ASTM D5194-96(2000)
(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:D5194–96 (Reapproved 2000)
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 D 4052 Test Method for Density and Relative Density of
Liquids by Digital Density Meter
1.1 This test method covers the determination of total
E29 Practice for Using Significant Digits in Test Data to
chloride (organic and inorganic) in liquid aromatic hydrocar-
Determine Conformance with Specifications
bons and cyclohexane.
2.2 Other Documents:
1.2 The test method is applicable to samples with chloride
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
concentrations of 1 to 25 mg/kg.
1910.1200
1.3 Bromides and iodides, if present, will be calculated as
chlorides.
3. Summary of Test Method
1.4 Materials, such as styrene, that are polymerized by
3.1 A known amount of hydrocarbon sample is transferred
sodium biphenyl reagent cannot be analyzed by this test
into a separatory funnel containing toluene. Sodium biphenyl
method.
reagent is added to convert organic halogens into inorganic
1.5 The following applies to all specified limits in this test
halides. The excess reagent is decomposed with water and the
method: for purposes of determining conformance with this
phases are separated. The aqueous phase is acidified, washed,
test method, an observed value or a calculated value shall be
and concentrated. Acetone is added and the solution is titrated
rounded off “to the nearest unit” in the last right-hand digit
with silver nitrate solution.
used in expressing the specification limit, in accordance with
the rounding-off method of PracticeE29.
4. Significance and Use
1.6 This standard does not purport to address all of the
4.1 Organic and inorganic chlorine compounds can have a
safety concerns, if any, associated with its use. It is the
deleterious effect on equipment and reactions in processes
responsibility of the user of this standard to establish appro-
involving aromatic hydrocarbons.
priate safety and health practices and determine the applica-
4.2 Maximum chloride levels are often specified for process
bility of regulatory limitations prior to use. For a specific
streams and for aromatic hydrocarbon products.
hazard statement, see Section 7.
5. Apparatus
2. Referenced Documents
5.1 Titrator, potentiometric, recording, + 2000 mV range, 1
2.1 ASTM Standards:
mV resolution with dispenser having a volume readout of 0.00
D 891 Test Method for Specific Gravity, Apparent, of Liq-
to 9.99 mL or 0.00 to 99.99 mL and 0.01 % resolution.
uid Industrial Chemicals
3 5.2 Electrode, glass, reference.
D 1193 Specification for Reagent Water
5.3 Electrode, silver, billet type.
D 3437 Practice for Sampling and Handling Liquid Cyclic
Products
6. Reagents and Materials
D 3505 Test Method for Density or Relative Density of
6.1 Purity of Reagents—Reagent grade chemicals shall be
Pure Liquid Chemicals
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
Analytical Reagents of theAmerican Chemical Society, where
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.04 on Instrumental Analysis.
Current edition approved Feb. 10, 1996. Published April 1996. Originally
e1 5
published as D 5194 – 91. Last previous edition D 5194 – 91 . Annual Book of ASTM Standards, Vol 05.02.
2 6
Annual Book of ASTM Standards, Vol 15.05. Annual Book of ASTM Standards, Vol 14.02.
3 7
Annual Book of ASTM Standards, Vol 11.01. Available from Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 06.04. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5194–96 (2000)
such specifications are available. Other grades may be used, 9. Electrode Preparation
provided it is first ascertained that the reagent is of sufficiently
9.1 Clean the surface of the silver electrode with mild
high purity to permit its use without lessening the accuracy of
detergent and scouring powder, and rinse with water.
the determination.
9.2 Immerse the electrode in the saturated potassium chlo-
6.2 Purity of Water—Unless otherwise indicated, references
ride solution until the electrode tip turns light gray.
to water shall be understood to mean reagent water as defined
9.3 Rinse well with water and attach to the titrimeter.
by Types II or III of Specification D 1193.
9.4 Repeat the electrode preparation when the silver chlo-
6.3 Acetone, 99.9 % purity.
ride film begins to peel from the surface, or if the film becomes
6.4 Congo Red Paper.
discolored.
6.5 Detergent, residue free.
6.6 Isobutanol, 99.9 % minimum purity.
10. Procedure for Total Chloride
6.7 Isooctane.
10.1 Extreme care must be used to prevent contamination
6.8 Nitric Acid, concentrated.
and all glassware should be exclusively reserved for this
6.9 NitricAcid, 5-M. Dilute 160 mLconcentrated nitric acid
analysis. Just prior to use, the glassware should be rinsed with
to 500 mL with water.
water followed by acetone and then air dried.
6.10 Potassium Chloride, primary standard.
10.2 Place 50 mL of toluene into a 250-mL separatory
6.11 Potassium Chloride Solution, saturated.
funnel and pipet in the amount of the liquid sample that
6.12 Scouring Powder, cleanser.
corresponds to the estimated chloride content as prescribed in
6.13 Silver Nitrate, 99.99 % minimum purity.
Table 1.
6.14 Silver Nitrate Solution, 0.01 N, standardized to 0.1 %.
NOTE 2—It is generally more convenient to measure the liquid samples
NOTE 1—This solution may be obtained as follows:
by volume and then convert to mass using density or relative density.
(1) Purchase from a laboratory supply company, (2) Weigh to four
Table 2 lists the relative densities of several pure hydrocarbons. Densities
places, 1.680 to 1.720 g silver nitrate, transfer quantitatively into a
of unknowns may be determined by usingTest Methods D 891, D 3505 or
1000-mL volumetric flask, make to mark with water, and mix well.
D 4052.
NOTE 3—Alternately, place the sample into a 125-mLbottle and weigh.
Weight AgNO
Normality of solution 5
From the contents of this bottle add the appropriate amount of the sample
169.9
to the toluene in the separatory funnel. Reweigh the bottle, and determine
the weight of the analytical specimen.
or (3) Dissolve 8.5 g silver nitrate in 500 mL water to give a 0.1 N
solution. Weigh 0.09 to 0.10 g of dried (105°C) potassium chloride to the
10.3 Add the contents of one vial of sodium biphenyl
nearest0.1mgintoa250-mLelectrolyticbeaker,add100mLofwaterand
reagent, stopper the separato
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