INTERNATIONAL STANDARD

Transcription

1 INTERNATIONAL STANDARD ISO Second edition Plastics Polyols for use in the production of polyurethanes Determination of hydroxyl number by NIR spectroscopy Plastiques Polyols pour la production de polyuréthannes Détermination de l indice d hydroxyle par spectroscopie dans le proche infrarouge Reference number ISO 2011

2 COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO s member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel Fax copyright@iso.org Web Published in Switzerland ii ISO 2011 All rights reserved

3 Contents Foreword... iv Introduction... v 1 Scope Normative references Terms and definitions Principle General Procedure employed Limitations Instrumentation General Light source and detector Spectrometer Sampling system Software Developing a calibration model Selection of calibration materials Reference method and reference values Determining wavelength regions and pathlength Reduction of sources of spectral variation Multivariate mathematical treatments Evaluating calibration models Validation of a multivariate calibration model Calibration transfer Calibration quality control Procedure General Calibration curve Measurement Illustrative results Precision of NIR estimated values Test report... 7 Annex A (informative) Illustrative results... 8 Annex B (informative) NIR spectral measurements...15 Annex C (informative) Spectrometers...16 Annex D (informative) Sampling systems...17 Annex E (informative) Selection of calibration materials...18 Annex F (informative) Multivariate analysis...20 Annex G (informative) Statistical tools used to optimize calibration models Annex H (informative) Sources of calibration and analysis error...25 Annex I (informative) Monitoring the performance of the instrument and calibration model Bibliography...27 Page ISO 2011 All rights reserved iii

4 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 15063:2004), which has been technically revised so that the document is no longer a guidance document (as it was in the first edition) but specifies the precise requirements which have to be met when determining the hydroxyl number of a polyol. Subject matter which has remained informative in nature has been transferred to informative annexes. iv ISO 2011 All rights reserved

5 Introduction International Standards have been published which deal with the determination of hydroxyl values of polyols and surface-active agents using conventional chemistry based on esterification reactions (ISO 14900, ISO 4326, ISO 4327, ISO 4629, ISO 2554 and ISO 6796). This International Standard provides a method for the determination of hydroxyl numbers of polyols using NIR spectroscopy. It is based on ASTM D6342 and on work conducted by laboratories associated with the Japan Urethane Raw Materials Association. ISO 2011 All rights reserved v

6 COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO s member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel Fax copyright@iso.org Web Published in Switzerland ii ISO 2011 All rights reserved

7 Contents Foreword... iv Introduction... v 1 Scope Normative references Terms and definitions Principle General Procedure employed Limitations Instrumentation General Light source and detector Spectrometer Sampling system Software Developing a calibration model Selection of calibration materials Reference method and reference values Determining wavelength regions and pathlength Reduction of sources of spectral variation Multivariate mathematical treatments Evaluating calibration models Validation of a multivariate calibration model Calibration transfer Calibration quality control Procedure General Calibration curve Measurement Illustrative results Precision of NIR estimated values Test report... 7 Annex A (informative) Illustrative results... 8 Annex B (informative) NIR spectral measurements...15 Annex C (informative) Spectrometers...16 Annex D (informative) Sampling systems...17 Annex E (informative) Selection of calibration materials...18 Annex F (informative) Multivariate analysis...20 Annex G (informative) Statistical tools used to optimize calibration models Annex H (informative) Sources of calibration and analysis error...25 Annex I (informative) Monitoring the performance of the instrument and calibration model Bibliography...27 Page ISO 2011 All rights reserved iii

8 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 15063:2004), which has been technically revised so that the document is no longer a guidance document (as it was in the first edition) but specifies the precise requirements which have to be met when determining the hydroxyl number of a polyol. Subject matter which has remained informative in nature has been transferred to informative annexes. iv ISO 2011 All rights reserved

9 Introduction International Standards have been published which deal with the determination of hydroxyl values of polyols and surface-active agents using conventional chemistry based on esterification reactions (ISO 14900, ISO 4326, ISO 4327, ISO 4629, ISO 2554 and ISO 6796). This International Standard provides a method for the determination of hydroxyl numbers of polyols using NIR spectroscopy. It is based on ASTM D6342 and on work conducted by laboratories associated with the Japan Urethane Raw Materials Association. ISO 2011 All rights reserved v

10 COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO s member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel Fax copyright@iso.org Web Published in Switzerland ii ISO 2011 All rights reserved

11 Contents Foreword... iv Introduction... v 1 Scope Normative references Terms and definitions Principle General Procedure employed Limitations Instrumentation General Light source and detector Spectrometer Sampling system Software Developing a calibration model Selection of calibration materials Reference method and reference values Determining wavelength regions and pathlength Reduction of sources of spectral variation Multivariate mathematical treatments Evaluating calibration models Validation of a multivariate calibration model Calibration transfer Calibration quality control Procedure General Calibration curve Measurement Illustrative results Precision of NIR estimated values Test report... 7 Annex A (informative) Illustrative results... 8 Annex B (informative) NIR spectral measurements...15 Annex C (informative) Spectrometers...16 Annex D (informative) Sampling systems...17 Annex E (informative) Selection of calibration materials...18 Annex F (informative) Multivariate analysis...20 Annex G (informative) Statistical tools used to optimize calibration models Annex H (informative) Sources of calibration and analysis error...25 Annex I (informative) Monitoring the performance of the instrument and calibration model Bibliography...27 Page ISO 2011 All rights reserved iii

12 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 15063:2004), which has been technically revised so that the document is no longer a guidance document (as it was in the first edition) but specifies the precise requirements which have to be met when determining the hydroxyl number of a polyol. Subject matter which has remained informative in nature has been transferred to informative annexes. iv ISO 2011 All rights reserved

13 Introduction International Standards have been published which deal with the determination of hydroxyl values of polyols and surface-active agents using conventional chemistry based on esterification reactions (ISO 14900, ISO 4326, ISO 4327, ISO 4629, ISO 2554 and ISO 6796). This International Standard provides a method for the determination of hydroxyl numbers of polyols using NIR spectroscopy. It is based on ASTM D6342 and on work conducted by laboratories associated with the Japan Urethane Raw Materials Association. ISO 2011 All rights reserved v

14 COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO s member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel Fax copyright@iso.org Web Published in Switzerland ii ISO 2011 All rights reserved

15 Contents Foreword... iv Introduction... v 1 Scope Normative references Terms and definitions Principle General Procedure employed Limitations Instrumentation General Light source and detector Spectrometer Sampling system Software Developing a calibration model Selection of calibration materials Reference method and reference values Determining wavelength regions and pathlength Reduction of sources of spectral variation Multivariate mathematical treatments Evaluating calibration models Validation of a multivariate calibration model Calibration transfer Calibration quality control Procedure General Calibration curve Measurement Illustrative results Precision of NIR estimated values Test report... 7 Annex A (informative) Illustrative results... 8 Annex B (informative) NIR spectral measurements...15 Annex C (informative) Spectrometers...16 Annex D (informative) Sampling systems...17 Annex E (informative) Selection of calibration materials...18 Annex F (informative) Multivariate analysis...20 Annex G (informative) Statistical tools used to optimize calibration models Annex H (informative) Sources of calibration and analysis error...25 Annex I (informative) Monitoring the performance of the instrument and calibration model Bibliography...27 Page ISO 2011 All rights reserved iii

16 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 15063:2004), which has been technically revised so that the document is no longer a guidance document (as it was in the first edition) but specifies the precise requirements which have to be met when determining the hydroxyl number of a polyol. Subject matter which has remained informative in nature has been transferred to informative annexes. iv ISO 2011 All rights reserved

17 Introduction International Standards have been published which deal with the determination of hydroxyl values of polyols and surface-active agents using conventional chemistry based on esterification reactions (ISO 14900, ISO 4326, ISO 4327, ISO 4629, ISO 2554 and ISO 6796). This International Standard provides a method for the determination of hydroxyl numbers of polyols using NIR spectroscopy. It is based on ASTM D6342 and on work conducted by laboratories associated with the Japan Urethane Raw Materials Association. ISO 2011 All rights reserved v