scholarly journals Preparation of Three New Certified Reference Materials for Food and Environmental Analysis and Certification Using Laboratory Intercomparison as well as Primary Reference Measurement Procedures

2021 ◽  
Author(s):  
Halina Polkowska-Motrenko ◽  
Zbigniew Samczyński ◽  
Rajmund S. Dybczyński ◽  
Ewelina Chajduk ◽  
Bożena Danko ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Reference Materials ◽  
Trace Analysis ◽  
Inductively Coupled Plasma ◽  
Certified Reference Materials ◽  
Isotope Dilution Mass Spectrometry ◽  
Analytical Techniques ◽  
Reference Measurement ◽  
Certification Procedure ◽  
Primary Reference

AbstractThree new reference materials: MODAS-3 Herring Tissue (M-3 HerTis), MODAS-4 Cormorant Tissue (M-4 CormTis), and MODAS-5 Cod Tissue (M-5 CodTis) were prepared and certified on the basis of results of a worldwide intercomparison exercise. Independently of our proven method of establishing the certified and information values, the content of several essential and toxic elements was additionally determined by the use of ratio primary reference measurement procedures (definitive methods) based on radiochemical neutron activation analysis (RNAA) in the case of As, Cd, Co, Cr, Fe, Mo, Se, and U and isotope dilution mass spectrometry (IDMS) in the case of Hg, respectively. Good agreement of the established certified values and the results obtained by ratio primary reference measurement procedures confirmed the validity of the certification procedure. The total number of elements which could be certified amounted to 30, 21, 18 in M-3 HerTis, M-4 CormTis, and M-5 CodTis, respectively. The relative frequency of use of individual analytical techniques in this intercomparison campaign was calculated and discussed. Inductively coupled plasma mass spectrometry (ICP-MS) is now a dominant technique, followed by atomic absorption spectroscopy (AAS), NAA, and emission spectroscopy (ES). The decreasing share of NAA as compared to several earlier intercomparison exercises should be noticed. NAA is the only method in the array of highly sensitive methods of inorganic trace analysis, which is essentially free from blank. The lack of this method in the foreseeable future may be an obstacle in the prospective certification campaigns and may endanger the implementation of quality assurance in trace analysis.

An optimized HNO3 and HBF4 digestion method for multielemental soil and sediment analysis using inductively coupled plasma quadrupole mass spectrometry

2020 ◽  
Vol 100 (4) ◽  
pp. 393-407
Author(s):  
Muhammad Babar Javed ◽  
Iain Grant-Weaver ◽  
William Shotyk
Keyword(s):  
Mass Spectrometry ◽  
Trace Elements ◽  
Nitric Acid ◽  
Reference Materials ◽  
Inductively Coupled Plasma ◽  
Certified Reference Materials ◽  
Quadrupole Mass ◽  
Quadrupole Mass Spectrometry ◽  
Inductively Coupled ◽  
Almost All

A robust and reliable analytical procedure for the determination of trace (mg∙kg−1) and ultra-trace elements (μg∙kg−1) in soil and sediments by inductively coupled plasma quadrupole mass spectrometry (ICP-QMS) was optimized. Aliquots of ∼200 mg of two certified reference materials (IAEA Soil-7, soil and IAEA SL-1, lake sediments) were digested in nitric acid (HNO3) purified twice by sub-boiling distillation using a microwave-heated high-pressure autoclave. Incremental addition of tetrafluoroboric acid (HBF4, 0.1–2 mL) to HNO3 was evaluated for yield. The selection of appropriate proportions of digestion acids was crucial to obtain accurate results. Digested samples were analyzed for a range of trace elements including those that are potentially toxic (Ag, Cd, Pb, Sb, and Tl), plant micronutrients (Cu, Fe, Mn, and Zn), those enriched in bitumen (Mo, Ni, and V), and lithophile elements (Al, Ba, Co, Cr, Rb, Sr, Th, Ti, Y, and Zr). Nitric acid alone proved to be sufficient to completely liberate Cd, Co, Cr, Fe, Mn, Ni, Pb, V, and Zn in both soil and sediments (87%–120% recovery). For almost all the other elements, addition of HBF4 was needed for improved recovery. A combination of 3 mL of HNO3 and 1.5 mL of HBF4 was optimal to fully liberate an extended list of elements including Ba, Sb, and Sr from both the reference materials. Conservative lithophile elements (Th, Ti, Y, and Zr) could not be completely recovered with the proposed method, requiring hydrofluoric acid for complete dissolution of recalcitrant minerals.

scholarly journals A Microwave Digestion Technique for the Analysis of Rare Earth Elements, Thorium and Uranium in Geochemical Certified Reference Materials and Soils by Inductively Coupled Plasma Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5178 ◽  
Author(s):  
Sharayu Kasar ◽  
Rajamanickam Murugan ◽  
Hideki Arae ◽  
Tatsuo Aono ◽  
Sarata Kumar Sahoo
Keyword(s):  
Mass Spectrometry ◽  
Rare Earth ◽  
Rare Earth Elements ◽  
Reference Materials ◽  
Inductively Coupled Plasma ◽  
Certified Reference Materials ◽  
Microwave Digestion ◽  
Inductively Coupled ◽  
Digestion Technique ◽  
Plasma Mass Spectrometry

Two different digestion methods—microwave digestion (Mw) and Savillex digestion (Sx)—were used to evaluate the best quality control for analysis of the rare earth elements, Th and U in the geochemical certified reference material JSd-2, supplied by the Geological Survey of Japan (GSJ). The analysis of trace elements was carried out using inductively coupled plasma mass spectrometry (ICP-MS). The digestion recovery was > 90% for almost all elements by both methods. Mw-4 (four repeats of the microwave digestion) was found to be more effective and faster than Sx. In order to evaluate the efficiency of Mw-4, three other GSJ certified reference materials, JLk-1, JB-1 and JB-3, as well as five different soil samples from Belarus, Japan, Serbia and Ukraine were also analyzed. The Mw-4 method was seen to be promising for complete digestion and recovery of most of the elements. The U/Th ratio showed some heterogeneity for Ukraine and Serbia soils affected by Chernobyl nuclear power plant accident and depleted uranium contamination, respectively. This method can be successfully applied to any type of soils for elemental analyses.

scholarly journals 30 years of IRMM-1027 reference materials for fissile material accountancy and control: development, production and characterisation

2021 ◽  
Author(s):  
Rožle Jakopič ◽  
Kalman Toth ◽  
Jeroen Bauwens ◽  
Renata Buják ◽  
Carmel Hennessy ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Isotopic Composition ◽  
Reference Materials ◽  
Isotope Dilution ◽  
Organic Substance ◽  
Certified Reference Materials ◽  
Isotope Dilution Mass Spectrometry ◽  
Fissile Material ◽  
High Quality ◽  
And Control

AbstractThe IRMM-1027 Large-sized dried (LSD) spikes are certified reference materials applied to measure the uranium and plutonium content of dissolved fuel solutions using isotope dilution mass spectrometry. High quality starting metals of uranium and plutonium are dissolved to produce a stock solution, which is dispensed into individual vials and dried down. The present spikes are mixtures of typically 50 mg 20% enriched U and 2 mg enriched 239Pu as dried nitrates, conditioned in an organic substance for stability. Each vial of an IRMM-1027 LSD spike comes with certified masses of uranium (235U and 238U) and 239Pu and isotopic composition with associated uncertainty. This article will discuss major developments since the production of the first batch of LSD spikes and will reflect on the current preparation and certification approaches.

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