ANALYSIS OF GEOLOGICAL MATERIALS BY ICP-AES WITH CALIBRATION IN CONCENTRATION RATIO

2019 ◽  
Vol 85 (6) ◽  
pp. 24-29
Author(s):  
T. A. Karimova ◽  
G. L. Buchbinder

A method of calibration in relative concentrations (concentration ratio) previously used only in analysis of non-ferrous and ferrous metals was first implemented when performing silicate analysis of geological materials using atomic emission spectrometry with inductively coupled plasma (AES-ICP). Prior to apply the Concentration Calibration Ratio to analysis of geological materials it is necessary to consider and address the following problems: some of the components are not determined by ICP-AES, matrix elements may be present in different oxidation states. Sample preparation of ores and geological materials was carried out in autoclaves heated at 180°C using HotBlock 200 system. A mixture HCl/HNO3/HF was used at the first step and then added with a 4% H3BO3 solution. The repeatability and intermediate precision of determination when using Concentration Ratio Calibration, calibration without internal standard and Calibration with In as internal standard are compared for determination of SiO2 (content 40 – 75%), Al2O3 (5 – 20%), CaO (0.25 – 15%), MgO (0.1 – 15%), Fe2O3 (0.5 – 15%), Na2O (0.5 – 10%), K2O (0.5 – 5%), P2O5 (0.01 – 0.3%), MnO (0.03 – 0.5%), and TiO2 (0.05 – 2%). The use of Concentration Ratio Calibration provides better metrological characteristics, repeatability and precision in analysis of geological materials compared to other calibration procedures due to elimination of the calibration error of balances and volumetric flasks from total error of analysis; measuring the large intensities of the base element; and better accuracy of measuring the intensity ratio compared to absolute intensity measurements.

2020 ◽  
Vol 86 (5) ◽  
pp. 16-21
Author(s):  
T. A. Karimova ◽  
G. L. Buchbinder ◽  
S. V. Kachin

Calibration by the concentration ratio provides better metrological characteristics compared to other calibration modes when using the inductively coupled plasma atomic emission spectrometry (ICP-AES) for analysis of geological samples and technical materials on their base. The main reasons for the observed improvement are: i) elimination of the calibration error of measuring vessels and the error of weighing samples of the analyzed materials from the total error of the analysis; ii) high intensity of the lines of base element; and iii) higher accuracy of measuring the ratio of intensities compared to that of measuring the absolute intensities. Calcium oxide is better suited as a base when using calibration by the concentration ratio in analysis of carbonate rocks, technical materials, slags containing less than 20% SiO2 and more than 20% CaO. An equation is derived to calculate the content of components determined in carbonate materials when using calibration by the concentration ratio. A method of ICP-AES with calibration by the concentration ratio is developed for determination of CaO (in the range of contents 20 – 100%), SiO2 (2.0 – 35%), Al2O3 (0.1 – 30%), MgO (0.1 – 20%), Fe2O3 (0.5 – 40%), Na2O (0.1 – 15%), K2O (0.1 – 5%), P2O5 (0.001 – 2%), MnO (0.01 – 2%), TiO2 (0.01 – 2.0%) in various carbonate materials. Acid decomposition of the samples in closed vessels heated in a HotBlock 200 system is proposed. Correctness of the procedure is confirmed in analysis of standard samples of rocks. The developed procedure was used during the interlaboratory analysis of the standard sample of slag SH17 produced by ZAO ISO (Yekaterinburg, Russia).


2011 ◽  
Vol 9 (2) ◽  
pp. 213-217 ◽  
Author(s):  
George Zachariadis ◽  
Efrosini Sahanidou

AbstractA multi-element analytical method based on inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed for trace elements in pharmaceutical tablets and cosmetics. Titanium was also included in the analytes since it is widely used in pharmaceuticals. Critical ICP conditions, like RF incident power, argon gas flow rate and nebulizer sample uptake flow rate were optimized. The most sensitive spectral line of each analyte was selected as optimum for further study. Detection limits in the low µg g−1 range were obtained. Prior to chemical analysis, the samples were decomposed by acid digestion, using various mixtures of HCl, HNO3 and HF. Yttrium was used as a suitable internal standard in order to correct for possible matrix effects. The method was applied to the analysis of six different pharmaceutical products (anti-biotic, anti-inflammatory, anti-hypertensive) in the form of tablets with film coating and also three cosmetic products like hair and face masks.


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