ASTM D1157-91(2000)e1
(Test Method)Standard Test Method for Total Inhibitor Content (TBC) of Light Hydrocarbons
Standard Test Method for Total Inhibitor Content (TBC) of Light Hydrocarbons
SCOPE
1.1 This test method covers the determination of total p-tertiary-butylcatechol inhibitor added to polymerization and recycle grades of butadiene or to other C 4 hydrocarbon mixtures containing no phenolic material other than catechol or no oxidized phenolic material other than that derived from oxidation of catechol. In general, all phenols and their quinone oxidation products are included in the calculated catechol content. Small amounts of polymer do not interfere. This test method is applicable over the range of TBC from 50 to 500 mg/kg.
1.2 The values stated in SI units are to be regarded as standard. The values stated in inch-pound units are for information only.
1.3This 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.
General Information
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
An American National Standard
e1
Designation: D 1157 – 91 (Reapproved 2000)
Standard Test Method for
Total Inhibitor Content (TBC) of Light Hydrocarbons
This standard is issued under the fixed designation D1157; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Warning notes were placed in the text in November 2000.
1. Scope 4. Significance and Use
1.1 This test method covers the determination of total 4.1 p-tertiary-butylcatecholiscommonlyaddedtocommer-
p-tertiary-butylcatechol inhibitor added to polymerization and cial butadiene in amounts of 50 to 250 mg/kg as an oxidation
recycle grades of butadiene or to other C hydrocarbon inhibitor.Thistestmethodissuitableforusebybothproducers
mixturescontainingnophenolicmaterialotherthancatecholor and users of butadiene within the limitations described in the
no oxidized phenolic material other than that derived from scope.
oxidation of catechol. In general, all phenols and their quinone
5. Apparatus
oxidation products are included in the calculated catechol
5.1 Photometer—A sensitive photoelectric photometer ca-
content. Small amounts of polymer do not interfere. This test
method is applicable over the range of TBC from 50 to 500 pable of producing light of narrow spectral range that is
predominantly blue (425 nm).
mg/kg.
1.2 The values stated in SI units are to be regarded as 5.2 Graduates, 100-mL.
5.3 Volumetric Flasks, 100-mL; or stoppered graduated
standard. The values stated in inch-pound units are for infor-
mation only. mixing cylinder, 100-mL.
5.4 Erlenmeyer Flasks, 250-mL.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.5 Funnels, 75-mm diameter.
5.6 Pipet, 5-mL.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6. Reagents
bility of regulatory limitations prior to use.
6.1 Purity of Reagents—Reagent grade chemicals shall be
2. Referenced Documents
used in all tests. Unless otherwise indicated, it is intended that
2.1 ASTM Standards: all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
D1265 Practice for Sampling Liquified Petroleum (LP)
Gases where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
3. Summary of Test Method
sufficiently high purity to permit its use without lessening the
3.1 The catechol is separated from the butadiene by evapo- accuracy of the determination.
ration.Theresidueisdissolvedinwaterandanexcessofferric 6.2 Purity of Water—References to water shall be under-
chloride is added.The intensity of the yellow-colored complex stood to mean distilled water.
is compared in a photoelectric colorimeter with that produced 6.3 Ferric Chloride, Standard Solution—Dissolve20.0gof
by known concentrations of the catechol. ferric chloride (FeCl ·6H O) in ethanol (95%).Add 9.2 mLof
3 2
HCl (sp gr 1.19), and then dilute with ethanol (95%) to 1000
mL in a volumetric flask.
6.4 p-Tertiary-Butylcatechol, Standard—(Warning—
This test method is under the jurisdiction of ASTM Committee D02 on
Potentially hazardous. May cause skin irritation or burns; can
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.04 on C Hydrocarbons.
Current edition approved March 15, 1991. Published May 1991. Originally
published as D1157–51. Last previous edition D1157–84. Reagent Chemicals, American Chemical Society Specifications, American
This method was derived from the method developed and cooperatively tested Chemical Society, Washington, DC. For suggestions on the testing of reagents not
by the Butadiene Producers’ Committee on Specifications and Methods ofAnalysis listed by the American Chemical Society, see Analar Standards for Laboratory
oftheOfficeofRubberReserve,whichappearsintheButadieneLaboratoryManual Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
as Method 2.1.9.1. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 05.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D 1157
be absorbed through the skin. May be harmful or fatal if and filter through a rapid, hardened, low-ash paper that has
swallowed. Avoid contact with eyes; may burn and impair previously been moistened. Repeat with two more 30-mL
vision. May be harmful to respiratory system. May produce portions of water. Combine all filtrates, add from a pipet 5.0 6
quinonesandflammablebutylenesondecomposition.Usewith 0.1 mLof standard FeCl solution, dilute to 100 mL, and mix
adequate ventilation. Store in flammable liquids storage area.) well.
Dissolve 0.63 g of p-tertiary-butylcatechol (95% minimum 9.2 Measurement of Sample—After the addition of the
purity)in10mLofethanol(95%)anddilutewithwaterto100 FeCl reagent,allowthesolutiontostandforfrom5to15min;
mLinavolumetricflask.Whenusedinplaceof100mL(63g) then measure the absorbance of the solution by means of a
ofsample,consider1.00mLofthissolutiontobeequivalentto photoelectric photometer, using water as a
...
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