ASTM D1157-91(2019)
(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 mg/kg 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 mg/kg 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
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Designation: D1157 − 91 (Reapproved 2019)
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 3. Summary of Test Method
1.1 This test method covers the determination of total 3.1 The catechol is separated from the butadiene by evapo-
p-tertiary-butylcatechol inhibitor added to polymerization and ration. The residue is dissolved in water and an excess of ferric
recycle grades of butadiene or to other C hydrocarbon chloride is added. The intensity of the yellow-colored complex
mixtures containing no phenolic material other than catechol or is compared in a photoelectric colorimeter with that produced
no oxidized phenolic material other than that derived from by known concentrations of the catechol.
oxidation of catechol. In general, all phenols and their quinone
oxidation products are included in the calculated catechol 4. Significance and Use
content. Small amounts of polymer do not interfere. This test
4.1 p-tertiary-butylcatechol is commonly added to commer-
method is applicable over the range of TBC from 50 mg ⁄kg to
cial butadiene in amounts of 50 mg ⁄kg to 250 mg ⁄kg as an
500 mg ⁄kg.
oxidation inhibitor. This test method is suitable for use by both
1.2 The values stated in SI units are to be regarded as producers and users of butadiene within the limitations de-
standard. No other units of measurement are included in this scribed in Section 1.
standard.
5. Apparatus
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5.1 Photometer—A sensitive photoelectric photometer ca-
responsibility of the user of this standard to establish appro-
pable of producing light of narrow spectral range that is
priate safety, health, and environmental practices and deter-
predominantly blue (425 nm).
mine the applicability of regulatory limitations prior to use.
5.2 Graduates, 100 mL.
1.4 This international standard was developed in accor-
5.3 Volumetric Flasks, 100 mL; or stoppered graduated
dance with internationally recognized principles on standard-
mixing cylinder, 100 mL.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5.4 Erlenmeyer Flasks, 250 mL.
mendations issued by the World Trade Organization Technical
5.5 Funnels, 75 mm diameter.
Barriers to Trade (TBT) Committee.
5.6 Pipet, 5 mL.
2. Referenced Documents
6. Reagents
2.1 ASTM Standards:
6.1 Purity of Reagents—Reagent grade chemicals shall be
D1265 Practice for Sampling Liquefied Petroleum (LP)
used in all tests. Unless otherwise indicated, it is intended that
Gases, Manual Method
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
This test method is under the jurisdiction of ASTM Committee D02 on where such specifications are available. Other grades may be
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
used, provided it is first ascertained that the reagent is of
Subcommittee D02.D0.04 on C4 and C5 Hydrocarbons.
sufficiently high purity to permit its use without lessening the
Current edition approved Dec. 1, 2019. Published December 2019. Originally
accuracy of the determination.
approved in 1951. Last previous edition approved in 2014 as D1157 – 91 (2014).
DOI: 10.1520/D1157-91R19.
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 ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Laboratory Manual as Method 2.1.9.1. Standard-Grade Reference Materials, American Chemical Society, Washington,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by the American Chemical
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1157 − 91 (2019)
6.2 Purity of Water—References to water shall be under- pressure. May form explosive peroxides upon exposure to air.
stood to mean distilled water. Harmful if inhaled. Irritating to eyes, skin, and mucous
membranes.) into a graduate that has been cooled to be-
6.3 Ferric Chloride, Standard Solution— Dissolve 20.0 g of
low −20 °C. Pour the sample into a 250 mL Erlenmeyer flask
ferric chloride (FeCl ·6H O) in ethanol (95 %). Add 9.2 mL of
3 2
and allow the liquid to evaporate at room temperature behind
HCl (sp gr 1.19), and then dilute with ethanol (95 %) to
a shield in a well-ventilated hood. A steam bath may be used to
1000 mL in a volumetric flask.
complete the evaporation. Add 30 mL of water to the flask,
6.4 p-Tertiary-Butylcatechol, Standard—(Warning—
stopper, shake, and filter through a rapid, hardened, low-ash
Potentially hazardous. May cause skin irritation or burns; can
paper that has previously been moistened. Repeat with two
be absorbed through the skin. May be harmful or fatal if
more 30 mL portions of water. Combine all filtrates, add from
swallowed. Avoid contact with eyes; may burn and impair
a pipet 5.0 mL 6 0.1 mL of standard FeCl solution, dilute to
vision. May be harmful
...
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 2014) D1157 − 91 (Reapproved 2019)
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 5050 mg ⁄kg 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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 5050 mg ⁄kg to 250250 mg mg/kg ⁄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).(425 nm).
5.2 Graduates, 100-mL.100 mL.
5.3 Volumetric Flasks, 100-mL;100 mL; or stoppered graduated mixing cylinder, 100-mL.100 mL.
5.4 Erlenmeyer Flasks, 250-mL.250 mL.
5.5 Funnels, 75-mm75 mm diameter.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of Subcommittee
D02.D0.04 on C4 and C5 Hydrocarbons.
Current edition approved May 1, 2014Dec. 1, 2019. Published July 2014December 2019. Originally approved in 1951. Last previous edition approved in 20092014 as
D1157 – 91 (2009).(2014). DOI: 10.1520/D1157-91R14.10.1520/D1157-91R19.
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 (2019)
5.6 Pipet, 5-mL.5 mL.
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 20.0 g of ferric chloride (FeCl ·6H O) in ethanol (95 %). Add 9.2 mL
3 2
9.2 mL of 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—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 0.63 g of p-tertiary-butylcatechol (95 % minimum purity) in 10 mL of ethanol
(95 %) and dilute with water to 100 mL in a volumetric flask. When used in place of 100 mL (63 g) 100 mL (63 g) of sample,
consider 1.00 mL 1.00 mL of this solution to be equivalent to 100 ppm 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-mL0 mL, 1 mL, 2 mL,
3 mL, 4 mL, and 5 mL portions of the standard catechol
...
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