CCQM-K108.2014: determination of arsenic species and total arsenic in brown rice flour

Abstract

The key comparison CCQM-K108.2014 was organised by the Inorganic Analysis Working Group (IAWG) of CCQM to test the abilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of inorganic arsenic (i-As, sum of the amount of arsenite [As(III)] and arsenate [As(V)]), dimethylarsinic acid (DMAA), and total arsenic (total As) in brown rice flour. This was the follow-up comparison for the CCQM-K108 & CCQM-P147 (Cd, As, inorganic arsenic, and DMAA in brown rice flour).For total As, no strong outliers among the reported values were observed, and the distribution of the results was narrow, within 3% around the median. For i-As and DMAA, the distributions of the results were slightly wider than that for total arsenic, but no strong outliers among the reported values of i-As and DMAA were observed. Two potentially bias sources, an extraction efficiency of As species (the ratio of the sum of i-As and DMAA to total As) and the quality of primary standard of DMAA, were discussed. The extraction efficiency was estimated as the ratio of the sum of i-As and DMAA to total As. In the previous comparison (CCQM-K108 & CCQM-P147), the extraction efficiency was one of the largest bias sources for i-As and DMAA. However, in this study, all the extraction efficiencies estimated from the reported values were close to 100 %. Regarding the quality of the primary standard solutions, no significant difference was observed among the primary standard solution used by the participants. These results suggest the two potential bias sources mentioned above would not have been majors in this study, and then the technical issues in the previous comparison had been overcome.Accounting for relative expanded uncertainty, a comparability of measurement was successfully demonstrated by the participating NMIs and DIs for the measurement of total As at the level of less than 0.7 mg/kg, i-As at the level of less than 0.6 mg/kg, and DMAA at the level of less than 0.1 mg/kg. These are expected that total arsenic and i-As at mass fractions greater than 0.1 mg/kg and DMAA at mass fractions greater than 0.005 mg/kg in rice flour can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. Furthermore, the results of this key comparison can be utilised along with the IAWG core capability approach.Main textTo reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).