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BS EN ISO 14896:2001:2002 Edition

$102.76

Plastics. Polyurethane raw materials. Determination of isocyanate content

Published By Publication Date Number of Pages
BSI 2002 20
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5 Plastics�— Polyurethane raw materials�— Determination of isocyanate content
7 Contents Page
8 Foreword
9 Plastics�— Polyurethane raw materials�— Determination of isocyanate content
1��� Scope
2��� Normative references
3��� Terms and definitions
10 4��� Principle
4.1��� Method�A
4.2��� Method�B
5��� Application
6��� Interferences
7��� Sampling
11 8��� Test conditions
9��� Reagents
9.1��� Acetone
9.2��� Toluene
9.3��� di-
9.4��� di-
9.5��� Aqueous hydrochloric acid
9.6��� Methanolic hydrochloric acid
9.7��� Bromophenol blue indicator solution
9.8��� 1,2,4-Trichlorobenzene
9.9��� Methanol
10��� Apparatus
10.1��� Potentiometric titrator
10.2��� Syringes
10.3��� Magnetic stirrer
10.4��� Analytical balance
12 10.5��� Iodine flask
10.6��� Conical flask
10.7��� Volumetric pipettes
10.8��� Measuring pipette
10.9��� Graduated cylinders
10.10��� Beaker
10.11��� Burette
11��� Method�A — Toluene/dibutylamine with aqueous HCl
11.1��� Procedure
11.1.1��� Using a volumetric pipette (
11.1.2��� Weigh a sample of the product to be analysed to the nearest
11.1.3��� After complete dissolution, allow to react for
11.1.4��� Using a graduated cylinder (
11.1.5��� Titrate the excess dibutylamine using one of the two following procedures:
11.1.5.1��� Potentiometric titration (recommended)
11.1.5.2��� Colorimetric titration
13 11.1.6��� Conduct a blank determination under identical conditions, except omit the test portion.
11.2��� Expression of results
11.2.1��� Calculate the %�NCO as follows:
11.2.2��� The amine equivalent may be calculated as follows:
11.2.3��� For isocyanates based on a single isomer or isomer mixture (for example, “pure” TDI or …
11.2.4��� The number of equivalents per kilogram (equiv/kg) may be calculated as follows:
14 11.2.5��� In refined isocyanates, acidic impurities are usually present in such low amounts that …
11.3��� Precision and bias
11.3.1��� Precision
11.3.2��� Bias
11.4��� Test report
12��� Method�B — Toluene/TCB/DBA with methanolic HCl
12.1��� Procedure
12.1.1��� Introduce
15 12.1.2��� Transfer the approximate amount of sample required, weighed to the nearest
12.1.3��� Cover the flask and swirl the contents until the solution is homogeneous. The reaction …
12.1.4��� Let the reaction mixture stand until it reaches room temperature (
12.1.5��� Titrate potentiometrically with
12.1.6��� Prepare a blank exactly as described above, but without adding the test portion. Titrat…
12.1.7��� If a potentiometric titrator is not available, the titration can be performed using a c…
12.2��� Expression of results
12.2.1��� As required, calculate the %�NCO, amine equivalent, or equivalents per kilogram followi…
12.2.2��� In refined isocyanates, acidic impurities are usually present in such low amounts that …
16 12.2.3��� The amine equivalent, corrected for acidity, may be calculated as follows:
12.3��� Precision and bias
12.3.1��� Use the following criteria to judge the acceptability of results for crude or modified …
12.3.1.1��� Repeatability (single analyst)
12.3.1.2��� Reproducibility (multilaboratory)
12.3.2��� Use the following criteria to judge the acceptability of results for MDI isomers:
12.3.2.1��� Repeatability
12.3.2.2��� Reproducibility
12.3.3��� TDI isomers were evaluated. However, there were insufficient degrees of freedom to make…
12.3.4��� Bias is the difference between the expectation of the test results and an accepted refe…
12.4��� Test report
BS EN ISO 14896:2001
$102.76