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ASTM E1899-23

(Test Method)

Standard Test Method for Hydroxyl Groups Using Reaction with p-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide

Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide

SIGNIFICANCE AND USE
5.1 Hydroxyl is an important functional group and knowledge of its content is required in many intermediate and end use applications. This test method is for the determination of primary and secondary hydroxyl groups and can be used for the assay of compounds containing them.  
5.2 This test method has the following advantages over other hydroxyl number methods: It is rapid (10 min), pyridine-free, ambient temperature, small sample size, applicable to extremely low hydroxyl numbers (
SCOPE
1.1 This test method covers the determination of hydroxyl groups attached to primary and secondary carbon atoms in aliphatic and cyclic compounds and phenols from 0.5 to 367 hydroxyl number. It is not suitable for determination of hydroxyl groups attached to tertiary carbon atoms. This test method is applicable to polyacetals, temperature sensitive materials, high solids polymer polyols, and rigid polyols. Other available test methods listed in Note 1 are not suitable for many of the sample types listed above.  
1.1.1 This test method is currently recommended for neutral refined products. Successful application has been made, however, to some in-process samples that contain an excess of acidic species. Proper validation must be performed, of course, to show that the acidic species either does not interfere, or that the acidic species interference has been obviated.
Note 1: Other methods for determination of hydroxyl groups are given in Test Methods D817, D871, D4252, D4273, D4274, E222, E326, and E335.  
1.2 The Limit of Detection (LOD) is 0.18 units and the Limit of Quantitation (LOQ) is 0.59 units. Unit = hydroxyl number (OH#).
Note 2: LOD and LOQ were calculated using Standard deviations from 14.1.2.1.  
1.3 Review the current appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 The following applies for the purposes of determining the conformance of the test results using this test method to applicable specifications. Results shall be rounded off in accordance with the rounding-off method of Practice E29.  
1.6 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. For specific hazards see Section 9.  
1.7 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

Status
Published
Publication Date
31-Mar-2023
ICS
71.040.40 - Chemical analysis
Technical Committee
D16 - Aromatic, Industrial, Specialty and Related Chemicals
Drafting Committee
D16.12 - Caustics and Peroxides
Current Stage
Ref Project

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ASTM E1899-23 - Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium HydroxideASTM E1899-23 - Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide
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REDLINE ASTM E1899-23 - Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide
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Standards Content (Sample)

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.
Designation: E1899 − 23
Standard Test Method for
Hydroxyl Groups Using Reaction with p-Toluenesulfonyl
Isocyanate (TSI) and Potentiometric Titration with
1
Tetrabutylammonium Hydroxide
This standard is issued under the fixed designation E1899; 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* 1.5 The following applies for the purposes of determining
the conformance of the test results using this test method to
1.1 This test method covers the determination of hydroxyl
applicable specifications. Results shall be rounded off in
groups attached to primary and secondary carbon atoms in
accordance with the rounding-off method of Practice E29.
aliphatic and cyclic compounds and phenols from 0.5 to 367
1.6 This standard does not purport to address all of the
hydroxyl number. It is not suitable for determination of
safety concerns, if any, associated, with its use. It is the
hydroxyl groups attached to tertiary carbon atoms. This test
responsibility of the user of this standard to establish appro-
method is applicable to polyacetals, temperature sensitive
priate safety, health, and environmental practices and deter-
materials, high solids polymer polyols, and rigid polyols. Other
mine the applicability of regulatory limitations prior to use.
available test methods listed in Note 1 are not suitable for many
For specific hazards see Section 9.
of the sample types listed above.
1.7 This international standard was developed in accor-
1.1.1 This test method is currently recommended for neutral
dance with internationally recognized principles on standard-
refined products. Successful application has been made,
ization established in the Decision on Principles for the
however, to some in-process samples that contain an excess of
Development of International Standards, Guides and Recom-
acidic species. Proper validation must be performed, of course,
mendations issued by the World Trade Organization Technical
to show that the acidic species either does not interfere, or that
Barriers to Trade (TBT) Committee.
the acidic species interference has been obviated.
NOTE 1—Other methods for determination of hydroxyl groups are given
2. Referenced Documents
in Test Methods D817, D871, D4252, D4273, D4274, E222, E326, and
2
E335. 2.1 ASTM Standards:
D817 Test Methods of Testing Cellulose Acetate Propionate
1.2 The Limit of Detection (LOD) is 0.18 units and the
and Cellulose Acetate Butyrate
Limit of Quantitation (LOQ) is 0.59 units. Unit = hydroxyl
D871 Test Methods of Testing Cellulose Acetate
number (OH#).
D1193 Specification for Reagent Water
NOTE 2—LOD and LOQ were calculated using Standard deviations
D4252 Test Methods for Chemical Analysis of Alcohol
from 14.1.2.1.
Ethoxylates and Alkylphenol Ethoxylates
1.3 Review the current appropriate Safety Data Sheets
D4273 Test Method for Polyurethane Raw Materials: Deter-
(SDS) for detailed information concerning toxicity, first aid
mination of Primary Hydroxyl Content of Polyether Poly-
procedures, and safety precautions.
ols
D4274 Test Methods for Testing Polyurethane Raw Materi-
1.4 The values stated in SI units are to be regarded as
als: Determination of Hydroxyl Numbers of Polyols
standard. No other units of measurement are included in this
D6809 Guide for Quality Control and Quality Assurance
standard.
Procedures for Aromatic Hydrocarbons and Related Ma-
terials
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
2
bility of Subcommittee D16.12 on Caustics and Peroxides. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2023. Published June 2023. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1997. Last previous edition approved in 2016 as E1899 – 16. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1899-23. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1899 − 23
E29 Practice for Using Significant Digits in Test Data to 5.2 This test method has the following advantages over
Determine Conformance with Specifications other hydroxyl number methods: It is rapid (1
...

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: E1899 − 16 E1899 − 23
Standard Test Method for
Hydroxyl Groups Using Reaction with p-Toluenesulfonyl
Isocyanate (TSI) and Potentiometric Titration with
1
Tetrabutylammonium Hydroxide
This standard is issued under the fixed designation E1899; 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 hydroxyl groups attached to primary and secondary carbon atoms in aliphatic
and cyclic compounds and phenols. phenols from 0.5 to 367 hydroxyl number. It is not suitable for determination of hydroxyl
groups attached to tertiary carbon atoms. This test method is applicable to polyacetals, temperature sensitive materials, high solids
polymer polyols, and rigid polyols. Other available test methods listed in Note 1 are not suitable for many of the sample types listed
above.
1.1.1 This test method is currently recommended for neutral refined products. Successful application has been made, however, to
some in-process samples that contain an excess of acidic species. Proper validation must be performed, of course, to show that the
acidic species either does not interfere, or that the acidic species interference has been obviated.
NOTE 1—Other methods for determination of hydroxyl groups are given in Test Methods D817, D871, D1957, D2195, D4252, D4273, D4274, E222,
E326, and E335.
1.2 The Limit of Detection (LOD) is 0.18 units and the Limit of Quantitation (LOQ) is 0.59 units. Unit = hydroxyl number (OH#).
NOTE 2—LOD and LOQ were calculated using Standard deviations from 14.1.2.1.
1.3 Review the current appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and
safety precautions.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 The following applies for the purposes of determining the conformance of the test results using this test method to applicable
specifications. Results shall be rounded off in accordance with the rounding-off method of Practice E29.
1.6 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. For specific hazards see Section 9.
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.12 on Caustics and Peroxides.
Current edition approved April 1, 2016April 1, 2023. Published May 2016June 2023. Originally approved in 1997. Last previous edition approved in 20082016 as
E1899 – 08.E1899 – 16. DOI: 10.1520/E1899-16.10.1520/E1899-23.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1899 − 23
1.7 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
2.1 ASTM Standards:
D817 Test Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate
D871 Test Methods of Testing Cellulose Acetate
D1193 Specification for Reagent Water
3
D1957 Test Method for Hydroxyl Value of Fatty Oils and Acids (Withdrawn 2007)
3
D2195 Test Methods for Pentaerythritol (Withdrawn 2011)
D4252 Test Methods for Chemical Analysis of Alcohol Ethoxylates and Alkylphenol Ethoxylates
D4273 Test Method for Polyurethane Raw Materials: Determination of Primary Hydroxyl Content of Polyether Polyols
D4274 Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E180 Practice for D
...

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4.2 This practice is useful to reduce potential fractionation during separation, such as when attempting to distinguish between various grades of fuel oil.  
4.3 This practice is particularly useful for extraction from nonporous surfaces such as glass, or the interior of burned containers. It is also well suited to the extraction of ignitable liquid residues from samples that are not amenable to extraction using Practice E1412.  
4.4 This practice lacks specificity to separate and isolate ignitable liquids from interfering compounds present in the fire debris.  
4.5 This practice is not suitable for the extraction of extremely volatile compounds and ignitable liquids (for example, acetone, butane, ethanol, propane, some cigarette lighter fluids), which could evaporate during the concentration step.  
4.6 This is a destructive technique. Whenever possible, this technique should only be used when a representative portion of the sample can be preserved for reanalysis. Those portions of the sample subjected to this procedure could be unsuitable for resampling. If sample spoliation is an issue, a nondestructive extraction technique (for example, Practices E1412, E2154) should be used prior to this technique.
SCOPE
1.1 This practice covers the procedure for removing small quantities of ignitable liquid residue from samples of fire debris using solvent to extract the residue.  
1.2 This practice is suitable for extracting ignitable liquid residues over a wide range of concentrations.  
1.3 Alternate separation and concentration procedures are listed in the referenced documents (Practices E1388, E1412, E1413, E2154, and E3189).  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

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ASTM
ASTM E1641-23(Test Method)
Standard Test Method for Decomposition Kinetics by Thermogravimetry Using the Ozawa/Flynn/Wall Method

SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the temperature-decomposition profile of a material.  
5.2 This test method can be used for estimating lifetimes of materials, using Practice E1877 provided that a relationship has been established between the thermal endurance test results and actual lifetime tests.
SCOPE
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and pre-exponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kinetics using the Ozawa/Flynn/Wall isoconversional method (1, 2).2  
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change with a single maximum rate.  
1.3 This test method is normally applicable to decomposition occurring in the range from 400 K to 1300 K (nominally 100 °C to 1000 °C). The temperature range may be extended depending on the instrumentation used.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

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ASTM
ASTM E2403-23(Test Method)
Standard Test Method for Sulfated Ash of Organic Materials by Thermogravimetry

SIGNIFICANCE AND USE
5.1 The sulfated ash value indicates the level of known metal-containing additives or impurities in an organic material. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates. Tin and zinc are converted to their oxides.  
5.2 This test method may be used for research and development, specification acceptance, and quality assurance purposes.
SCOPE
1.1 This test method describes the determination of sulfated ash content (sometimes called residue-on-ignition) of organic materials by thermogravimetry. This test method converts common metals found in organic materials (such as sodium, potassium, lithium, calcium, magnesium, zinc, and tin) into their sulfate salts permitting estimation of their total content as sulfates or oxides. The range of this test method is from 0.1 % to 100 % metal content.  
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.

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