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A novel approach for chlorine determination in acidic medium by total reflection x‐ray fluorescence
Author(s) -
Misra N. L.,
Varga Imre,
Dhara Sangita,
Aggarwal Suresh K.
Publication year - 2009
Publication title -
x‐ray spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.447
H-Index - 45
eISSN - 1097-4539
pISSN - 0049-8246
DOI - 10.1002/xrs.1139
Subject(s) - chlorine , chemistry , x ray fluorescence , reagent , analytical chemistry (journal) , tungsten , analyte , nitric acid , detection limit , fluorescence , silver chloride , chloride , limiting , standard solution , chromatography , inorganic chemistry , electrode , optics , mechanical engineering , engineering , physics , organic chemistry
A novel approach for chlorine (Cl) determination in acidic medium using total reflection x‐ray fluorescence (TXRF) is reported. It is based on the addition of a known excess amount of AgNO 3 solution to the sample containing Cl for precipitating silver chloride (AgCl). This is followed by TXRF determination of Ag in supernatant after filtering, employing Cd as an internal standard. Tungsten (W) continuum excitation at 50 kV and 38 mA was used for TXRF measurements. Ag Kα line of the analyte, Ag and Cd Kα line of the internal standard, Cd were used for such determinations of Ag. Six samples of NaCl were prepared in HNO 3 medium of different molarities to obtain the Cl concentrations ranging from 1 to 60 µg/ml. The precision of such TXRF determinations of Cl in nitric acid medium samples was found to be better than 10% (1σ) and the results deviated from the expected Cl concentrations by less than 15%. An overall laboratory and reagents blank of 1.5 ± 0.5 µg/ml was obtained limiting the applicability of this approach to Cl levels of about 5 µg/ml. This can be improved by using ultra clean laboratory and high purity reagents. Copyright © 2009 John Wiley & Sons, Ltd.