Tadeusz Gorewoda

Certyfikowane materiały odniesienia (certified reference materials − CRM) są nierozłącznym elementem analizy składu chemicznego w kontroli jakości surowców i produktów. Ich wykorzystanie w takich technikach, jak fluorescencyjna spektrometria rentgenowska (XRF) oraz optyczna spektrometria emisyjna ze wzbudzeniem w iskrze niskowoltowej (spark-OES) umożliwia kalibracje spektrometrów, weryfikacje poprawności uzyskiwanych wyników, a także wykazanie spójności pomiarowej wyników otrzymanych za pomocą danej procedury analitycznej.

Matrix certified reference materials (mCRMs) are materials characterized by suitable homogeneity, stability, and traceability, with certified values, including uncertainties, and a specific matrix. mCRMs constitute a reference for instrumental analytical methods and ensure their metrological consistency. Matrix certified reference materials (mCRMs) are essential tools for ensuring the accuracy and traceability of analytical measurements, particularly for samples with complex matrices. These mCRMs are carefully manufactured materials that closely mimic the composition and properties of real samples, allowing laboratories to validate their analytical methods, calibrate analytical instruments, or check the classical methods. This article highlights the challenges associated with the production and characterization of these complex mCRMs, including obtaining homogeneous materials, establishing accurate target values, and ensuring stability for different types of materials, such as gases, liquids, and metal alloys. Additionally, the process of statistical evaluation through the use of advanced statistical methods is discussed, as is the systems approach associated with the implementation of the ISO 17034 standard, which specifies the requirements for manufacturers of reference materials. This paper also includes a summary of the current status in trends of normalization as well as mCRM production.

This paper evaluates the possibility of analyzing the composition of high-quality copper scrap with X-ray fluorescence spectrometry (XRF) instead of electrogravimetry combined with flame atomic absorption spectroscopy (EG+FAAS) method. The evaluation of the methods was performed on three real copper scraps, the composition of which were estimated in average samples taken after re-melting. Traceability of XRF results was ensured by the use of new certified reference materials (CRMs) dedicated to copper scrap analysis. The copper content results obtained by XRF were characterized by high agreement with the reference results obtained by EG+FAAS method. The estimated expanded uncertainty for Cu of both methods was 0.23%. In addition to significant time savings without compromising accuracy, the XRF method additionally provided information on the content of 12 other elements, such as Sn, Zn, Co, Cd, Sb, Ni, Fe, Pb, Bi, Ag, Al, and P. This may make the XRF method attractive compared to the commonly used EG+FAAS method.

This paper presents a practical approach to the production of certified reference materials (CRMs) for ferrosilicon magnesium alloys. These new CRMs are predicted to be used in fast X-ray fluorescence spectrometry (XRF) analysis, which does not require sample digestion and does not result in the production of acidic sewage and emissions, contrary to the classical and instrumental techniques currently used in laboratories. Four new certified reference materials (CRMs) were developed to fill the gap in the reference materials market and ensure fast and traceable analyses. The materials were produced with an industrial process and then homogenized and mixed to achieve the required compositions and level of homogeneity. The homogeneity was determined using specially developed analytical methods and confirmed statistically by ANOVA. Additionally, the results of the tests show the short- and long-term stabilities of the new materials. The certified values for specific element contents were determined in interlaboratory tests. All results were assessed statistically for outliers. The results from three or more independent and different analytical methods were used for the calculations. In parallel homogeneity, the stability, and characterization standard uncertainties were calculated and used in the estimation of the final expanded uncertainties of the certified values. Finally, four new CRMs were assisted with the proper certificates according to ISO standards.

Total Productive Maintenance (TPM) is an infrastructure-managing methodology that leads to improvements in production efficiency, quality, and safety. It includes a set of processes, techniques, and strategies based on forecasting, maintenance, the optimized cooperation of different company departments, and the minimization of costs related to downtime or accidents caused by equipment failure. This article discusses the history, assumptions of the TPM concept, and approach to implementing Total Productive Maintenance in organizations in detail. The right ingredients required for successful TPM implementation and barriers to implementation are also reviewed. The benefits of implementing TPM in organizations are presented and supported with examples of implementations in production and non-production organizations. The article is addressed to representatives of the manufacturing industry. TPM also indicates a high potential for implementation in non-production areas, which may be interesting, for example, for the service, medical, or laboratory industries.

According to the idea of sustainable development, humanity should make every effort to care for the natural environment along with economic development. Decreasing water resources in the world makes it necessary to take action to reduce the consumption of this resource. This article presents the results of research conducted to improve the use of recyclable materials in line with the circular economy model. The research focused on the development of a technological solution for the recovery of raw materials from galvanic wastewater. The concept of a galvanic wastewater treatment system presented in the article includes wastewater pre-treatment in the ultrafiltration (UF) process and water recovery in the reverse osmosis (RO) process. In addition, the purpose of the work was to manage post-filtration waste (RO retentate) containing high concentrations of zinc in the process of galvanizing metal details. The obtained results indicate that it is possible to reduce the amount of sewage from the galvanizing industry by reusing the recovered water as technical water in the process line. The carried-out model tests of galvanizing confirmed the possibility of using RO retentate for the production of metal parts. The achieved results are a proposal to solve the problem of reducing the impact of galvanic wastewater on the environment and to improve the profitability of existing galvanizing technologies by reducing the consumption of water and raw materials.

Information about copper speciation forms is essential for analytical laboratories in the copper industry. Because of the technological importance of this analytical information, many laboratories have developed different methods for the speciation of this metal over the past few decades. This review covers over one hundred years (from 1901 to the present) of published work focused on analytical procedures for copper speciation. The analytical techniques used for speciation analysis are classified into two main groups: instrumental techniques and classical methods, which can be based on selective solutions or titration methods implemented after the required sample preparation.

The electronic components mounted on the printed circuit boards (PCBs) of mobile phones represent a resource that is rich in metals, and after separation from the boards, these components could be considered secondary raw materials. The concentrations of the valuable metals are insignificant when compared with those of complete PCBs; however, they could be significantly higher in a fraction formed from the separated components. This study focused on the analysis of Ag, Au, Cu, Nd, Nb, Ni, Pb, Pd, Sn, and Ta in fractions produced by the separation of all the components mounted on PCBs from several types of mobile phones. Atomic absorption spectrometry, atomic emission spectrometry, and mass spectrometry techniques were utilized, and a comparison of five older models of “brick” phones and five modern smartphones was conducted. Additionally, 50 kg of PCBs from the current recycling market were analyzed in the same way to create a summary of the current recycling stream.

This article describes the effects of microstructures in an analysis of lead-free solders, namely SnAg, SnBi and SnIn, using X-ray fluorescence spectrometry (XRF). The size of the microstructures in the samples and calibration materials has a strong impact on the calibration accuracy and results. A comparison of the microstructure size and critical thickness values demonstrated the importance of the former parameter in terms of the analyzed volume of the specimen. The re-melting and casting in an induction furnace at developed conditions were determined to be a way to obtain samples with fine-grained microstructures. Calibration with re-melted reference materials yielded more accurate calibration curves than calibration using the materials in their original state. Re-melting of the samples resulted in improvements in the XRF results in comparison to the reference values. This improvement is especially important in case of alloying elements with concentrations that determine the recognition of a specific solder grade.

The accurate analysis of hard CuP and CuPAg‐type solders using X‐ray fluorescence spectrometry is a difficult task. Surface milling, the most common sample preparation method for calibration materials, results in poor accuracy for the phosphorus analysis, as evidenced by the unacceptable values of the root mean square error. Meanwhile, the analysis of real samples provides incorrect results, and microstructural effects are the main source of error. Thus, this effect was negated by considering the information depth of the phosphorus Kα line and the microstructure size of the alloys. Phosphorus was measured using a thin layer of the sample (a thickness of several micrometers). As a result, the analyzed layer was a poor representative of the sample. Two different approaches for solving the microstructural effect issue were proposed. In the first method, the alloy was remelted under controlled conditions to obtain fine‐grain samples, which successfully limited the microstructural effects. The second solution used specially prepared thin layer samples, and the sample dissolution eliminated the microstructural effect. Using the developed sample treatment methods resulted in an improvement in the accuracy of the phosphorus calibration curves. This allowed for the correct determination of phosphorus and other alloying elements in the Cu‐based alloys with low uncertainties.