Elemental characterization of electronic waste: a review of research methodologies and applicability to the practice of e-waste recycling.

Economic and environmental considerations have elucidated research interests on the best approach to managing electronic waste (e-waste), which has increasing social, environmental, and economic impacts. Proper e-waste managementis essential for resource recovery, environmental sustainability, and public health protection, and effective management of e-waste necessitates analytical techniques to assess and characterize their elemental composition. Despite expansive literature published on the topic of e-waste, there is scarce coverage of the various analytical techniques employed to characterize the inorganic contents of e-waste. This review discusses the various e-waste characterization techniques used in studies published between 2013 and 2023. Specifically, this review covers the analytical approaches employed to characterize the inorganic content of e-waste, the electronic devices or their components analyzed, the elements identified, the sample preparation methods adopted, and the merits and demerits of the analytical procedures. This review highlights the disparate approaches to e-waste characterization and the need for reliable and repeatable e-waste analysis and sample preparation methods.

Prompt gamma ray activation analysis for determining chemical composition of 3D printing and casting materials used in biomedical applications.

Three-dimensional printing and casting materials were analyzed by prompt gamma-ray activation analysis (PGAA) to determine their suitability as human tissue surrogates for the fabrication of phantoms for medical imaging and radiation dosimetry applications. Measured elemental compositions and densities of five surrogate materials simulating soft tissue and bone were used to determine radiological properties (x-ray mass attenuation coefficient and electron stopping power). When compared with radiological properties of International Commission on Radiation Units and Measurements (ICRU) materials, it was determined that urethane rubber and PLA plastic yielded the best match for soft tissue, while silicone rubber and urethane resin best simulated the properties of bone.

Gross handling of pulmonary resection specimen: maintaining the 3-dimensional orientation.

There is limited literature on the gross handling of lung resection specimens. Microscopic examination of the specimen, TNM staging and predictive biomarker testing are fully dependent on an adequate gross handling. In this paper, we present a 3-dimensional (3D) grossing method of oncological lung resection specimens, which ensures proper fixation of the tumor tissue, but also enables accurate correlation with the pre-surgical imaging.

Glassy carbon, NIST Standard Reference Material (SRM 3600): hydrogen content, neutron vibrational density of states and heat capacity.

Commercial glassy carbon plates being used as absolute intensity calibration standards in small-angle X-ray scattering applications (NIST SRM 3600) have been characterized in several recent publications. This contribution adds to the characterization by measuring the hydrogen content of a plate to be (4.8 ± 0.2) × 10-4 (mol H)/(mol C), and by measuring the vibrational spectrum by neutron inelastic scattering. The spectrum bears a strong resemblance to published measurements on graphite, allowing the identification of several spectral features. The measured spectrum is used to calculate the heat capacity of low-hydrogen-content glassy carbon for comparison with measurements reported here from 20 to 295 K.

Development of a kelp powder (Thallus laminariae) Standard Reference Material.

A Standard Reference Material (SRM) of seaweed, SRM 3232 Kelp Powder (Thallus laminariae) has been developed to support food and dietary supplement measurements in compliance with the Food Safety Modernization Act (FSMA) and the Dietary Supplement Health and Education Act of 1994 (DSHEA). The material was characterized for nutritional minerals, arsenic species, isomers of vitamin K1, proximates, and toxic elements. Kelp is a rich source of vitamins and minerals, and it is an excellent source of dietary iodine. Kelp also contains a large amount of arsenic, which is toxic as inorganic species but much less so as organic species. To capture the dietary profile of kelp, certified values were issued for As, Ca, Cd, Cr, Cu, Fe, Hg, I, K, Mg, Mn, Mo, Na, Pb, and Zn. Reference values for proximates were assigned. For the first time, a certified value for iodine, reference values for isomers of vitamin K1, and reference values for arsenic species including arsenosugars were assigned in a seaweed. SRM 3232 fills a gap in Certified Reference Materials (CRMs) needed for quality assurance and method validation in the compositional measurements of kelp and similar seaweeds used as food and as dietary supplements. Graphical Absract Arsenic species and isomers of vitamin K1 were determined in the development of SRM 3232 Kelp Powder (Thallus laminariae).

Assessment of PGAA capability for low-level measurements of H in Ti alloys.

The accuracy of low-level hydrogen measurements with prompt gamma-ray activation analysis (PGAA) depends on identifying and accounting for all background H signals, including interfering signals. At the cold-neutron (CN)PGAA facility at the NIST Center for Neutron Research, the sources of background H signals were investigated in the context of titanium-based matrices containing low-levels of H (<300 mg H per kg Ti) with the measurements of prepared standards (mixtures of polyvinyl chloride and titanium oxide) and Ti alloy (Ti6Al4V) samples. The sensitivity ratio, defined as the ratio of the H signal to the Ti signal per unit mass ratio of H in Ti, was determined (1) with the measurements of prepared standards and (2) based on partial gamma-ray production cross sections and full-energy detection efficiencies. The resulting calibrations from these two approaches agreed within experimental uncertainty. A series of Ti alloy NIST Standard Reference Materials (SRMs) previously certified for the H content (SRMs 2452, 2453, 2453a, 2454) were used as test cases, with the mass fractions determined based on the sensitivity ratios derived from method 1 and method 2, respectively. The results agreed with the certified values within experimental uncertainties, validating the analysis performed on the new instrument with newly-prepared standards at low H mass fractions (method 1), and with the standard-independent analysis (method 2). Various sample mounting improvements were made to lower the background H signal. Spectral interferences near the H peak were identified as potential sources of bias and as a limiting factor in the detection limit of H in Ti alloy samples.

Prompt Gamma-ray Activation Analysis for Certification of Sulfur in Fuel Oil SRMs.

A combination of cold neutron prompt gamma-ray activation analysis (CNPGAA) and thermal neutron (TN) PGAA was used to determine sulfur in fuel oils to develop a method to provide values for certification. CNPGAA was used to measure S/H mass ratios, and TNPGAA to measure hydrogen mass fractions. Measurements were combined to determine sulfur mass fractions (with expanded uncertainties) of 2.159 % ± 0.072 % for SRM 1622e, 0.7066 % ± 0.0120 % for SRM 1619b, and 0.1266 % ± 0.0030 % for SRM 1617b, in agreement with certified values. The results validate the method as suitable for certification of sulfur at mass fractions ≥ 0.1 %.

Elemental characterization of single-wall carbon nanotube certified reference material by neutron and prompt γ activation analysis.

Instrumental neutron activation analysis with both relative and k0 standardization was used in four experienced laboratories to determine element mass fractions in single-wall carbon nanotube certified reference material (CRM) SWCNT-1. Results obtained were evaluated using the National Institute of Standards and Technology (NIST) "Type B On Bias" approach and yielded consensus values in agreement with National Research Council Canada (NRCC) certified values for Fe, Co, Ni, and Mo and provided mass fraction values for 13 additional elements, namely, Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Br, La, W, and Au. In addition, prompt γ neutron activation analysis was employed to determine mass fractions of H, B, Co, Ni, and Mo. Results of this work provide a basis for the establishment of reference values of element mass fractions in CRM SWCNT-1, thus expanding its usability for more accurate characterization and benchmarking of similar nanotechnology materials.

Certification of Total Arsenic in Blood and Urine Standard Reference Materials by Radiochemical Neutron Activation Analysis and Inductively Coupled Plasma - Mass Spectrometry.

A newly developed procedure for determination of arsenic by radiochemical neutron activation analysis (RNAA) was used to measure arsenic at four levels in SRM 955c Toxic Elements in Caprine Blood and at two levels in SRM 2668 Toxic Elements in Frozen Human Urine for the purpose of providing mass concentration values for certification. Samples were freeze-dried prior to analysis followed by neutron irradiation for 3 h at a fluence rate of 1×1014cm-2s-1. After sample dissolution in perchloric and nitric acids, arsenic was separated from the matrix by extraction into zinc diethyldithiocarbamate in chloroform, and 76As quantified by gamma-ray spectroscopy. Differences in chemical yield and counting geometry between samples and standards were monitored by measuring the count rate of a 77As tracer added before sample dissolution. RNAA results were combined with inductively coupled plasma - mass spectrometry (ICP-MS) values from NIST and collaborating laboratories to provide certified values of (10.81 ± 0.54) µg/kg and (213.1 ± 0.73) µg/kg for SRM 2668 Levels I and II, and certified values of (21.66 ± 0.73) µg/kg, (52.7 ± 1.1) µg/kg, and (78.8 ± 4.9) µg/kg for SRM 955c Levels 2, 3, and 4 respectively. Because of discrepancies between values obtained by different methods for SRM 955c Level 1, an information value of < 5 µg/kg was assigned for this material.

Evaluation of the phenotypic test and genetic analysis in the detection of glucose-6-phosphate dehydrogenase deficiency.

BACKGROUND: Glucose-6-phosphate dehydrogenase (G6PD) deficiency is particularly prevalent in historically malaria-endemic countries. Although most individuals with G6PD deficiency are asymptomatic, deficiency can result in acute haemolytic anaemia after exposure to oxidative agents. A reliable test is necessary for diagnosing the deficiency to prevent an acute haemolytic crisis following, for example, anti-malarial treatment. The aim of this study was to investigate which method was the best predictor of this disorder. METHODS: The present study investigated four G6PD activity detections (fluorescence spot (FS), methaemoglobin reduction (MR), biochemical and cytochemical test). These methods accompanied with mutation analysis of blood samples were taken from 295 apparently healthy individuals with unknown G6PD deficiency status. RESULTS: Molecular characterization of 295 Thai adults revealed an overall prevalence of 14.2%. The G6PD Viangchan (871 G>A) was the most common (83.3%), followed by G6PD Mahidol (487G>A) (11.9%), and G6PD Union (1360 C>T) (4.8%). There were two cases of G6PD deficiency carrying the double mutations of Viangchan (871G > A)-Mahidol (487G > A) and Viangchan (871G > A)-Union (1360C > T). In comparison, the prevalence of G6PD deficiency was 6.1% by FS test and 7.1% by MR test. G6PD activity was 11 ± 2.5 IU/gHb in non-deficient females (mean ± SD), and 10.9 ± 0.6 IU/gHb in non-deficient males. The upper and lower limit cut-off points for partial and severe deficiency in adults were 5.7 IU/gHb (60% of the normal mean) and 0.95 IU/gHb (10% of the normal mean), respectively. All hemizygote, homozygote and double mutations were associated with severe enzyme deficiency (the residual enzyme activity <10% of the normal mean), whereas only 14.3% of the heterozygote mutations showed severe enzyme deficiency. Based on the cut-off value <5.7 IU/gHb, the quantitative G6PD assay diagnosed 83% of cases as G6PD-deficient. Using a cut-off number of negative cell >20% in the cytochemical assay to define G6PD deficiency, the prevalence of G6PD deficiency was closest to the molecular analysis (12.9% G6PD-deficient) compared to the others methods. CONCLUSION: The cytochemical method is a significant predictor of this disease, while FS and MR test are recommended for the detection of severe G6PD deficiency in developing countries.

Structure and stability of SnO2 nanocrystals and surface-bound water species.

The structure of SnO2 nanoparticles (avg. 5 nm) with a few layers of water on the surface has been elucidated by atomic pair distribution function (PDF) methods using in situ neutron total scattering data and molecular dynamics (MD) simulations. Analysis of PDF, neutron prompt gamma, and thermogravimetric data, coupled with MD-generated surface D2O/OD configurations demonstrates that the minimum concentration of OD groups required to prevent rapid growth of nanoparticles during thermal dehydration corresponds to ~0.7 monolayer coverage. Surface hydration layers not only stabilize the SnO2 nanoparticles but also induce particle-size-dependent structural modifications and are likely to promote interfacial reactions through hydrogen bonds between adjacent particles. Upon heating/dehydration under vacuum above 250 °C, nanoparticles start to grow with low activation energies, rapid increase of nanoparticle size, and a reduction in the a lattice dimension. This study underscores the value of neutron diffraction and prompt-gamma analysis, coupled with molecular modeling, in elucidating the influence of surface hydration on the structure and metastable persistence of oxide nanomaterials.

Certification of elements in and use of standard reference material 3280 multivitamin/multielement tablets.

Standard Reference Material 3280 Multivitamin/ Multielement Tablets was issued by the National Institute of Standards and Technology in 2009, and has certified and reference mass fraction values for 13 vitamins, 26 elements, and two carotenoids. Elements were measured using two or more analytical methods at NIST with additional data contributed by collaborating laboratories. This reference material is expected to serve a dual purpose: to provide quality assurance in support of a database of dietary supplement products and to provide a means for analysts, dietary supplement manufacturers, and researchers to assess the appropriateness and validity of their analytical methods and the accuracy of their results.

Determination of moisture content of single-wall carbon nanotubes.

Several techniques were evaluated for the establishment of reliable water/moisture content of single-wall carbon nanotubes. Karl Fischer titration (KF) provides a direct measure of the water content and was used for benchmarking against results obtained by conventional oven drying, desiccation over anhydrous magnesium perchlorate as well as by thermogravimetry and prompt gamma-ray activation analysis. Agreement amongst results was satisfactory with the exception of thermogravimetry, although care must be taken with oven drying as it is possible to register mass gain after an initial moisture loss if prolonged drying time or elevated temperatures (120 °C) are used. Thermogravimetric data were precise but a bias was evident that could be accounted for by considering the non-selective loss of mass as volatile carbonaceous components. Simple drying over anhydrous magnesium perchlorate for a minimum period of 8-10 days is recommended if KF is not available for this measurement.

Evaluation of radiochemical neutron activation analysis methods for determination of arsenic in biological materials.

Radiochemical neutron activation analysis (RNAA) with retention on hydrated manganese dioxide (HMD) has played a key role in the certification of As in biological materials at NIST. Although this method provides very high and reproducible yields and detection limits at low microgram/kilogram levels, counting geometry uncertainties may arise from unequal distribution of As in the HMD, and arsenic detection limits may not be optimal due to significant retention of other elements. An alternate RNAA procedure with separation of arsenic by solvent extraction has been investigated. After digestion of samples in nitric and perchloric acids, As(III) is extracted from 2 M sulfuric acid solution into a solution of zinc diethyldithiocarbamate in chloroform. Counting of (76)As allows quantitation of arsenic. Addition of an (77)As tracer solution prior to dissolution allows correction for chemical yield and counting geometries, further improving reproducibility. The HMD and solvent extraction procedures for arsenic were compared through analysis of SRMs 1577c (bovine liver), 1547 (peach leaves), and 1575a (pine needles). Both methods gave As results in agreement with certified values with comparable reproducibility. However, the solvent extraction method yields a factor of 3 improvement in detection limits and is less time-consuming than the HMD method. The new method shows great promise for use in As certification in reference materials.

Heritability of the human infectious reservoir of malaria parasites.

BACKGROUND: Studies on human genetic factors associated with malaria have hitherto concentrated on their role in susceptibility to and protection from disease. In contrast, virtually no attention has been paid to the role of human genetics in eliciting the production of parasite transmission stages, the gametocytes, and thus enhancing the spread of disease. METHODS AND FINDINGS: We analysed four longitudinal family-based cohort studies from Senegal and Thailand followed for 2-8 years and evaluated the relative impact of the human genetic and non-genetic factors on gametocyte production in infections of Plasmodium falciparum or P. vivax. Prevalence and density of gametocyte carriage were evaluated in asymptomatic and symptomatic infections by examination of Giemsa-stained blood smears and/or RT-PCR (for falciparum in one site). A significant human genetic contribution was found to be associated with gametocyte prevalence in asymptomatic P. falciparum infections. By contrast, there was no heritability associated with the production of gametocytes for P. falciparum or P. vivax symptomatic infections. Sickle cell mutation, HbS, was associated with increased gametocyte prevalence but its contribution was small. CONCLUSIONS: The existence of a significant human genetic contribution to gametocyte prevalence in asymptomatic infections suggests that candidate gene and genome wide association approaches may be usefully applied to explore the underlying human genetics. Prospective epidemiological studies will provide an opportunity to generate novel and perhaps more epidemiologically pertinent gametocyte data with which similar analyses can be performed and the role of human genetics in parasite transmission ascertained.

Characterization of SiGe films for use as a National Institute of Standards and Technology Microanalysis Reference Material (RM 8905).

Bulk silicon-germanium (SiGe) alloys and two SiGe thick films (4 and 5 microm) on Si wafers were tested with the electron probe microanalyzer (EPMA) using wavelength dispersive spectrometers (WDS) for heterogeneity and composition for use as reference materials needed by the microelectronics industry. One alloy with a nominal composition of Si0.86Ge0.14 and the two thick films with nominal compositions of Si0.90Ge0.10 and Si0.75Ge0.25 on Si, evaluated for micro- and macroheterogeneity, will make good microanalysis reference materials with an overall expanded heterogeneity uncertainty of 1.1% relative or less for Ge. The bulk Ge composition in the Si0.86Ge0.14 alloy was determined to be 30.228% mass fraction Ge with an expanded uncertainty of the mean of 0.195% mass fraction. The thick films were quantified with WDS-EPMA using both the Si0.86Ge0.14 alloy and element wafers as reference materials. The Ge concentration was determined to be 22.80% mass fraction with an expanded uncertainty of the mean of 0.12% mass fraction for the Si0.90Ge0.10 wafer and 43.66% mass fraction for the Si0.75Ge0.25 wafer with an expanded uncertainty of the mean of 0.25% mass fraction. The two thick SiGe films will be issued as National Institute of Standards and Technology Reference Materials (RM 8905).

Quantification of hydroxyl content in ceramic oxides: a prompt gamma activation analysis study of BaTiO3.

Thermogravimetric analysis (TGA) and Fourier transform-infrared spectroscopy (FT-IR) techniques for water content determination were compared with a neutron characterization technique, prompt gamma activation analysis (PGAA). Residual H content in the samples, heat treated at various temperatures, was measured with PGAA and compared with the results obtained from TGA. Two major difficulties in TGA were overlapping of mass loss regimes due to removal of different species and residual water that could not be removed, even though the samples were heated above 900 degrees C. After 3 h of heat treatment at 900 degrees C, 0.007% mass fraction H remained in the sample. FT-IR spectra confirmed the presence of H semiquantitatively. It is concluded that residual H remains even after high-temperature treatments.

Internal thoracic vessels used as pedicle graft for anastomosis with vascularized bone graft to reconstruct C7-T3 spinal defects: a new technique.

STUDY DESIGN: A report of 4 cases of primary bone tumors (3 cases) or infection (1 case) at the cervicothoracic junction treated with resection-reconstruction. OBJECTIVES: To document a new technique using the internal thoracic vessels as recipient vessels for reconstruction of the cervicothoracic spine with free vascularized fibula grafts. SUMMARY OF BACKGROUND DATA: The cervicothoracic junction is a difficult region in reconstructive spinal surgery. Although nonvascularized fibula grafts can be used to reconstruct the osseous defect, compared with free vascularized fibula grafts they are biomechanical weaker, incorporate less well, are less resistant to infection, and remodel incomplete in time. However, when using free vascularized bone grafts, the selection of suitable recipient vessels remains one of the most critical decisions. MATERIALS AND METHODS: Four patients who had a primary tumor (3 cases) or a severe progressive kyphotic deformity and progressive neurologic symptoms due to tuberculosis (1 case) were treated by resection and vascularized reconstruction. In 3 patients, a staged anteroposterior en bloc resection of T1-T3 (2 cases) or T1-T2 (1 case) was performed; the ventral reconstruction of the osseous defect consisted of a vascularized fibula graft interposition between C7-T4 (2 cases) or C7-T3 (1 case). In another case, an axial slot was milled through the T1-T2 vertebral bodies to accept an osteotomized vascularized fibular graft. In all cases, a free vascularized fibula graft was used: the vascular anastomosis was performed between the peroneal and the dissected and rerouted internal thoracic vessels. The anterior construction was strengthened by a ventral plate-screw system. RESULTS: The resection-reconstruction procedures, including the dissection, rerouting, and anastomosis between the internal thoracic vessels and the peroneal vessels, were successfully performed. At present, all patients are alive, and there is no evidence of recurrent disease, unchanged, or improved neurologic with a mean follow-up of 28 months. All grafts are well incorporated. CONCLUSIONS.: A combined low anterolateral cervical and midsternal approach or a midline sternotomy allows not only a safe and excellent exposure to the cervicothoracic junction but also to the internal thoracic vessels. The internal thoracic vessels are appropriate donor vessels: its longevity, diameter, length, and rerouting capacity allow vascularized graft reconstruction of vertebral column defects of the low cervical (C6-C7) and/or upper thoracic (T1-T3) region.