Abstract
Purity assay of high-purity materials (HPMs) of phthalic acid esters (PAEs) was carried out by means of a mass balance method. In this method, chromatographic methods such as gas chromatography-flame ionization detector (GC-FID) and/or high-performance liquid chromatography (HPLC) in combination with other methods such as Karl-Fischer (KF) titration and vacuum evaporation (VE) were applied. The sum of the impurities estimated by these methods allowed the estimation of the purity of the main component by difference. Seven PAEs with varying side chain structures and levels of impurities were analysed on a systematic way in which impurities were classified into several groups in terms of their abundance, availability of qualitative information and availability of authentic compounds, etc. The absolute quantity of each impurity was determined by GC-FID and/or HPLC based on the calibration made by the authentic compounds of impurities whenever available. The purities in mass fraction of these PAEs were certified at the National Metrology Institute of Japan (NMIJ), and the PAEs were registered as primary reference materials playing an essential role in linking the metrological traceability of the Japan Calibration Service System (JCSS) to the International System of Units (SI).
References
Mackintosh CE, Maldonado JA, Ikonomou MG, Gobas FAPC (2006) Environ Sci Technol 40:3481–3488
Liu Y, Guan Y, Yang Z, Cai Z, Mizuno T, Tsuno H, Zhu W, Zhang X (2006) Ecotoxicology 18:293–303
Internet: http://echa.europa.eu/chem_data/authorisation_process/candidate_list_table_en.asp
Internet: http://www.houko.com/00/01/S22/233.HTM
Kaarls R (2006) Accred Qual Assur 11:162–171
Internet: http://www.jcsslabo.or.jp/
Milton MJT, Quinn TJ (2001) Metrologia 38:289–296
Shimizu Y, Ohte Y, Bao X, Otsuka S, Kitamaki Y, Ishikawa K, Ihara T, Kato K (2008) Accred Qual Assur 13:389–396
Duewer D, Parris R, White E, May W, Elbaum H (2004) NIST Special Publication (SP 1012)
King B, Westwood S (2001) Fresenius J Anal Chem 370:194–199
International Organization for Standardization (2000) ISO guide 34: 2000 general requirements for the competence of reference material producers, 2nd edn. ISO, Geneva
International Organization for Standardization (1999) ISO/IEC 17025: 1999 General requirements for the competence of testing and calibration laboratories. ISO, Geneva
International Organization for Standardization (1989) ISO Guide 35: 1989 certification of reference materials-general and statistical principles, 2nd edn. ISO, Geneva
International Organization for Standardization (2006) ISO guide 35: 2006 reference materials-general and statistical principles for certification, 3rd edn. ISO, Geneva
Linsinger TP, Pauwels J, van der Veen AMH, Schimmel H, Lamberty A (2001) Accred Qual Assur 6:20–25
Fischer H (2011) History of the central limit theorem. Springer, New York
Rice J (1995) Mathematical statistics and data analysis, 2nd edn. Duxbury Press, Belmont
Internet: http://en.wikipedia.org/wiki/Central_limit_theorem
Wells RJ, Hook JM, Al-Deen TS, Hibbert DB (2002) J Agric Food Chem 50:3366–3374
Saito T, Ihara T, Koike M, Kinugasa S, Fujimine Y, Nose K, Hirai T (2009) Accred Qual Assur 14:79–86
Acknowledgments
We acknowledge the collaborators for the preparations of the candidate reference materials, and the NMIJ analysts who helped in the development of the CRMs described in this paper.
Author information
Authors and Affiliations
Corresponding author
Additional information
An erratum to this article can be found at http://dx.doi.org/10.1007/s00769-011-0776-z
Rights and permissions
About this article
Cite this article
Ishikawa, K., Hanari, N., Shimizu, Y. et al. Mass balance method for purity assay of phthalic acid esters: development of primary reference materials as traceability sources in the Japan Calibration Service System. Accred Qual Assur 16, 311–322 (2011). https://doi.org/10.1007/s00769-011-0767-0
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00769-011-0767-0