High-Resolution Atomic Absorption Spectrometry Combined with Machine Learning Data Processing for Isotope Amount Ratio Analysis of Lithium

<a>An alternative method for lithium isotope amount ratio analysis based on a combination of high-resolution atomic absorption spectrometry and spectral data analysis by machine learning (ML) is proposed herein. It is based on the well-known isotope shift of approximately 15 pm for the electronic transition 2²P←2²S at around the wavelength of 670.8 nm, which can be measured by state-of-the-art high-resolution continuum source graphite furnace atomic absorption spectrometry. For isotope amount ratio analysis, a scalable tree boosting ML algorithm (XGBoost) was employed and calibrated using a set of samples with ⁶Li isotope amount fractions ranging from 0.06 to 0.99 mol mol⁻¹, previously determined by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The calibration ML model was validated with two certified reference materials (LSVEC and IRMM-016). The procedure was applied to the isotope amount ratio determination of a set of stock chemicals (Li₂CO₃, LiNO₃, LiCl, and LiOH) and a BAM candidate reference material, that is, LiNi_1/3Mn_1/3Co_1/3O₂ (NMC111) cathode material. The results of these determinations were compared with those obtained by MC-ICP-MS and found to be metrologically comparable and compatible. The residual bias was −1.8‰ and the </a><a>precision obtained ranged from 1.9‰ to 6.2‰</a>. This precision was sufficient to resolve naturally occurring variations, as demonstrated for samples ranging from approximately −3‰ to +15‰. To assess its suitability to technical applications, the NMC111 cathode candidate reference material was analyzed using high-resolution continuum source molecular absorption spectrometry with and without matrix purification. The results obtained were metrologically compatible with each other.

High-Resolution Atomic Absorption Spectrometry Combined with Machine Learning Data Processing for Isotope Amount Ratio Analysis of Lithium

<a>An alternative method for lithium isotope amount ratio analysis based on a combination of high-resolution atomic absorption spectrometry and spectral data analysis by machine learning (ML) is proposed herein. It is based on the well-known isotope shift of approximately 15 pm for the electronic transition 2²P←2²S at around the wavelength of 670.8 nm, which can be measured by state-of-the-art high-resolution continuum source graphite furnace atomic absorption spectrometry. For isotope amount ratio analysis, a scalable tree boosting ML algorithm (XGBoost) was employed and calibrated using a set of samples with ⁶Li isotope amount fractions ranging from 0.06 to 0.99 mol mol⁻¹, previously determined by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The calibration ML model was validated with two certified reference materials (LSVEC and IRMM-016). The procedure was applied to the isotope amount ratio determination of a set of stock chemicals (Li₂CO₃, LiNO₃, LiCl, and LiOH) and a BAM candidate reference material, that is, LiNi_1/3Mn_1/3Co_1/3O₂ (NMC111) cathode material. The results of these determinations were compared with those obtained by MC-ICP-MS and found to be metrologically comparable and compatible. The residual bias was −1.8‰ and the </a><a>precision obtained ranged from 1.9‰ to 6.2‰</a>. This precision was sufficient to resolve naturally occurring variations, as demonstrated for samples ranging from approximately −3‰ to +15‰. To assess its suitability to technical applications, the NMC111 cathode candidate reference material was analyzed using high-resolution continuum source molecular absorption spectrometry with and without matrix purification. The results obtained were metrologically compatible with each other.

Method for Preparation of a Candidate Reference Material of PM10 and PM2.5 Airborne Particulate Filters Loaded with Incineration Ash-Inter Comparison Results for Metal Concentrations

Air pollution is an important issue that can have significant implications for human health. Consequently, air quality control is matter of great interest, and the ΕU has established strict legislation with respect to public health protection. A work package of the EMPIR project AEROMET focused on the investigation of traceable validated methods for chemical composition of airborne particulate matter (PM), including heavy metals. Incineration ash typically contains quantities of heavy and toxic metals in excess of the limits imposed for airborne PM, so it provides a candidate source for a Standard Reference Material (SRM). In this work, a method for loading incinerator ash (PM10 and PM2.5 fractions) on quartz filters with a good reproducibility and homogeneity was developed. An intercomparison exercise involving three separate laboratories was conducted for the elemental analysis of the prepared candidate reference material. The filters were treated by acid digestion and analyzed by Inductively Coupled Plasma–Mass Spectrometry (ICP-MS) according to the European standard EN 14902:2005. Eleven elements, including the regulated metals (As, Cd, Ni and Pb), were determined using different ICP-MS instruments and standardization methods. Data evaluation showed a good agreement between the results, with deviations below 10–15%. The development of a Standard Reference Material seems auspicious.

Development of a certified reference material for anti-β2-glycoprotein I IgG – commutability studies

ObjectivesIn this paper, we describe the steps followed for the development of a certified reference material for immunoglobulin G antibodies against β2-glycoprotein I (also known as apolipoprotein H). These steps include processing of the material, commutability, the impact of dilution, the appropriate reconstitution conditions, homogeneity and stability during transport and storage.MethodsWe analysed 69 clinical samples from patients suffering from antiphospholipid syndrome with several commercial enzyme-linked immunosorbent assays (ELISA) purchased from in vitro diagnostic manufacturers.ResultsAnalysis of the results indicated that the candidate reference material can be safely freeze-dried, and that the user should carefully follow the reconstitution instructions as small changes in e.g. temperature may have unwanted effects. The statistical analysis of the commutability studies indicated that the analytical response of the reference material upon dilution is similar to that of clinical samples, and that correlation between results may differ from assay to assay. Finally yet importantly, the presented and developed candidate reference material is commutable for most assays tested, homogeneous and stable.ConclusionsImmunoglobulin G antibodies against β2-glycoprotein I are associated with a higher risk of thrombosis and pregnancy complications. Their measurement is essential for the diagnosis and monitoring of antiphospholipid syndrome. These antibodies are detected by specific immunoassays, routinely used in clinical diagnostics, but various of these methods show enormous variability, in part due to the lack of a reference material.

Micro-homogeneity evaluation of a bovine kidney candidate reference material

The minimum sample intake for which a reference material remains homogeneous is one of the parameters that must be estimated in the homogeneity assessment study of reference materials. In this work, Instrumental Neutron Activation Analysis was used to evaluate this quantity in a bovine kidney candidate reference material. The mass fractions of 9 inorganic constituents were determined in subsamples between 1 and 2 mg in order to estimate the relative homogeneity factor (HE) and the minimum sample mass to achieve 5% and 10% precision on a 95% confidence level. Results obtained for HE in all the analyzed elements were satisfactory. The estimated minimum sample intake was between 2 mg and 40 mg, depending on the element.