ISO 11357-5:2013 pdf download.Plastics – Differential scanning calorimetry (DSC)一Part 5:Determination of characteristic reaction-curve temperatures and times, enthalpy of reaction and degree of conversion.
This part of Iso 11357 specifies a method for the determination of reaction temperatures and times, enthalpies of reaction, and degrees of conversion using differential scanning calorimetry (DSC).
The method applies to monomers, prepolymers, and polymers in the solid or liquid state. The material can contain fillers and/or initiators in the solid or liquid state.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 11357-1, Plastics — Differential scanning calorimetry (DSC) — Part 1: General principles
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 11357-1 and the following apply.
3.1
polymerization
process of converting a monomer or a mixture of monomers into a polymer
3.2
crosslinking
process of multiple intermolecular covalent or ionic bonding between polymer chains
3.3
degree of conversion
quantity of reacted product obtained during a reaction compared with the maximum possible quantity of the product
Note ito entry: The degree of conversion will depend on both time and temperature.
4 Principle
The principle is specified in ISO 11357-1.
The test method described indicates the various stages of the reaction by means of DSC curves.
5 Apparatus and materials
The apparatus and materials are specified in Iso 11357-1.
6 Test specimens
The test specimens are specified in ISO 11357-1.
If not specified otherwise, use a mass of 5 mg to 20 mg and adjust the specimen mass if the thermal
effect is too high or too low.
7 Test conditions and specimen conditioning
For polymers, the test conditions and specimen conditioning are specified in ISO 11357-1.
For specimens releasing volatile components, it may be necessary to carry out conditioning and testing with the specimen enclosed in a gas-tight specimen crucible which is resistant to high temperature and pressure.
Suitable conditioning procedures shall be agreed between involved parties and included in the test report.
8 Calibration
The calibration is specified in ISO 11357-1.
9 Procedure
9.1 General
The test may use one of two different methods, depending on what information is required:
— temperature-scanning method;
— isothermal method.
9.2 Temperature-scanning method
The temperature-scanning method is specified in ISO 11357-1.
Carry out a temperature scan, from ambient temperature to a temperature high enough to record the whole of the reaction peak, at a scan rate in the range 5 K/mm to 20 K/mm. Use the same scan rate for all tests which are intended to be comparative.
The final temperature shall be lower than the temperature corresponding to the onset of decomposition of the polymer.
A preliminary test can be useful in defining the decomposition temperature.
9.3 Isothermal method
9.3.1 General
The isothermal method can be carried out in two different ways once the specimen is loaded into the DSC sample holder:
— at constant temperature.ISO 11357-5 pdf download.