The Isotope-Dilution Determination of Platinum in Soil by Inductively Coupled Plasma Mass Spectrometry

2000 ◽  
Vol 65 (12) ◽  
pp. 1875-1887 ◽  
Author(s):  
Ivan Trešl ◽  
Oto Mestek ◽  
Miloslav Suchánek

A method of the determination of trace amounts of platinum in soils has been developed and validated. Samples were ignited, spiked by 198Pt and decomposed by acid digestion (HF-HClO4, HCl-HNO3). Platinum was separated from the matrix by tellurium coprecipitation (recovery 55-87%) and its content was calculated by the (194Pt + 195Pt + 196Pt)/198Pt ratio measurement. In spite of the separation step (hafnium and tungsten recovery below 1%), residual spectral interference caused by HfO+ ions was observed. This interference as well as that of 198Hg were removed by mathematical correction. Accuracy of the method was confirmed by analysis of certified reference material and by the standard addition method. Detection limit of the method was 0.08 ng g-1 Pt. It was found out that the main component of the standard uncertainty of results was sampling uncertainty. Analysis of soil samples taken in the neighbourhood of Hřensko (Northern Bohemia) showed high platinum contents near the road with heavy traffic.

2005 ◽  
Vol 88 (6) ◽  
pp. 1797-1810 ◽  
Author(s):  
Awad A Momen ◽  
George A Zachariadis ◽  
Aristidis N Anthemidis ◽  
John A Stratis

Abstract Various digestion procedures were carefully investigated and accurately evaluated with respect to their effect on the analysis of cereals and cereal flours. Multielement methods were selected and well developed for the determination of essential (Cr, Cu, Fe, Mg, Mn, and Zn), nonessential (Ag, Al, Ba, Bi, In, and Ga), and toxic (Cd and Pb) minor and trace elements by inductively coupled plasma–atomic emission spectrometry. Only Ag could be determined, either with aqueous standard or standard addition calibration methods, while the standard addition methods were more accurate for the determination of other elements. The recoveries were mostly within the range of 84.1–113% for the expected values of all analytes with respect to certified reference material NIST SRM 1586a (rice flour). The results proved that, for cereals and cereal flours, the use of H2O2 for wet digestion and HNO3 for dry ashing were not necessary. Linear regression analysis and Student's paired t-test were applied to evaluate the significant differences between different procedures and type of samples.


2014 ◽  
Vol 29 (9) ◽  
pp. 1720-1725 ◽  
Author(s):  
Krishnan Chandrasekaran ◽  
Dheram Karunasagar

Matrix precipitation for the sensitive determination of impurities in the Pb–Bi eutectic system by ICP-MS.


2013 ◽  
Vol 740 ◽  
pp. 665-669
Author(s):  
Yong Cheng ◽  
Hui Xian Peng ◽  
Jin Hong Yuan

The potassium metavanadate samples were digested by hydrochloric acid and diluted with water to a constant volume, then the inductively coupled plasma atomic emission spectrometry (ICP-OES) was used to directly determine the content of 10 to 45% matrix vanadium. The matrix effects, spectral interference, background noise and other interference factors in the high concentration of potassium ions coexistence system were all examined in the paper. The results showed that although the coexisting alkali metal potassium significantly increased the ICP flame, the 1g/L potassium standard solution did not produce peaks in the scanning window of analysis line which substantially coincide with the reagent blank signal line, i.e., the 28% (or 0.28g/L) potassium contained in the potassium metavanadate did not interfere with the determination. Therefore, only the standard solution of vanadium was used to draw a calibration curve without the need of potassium matrix matching. In order to obtain a wide linear range and improve the detection precision and the accuracy of the matrix element vanadium, the sample dilution ratio and ICP spectrometer detection parameters were optimized, and the suitable sensitivity spectral lines and their detection integral and background correction regional were selected, the detection signal intensity of the high concentration vanadium is effectively regulated moderate, the detection range is covered from 10 to 45%, which fully meet the need for determination of vanadium in the potassium metavanadate (qualified products containing 37% vanadium). The results also showed that the background equivalent concentration is less than 5 μg/L, the relative standard deviation (RSD) is less than 1.0%, the detection results consistent with the redox titration method. The method is simple and fast, accurate and reliable, the precision is high. The inspection cycle is 10 to 15 minutes, which is greatly shorter than the chemical titration that takes 2 to 3 hours, so that the method meet the requirements of fast-paced production site of the potassium metavanadate product quality inspection and control.


2019 ◽  
Vol 107 (3) ◽  
pp. 215-220
Author(s):  
Brijlesh Kumar Nagar ◽  
Sadhan Bijoy Deb ◽  
Manoj Kumar Saxena ◽  
Bhupendra Singh Tomar

Abstract A method has been developed for quantification of trace rare earth (Ce, Dy, Er, Eu, Gd, Ho, La, Nd, Pr, Sm, Tb and Yb) impurities in alumina and aluminum by inductively coupled plasma mass spectrometry (ICP-MS) after matrix separation. The matrix separation was achieved by selective precipitation of trace elements. Due to its refractory nature a microwave digestion method was developed and optimized for the quantitative dissolution of Al2O3. The analytical methodology was validated by recovery studies with standard addition as well as with an independent γ-spectrometry technique using 152,154Eu tracers. The observed recovery in the synthetic samples was in the range of 93–100% with precision within 6.1–11.6 (%RSD), while the same in the case of radio tracer technique were found to be >98% and <2% (RSD), respectively. The method detection limit was found within 0.5–8.3 μg kg−1, respectively. The procedure is simple, organic waste free and suitable for routine analysis.


1990 ◽  
Vol 44 (1) ◽  
pp. 91-95 ◽  
Author(s):  
Akio Makishima ◽  
Isamu Inamoto ◽  
Koichi Chiba

Isotope dilution analysis with inductively coupled plasma mass spectrometry (ICP-MS) was applied to the determination of gallium in pure aluminum. Furthermore, a solvent extraction procedure was combined with isotope dilution analysis as a preconcentration technique in order to determine ultra-trace levels of gallium with high precision. The accuracy and the precision of isotope dilution analysis using ICP-MS were compared with those of conventional standard addition analysis using ICP-MS. Isotope dilution analysis gave more accurate and precise results than did standard addition analysis. Isotope dilution analysis with solvent extraction made it possible to measure 0.029 µg/g gallium in 99.999% aluminum with analytical errors at less than 3%.


2011 ◽  
Vol 301-303 ◽  
pp. 569-572 ◽  
Author(s):  
Gao Wa Jin ◽  
Qian Gong ◽  
You Qiong Cai ◽  
Xiao Lei Li ◽  
Yong Fu Shi ◽  
...  

A method based on microwave digestion and inductively coupled plasma-mass spectrometry (ICP-MS) has been established for the sensitive determination of cadmium in bivalve molluscs. The application of the internal standards calibration improved the accuracy and precision values of the method. The relative standard deviation (RSD), the standard addition recovery value and the detection limit were determined as 4.25%, 94.74% and 0.005 μg/L, respectively. This method has been verified by the determination of cadmium in certified reference material kelp (GBW08517) and mussel (GBW08571). The method has been applied to determine the contamination concentration level of cadmium in seven kinds of bivalve mollusk samples. The results indicated that, among them, mud clam, scallop and oyster have relative high accumulation ability to cadmium.


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