Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide
用<emph type=“ital”>p</emph>-甲苯磺酰基异氰酸酯(TSI)反应和四丁基氢氧化铵电位滴定法测定羟基的标准试验方法
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.
====== 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 (<1), and is amenable to automation.