASTM D7713-18 - Standard Specification for Aqueous Engine Coolant Grade Glycol (53 % by Volume Nominal)
• Effective Date: 10-May-1999

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
e1
Designation:D3634–99
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.
e NOTE—Editorial changes were made in November 2001.
1. Scope zole to soluble, noninterfering sulfonate. The treated sample is
dissolved in glacial acetic acid and titrated potentiometrically
1.1 This test method covers the determination of chloride
with dilute standard silver nitrate solution. Since the solubility
ion in engine coolants in the range from 5 to 200 ppm in the
of silver chloride in this system is sufficient to prevent
presence of up to 0.6 weight % mercaptobenzothiazole.
obtaining a suitable inflection at the very low limit of the test
1.2 Other materials that react with silver ion will interfere.
method, some chloride is deliberately added to the glacial
1.3 Chloride in engine coolants containing an aryltriazole
acetic acid solvent and then corrected for by a blank titration.
instead of mercaptobenzothiazole can be determined directly
by this test method without pretreatment with hydrogen per-
4. Significance and Use
oxide.
4.1 This test method permits the determination of very low
1.4 The values stated in SI units are to be regarded as the
levels of chloride ion in engine coolants containing the
standard.
commoncorrosioninhibitor,mercaptobenzothiazole,orrelated
1.5 This standard does not purport to address all of the
mercaptans, which would normally interfere with the titration
safety concerns, if any, associated with its use. It is the
by also forming insoluble silver salts with silver nitrate.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use. Specific hazards
5.1 Manual Titrations:
statements are given in Section 7.
5.1.1 pH Meter — An expanded scale pH meter which can
2. Referenced Documents bereadto1or2mVisdesirablebutnotrequired.Asilverbillet
5 6
indicator electrode and glass reference electrode are used for
2.1 ASTM Standards:
the chloride titration. The silver electrode should be polished
D 1176 Test Method for Sampling and Preparing Aqueous
occasionally with fine steel wool or scouring powder and
Solutions of Engine Coolants or Antirusts for Testing
2 thoroughly rinsed.
Purposes
3 5.1.2 Buret, 10-mL, micro, Class A, calibrated in 0.02-mL
D 1193 Specification for Reagent Water
divisions.
E 200 Practice for Preparation, Standardization, and Stor-
5.1.3 Beakers, electrolytic, 250-mL tall form.
age of Standard and Reagent Solutions for Chemical
2 5.2 Automatic Titrators are satisfactory for this test method,
Analysis
4 provided they exhibit resolution and accuracy equivalent to
2.2 Manufacturing Chemists Association Document:
that specified for manual titrations.
MCA Chemical Safety Data Sheet SD-53
5.3 Pipets, 10, 20, and 100-mL, Class A.
3. Summary of Test Method 5.4 Flask, Erlenmeyer,250mL,witha24/40standardtaper,
female ground glass joint.
3.1 The sample is first treated at a pH of 12 to 13 with
aqueous hydrogen peroxide to oxidize the mercaptobenzothia-
This test method is under the jurisidiction ofASTM Committee D15 on Engine
Coolants and is the direct responsibility of Subcommittee D15.04 on Chemical
Properties.
Current edition approved May 10, 1999. Published August 1999. Originally The1993–1994FisherScientificCompanyCatalognumberfortheSilverBillet
published as D 3634 – 77. Last previous edition D 3634 – 93. Electrode is: 13-620-122 and it is available from 10700 Rockley Road, P.O. Box
Annual Book of ASTM Standards, Vol 15.05. 1307, Houston, TX 77251.
3 6
Annual Book of ASTM Standards, Vol 11.01. The 1993-1994 Fisher Scientific Company Catalog number for the reference
Available from the Manufacturing Chemists Association, 1825 Connecticut electrode is 13-620-216 and it is available from 10700 Rockley Road, P.O. Box
Ave., Washington, DC 20009. 1307, Houston, TX 77251.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3634
5.5 Condenser—The condenser shall be of the water- 7.3 Acetic Acid, Glacial—Poison, causes severe burns;
cooled, reflux, glass-tube type, having a condenser jacket combustible; harmful if swallowed or inhaled.
approximately 200 mm in length. The bottom end of the 7.4 Hydrogen Peroxide Solution—Strong oxidizer; contact
condenser shall have a 24/40 male ground glass joint to match with other material may cause fire; causes severe burns. Do not
the Erlenmeyer flask. tightlystoppercontainers.Forfurtherdetails,seeMCAChemi-
5.6 Flask, volumetric, 200 mL, Class A. cal Safety Data Sheet SD-53.
7.5 Silver Nitrate— May be fatal if swallowed; causes
NOTE 1—All glassware should be thoroughly cleaned and reserved for
severe burns.
use in this test method. Great care must be exercised to avoid contami-
7.6 Sodium Hydroxide Solution—Causes severe burns to
nation. Glassware should be cleaned with chromic acid (Warning—See
7.1.) cleaning solution, then thoroughly rinsed with water, then with skin and eyes.
acetone (Warning—See 7.2.), and dried.
8. Sampling
6. Reagents and Materials
8.1 Sampling of engine coolant should be carried out in
6.1 Purity of Reagents— Reagent grade chemicals shall be
accordance with Method D 1176.
used in all tests. Unless otherwise indicated, it is intended that
9. Preparation of Titration Solvent
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
9.1 Determine a titration blank on a full 5-lb (2.3-kg) bottle
where such specifications are available. Other grades may be
of glacial acetic acid b
...