CCQM-K125 Elements in infant formula : Final report

The Key Comparison CCQM-K125 “Elements in Infant Formula” was undertaken to demonstrate the capability of participating national metrology institutes (NMIs) and designated institutes (DIs) in measuring the mass fraction the analytes at mg/kg levels in a test sample of infant formula by various analytical techniques. According to the Inorganic Analysis Working Group’s (IAWG’s) five-year plan, it was recommended to have a key comparison under the measurement service category of food for the year 2015. In this regards, the Government Laboratory, Hong Kong (GLHK) proposed to coordinate a new key comparison and a parallel-run pilot study (CCQM-K125 and CCQM-P159) for the determination of elements in infant formula. At the CCQM IAWG Meeting held in October 2014, the proposed study was agreed by IAWG members to be organised as the fifth benchmarking exercise. It was important for benchmarking to select two exemplary elements which were reasonably easy for many IAWG members to measure. Having further discussed with concerned IAWG members, potassium and copper were selected as the exemplary elements for examination, whereas iodine was an optional element for analysis. This key comparison facilitates claims by participants on the Calibration and Measurement Capabilities (CMCs) as listed in Appendix C of the Key Comparison Database (KCDB) under the Mutual Recognition Arrangement of the International Committee for Weights and Measures (CIPM MRA). Participants are requested to complete the pertinent Inorganic Core Capabilities Tables as a means of providing evidence for their CMC claims. For registration of CCQM-K125, total 25 institutes registered for the examination of the exemplary analytes of potassium and copper, while 12 institutes registered for the optional analyte of iodine. For submission of results, 25 institutes submitted the results for potassium, 24 institutes submitted the results for copper and 8 institutes submitted the results for iodine. The information about registration and submission of participants’ results is summarised in Table A. For examination of potassium and copper, most of the participants used microwave-assisted acid digestion methods for sample dissolution. A variety of instrumental techniques including inductively coupled plasma mass spectrometry (ICP-MS), isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), flame atomic emission spectrometry (FAES) and microwave plasma atomic emission spectroscopy (MP-AES) were employed by the participants for determination. For analysis of iodine, most of the participants used alkaline extraction methods for sample preparation. ICP-MS and ID-ICP-MS were used by the participants for the determination. For this key comparison, inorganic core capabilities were demonstrated by the concerned participants with respect to the methods including ICP-MS (without isotope dilution), ID-ICP-MS, ICP-OES, AAS, FAES and MP-AES on the determination of elements (potassium, copper and iodine) in a food matrix of infant formula

Final report of the CCQM-K145: toxic and essential elements in bovine liver

Liver plays a major role in metabolism and acts as a source of energy for the body by storing glycogen. With the growing interest and investigation in the biological effects in recent years, it is important and necessary to develop accurate and comparable analytical methods for elements in bio-samples. It has, however, been 10 years since the tissue sample (bovine liver) of CCQM-K49 key comparison. The purpose of CCQM-K145 is to ensure the comparable and traceable measurement results for essential and toxic elements such as P, S, Zn, Mn, Ni, Mo, Sr, Cr, Co, Pb, As and Hg in bovine liver among NMIs and other designated measurement bodies worldwide. The comparison was agreed by IAWG as 6th IAWG Benchmarking Exercise with Zn and Ni as exemplary elements at the meeting in Korea in the early October 2016. The results of CCQM-K145 are expected to cover the measurement capability and support CMCs claiming for inorganic elements in the similar biological tissue materials and food samples. 30 NMIs and DIs registered in CCQM-K145. With respect to the methodology, a variety of techniques such as IDMS, ICP-OES, ICP-MS(non-ID), AAS and NAA were adopted by the participants. For Zn, Ni, Sr, Pb and Hg measurements, most participants chose ID-ICP-MS method, which showed the better performance in terms of consistency and reliability of the measurement results. In aspect of the traceability for the measurement results in CCQM-K145, most participants used their own (in house) CRMs or other NMI's CRMs to guarantee trace to SI unit. Most participants used similar matrix CRMs for quality control or method validation. Base on different statistic way to calculate the reference mass fraction values and associated uncertainties for each measurand, removal of the suspected extreme values, and discussion at the IAWG meetings, the median values are proposed as the KCRV for Zn, Ni, Mn, Mo, Cr, Pb and Hg; the arithmetic mean values are proposed as the KCRV for P, S, Sr, Co and As. In general, the performances of the majority of CCQM-K145 participants are very good, illustrating their measurement capabilities for Zn, Ni, P, S, Mn, Mo, Sr, Cr, As, Co, Pb and Hg in a complex biological tissue matrix. Bovine liver contains many kinds of nutrients and microelements, it can be regarded as a typical representative material of biological tissue and food. In CCQM-K145, the analytes involved alkali metals and transition elements, metalloids / semi-metals and non metals with a range of mass fraction from mg/g to μg/kg. CCQM-K145 also tested the ability of NMIs/DIs to determine elements that were easy to be lost and polluted, and interfered significantly. The chemical pretreatment methods of samples used in the comparison is suitable for general food and biological matrix samples. A variety of measurement methods used in the comparison represent the main instrumental technology for elemental analysis. Therefore, for supporting CMC claim, CCQM-K145 is readily applicable to measurement of more elements in a wide range of biological materials (including liquids and solids) and meat products

CCQM-K124 Trace elements and ehromium speciation in drinking water : Part A: Trace elements in drinking water Part B: chromium speciation in drinking water. Final report

CCQM-K124 was an activity of the Inorganic Analysis Working Group (IAWG) and was jointly coordinated by the National Metrology Institute of Japan (NMIJ) and the Government Laboratory, Hong Kong SAR (GLHK). The Part A of CCQM-K124 was organized by NMIJ and trace elements in drinking water were the measurands. The Part A of the key comparison was undertaken for NMIs and DIs to demonstrate their capabilities in measuring part-per-billion level (in μg/kg) or part-per-million level (in mg/kg) of trace elements in drinking water. It should also facilitate the acquisition of claims in Calibration and Measurement Capabilities (CMCs) as listed in Appendix C of Key Comparison Database (KCDB) under the Mutual Recognition Arrangement of the International Committee of Weights and Measures (CIPM MRA). Results were submitted by 14 NMIs and nine DIs. The participants used different measurement methods, though most of them used direct measurement using inductively coupled plasma-optical emission spectrometry (ICP-OES), inductively coupled plasma-mass spectrometry (ICP-MS) and high resolution ICP-MS and isotope dilution technique with ICP-MS. Other methods were graphite furnace atomic absorption spectrophotometry (GFAAS) and flame atomic absorption spectrophotometry (FAAS). The results of B, Ca, Cr, As and Cd show good agreement except some outliers. Concerning Hg, instability was observed when the sample was stored in the light. And some participants observed instability of Mo. Therefore, it was agreed to abandon the Hg and Mo analysis as this sample was not satisfactory for KC. Accounting for relative expanded uncertainty, comparability of measurement results for each of B, Ca, Cr, As and Cd was successfully demonstrated by the participating NMIs or DIs. Furthermore, the results of this key comparison can be utilized along with the IAWG core capability approach. It is expected that arsenic, boron, cadmium, calcium and chromium at mass fractions greater than approximately 0.1 µg/kg, 1 µg/kg, 0.01 µg/kg, 1 mg/kg and 0.1 µg/kg respectively in drinking water and similar matrices (groundwater and river water etc.) 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