ASTM D1157-91(2004)
(Test Method)Standard Test Method for Total Inhibitor Content (TBC) of Light Hydrocarbons
Standard Test Method for Total Inhibitor Content (TBC) of Light Hydrocarbons
SIGNIFICANCE AND USE
p-tertiary-butylcatechol is commonly added to commercial butadiene in amounts of 50 to 250 mg/kg as an oxidation inhibitor. This test method is suitable for use by both producers and users of butadiene within the limitations described in Section 1.
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 C4 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.
1.3 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.
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Designation:D1157–91(Reapproved 2004)
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This test method covers the determination of total 4.1 p-tertiary-butylcatechol is commonly added to commer-
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
no oxidized phenolic material other than that derived from Section 1.
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.
1.3 This standard does not purport to address all of the mixing cylinder, 100-mL.
5.4 Erlenmeyer Flasks, 250-mL.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.5 Funnels, 75-mm diameter.
5.6 Pipet, 5-mL.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
6. Reagents
2. Referenced Documents
6.1 Purity of Reagents—Reagent grade chemicals shall be
2.1 ASTM Standards: used in all tests. Unless otherwise indicated, it is intended that
D1265 Practice for Sampling Liquefied Petroleum (LP) all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
Gases, Manual Method
where such specifications are available. Other grades may be
3. Summary of Test Method
used, provided it is first ascertained that the reagent is of
3.1 The catechol is separated from the butadiene by evapo- sufficiently high purity to permit its use without lessening the
ration.Theresidueisdissolvedinwaterandanexcessofferric accuracy of the determination.
chloride is added.The intensity of the yellow-colored complex 6.2 Purity of Water—References to water shall be under-
is compared in a photoelectric colorimeter with that produced stood to mean distilled water.
by known concentrations of the catechol. 6.3 Ferric Chloride, Standard Solution—Dissolve20.0gof
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.
This test method is under the jurisdiction of ASTM Committee D02 on
6.4 p-Tertiary-Butylcatechol, Standard—(Warning—
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
Potentially hazardous. May cause skin irritation or burns; can
D02.D0 on Hydrocarbons for Chemical and Special Uses.
Current edition approved Nov. 1, 2004. Published November 2004. Originally
be absorbed through the skin. May be harmful or fatal if
´1
approved in 1951. Last previous edition approved in 2000 as D1157–91 (2000) .
swallowed. Avoid contact with eyes; may burn and impair
DOI: 10.1520/D1157-91R04.
This test method was derived from the method developed and cooperatively
tested by the Butadiene Producers’ Committee on Specifications and Methods of
Analysis of the Office of Rubber Reserve, which appears in the Butadiene Reagent Chemicals, American Chemical Society Specifications, American
Laboratory Manual as Method 2.1.9.1. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1157–91 (2004)
vision. May be harmful to respiratory system. May produce previously been moistened. Repeat with two more 30-mL
quinonesandflammablebutylenesondecomposition.Usewith portionsofwater.Combineallfiltrates,addfromapipet5.0 6
adequate ventilation. Store in flammable liquids storage area.) 0.1 mL of standard FeCl solution, dilute to 100 mL, and mix
Dissolve 0.63 g of p-tertiary-butylcatechol (95% minimum well.
purity)in10mLofethanol(95%)anddilutewithwaterto100 9.2 Measurement of Sample—After the addition of the
mLinavolumetricflask.Whenusedinplaceof100mL(63g) FeCl reagent,allowthesolutiontostandforfrom5to15min,
ofsample,consider1.00mLofthissolutiontobeequivalentto then measure the absorbance of the solution by means of a
100 ppm of catechol.
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