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Main text Cosmetics and personal care products are widely used globally. Although toxic elements are banned as intentional ingredients, they may exist as impurities either as contaminants in the raw ingredients, or as by-products of the manufacturing process. These toxic elements can accumulate in the body over time and cause adverse health effects. Different regions around the world have established relevant guidelines and regulations to safeguard the safety of consumers. Therefore, there is a need for metrology institutes to strengthen their measurement capabilities in this area. The supplementary comparison APMP.QM-S17: Elements in Lipstick Material was coordinated by the Health Sciences Authority, Singapore. Four measurands (arsenic, cadmium, mercury and lead) with maximum limits stated under the Association of Southeast Asian Nations (ASEAN) Guidelines on Limits of Contaminants for Cosmetics were chosen. Only one key comparison in the area of cosmetics (CCQM-K106: Lead, Arsenic and Mercury in Cosmetic Cream) was organised by the National Institute of Metrology (NIM) China in 2013. Hence, it was timely to organise another comparison in this area that covered cosmetics but in a different matrix. The study sample (lipstick) offered different analytical challenges as compared to the cream material used in the previous comparison. Moreover, it enabled National Metrology Institutes/Designated Institutes (NMIs/DIs) that did not participate in CCQM-K106 to demonstrate their measurement competencies. Seven institutes participated in the comparison for arsenic, nine for cadmium and lead, and eight for mercury. All participating NMIs/DIs employed microwave-assisted acid digestion for sample dissolution. Inductively coupled plasma mass spectrometry (ICP-MS) and sector field ICP-MS (SF-ICP-MS) were the two most commonly used instrumental techniques. Results of all participating NMIs/DIs were evaluated against the supplementary comparison reference value (SCRV). The SCRV and associated uncertainty were determined from results of NMIs/DIs that participated in the supplementary comparison using methods with demonstrated metrological traceability. For cadmium, mercury and lead, the median was used as estimator of the SCRVs. For arsenic, the arithmetic mean was used as estimator of the SCRV. The SCRVs (± expanded uncertainty) for arsenic, cadmium, mercury and lead (in mg/kg) were 4.188 (± 0.237), 2.0670 (± 0.0171), 2.732 (± 0.147) and 10.406 (± 0.080), respectively. The degree of equivalence and its associated uncertainty were calculated for each submitted result. Most participating institutes were able to demonstrate their capabilities in the determination of elements in lipstick material. Participating NMIs/DIs that have successfully participated in APMP.QM-S17 have demonstrated measurement capabilities in determining mass fraction of transition elements and metalloids/semi-metals, in mass fraction range from 0.1 mg/kg to 25 mg/kg in cosmetic matrices with high organic contents, such as lipstick. To 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 https://www.bipm.org/kcdb/. 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).

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.

Elements in serum serve as important biomarkers and reflect the well-being of an individual. The Key Comparison CCQM-K139 (Elements in human serum) aimed to enable participating National Metrology Institutes (NMIs) and Designated Institutes (DIs) to demonstrate their competence in the determination of elements (electrolytes and essential elements) in human serum. This is in line with the IAWG’s five year plan that a comparison under the Measurement Category 10 (Biological Fluids and Materials) is organised in order to best cover current and future CMCs. Table A summarises the list of measurands covered in this comparison, as well as the list of NMIs/DIs that registered and submitted their results for each measurand. For the analysis of sodium, copper, selenium and phosphorus, most of the participating institutes employed microwave-assisted digestion and acid digestion (with or without heating) sample dissolution. For the analysis of chloride, in addition to the microwave-assisted digestion and acid digestion, a wider variety of techniques were employed. These included matrix separation, alkaline extraction and coulometric titration. For sodium and phosphorus, inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES) were the two most commonly used instrumental techniques. Other techniques used included ion chromatography (IC) and flame atomic absorption spectrometry (FAAS). For chloride, copper and selenium, the most widely used instrumental technique was ICP-MS. Other techniques used included IC, titration, microcoulometry and ICP-OES. In this key comparison, the participating institutes have demonstrated the inorganic core capabilities in human serum matrix as listed in Table B.

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.