Interlaboratory Comparison Exercise Research Articles

Dose conversion in retrospective dosimetry: Results and implications from an inter-laboratory comparison featuring a realistic exposure scenario

Dose conversion coefficients attempt to harmonize the material-, location-, and exposure-dependent results from retrospective dosemeters. The issues and uncertainties arising from dose conversion are explored within the framework of an interlaboratory comparison exercise in which mobile phones were positioned around anthropomorphic phantoms and exposed to non-uniform photon fields, with the glass and resistors they contain employed as fortuitous dosemeters. The difficulties of adopting pre-calculated tables of generic conversion coefficients are evaluated first, and then compared against those arising through the use of bespoke data derived by Monte Carlo modelling, and also against not converting the doses measured by the phones. It is seen that the different subjective choices that users might make when selecting ‘optimal’ generic data can lead to a significant source of uncertainty (up to around 70 %), though may be improved (to around 30 %) by appropriate quality controls. Use of generic coefficients typically led to over-estimates of the organ doses: an average discrepancy of ca. a factor of 2 was found, but this is still better than the factor of around 3 observed when no conversion coefficients were applied. Use of bespoke conversion factors led to the best estimates of organ doses, although they still over-estimated by approximately 1.5 on average, and an uncertainty of around 20 % was associated with generating their values. Overall, applying bespoke conversion data improves but does not guarantee correct dose categorization of individuals, with the inconsistences in the measured results found generally to be the limiting factor in obtaining accurate dose assessments.

Interlaboratory comparison of gross alpha/beta activity of drinking water over a decade

Interlaboratory comparison exercises for determining the gross alpha and beta activity concentrations in drinking water, organized by the National Institute for Radiological Protection (NIRP), China CDC, have been carried out since 2012. The purpose of this study is to assess the accuracy and precision of gross alpha and beta analyses of low-level radioactivity concentrations. Natural water samples were used for the comparison, and the performance of the participating laboratories was evaluated with respect to the reference values using the Z-score performance indicator. The comparison data from 2012 to 2022 were analyzed, where the percentage of laboratories with acceptable results was 80–92%, and the dispersion of the measurement results across laboratories became smaller over time. The results demonstrate that these exercises can help laboratories to resolve issues in gross α/β analysis and improve the consistency of the measurement results.

LBDNet interlaboratory comparison for the dicentric chromosome assay by digitized image analysis applying weighted robust statistical methods

Purpose This interlaboratory comparison was conducted to evaluate the performance of the Latin-American Biodosimetry Network (LBDNet) in analyzing digitized images for scoring dicentric chromosomes from in vitro irradiated blood samples. The exercise also assessed the use of weighted robust algorithms to compensate the uneven expertise among the participating laboratories. Methods Three sets of coded images obtained through the dicentric chromosome assay from blood samples irradiated at 1.5 Gy (sample A) and 4 Gy (sample B), as well as a non-irradiated whole blood sample (sample C), were shared among LBDNet laboratories. The images were captured using the Metafer4 platform coupled with the AutoCapt module. The laboratories were requested to perform triage scoring, conventional scoring, and dose estimation. The dose estimation was carried out using either their laboratory calibration curve or a common calibration curve. A comparative statistical analysis was conducted using a weighted robust Hampel algorithm and z score to compensate for uneven expertise in dicentric analysis and dose assessment among all laboratories. Results Out of twelve laboratories, one had unsatisfactory estimated doses at 0 Gy, and two had unsatisfactory estimated doses at 1.5 Gy when using their own calibration curve and triage scoring mode. However, all doses were satisfactory at 4 Gy. Six laboratories had estimated doses within 95% uncertainty limits at 0 Gy, seven at 1.5 Gy, and four at 4 Gy. While the mean dose for sample C was significantly biased using robust algorithms, applying weights to compensate for the laboratory’s analysis expertise reduced the bias by half. The bias from delivered doses was only notable for sample C. Using the common calibration curve for dose estimation reduced the standard deviation (s*) estimated by robust methods for all three samples. Conclusions The results underscore the significance of performing interlaboratory comparison exercises that involve digitized and electronically transmitted images, even when analyzing non-irradiated samples. In situations where the participating laboratories possess different levels of proficiency, it may prove essential to employ weighted robust algorithms to achieve precise outcomes.

Interlaboratory comparison exercises for organically-bound tritium in the development of reference materials of environmental samples

The complex behavior of tritium and the probability of increasing tritium concentrations released in the environment were the promotors for the research and development of laboratory methods that enable to accurately determine the various forms of tritium including organically-bound tritium (OBT) for public and regulatory assurance. The measurement of tritium is a key step for dose and risk assessment. The Cernavoda Nuclear Power Plant (NPP) in Romania improved preparation methods and tested environmental matrices for OBT analysis through intercomparison exercises. This paper describes the international Organically-Bound Tritium (OBT) intercomparison exercise, organized by the Cernavoda Nuclear Power Plant (NPP) in 2019–2020, using fruit sample (quince) from Cernavoda town. Evaluation of the results from the participating laboratories was performed using both robust analysis (Algorithm A) method described in the ISO 13528:2015 standard and ANOVA method. The results obtained are encouraging as an increased number of participating laboratories did not change the observed dispersion of the results for activity concentration level around 50 Bq/L of combustion water. The stability of the remaining sample will be checked in time to investigate its use as a reference material for OBT analysis at the environmental levels.

An inter-laboratory comparison between 13 international laboratories for eight components relevant for hydrogen fuel quality assessment

The quality of the hydrogen delivered by refuelling stations is critical for end-users and society. The purity of the hydrogen dispensed at hydrogen refuelling points should comply with the technical specifications included in the ISO 14687:2019 and EN 17124:2022 standards. Once laboratories have set up methods, they need to verify their performances, for example through participation in interlaboratory comparisons. Due to the challenge associated with the production of stable reference materials and transport of these which are produced in hydrogen at high pressure (>10 bar), interlaboratory comparisons have been organized in different steps, with increasing extent.This study describes an inter-laboratory comparison exercise for hydrogen fuel involving a large number of participants (13 laboratories), completed in less than a year and included eight key contaminants of hydrogen fuel at level close to the ISO14687 threshold. These compounds were selected based on their high probability of occurrence or because they have been found in hydrogen fuel samples. For the results of the intercomparison, it appeared that fully complying with ISO 21087:2019 is still challenging for many participants and highlighted the importance of organising these types of exercises. Many laboratories performed corrective actions based on their results, which in turn significantly improved their performances.

Stable isotope composition of pesticides in commercial formulations: The ISOTOPEST database

By assessing the changes in stable isotope compositions within individual pesticide molecules, Compound Specific Isotope Analysis (CSIA) holds the potential to identify and differentiate sources and quantify pesticide degradation in the environment. However, the environmental application of pesticide CSIA is limited by the general lack of knowledge regarding the initial isotopic composition of active substances in commercially available formulations used by farmers. To address this limitation, we established a database aimed at cataloguing and disseminating isotopic signatures in commercial formulations to expand the use of pesticide CSIA. Our study involved the collection of 25 analytical standards and 120 commercial pesticide formulations from 23 manufacturers. Subsequently, 59 commercial formulations and 25 standards were extracted, and each of their active substance was analyzed for both δ13C (n = 84) and δ15N CSIA (n = 43). The extraction of pesticides did not cause significant isotope fractionation (Δ13C and Δ15N < 1‰). Incorporating existing literature data, stable carbon and nitrogen isotope signatures varied in a relatively narrow range among pesticide formulations for different pesticides (Δ13C and Δ15N < 10‰) and within different formulations for a single substance (Δ13C and Δ15N < 2‰). Overall, this suggests that pesticide CSIA is more suited for identifying pesticide transformation processes rather than differentiating pesticide sources. Moreover, an inter-laboratory comparison showed similar δ13C (Δ13C ≤ 1.2 ‰) for the targeted substances albeit varying GC-IRMS instruments. Insignificant carbon isotopic fractionation (Δ13C < 0.5‰) was observed after 4 years of storing the same pesticide formulations, confirming their viability for long-term storage at 4 °C and future inter-laboratory comparison exercises. Altogether, the ISOTOPEST database, in open access for public use and additional contributions, marks a significant advancement in establishing an environmentally relevant pesticide CSIA approach.

Certified reference material (CRM) of tea powder (BARC - D3201) for K, Ca, P, Mg, Mn, Al, Fe, Ba, Zn, Cu, Sr, Pb, As, Cd, and Hg: Method validation and its production

A certified reference material (CRM) for major and trace elements in black tea powder has been developed at National Centre for Compositional Characterization of Materials/Bhabha Atomic Research Centre (BARC), Hyderabad. The study describes an acid assisted microwave digestion of tea powder followed by quantitation of K, Ca, P, Mg, Mn, Al, Fe, Ba, Zn, Cu and Sr by ICP-AES; Pb, Cd by GFAAS and As, Hg by AFS in the digests. The method was validated in terms of selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), trueness, precision, traceability, ruggedness and combined uncertainty using a CRM of tea powder (NMIJ CRM 7505-a) and spike recovery studies. The obtained values of LOQ ranged from 0.018 % m/m for Ca to 0.35mg kg−1 for Hg. Precision of the method was found to be <5% for all the analytes (K, Ca, P, Mg, Mn, Al, Fe, Ba, Zn, Cu, Sr, Cd and Hg) excepting for Pb and As (6.5 % at 95% confidence level). The obtained LOQ values, trueness and precision established that the validated method could be used for the characterization of candidate tea CRM during homogeneity and stability studies. Candidate tea CRM (∼3.6 Kg) was processed (which included spiking, drying grinding and sieving) and its homogeneity was assessed at various levels with respect to all 15 property values. The assignment of the property values for each element was carried out after an interlaboratory comparison exercise (ILCE), where 11 laboratories from various government and private sectors participated. A total of four techniques inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES), graphite-furnace atomic-absorption spectrometry (GFAAS) and atomic-fluorescence spectrometry (AFS) were used during ILCE. Property values were assigned for 14 elements (K, Ca, P, Mg, Mn, Al, Fe, Ba, Zn, Cu, Sr, Pb, Cd, and Hg) along with combined uncertainties. The concentration with expanded uncertainties of the property values were between 0.458 ± 0.025 for Ca (% m/m) to 0.60 ± 0.084 mg kg−1 for Hg. Long-term stability studies suggested that the produced tea CRM is stable at storage temperature (4 °C) for the last two years, whereas, short-term stability studies (at temperatures 4, 25 and 40 °C) established its transportation stability at tested temperatures for a period of three weeks. Preparation and certification of tea CRM (BARC-D3201) was carried out in accordance with ISO Guides 17034 and 35.

Validation and interlaboratory comparison of anticoagulant rodenticide analysis in animal livers using ultra-performance liquid chromatography-mass spectrometry.

Anticoagulant rodenticides (ARs) are used to control rodent populations. Poisoning of non-target species can occur by accidental consumption of commercial formulations used for rodent control. A robust method for determining ARs in animal tissues is important for animal postmortem diagnostic and forensic purposes. We evaluated an ultra-performance liquid chromatography coupled with mass spectrometry (UPLC-MS) method to quantify 8 ARs (brodifacoum, bromadiolone, chlorophacinone, coumachlor, dicoumarol, difethialone, diphacinone, warfarin) in a wide range of animal (bovine, canine, chicken, equine, porcine) liver samples, including incurred samples. We further evaluated UPLC-MS in 2 interlaboratory comparison (ILC) studies; one an ILC exercise (ICE), the other a proficiency test (PT). The limits of detection of UPLC-MS were 0.3-3.1 ng/g, and the limits of quantification were 0.8-9.4 ng/g. The recoveries obtained using UPLC-MS were 90-115%, and relative SDs were 1.2-13% for each of the 8 ARs for the 50, 500, and 2,000 ng/g spiked liver samples. The overall accuracy from the laboratories participating in the 2 ILC studies (4 and 11 laboratories for ICE and PT studies, respectively) were 86-118%, with relative repeatability SDs of 3.7-11%, relative reproducibility SDs of 7.8-31.2%, and Horwitz ratio values of 0.5-1.5. Via the ILC studies, we verified the accuracy of UPLC-MS for AR analysis in liver matrices and demonstrated that ILC can be utilized to evaluate performance characteristics of analytical methods.

Successful Detection of Delta and Omicron Variants of SARS-CoV-2 by Veterinary Diagnostic Laboratory Participants in an Interlaboratory Comparison Exercise.

Throughout the COVID-19 pandemic, veterinary diagnostic laboratories have tested diagnostic samples for SARS-CoV-2 both in animals and over 6 million human samples. An evaluation of the performance of those laboratories is needed using blinded test samples to ensure that laboratories report reliable data to the public. This interlaboratory comparison exercise (ILC3) builds on 2 prior exercises to assess whether veterinary diagnostic laboratories can detect Delta and Omicron variants spiked in canine nasal matrix or viral transport medium. The ILC organizer was an independent laboratory that prepared inactivated Delta variant at levels of 25 to 1000 copies per 50 µL of nasal matrix for blinded analysis. Omicron variant at 1000 copies per 50 µL of transport medium was also included. Feline infectious peritonitis virus (FIPV) RNA was used as a confounder for specificity assessment. Fourteen test samples were prepared for each participant. Participants used their routine diagnostic procedures for RNA extraction and real-time reverse transcriptase-PCR. Results were analyzed according to International Organization for Standardization (ISO) 16140-2:2016. Overall, laboratories demonstrated 93% detection for Delta and 97% for Omicron at 1000 copies per 50 µL. Specificity was 97% for blank samples and 100% for blank samples with FIPV. No differences in Cycle Threshold (Ct) values were significant for samples with the same virus levels between N1 and N2 markers, nor between the 2 variants. The results indicated that all ILC3 participants were able to detect both Delta and Omicron variants. The canine nasal matrix did not significantly affect SARS-CoV-2 detection.

Data quality control considerations in multivariate environmental monitoring: experience of the French coastal network SOMLIT

IntroductionWhile crucial to ensuring the production of accurate and high-quality data—and to avoid erroneous conclusions—data quality control (QC) in environmental monitoring datasets is still poorly documented.MethodsWith a focus on annual inter-laboratory comparison (ILC) exercises performed in the context of the French coastal monitoring SOMLIT network, we share here a pragmatic approach to QC, which allows the calculation of systematic and random errors, measurement uncertainty, and individual performance. After an overview of the different QC actions applied to fulfill requirements for quality and competence, we report equipment, accommodation, design of the ILC exercises, and statistical methodology specially adapted to small environmental networks (&amp;lt;20 laboratories) and multivariate datasets. Finally, the expanded uncertainty of measurement for 20 environmental variables routinely measured by SOMLIT from discrete sampling—including Essential Ocean Variables—is provided.Results, Discussion, ConclusionThe examination of the temporal variations (2001–2021) in the repeatability, reproducibility, and trueness of the SOMLIT network over time confirms the essential role of ILC exercises as a tool for the continuous improvement of data quality in environmental monitoring datasets.

Production of Bauxite Certified Reference Material (BARC‐B1201) for Nine Property Values (Al2O3, Fe2O3, SiO2, TiO2, V2O5,MnO, Cr2O3, MgO and LOI) Traceable to SI Units

The National Centre for Compositional Characterisation of Materials (NCCCM) / Bhabha Atomic Research Centre (BARC) and National Aluminium Company Limited (NALCO), India have produced an Indian origin bauxite certified reference material (CRM), referred to as BARC‐B1201, certified for major (Al2O3, Fe2O3, SiO2, TiO2, loss on ignition ‐ LOI) and trace contents (V2O5, MnO, Cr2O3, MgO). Characterisation was undertaken by strict adherence to ISO Guides. A method previously developed and validated in our laboratory, using single step bauxite dissolution and subsequent quantitation (of Al2O3, Fe2O3, SiO2, TiO2, V2O5, MnO, Cr2O3 and MgO) by ICP‐AES (SSBD ICP‐AES) was used for homogeneity studies and an inter‐laboratory comparison exercise (ILCE) of the candidate CRM. LOI was determined by thermo‐gravimetric analysis. Property values were assigned after an ILCE with participation from seventeen reputed government and private sector laboratories in India. The CRM was certified for nine property values: Al2O3, Fe2O3, SiO2, TiO2, V2O5, MnO, Cr2O3, MgO and LOI, which are traceable to SI units.

RENEB Inter-Laboratory Comparison 2021: The Gamma-H2AX Foci Assay.

The Running the European Network of biological and retrospective dosimetry (RENEB) network of laboratories has a range of biological and physical dosimetry assays that can be deployed in the event of a radiation incident to provide exposure assessment. To maintain operational capability and provide training, RENEB runs regular inter-laboratory comparison (ILC) exercises. The RENEB ILC2021 was carried out with all the biological and physical dosimetry assays employed in the network. The focus of this paper is to evaluate the results from 6 laboratories that took part using the gamma-H2AX radiation-induced foci assay. For two laboratories this was their first RENEB ILC. Blood samples were homogenously exposed to 240 kVp X rays (1 Gy/min) to provide calibration data, (0-4 Gy), and a few weeks later three blind coded test samples, (0, 1.2 and 3.5 Gy) were prepared. All samples were allowed a 2 h repair time at 37°C before being transported, on ice packs, to the participating laboratories. On arrival, the samples were processed, scored either manually or automatically for gamma-H2AX foci and dose estimates for the 3 blind coded samples sent to the organizing laboratory. The temperature of samples during transit and the time taken to report the dose estimates were recorded. Subsequent examination of the data from each laboratory used the doses estimates to assign triage categories to the samples. After receipt of the samples, the quickest report of dose estimates was 4.6 h. Analysis of variance revealed that the laboratory carrying out the assay had a significant effect on the foci yield (P < 0.001) for the calibration data, but not on the dose estimates of the blind coded samples (P = 0.101). All laboratories correctly identified the unirradiated and irradiated samples, although the dose estimates for the latter tended to under-estimate the dose. Two participants seriously under-estimated the dose for the highly exposed sample, which resulted in the sample being placed in the lowest triage category not the highest. However, this under-estimation resulted from the samples not remaining cold during shipment, due to a delay in transit and was not related to the experience of the participating laboratory. Overall, the RENEB network laboratories have demonstrated it is possible to quickly identify a recent whole-body acute exposure using the gamma-H2AX assay within the conditions of the ILC. In addition, an ILC provides a useful training and harmonization exercise for laboratories.

A Single Step Acid Assisted Microwave Digestion Method for the Complete Dissolution of Bauxite and Quantitation of its Composition (Al2O3, Fe2O3, SiO2, TiO2, Cr2O3, MgO, MnO and V2O5) by ICP‐AES

An acid assisted microwave‐based method for the complete dissolution of bauxite using mixture of H2SO4, H3PO4 and HF acids in a single step was developed for the determination of various analytes (Al2O3, Fe2O3, SiO2, TiO2, Cr2O3, MgO, MnO and V2O5) using ICP‐AES. The method was validated with respect to ruggedness, linearity, trueness, precision, limit of detection (LOD), limit of quantification (LOQ), working range and measurement uncertainties by analysing a bauxite reference material (Alcan BXT‐12) and four certified reference materials (IPT‐131, BXBA‐4, NIST SRM 600, NIST SRM 697). The expanded uncertainties obtained for Al2O3 (40.0%), Fe2O3 (17.0%), SiO2 (20.3%), TiO2 (1.31%), Cr2O3 (0.024%), MgO (0.05), MnO (0.013), and V2O5 (0.60%), were 0.80, 0.40, 0.50, 0.033, 0.0008, 0.002, 0.0007 and 0.002 respectively, which are fit for the intended use to characterise bauxite. The developed method was also evaluated through participation in an interlaboratory comparison exercise organised by the Jawaharlal Nehru Aluminium Research Development and Design Centre (JNARDDC), Nagpur, India, using bauxite sample (BXT‐JNA), with satisfactory z‐scores achieved.

RENEB Inter-Laboratory Comparison 2021: The Gene Expression Assay.

Early and high-throughput individual dose estimates are essential following large-scale radiation exposure events. In the context of the Running the European Network for Biodosimetry and Physical Dosimetry (RENEB) 2021 exercise, gene expression assays were conducted and their corresponding performance for dose-assessment is presented in this publication. Three blinded, coded whole blood samples from healthy donors were exposed to 0, 1.2 and 3.5 Gy X-ray doses (240 kVp, 1 Gy/min) using the X-ray source Yxlon. These exposures correspond to clinically relevant groups of unexposed, low dose (no severe acute health effects expected) and high dose exposed individuals (requiring early intensive medical health care). Samples were sent to eight teams for dose estimation and identification of clinically relevant groups. For quantitative reverse transcription polymerase chain reaction (qRT-PCR) and microarray analyses, samples were lysed, stored at 20°C and shipped on wet ice. RNA isolations and assays were run in each laboratory according to locally established protocols. The time-to-result for both rough early and more precise later reports has been documented where possible. Accuracy of dose estimates was calculated as the difference between estimated and reference doses for all doses (summed absolute difference, SAD) and by determining the number of correctly reported dose estimates that were defined as ±0.5 Gy for reference doses <2.5 Gy and ±1.0 Gy for reference doses >3 Gy, as recommended for triage dosimetry. We also examined the allocation of dose estimates to clinically/diagnostically relevant exposure groups. Altogether, 105 dose estimates were reported by the eight teams, and the earliest report times on dose categories and estimates were 5 h and 9 h, respectively. The coefficient of variation for 85% of all 436 qRT-PCR measurements did not exceed 10%. One team reported dose estimates that systematically deviated several-fold from reported dose estimates, and these outliers were excluded from further analysis. Teams employing a combination of several genes generated about two-times lower median SADs (0.8 Gy) compared to dose estimates based on single genes only (1.7 Gy). When considering the uncertainty intervals for triage dosimetry, dose estimates of all teams together were correctly reported in 100% of the 0 Gy, 50% of the 1.2 Gy and 50% of the 3.5 Gy exposed samples. The order of dose estimates (from lowest to highest) corresponding to three dose categories (unexposed, low dose and highest exposure) were correctly reported by all teams and all chosen genes or gene combinations. Furthermore, if teams reported no exposure or an exposure >3.5 Gy, it was always correctly allocated to the unexposed and the highly exposed group, while low exposed (1.2 Gy) samples sometimes could not be discriminated from highly (3.5 Gy) exposed samples. All teams used FDXR and 78.1% of correct dose estimates used FDXR as one of the predictors. Still, the accuracy of reported dose estimates based on FDXR differed considerably among teams with one team's SAD (0.5 Gy) being comparable to the dose accuracy employing a combination of genes. Using the workflow of this reference team, we performed additional experiments after the exercise on residual RNA and cDNA sent by six teams to the reference team. All samples were processed similarly with the intention to improve the accuracy of dose estimates when employing the same workflow. Re-evaluated dose estimates improved for half of the samples and worsened for the others. In conclusion, this inter-laboratory comparison exercise enabled (1) identification of technical problems and corrections in preparations for future events, (2) confirmed the early and high-throughput capabilities of gene expression, (3) emphasized different biodosimetry approaches using either only FDXR or a gene combination, (4) indicated some improvements in dose estimation with FDXR when employing a similar methodology, which requires further research for the final conclusion and (5) underlined the applicability of gene expression for identification of unexposed and highly exposed samples, supporting medical management in radiological or nuclear scenarios.

Innovative reference materials for method validation in microplastic analysis including interlaboratory comparison exercises

Reference materials (RMs) are vital tools in the validation of methods used to detect environmental pollutants. Microplastics, a relatively new environmental pollutant, require a variety of complex approaches to address their presence in environmental samples. Both interlaboratory comparison (ILC) studies and RMs are essential to support the validation of methods used in microplastic analysis. Presented here are results of quality assurance and quality control (QA/QC) performed on two types of candidate microplastic RMs: dissolvable gelatin capsules and soda tablets. These RMs have been used to support numerous international ILC studies in recent years (2019–2022). Dissolvable capsules containing polyethylene terephthalate (PET), polyvinyl chloride (PVC), polyethylene (PE), and polystyrene (PS), in different size fractions from 50 to 1000 µm, were produced for one ILC study, obtaining relative standard deviation (RSD) from 0 to 24%. The larger size fraction allowed for manual addition of particles to the capsules, yielding 0% error and 100% recovery during QA/QC. Dissolvable capsules were replaced by soda tablets in subsequent ILC studies and recovery test exercises because they were found to be a more reliable carrier for microplastic RMs. Batches of soda tablets were produced containing different single and multiple polymer mixtures, i.e., PE, PET, PS, PVC, polypropylene (PP), and polycarbonate (PC), with RSD ranging from 8 to 21%. Lastly, soda tablets consisting of a mixture of PE, PVC, and PS (125–355 µm) were produced and used for recovery testing during pretreatment of environmental samples. These had an RSD of 9%. Results showed that soda tablets and capsules containing microplastics >50 µm could be produced with sufficient precision for internal recovery tests and external ILC studies. Further work is required to optimize this method for smaller microplastics (< 50 µm) because variation was found to be too large during QA/QC. Nevertheless, this approach represents a valuable solution addressing many of the challenges associated with validating microplastic analytical methods.

Instrument comparability of non-targeted UHPLC-HRMS for wine authentication

Instrument comparability is a major prerequisite for the harmonization of non-targeted analytical approaches for food authentication. While non-targeted liquid chromatography coupled with mass spectrometry (LC-MS) is a powerful and widely used technique in authenticity studies, inter-laboratory or instrument comparison exercises are rare. For the first time, in the present study a comparison of two LC-MS platforms using identical setups and conditions except for the mass spectrometer (Orbitrap Q Exactive™ Focus vs. Plus) was carried out in order to assess the impact of instrumental differences on the classification of grape varieties in wine. A set of 201 red and white wine samples comprising 10 grape varieties was analyzed with both platforms and subjected to multivariate statistical analysis. Using unsupervised and supervised methods, the same correlation pattern between samples was observed with both platforms. Partial Least Squares – Discriminant Analysis (PLS-DA) classification models achieved comparable accuracies in the internal validation (90–95%). The percentage of common discriminating features was about 46–69% between both platforms. The common features were used to merge data from both instruments and joint PLS-DA models produced excellent results. The prediction of data from one platform with the model from the other platform, as well as a model using data from both platforms, resulted in correct classification rates of 92–98%. Putative identification of common features was performed to determine potential marker substances for grape varieties. With this study, a first step towards harmonization of non-targeted LC-MS approaches for wine authentication is taken, advancing their potential application in official food control.

Interlaboratory comparison exercise using OSL personal dosimeters between the LMRI-DEN/UFPE, Brazil, and LCD/LAF-RAM, Nicaragua.

The aim of this paper is to present the results obtained in the intercomparison exercise organized by the Ionizing Radiation Metrology Laboratory at the Federal University of Pernambuco (LMRI-DEN/UFPE) and the Radiation Physics and Metrology Laboratory (LAF-RAM) of the National Autonomous University of Nicaragua, Managua (UNAN-Managua). The comparison aimed to assess the technical capabilities of the Dosimetry Calibration Laboratory (LCD) belonging to LAF-RAM for the irradiation of personal dosimeters in terms of Hp(d) magnitudes with a 137Cs radiation beam. The BeO OSL dosimeters were shipped by LMRI-DEN/UFPE to LAF-RAM for irradiation in March 2020. The evaluation of the Z-Score value obtained in the intercomparison was satisfactory for all irradiations of the dosimeters in the Hp (d) magnitude.

The reproducibility of corrosion testing in supercritical water—Results of a second international interlaboratory comparison exercise

Supercritical water-cooled reactor candidate materials are typically corrosion-resistant alloys whose mass changes in supercritical water fluctuate around zero. A previous interlaboratory corrosion experiment exercise revealed large scatter in mass change results between laboratories. Here, we reduced systemic differences between laboratories by unilateral preparation of coupons and unilateral chemical cleaning. Type 310S stainless steel and Alloy 800HT test coupons were exposed for 1000 h to 550 °C, 25 MPa, deaerated water. Average mass loss for 310S and 800HT was 38 ± 26 and 51 ± 31 mg/dm2, respectively. Differences in mass transfer, galvanic and local corrosion, and average coupon temperature may explain the poor reproducibility.

A comparative validation of biodosimetry and physical dosimetry techniques for possible triage applications in emergency dosimetry

Large-scale radiological accidents or nuclear terrorist incidents involving radiological or nuclear materials can potentially expose thousands, or hundreds of thousands, of people to unknown radiation doses, requiring prompt dose reconstruction for appropriate triage. Two types of dosimetry methods namely, biodosimetry and physical dosimetry are currently utilized for estimating absorbed radiation dose in humans. Both methods have been tested separately in several inter-laboratory comparison exercises, but a direct comparison of physical dosimetry with biological dosimetry has not been performed to evaluate their dose prediction accuracies. The current work describes the results of the direct comparison of absorbed doses estimated by physical (smartphone components) and biodosimetry (dicentric chromosome assay (DCA) performed in human peripheral blood lymphocytes) methods. For comparison, human peripheral blood samples (biodosimetry) and different components of smartphones, namely surface mount resistors (SMRs), inductors and protective glasses (physical dosimetry) were exposed to different doses of photons (0–4.4 Gy; values refer to dose to blood after correction) and the absorbed radiation doses were reconstructed by biodosimetry (DCA) and physical dosimetry (optically stimulated luminescence (OSL)) methods. Additionally, LiF:Mg,Ti (TLD-100) chips and Al2O3:C (Luxel) films were used as reference TL and OSL dosimeters, respectively. The best coincidence between biodosimetry and physical dosimetry was observed for samples of blood and SMRs exposed to γ-rays. Significant differences were observed in the reconstructed doses by the two dosimetry methods for samples exposed to x-ray photons with energy below 100 keV. The discrepancy is probably due to the energy dependence of mass energy-absorption coefficients of the samples extracted from the phones. Our results of comparative validation of the radiation doses reconstructed by luminescence dosimetry from smartphone components with biodosimetry using DCA from human blood suggest the potential use of smartphone components as an effective emergency triage tool for high photon energies.

Development of Kudzu (Pueraria Montana var. lobata) Reference Materials for the Determination of Isoflavones and Toxic Elements.

In collaboration with the Office of Dietary Supplements at the National Institutes of Health, the National Institute of Standards and Technology issued a suite of botanical matrix reference materials (RMs) and Standard Reference Material® (SRM) for determination of isoflavones and toxic elements in kudzu dietary supplement ingredients. RM 8650 Pueraria montana var. lobata (Kudzu) Rhizome, SRM 3268 Pueraria montana var. lobata (Kudzu) Extract, and RM 8652 Kudzu-Containing Solid Oral Dosage Form were issued with values assigned for isoflavones (puerarin, daidzin, and daidzein), toxic elements (arsenic, cadmium, and lead), and selenium. Isoflavone values were assigned using liquid chromatography with UV absorbance or mass spectrometry detection. Element values were assigned using inductively coupled plasma mass spectrometry and results from an interlaboratory comparison exercise. Mass fractions for puerarin were 32.2 ± 3.2 mg/g, 128 ± 13 mg/g, and 68.2 ± 6.9 mg/g in RM 8650, SRM 3268, and RM 8652, respectively. Arsenic increases from 156 ± 14 ng/g to 849 ± 83 ng/g and cadmium decreases from 348 ± 14 ng/g to 82.1 ± 4.9 ng/g from rhizome to extract. The kudzu RM/SRM suite complements previously issued soy-related SRMs with values assigned for isoflavones, which have been studied for their potential health benefits, and expands the analytical resource by providing values for puerarin, an isoflavone not found in soy. The three new kudzurmaterials are for use in the determination of isoflavones, toxic elements, and selenium. For the isoflavones, these new kudzu materials provide higher levels of daidzin and daidzein than existing soy-related SRMs, and they provide a value for an isoflavone not in existing SRMs (puerarin). Toxic elements in RM 8650 and SRM 3268 provide new botanical matrixes for use by dietary supplement manufacturers for the verification of the safety of their raw materials.