CERTIFICATION REPORT: The certification of electrophoretic mobility/zeta potential of silica particles in aqueous solution: ERM-FD306/SRM 1993

This report describes the production of ERM-FD306/SRM 1993, silica particles suspended in a borate buffer, certified for electrophoretic mobility and zeta potential by electrophoretic light scattering (ELS). This material was produced following ISO 17034:2016 and is certified in accordance with ISO Guide 35:2017. The certified reference material (CRM) was jointly produced by the Directorate F - Health, Consumers and Reference Materials of the European Commission’s Joint Research Centre (JRC) in Geel (Belgium) and the US National Institute of Standards and Technology (NIST), Gaithersburg (USA). The CRM was produced from a buffer-modified and diluted commercial colloidal silica slurry. Between-ampoule homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2017. The minimum sample intake for the ELS method was determined from the results and information provided by the laboratories that participated in the interlaboratory comparison (ILC) exercise. The material was characterised by an interlaboratory comparison between laboratories of demonstrated competence and adhering to ISO/IEC 17025. Technically invalid results were removed but no outlier was eliminated solely on statistical grounds. Uncertainties of the certified values were calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for quality control and assessment of method performance. The method-defined certified values are regarded as reliable estimates of the true values and ERM-FD306/SRM 1993 can therefore be used for calibration purposes. The CRM is available in 25 mL pre-scored amber glass ampoules each containing approximately 25 mL of suspension.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of electrophoretic mobility/zeta potential of silica particles in aqueous solution: ERM-FD305/SRM 1992

This report describes the production of ERM-FD305/SRM 1992, silica particles suspended in a borate buffer, certified for electrophoretic mobility and zeta potential by electrophoretic light scattering (ELS). This material was produced following ISO 17034:2016 and is certified in accordance with ISO Guide 35:2017. The certified reference material (CRM) was jointly produced by the Directorate F - Health, Consumers and Reference Materials of the European Commission’s Joint Research Centre (JRC) in Geel (Belgium) and the US National Institute of Standards and Technology (NIST), Gaithersburg (USA). The CRM was produced from a buffer-modified and diluted commercial colloidal silica slurry. Between-ampoule homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2017. The minimum sample intake for the ELS method was determined from the results and information provided by the laboratories that participated in the interlaboratory comparison (ILC) exercise. The material was characterised by an interlaboratory comparison between laboratories of demonstrated competence and adhering to ISO/IEC 17025. Technically invalid results were removed but no outlier was eliminated solely on statistical grounds. Uncertainties of the certified values were calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for quality control and assessment of method performance. The CRM is available in 5 mL pre-scored amber glass ampoules each containing approximately 5 mL of suspension.JRC.F.6-Reference Material

USGS44, a new high purity calcium carbonate reference material for δ13 C measurements

RATIONALE: The stable carbon isotopic (δ13 C) reference material (RM) LSVEC Li2 CO3 has been found to be unsuitable for δ13 C standardization work because its δ13 C value increases with exposure to atmospheric CO2 . A new CaCO3 RM, USGS44, has been prepared to alleviate this situation. METHODS: USGS44 was prepared from 8 kg of Merck high purity CaCO3 . Two sets of δ13 C values of USGS44 were determined. The first set of values was determined by on-line combustion, continuous-flow (CF) isotope-ratio mass spectrometry (IRMS) of NBS 19 CaCO3 (δ13 CVPDB = +1.95 milliurey (mUr) exactly, where mUr = 0.001 = 1 ‰), and LSVEC Li2 CO3 (δ13 CVPDB = -46.6 mUr exactly), and normalized to the two-anchor δ13 CVPDB-LSVEC isotope-delta scale. The second set of values was obtained by dual-inlet (DI) IRMS of CO2 evolved by reaction of H3 PO4 with carbonates, corrected for cross contamination, and normalized to the single anchor δ13 CVPDB scale. RESULTS: USGS44 is stable and isotopically homogeneous to within 0.02 mUr in 100-μg amounts. It has a δ13 CVPDB-LSVEC value of -42.21 ± 0.05 mUr. Single-anchor δ13 CVPDB values of -42.08 ± 0.01 and -41.99 ± 0.02 mUr were determined by DI-IRMS with corrections for cross contamination. CONCLUSIONS: The new high-purity, well homogenized calcium carbonate isotopic reference material USGS44 is stable and has a δ13 CVPDB-LSVEC value of -42.21 ± 0.05 mUr for both EA-IRMS and DI-IRMS measurements. As a carbonate relatively depleted in 13 C, it is intended for daily use as a secondary isotopic reference material to normalize stable carbon isotope-delta measurements to the δ13 CVPDB-LSVEC scale. It is useful in quantifying drift with time, determining mass-dependent isotopic fractionation (linearity correction), and adjusting isotope-ratio-scale contraction. Due to its fine grain size (smaller than 63 μm), it is not suitable as a δ18 O reference material. A δ13 CVPDB-LSVEC value of -29.99 ± 0.05 mUr was determined for NBS 22 oil

Organic Reference Materials for Hydrogen, Carbon, and Nitrogen Stable Isotope-Ratio Measurements: Caffeines, n-Alkanes, Fatty Acid Methyl Esters, Glycines, L-Valines, Polyethylenes, and Oils

An international project developed, quality-tested, and determined isotope−δ values of 19 new organic reference materials (RMs) for hydrogen, carbon, and nitrogen stable isotope-ratio measurements, in addition to analyzing pre-existing RMs NBS 22 (oil), IAEA-CH-7 (polyethylene foil), and IAEA-600 (caffeine). These new RMs enable users to normalize measurements of samples to isotope−δ scales. The RMs span a range of δ^2H_(VSMOW-SLAP) values from −210.8 to +397.0 mUr or ‰, for δ^(13)C_(VPDB-LSVEC) from −40.81 to +0.49 mUr and for δ^(15)N_(Air) from −5.21 to +61.53 mUr. Many of the new RMs are amenable to gas and liquid chromatography. The RMs include triads of isotopically contrasting caffeines, C_(16) n-alkanes, n-C_(20)-fatty acid methyl esters (FAMEs), glycines, and L-valines, together with polyethylene powder and string, one n-C_(17)-FAME, a vacuum oil (NBS 22a) to replace NBS 22 oil, and a ^2H-enriched vacuum oil. A total of 11 laboratories from 7 countries used multiple analytical approaches and instrumentation for 2-point isotopic normalization against international primary measurement standards. The use of reference waters in silver tubes allowed direct normalization of δ2H values of organic materials against isotopic reference waters following the principle of identical treatment. Bayesian statistical analysis yielded the mean values reported here. New RMs are numbered from USGS61 through USGS78, in addition to NBS 22a. Because of exchangeable hydrogen, amino acid RMs currently are recommended only for carbon- and nitrogen-isotope measurements. Some amino acids contain ^(13)C and carbon-bound organic ^2H-enrichments at different molecular sites to provide RMs for potential site-specific isotopic analysis in future studies

A Reference High-Pressure CO2 Adsorption Isotherm for Ammonium ZSM-5 Zeolite: Results of an Interlaboratory Study

© 2018, The Author(s). This paper reports the results of an international interlaboratory study led by the National Institute of Standards and Technology (NIST) on the measurement of high-pressure surface excess carbon dioxide adsorption isotherms on NIST Reference Material RM 8852 (ammonium ZSM-5 zeolite), at 293.15 K (20 °C) from 1 kPa up to 4.5 MPa. Eleven laboratories participated in this exercise and, for the first time, high-pressure adsorption reference data are reported using a reference material. An empirical reference equation nex=d(1+exp[(-ln(P)+a)/b])c, [nex-surface excess uptake (mmol/g), P-equilibrium pressure (MPa), a = −6.22, b = 1.97, c = 4.73, and d = 3.87] along with the 95% uncertainty interval (Uk = 2 = 0.075 mmol/g) were determined for the reference isotherm using a Bayesian, Markov Chain Monte Carlo method. Together, this zeolitic reference material and the associated adsorption data provide a means for laboratories to test and validate high-pressure adsorption equipment and measurements. Recommendations are provided for measuring reliable high-pressure adsorption isotherms using this material, including activation procedures, data processing methods to determine surface excess uptake, and the appropriate equation of state to be used

Optimal scaling of two-level factorial experiments

The relationship of a response variable with k continuous explanatory variables can be effectively studied by imbedding a 2k factorial design in the k space. A Bayesian model enables us to use prior information to select the scale of the experiment design. In this paper, the experimental design is scaled according to a criterion based on the Shannon entropy and on a criterion based on the maximum posterior variance within the experimental region. The designs are optimal if the observations are made without error, as in computer experiments, and are approximately optimal in the setting where experimental error is possible, and the ratio of error variance to prior variance is small.Bayesian experimental design computer experiments design scale factorial experiment

Development of a 96-Well Electrophilic Allergen Screening Assay for Skin Sensitization Using a Measurement Science Approach

The Electrophilic Allergen Screening Assay (EASA) has emerged as a promising in chemico method to detect the first key event in the adverse outcome pathway (AOP) for skin sensitization. This assay functions by assessing the depletion of one of two probe molecules (4-nitrobenzenethiol (NBT) and pyridoxylamine (PDA)) in the presence of a test compound (TC). The initial development of EASA utilized a cuvette format resulting in multiple measurement challenges such as low throughput and the inability to include adequate control measurements. In this study, we describe the redesign of EASA into a 96-well plate format that incorporates in-process control measurements to quantify key sources of variability each time the assay is run. The data from the analysis of 67 TCs using the 96-well format had 77% concordance with animal data from the local lymph node assay (LLNA), a result consistent with that for the direct peptide reactivity assay (DPRA), an OECD test guideline (442C) protein binding assay. Overall, the measurement science approach described here provides steps during assay development that can be taken to increase confidence of in chemico assays by attempting to fully characterize the sources of variability and potential biases and incorporate in-process control measurements into the assay