Abstract
A new simple method for chlorine percentage calculations (method C), from proton nuclear magnetic resonance (1H NMR) spectroscopy, has been established and applied to an industrial chlorinated paraffin (CP) mixture and 13 single-chain CPs of known carbon chain lengths. Two modified methods (method A and B), originating from the work of Sprengel et al., have been utilized on the same single-chain mixtures. All samples were analysed by 1H NMR and two-dimensional heteronuclear quantum coherence (HSQC) for this purpose. All three methods worked well for medium chlorinated (45–55% Cl) single-chain mixtures of known carbon chain lengths. Method A yielded the best result for mixtures of lower chlorine content (<45% Cl), method C gave better estimations for higher chlorine contents (>55% Cl). Compared to Mohr's titration, method A showed a deviation of 0.7–7.8% (3.6% average), method B 4.1–11.3% (7.0% average) and method C 0.6–11.6% (5.2% average), for all 13 single-chain mixtures. The new method C is the only method that could be applied for determining the chlorine percentage of industrial mixtures of multiple, unknown chain lengths.
Original language | English |
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Article number | 136312 |
Pages (from-to) | 1-7 |
Number of pages | 7 |
Journal | Chemosphere |
Volume | 308 |
Issue number | Part 3 |
Early online date | 9 Sept 2022 |
DOIs | |
Publication status | Published - Dec 2022 |
Bibliographical note
Funding Information:We would like to acknowledge the Norwegian research council ( NFR , 298628 ) and Eurostars ( E!113388-CHLOFFIN project ) for financial support. We also thank Quimica del Cinca for providing the C 14-15 chlorinated n-alkane mixtures and sharing their titration procedure, and Andrew Jaques of the Chlorinated Paraffins Industry Association (CPIA) for arranging the provision of the mixtures. The support from NFR to the Norwegian NMR Platform (226244/F50) is greatly appreciated.
Funding Information:
We would like to acknowledge the Norwegian research council (NFR, 298628) and Eurostars (E!113388-CHLOFFIN project) for financial support. We also thank Quimica del Cinca for providing the C14-15 chlorinated n-alkane mixtures and sharing their titration procedure, and Andrew Jaques of the Chlorinated Paraffins Industry Association (CPIA) for arranging the provision of the mixtures. The support from NFR to the Norwegian NMR Platform (226244/F50) is greatly appreciated.
Publisher Copyright:
© 2022 The Author(s)
Keywords
- Chlorinated paraffins
- Chlorine percentage calculation
- Industrial chlorinated paraffins
- NMR spectroscopy
- Reference standards