Standard Test Method for Determining Organic Chloride in Aromatic Hydrocarbons and Related Chemicals by Microcoulometry

SIGNIFICANCE AND USE
Organic as well as inorganic chlorine compounds can prove harmful to equipment and reactions in processes involving hydrocarbons.
Maximum chloride levels are often specified for process streams and for hydrocarbon products.
Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and this acid accumulates in condensing regions of the refinery.
SCOPE
1.1 This test method covers the organic chlorides in aromatic hydrocarbons, their derivatives, and related chemicals.
1.2 This test method is applicable to samples with chloride concentrations from 1 to 25 mg/kg.
1.3 This test method is preferred over Test Method D 5194 for products, such as styrene, that are polymerized by the sodium biphenyl reagent.
1.4 The following applies to all specified limits in this standard: for purposes of determining conformance with this standard, 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 E 29.
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. For specific hazard statements, see 7.3 and Section 9.

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Publication Date
09-Aug-2003
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ASTM D5808-03 - Standard Test Method for Determining Organic Chloride in Aromatic Hydrocarbons and Related Chemicals by Microcoulometry
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5808–03
Standard Test Method for
Determining Organic Chloride in Aromatic Hydrocarbons
1
and Related Chemicals by Microcoulometry
This standard is issued under the fixed designation D 5808; 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.
4
1. Scope Determine the Precision of a Test Method
2.2 Other Document:
1.1 This test method covers the organic chlorides in aro-
OSHA Regulations—29CFR paragraphs 1910.1000 and
matic hydrocarbons, their derivatives, and related chemicals.
5
1910.1200
1.2 This test method is applicable to samples with chloride
concentrations from 1 to 25 mg/kg.
3. Terminology
1.3 This test method is preferred over Test Method D 5194
3.1 Definitions:
for products, such as styrene, that are polymerized by the
3.1.1 dehydration tube—chamber containing concentrated
sodium biphenyl reagent.
sulfuric acid that scrubs the effluent gases from combustion to
1.4 The following applies to all specified limits in this
remove water vapor.
standard: for purposes of determining conformance with this
3.1.2 oxidative pyrolysis—a process in which a sample is
standard, an observed value or a calculated value shall be
combusted in an oxygen-rich atmosphere at high temperature
rounded off “to the nearest unit” in the last right-hand digit
to break down the components of the sample into elemental
used in expressing the specification limit, in accordance with
oxides.
the rounding-off method of Practice E 29.
3.1.3 recovery factor—an indication of the efficiency of the
1.5 This standard does not purport to address all of the
measurement computed by dividing the measured value of a
safety concerns, if any, associated with its use. It is the
standard by its theoretical value.
responsibility of the user of this standard to establish appro-
3.1.4 reference sensor pair—detects changes in silver ion
priate safety and health practices and determine the applica-
concentration.
bility of regulatory limitations prior to use. For specific hazard
3.1.5 test titration—a process that allows the coulometer to
statements, see 7.3 and Section 9.
set the endpoint and gain values to be used for sample analysis.
2. Referenced Documents 3.1.6 titration parameters—various instrumental conditions
that can be changed for different types of analysis.
2.1 ASTM Standards:
2 3.1.7 workingelectrode(generatorelectrode)—anelectrode
D 1193 Specification for Reagent Water
consistingofananodeandacathodeseparatedbyasaltbridge;
D 3437 Practice for Sampling and Handling Liquid Cyclic
3 maintains a constant silver ion concentration.
Products
D 5194 Test Method for Trace Chloride in LiquidAromatic
4. Summary of Test Method
3
Hydrocarbons
4.1 A liquid specimen is injected into a combustion tube
E 29 Practice for Using Significant Digits in Test Data to
4 maintained at 900°C having a flowing stream of oxygen and
Determine Conformance with Specifications
argon carrier gas. Oxidative pyrolysis converts the organic
E 691 Practice for Conducting an Interlaboratory Study to
halides to hydrogen halides that then flow into a titration cell
where it reacts with silver ions present in the electrolyte. The
silver ion thus consumed is coulometrically replaced and the
1
This test method is under the jurisdiction of ASTM Committee D16 on
total electrical work to replace it is a measure of the organic
Aromatic Hydrocarbons and Related Chemicals is the direct responsibility of
Subcommittee D16.04 on Instrumental Analysis. halides in the specimen injected (see Annex A1).
Current edition approved Aug. 10, 2003. Published August 2003. Originally
approved in 1995. Last previous edition approved in 1995 as D 5808 - 95.
2
Annual Book of ASTM Standards, Vol 11.01.
3 5
Annual Book of ASTM Standards, Vol 06.04. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
4
Annual Book of ASTM Standards, Vol 14.02. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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D5808–03
5. Significance and Use 7.7 Dehydration Tube, positioned at the end of the pyrolysis
tube so that effluent gases are bubbled through a sulfuric acid
5.1 Organic as well as inorganic chlorine compounds can
solution, and water vapor is subsequently trapped, while all
prove harmful to equipment and reactions in processes involv-
other gases are allowed to flow into the titration cell.
ing hydrocarbons.
7.8 Gas-Tight Sampling Syringe, having a 50 µl capacity,
5.2 Maximum chloride levels are often specified for pr
...

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