ASTM D5194-96
(Test Method)Standard Test Method for Trace Chloride in Liquid Aromatic Hydrocarbons
Standard Test Method for Trace Chloride in Liquid Aromatic Hydrocarbons
SCOPE
1.1 This test method covers the determination of total chloride (organic and inorganic) in liquid aromatic hydrocarbons and cyclohexane.
1.2 The test method is applicable to samples with chloride concentrations of 1 to 25 mg/kg.
1.3 Bromides and iodides, if present, will be calculated as chlorides.
1.4 Materials, such as styrene, that are polymerized by sodium biphenyl reagent cannot be analyzed by this test method.
1.5 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.
1.6 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. For a specific hazard statement, see Section 7.
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Designation: D 5194 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Trace Chloride in Liquid Aromatic Hydrocarbons
This standard is issued under the fixed designation D 5194; 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.
1. Scope Determine Conformance with Specifications
2.2 Other Documents:
1.1 This test method covers the determination of total
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
chloride (organic and inorganic) in liquid aromatic hydrocar-
1910.1200
bons and cyclohexane.
1.2 The test method is applicable to samples with chloride
3. Summary of Test Method
concentrations of 1 to 25 mg/kg.
3.1 A known amount of hydrocarbon sample is transferred
1.3 Bromides and iodides, if present, will be calculated as
into a separatory funnel containing toluene. Sodium biphenyl
chlorides.
reagent is added to convert organic halogens into inorganic
1.4 Materials, such as styrene, that are polymerized by
halides. The excess reagent is decomposed with water and the
sodium biphenyl reagent cannot be analyzed by this test
phases are separated. The aqueous phase is acidified, washed,
method.
and concentrated. Acetone is added and the solution is titrated
1.5 The following applies to all specified limits in this test
with silver nitrate solution.
method: for purposes of determining conformance with this
test method, an observed value or a calculated value shall be
4. Significance and Use
rounded off “to the nearest unit” in the last right-hand digit
4.1 Organic and inorganic chlorine compounds can have a
used in expressing the specification limit, in accordance with
deleterious effect on equipment and reactions in processes
the rounding-off method of Practice E 29.
involving aromatic hydrocarbons.
1.6 This standard does not purport to address all of the
4.2 Maximum chloride levels are often specified for process
safety concerns, if any, associated with its use. It is the
streams and for aromatic hydrocarbon products.
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. For a specific
5.1 Titrator, potentiometric, recording, + 2000 mV range, 1
hazard statement, see Section 7.
mV resolution with dispenser having a volume readout of 0.00
to 9.99 mL or 0.00 to 99.99 mL and 0.01 % resolution.
2. Referenced Documents
5.2 Electrode, glass, reference.
2.1 ASTM Standards:
5.3 Electrode, silver, billet type.
D 891 Test Method for Specific Gravity, Apparent, of Liq-
uid Industrial Chemicals
6. Reagents and Materials
D 1193 Specification for Reagent Water
6.1 Purity of Reagents—Reagent grade chemicals shall be
D 3437 Practice for Sampling and Handling Liquid Cyclic
used in all tests. Unless otherwise indicated, it is intended that
Products
all reagents conform to the specifications of the Committee on
D 3505 Test Method for Density or Relative Density of
Analytical Reagents of the American Chemical Society, where
Pure Liquid Chemicals
such specifications are available. Other grades may be used,
D 4052 Test Method for Density and Relative Density of
provided it is first ascertained that the reagent is of sufficiently
Liquids by Digital Density Meter
high purity to permit its use without lessening the accuracy of
E 29 Practice for Using Significant Digits in Test Data to
the determination.
1 6
This test method is under the jurisdiction of ASTM Committee D-16 on Annual Book of ASTM Standards, Vol 14.02.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Available from Superintendent of Documents, U.S. Government Printing
Subcommittee D16.0E on Instrumental Analysis. Office, Washington, DC 20402.
Current edition approved Feb. 10, 1996. Published April 1996. Originally Reagent Chemicals, American Chemical Society Specifications, American
e1
published as D 5194 – 91. Last previous edition D 5194 – 91 . Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 15.05. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 06.04. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 05.02. MD.
D 5194
6.2 Purity of Water—Unless otherwise indicated, references 9.3 Rinse well with water and attach to the titrimeter.
to water shall be understood to mean reagent water as defined 9.4 Repeat the electrode preparation when the silver chlo-
by Types II or III of Specification D 1193. ride film begins to peel from the surface, or if the film becomes
6.3 Acetone, 99.9 % purity. discolored.
6.4 Congo Red Paper.
10. Procedure for Total Chloride
6.5 Detergent.
10.1 Extreme care must be used to prevent contamination
6.6 Isobutanol, 99.9 % minimum purity.
and all glassware should be exclusively reserved for this
6.7 Isooctane.
analysis. Just prior to use, the glassware should be rinsed with
6.8 Nitric Acid, concentrated.
water followed by acetone and then air dried.
6.9 Nitric Acid, 5-M. Dilute 160 mL concentrated nitric acid
10.2 Place 50 mL of toluene into a 250-mL separatory
to 500 mL with water.
funnel and pipet in the amount of the liquid sample that
6.10 Potassium Chloride, primary standard.
corresponds to the estimated chloride content as prescribed in
6.11 Potassium Chloride Solution, saturated.
Table 1.
6.12 Scouring Powder, cleanser.
6.13 Silver Nitrate, 99.99 % minimum purity.
NOTE 2—It is generally more convenient to measure the liquid samples
6.14 Silver Nitrate Solution, 0.01 N, standardized to 0.1 %. by volume and then convert to mass using density or relative density.
Table 2 lists the relative densities of several pure hydrocarbons. Densities
NOTE 1—This solution may be obtained as follows:
of unknowns may be determined by using Test Methods D 891, D 3505 or
(1) Purchase from a laboratory supply company, (2) Weigh to four
D 4052.
places, 1.680 to 1.720 g silver nitrate, transfer quantitatively into a
NOTE 3—Alternately, place the sample into a 125-mL bottle and weigh.
1000-mL volumetric flask, make to mark with water, and mix well.
From the contents of this bottle add the appropriate amount of the sample
to the toluene in the separatory funnel. Reweigh the bottle, and determine
Weight AgNO
Normality of solution 5
the weight of the analytical specimen.
169.9
or (3) Dissolve 8.5 g silver nitrate in 500 mL water to give a 0.1 N
10.3 Add the contents of one vial of sodium biphenyl
solution. Weigh 0.09 to 0.10 g of dried (105°C) potassium
...
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