INVESTIGATION OF DIRECT DETEMINATION OF MANY IMPURITIES IN HIGH PURITY ZrCl4 MATERIAL AND AFTER SEPARATION OF THE MATRIX Zr USING SOLVENT EXTRACTION USING 2-ETHYL HEXYL PHOSPHONIC ACID MONO 2-ETHYL HEXYL ESTER (PC88A) BY ICP-MS.

Abstract

ICP-MS using matching matrix and internal standard In is believed direct detemination some impurities such as Al, Si, Ti, V, Cr, Fe, Ni, Zn, Nb, Mo, Sn, Hf, Ta and W in high purity ZrCl 4 . The study on capability extraction of Zr(IV) by di-2-ethyl hexyl phosphonic acid mono 2-ethyl hexyl ester (PC88A) were examined by infrared spectrum (IR) of ZrO(NO 3 ) 2 , PC88A-kerosene and Zr-PC88A-kerosene. Impurities in ZrCl 4 were also determinated when using internal standard In after separation of them from the matrix Zr by extracting in 50% of dissolved (PC88A) in kerosene. Investigation of separation of so many impurities from the matrix Zr showed that with using 50% PC88A/kerosene solvent, after one cycle extraction using 3M HNO 3 and 1-2 cycles stripping Zr and scrubbing impurities by 4M HNO 3 can recovery for 95-100% of almost investigated impurity elements and stripping about 22-28% of Zr(IV). Our results indicated that with the mentioned amount of Zr, effect of the matrix Zr on the determination of almost elements by ICP-MS can be negligible. Levels of impurities were relative standard deviations (RSD) less than 8.3% and recoveries (Rev) of 95.0-104.5%, so detemination of impurities was high reliability and accuracy.

Nano ZrO2 Synthesis by Extraction of Zr(IV) from ZrO(NO3)2 by PC88A, and Determination of Extraction Impurities by ICP-MS

“…Inductively coupled plasma mass spectrometry (ICP-MS) is a modern analytical method having the advantages of high sensitivity, low spectral interference, and low matrix effects. Some applications of ICP-MS for determination of impurities in Zr materials (ZrO 2 , Zircaloy 360a, ZrOCl 2 , ZrCl 4 ) are detailed in many studies [5][6][7][8][9][10][11][12][13]. Impurities (or trace elements) with high content can be directly determined by ICP-MS using matching matrix and internal standard (e.g., In, Bi, Rh).…”