scholarly journals Development and Validation of an Analytical Method for Determination of Al, Ca, Cd, Fe, Mg and P in Calcium-Rich Materials by ICP OES

Molecules ◽  
2021 ◽  
Vol 26 (20) ◽  
pp. 6269
Author(s):  
Anna Szymczycha-Madeja ◽  
Maja Welna ◽  
Monika Zabłocka-Malicka ◽  
Pawel Pohl ◽  
Włodzimierz Szczepaniak

Four procedures based on closed-vessel microwave-assisted wet digestion with different oxidative reagents, including HNO3 (P1), HNO3 + H2O2 (P2), aqua regia (P3) and Lefort aqua regia (P4), for preparation of calcium (Ca)-rich materials prior to determination of total concentrations of Al, Ca, Cd, Fe, Mg and P by inductively coupled optical emission spectrometry (ICP OES) were compared. It was found that digestion with Lefort aqua regia (P4) provided the best results for all examined elements, i.e., precision of 0.30–4.4%, trueness better than 2%, recoveries of added elements between 99.5–101.9%, and limits of detection within 0.08–1.8 ng g−1. Reliability of this procedure was verified by analysis of relevant certified reference materials (CRMs), i.e., Natural Moroccan Phosphate Rock—Phosphorite (BCR-O32). Additionally, selection of appropriate analytical lines for measurements of element concentrations, linear dynamic ranges of calibration curves and matrix effects on the analyte response were extensively investigated. Finally, the selected procedure was successfully applied for routine analysis of other Ca-rich materials, i.e., CRMs such as NIST 1400 (Bone Ash), CTA-AC-1 (Apatite Concentrate Kola Peninsula) and NCS DC70308 (Carbonate Rock), and six natural samples, such as a dolomite, a phosphate rock, an enriched superphosphate fertilizer, pork bones, pork bones after incineration, and after steam gasification.

Author(s):  
Stanislav Malý ◽  
Jiří Zbíral ◽  
Eva Čižmárová

Legislation limits for risk elements (As, Be, Cd, Co, Cr, Cu, Ni, Pb, V, Zn) in agricultural soil in the Czech Republic are given for the content of elements extracted by aqua regia. This extraction is time consuming and environmentally unfriendly. The regular soil survey is based on Mehlich 3 universal soil extractant and covers the simultaneous determination of macronutrients, sulphur, and micronutrients by inductively coupled plasma optical emission spectrometry (ICP-OES). Our study focused on the possibility to use Mehlich 3 extractant also for preliminary screening for the determination of the risk elements simultaneously with the other elements by the ICP-OES method. Mehlich 3 was confirmed as a reliable screening method for Cd regarding sensitivity, specificity and precision (> 0.8) when the cut-off value of 0.27 mg/kg in Mehlich 3 extracts was used for the prediction of soils to be above or below the legislation limit, which in turn is based on aqua regia extraction. Very good results were obtained for Be and promising results were received for As, Cu and V. But the available data were not sufficient for the determination of reliable cut-off values for Co, Cr, Ni, Pb and Zn.


Author(s):  
Masoud Aghahoseini ◽  
Gholamhassan Azimi ◽  
M. K. Amini

Determination of traces of Cd, Co, Cu, Mn and Pb elements in zirconium and its alloys by inductively coupled plasma optical emission spectrometry (ICP OES) suffers from severe spectral interferences...


2014 ◽  
Vol 97 (3) ◽  
pp. 687-699 ◽  
Author(s):  
James M Bartos ◽  
Barton L Boggs ◽  
J Harold Falls ◽  
Sanford A Siegel

Abstract A two-part single-laboratory validation study was conducted for determination of the P and K content in commercial fertilizer materials by inductively coupled plasma-optical emission spectrometry (ICP- OES). While several methods exist for determination of P and K in fertilizer products, the main focus of this study was on ICP-OES determination, which offers several unique advantages. Fertilizer samples with consensus P and K values from the Magruder and Association of Fertilizer and Phosphate Chemists (AFPC) check sample programs were selected for this study. Validation materials ranging from 4.4 to 52.4% P2O5 (1.7 to 22.7% P) and 3 to 62% K2O (2.5 to 51.5% K) were utilized. Because all P and K compounds contained in fertilizer materials are not "available" for plants to use, this study was conducted in two parts. Part A focused on ammonium citrate–disodium EDTA as the extraction solvent, as it estimates the pool of fertilizer P and K that is considered available to plants. Part B focused on hydrochloric acid as the digestion solvent, as it estimates the total P and K content of the fertilizer product. Selectivity studies indicated that this method can have a high bias for fertilizer products containing sources of phosphite or organic P compared to gravimetric or colorimetric methods that measure just orthophosphate. Provided the analytical challenges outlined in this study are addressed, this method offers the potential for a quick, accurate, and safe alternative for determining the P and K content of commercial inorganic fertilizer materials.


Author(s):  
Alexandra Schuh ◽  
Dirce Pozebon

This work deals with method validation for regulated metals (Cd, Pb, Ba, Sn, Cr and Cu) determination in infusion and transfusion medical devices. The investigated metals were extracted with water at (37 ± 1) °C followed by their determination in the extract by using inductively coupled plasma optical emission spectrometry (ICP-OES). The validated method was applied in the analysis of infusion and transfusion devices commercialized in Brazil to verify compliance with current legislation, which establishes that the sum of Pb, Ba, Sn, Cr and Cu in the extract must not exceed 1 mg L-1 and that of Cd must not 0.1 mg L-1. Samples from five manufacturers of infusion and transfusion devices, produced in Brazil or imported, were analysed. The results of the analysis showed that all devices complied with the legislation, whereas the sum of Pb, Ba, Sn, Cr and Cu concentrations and that of Cd in the extract were lower than the maximum permissible; Cd was not detected in any sample extract and the sum of the other elements was < 0.14 mg L-1 in all extracts of the analysed samples.


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