ASTM D1157-91(2014)
(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
4.1 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. No other units of measurement are included in this 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.
General Information
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Designation: D1157 − 91 (Reapproved 2014)
Standard Test Method for
1,2
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
content. Small amounts of polymer do not interfere. This test 5.1 Photometer—A sensitive photoelectric photometer ca-
method is applicable over the range of TBC from 50 to pable of producing light of narrow spectral range that is
500mg⁄kg. predominantly blue (425 nm).
1.2 The values stated in SI units are to be regarded as 5.2 Graduates, 100-mL.
standard. No other units of measurement are included in this
5.3 Volumetric Flasks, 100-mL; or stoppered graduated
standard.
mixing cylinder, 100-mL.
1.3 This standard does not purport to address all of the
5.4 Erlenmeyer Flasks, 250-mL.
safety concerns, if any, associated with its use. It is the
5.5 Funnels, 75-mm diameter.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.6 Pipet, 5-mL.
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
D1265Practice for Sampling Liquefied Petroleum (LP)
all reagents shall conform to the specifications of the Commit-
Gases, Manual Method
tee onAnalytical Reagents of theAmerican Chemical Society,
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
This test method is under the jurisdiction of ASTM Committee D02 on
HCl (sp gr 1.19), and then dilute with ethanol (95%) to
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.D0.04 on C4 Hydrocarbons.
1000mL in a volumetric flask.
CurrenteditionapprovedMay1,2014.PublishedJuly2014.Originallyapproved
6.4 p-Tertiary-Butylcatechol, Standard—(Warning—
in 1951. Last previous edition approved in 2009 as D1157–91(2009). DOI:
10.1520/D1157-91R14.
Potentially hazardous. May cause skin irritation or burns; can
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 Annual 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 (2014)
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
quinonesandflammablebutylenesondecomposition.Usewith 5.0 60.1mLofstandardFeCl solution,diluteto100mL,and
adequate ventilation. Store in flammable liquids storage area.) mix well.
Dissolve 0.63 g of p-tertiary-butylcatechol (95% minimum
9.2 Measurement of Sample—After the addition of the
purity) in 10 mL of ethanol (95%) and dilute with water to
FeCl reagent,allowthesolutiontostandforfrom5to15min,
100mL in a volumetric flask. When used in place of 100 mL
then measure the absorbance of the solution by means of a
(63 g) of sample, consider 1.00 mL of this solution to be
photoelectric photometer, using water as a ref
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D1157 − 91 (Reapproved 2009) D1157 − 91 (Reapproved 2014)
Standard Test Method for
1,2
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
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 C 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 500 500 mg mg/kg.⁄kg.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.
2. Referenced Documents
2.1 ASTM Standards:
D1265 Practice for Sampling Liquefied Petroleum (LP) Gases, Manual Method
3. Summary of Test Method
3.1 The catechol is separated from the butadiene by evaporation. The residue is dissolved in water and an excess of ferric
chloride is added. The intensity of the yellow-colored complex is compared in a photoelectric colorimeter with that produced by
known concentrations of the catechol.
4. Significance and Use
4.1 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.
5. Apparatus
5.1 Photometer—A sensitive photoelectric photometer capable of producing light of narrow spectral range that is predominantly
blue (425 nm).
5.2 Graduates, 100-mL.
5.3 Volumetric Flasks, 100-mL; or stoppered graduated mixing cylinder, 100-mL.
5.4 Erlenmeyer Flasks, 250-mL.
5.5 Funnels, 75-mm diameter.
5.6 Pipet, 5-mL.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.D0.04 on C4 Hydrocarbons.
Current edition approved July 1, 2009May 1, 2014. Published November 2009July 2014. Originally approved in 1951. Last previous edition approved in 20042009 as
D1157–91(2004).D1157 – 91 (2009). DOI: 10.1520/D1157-91R0910.1520/D1157-91R14.
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 Laboratory Manual as Method 2.1.9.1.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1157 − 91 (2014)
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—References to water shall be understood to mean distilled water.
6.3 Ferric Chloride, Standard Solution— Dissolve 20.0 g of ferric chloride (FeCl ·6H O) in ethanol (95 %). Add 9.2 mL of HCl
3 2
(sp gr 1.19), and then dilute with ethanol (95 %) to 1000 mL 1000 mL in a volumetric flask.
6.4 p-Tertiary-Butylcatechol, Standard—(Warning—Potentially hazardous. May cause skin irritation or burns; can be absorbed
through the skin. May be harmful or fatal if swallowed. Avoid contact with eyes; may burn and impair vision. May be harmful
to respiratory system. May produce quinones and flammable butylenes on decomposition. Use with adequate ventilation. Store in
flammable liquids storage area.) Dissolve 0.63 g of p-tertiary-butylcatechol (95 % minimum purity) in 10 mL of ethanol (95 %)
and dilute with water to 100 mL 100 mL in a volumetric flask. When used in place of 100 mL (63 g) of sample, consider 1.00 mL
of this solution to be equivalent to 100 ppm of catechol. This solution is not stable and should be prepared as needed.
7. Sampling
7.1 Supply samples to the laboratory in high-pressure sample cylinders. Use the procedures described in Practice D1265 or
similar methods.
8. Calibration and Standardization
8.1 Preparation of Standard Solutions—Prepare a standardization curve showing the relation between the absorbance and the
catechol content as follows: Make up solutions of known catechol content by pipetting 0, 1, 2, 3, 4, and 5-mL portions of the
standard catechol solution (1.00 mL = 100 mg/kg) into separate 100-mL volumetric flasks, or stoppered, graduated mixing
cylinders. Then add e
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