ISO_NWIPs-for-Ballot

ISO/NP

Contents

page

Foreword .......................................................................................................................................................................... 4 Introduction..................................................................................................................................................................... 5 1 Scope .................................................................................................................................................................... 6 2 Normative references .................................................................................................................................... 6 3 Terms and definitions.................................................................................................................................... 6 4 Principles ........................................................................................................................................................ 11 4.1 Nuclear magnetic resonance spectroscopy ............................................................................................... 11 4.2 1 H quantitative NMR ( 1 H qNMR).................................................................................................................... 13 5 Apparatus and equipment ........................................................................................................................ 16 5.1 General...................................................................................................................................................................... 16 5.2 Installation conditions and safety ................................................................................................................. 17 5.3 Outline of apparatus configuration............................................................................................................... 19 6 Preparation for 1 H qNMR........................................................................................................................... 20 6.1 General...................................................................................................................................................................... 20 6.2 Samples and reference material preparation with a balance ............................................................ 21 6.3 R eference materials ............................................................................................................................................. 22 6.4 Selection of a deuterated solvent................................................................................................................... 22 6.5 NMR tubes ............................................................................................................................................................... 23 6.6 NMR apparatus optimization .......................................................................................................................... 23 6.7 Weighing of sample and reference materials for qNMR ...................................................................... 23 6.8 Sample solution preparation ........................................................................................................................... 24 6.9 Measurement conditions for 1 H qNMR........................................................................................................ 25 7 Measurement ................................................................................................................................................. 26 7.1 1 H qNMR measurement condition settings ............................................................................................... 26 7.2 Measurement procedure................................................................................................................................... 26 7.3 Saving and processing FID data...................................................................................................................... 26 8 Analysis ............................................................................................................................................................ 27 8.1 General...................................................................................................................................................................... 27 8.2 Calculation............................................................................................................................................................... 27 9 Quality assurance requirements ............................................................................................................ 28 9.1 General...................................................................................................................................................................... 28 9.2 Qualification of the NMR apparatus.............................................................................................................. 28 9.3 System suitability test ........................................................................................................................................ 28 9.4 Ensuring traceability........................................................................................................................................... 29 9.5 Ensuring the reliability of analysis values ................................................................................................. 29 10 Test report ...................................................................................................................................................... 30 Bibliography ................................................................................................................................................................. 31

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