Vol.5 No.4 2013
54/70

Research paper : Standardization of environmental analysis methods of hazardous chemicals (S. Taniyasu et al.)−278−Synthesiology - English edition Vol.5 No.4 (2013) Industrial Competitiveness and Environmental Preservation,” the necessity for describing the results of the quality control studies was indicated from the perspective of meeting the ISO standard that requires the inclusion of the performance data of the standardized analysis method. This was indicated as part of the revision of the conventional JIS system for the measurements of water quality and atmosphere.4.1 Quality control study for nonylphenolFor NP, participation in the quality control study for the analysis of NP isomers in the water sample was solicited under the project leadership of Japan for ISO/TC147/SC2/WG17 (phenols) from July to September 2008. There were applications from 17 institutes from Japan and overseas. After conducting statistical analysis of the study results, the results were organized and reported to the participating institutes as an interim report, and a report was submitted to the ISO/TC147/SC2/WG17 as the performance data for the ISO/DIS 24293 (draft standard) in December 2008. The intermediate precision coefficient of variation (CVr) that looked at the variation of the analysis value within a laboratory was average of 10 % (minimum 4.4 % ~ maximum 21.6 %), and no difference was observed in intermediate precision due to the type of sample and difference in isomer composition. On the other hand, the reproducibility coefficient of variation (CVR) that looked at the variation of the analysis results when the measurements were done among different laboratories was approximately 30 % or less, but it surpassed 50 % in some isomers. Particularly, there was large variation in the inter-laboratory variation of isomers with small composition among the NP mixtures (NP8 and NP12, refer to Fig. 5), and the reproducibility tended to be poor. It was reported that there were slight differences in the isomer separation by different column manufacturers or due to the deterioration of the column even when equivalent separation columns were used. In this analysis method where the NP mixture was used as the quantifying standard, the effect of the slight difference in the peak separation capacity on the quantitative value could not be prevented for some isomers.[22]To check the effect on the analysis precision due to the difference of SS amount, river water (SS amount of 13 mg/L) and influx water of sewage treatment plant that contained large amount of SS (SS amount of 140 mg/L) were used as the quality control study samples. As described above, poor reproducibility was seen in some isomers (NP8 and NP12, refer to Fig. 5), but good results of CVR within 30 % was obtained for other isomers.[22]This analysis method was published as the ISO 24293:2009[1] in July 2009 after obtaining 15 votes of approval among 17 countries in the final vote. This analysis method was b) Example of separation using the multimode (reverse phase + anion exchange) column (JJ50 2D) (elution occurs in the order from long to short chain)a) Example of separation using the reverse phase column (Betasil C18) (elution occurs in the order from short to long chain)14.0012.0010.006.004.00PFOcDAPFOcDAPFHxDAPFHxDAPFTeDAPFTeDAPFTrDAPFTrDAPFDoDAPFDoDAPFUnDAPFUnDAPFDAPFDAPFNAPFNAPFOAPFOAPFHpAPFHpAPFHxAPFHxAPFPeAPFPeAPFBAPFBATime(min)Time(min)≫14.0012.0010.006.008.004.00Fig. 7 Example of the separation by chromatograph for perfluoroalkylcarbonic acid

元のページ 

page 54

※このページを正しく表示するにはFlashPlayer10.2以上が必要です