Selective Precipitation Separation and Inductively Coupled Plasma Mass Spectrometric Determination of Trace Metal Impurities in High Purity Silver

Abstract

A simple and rapid method for the determination of some trace element impurities in high purity silver, combining the isolation of analytes from the silver matrix with selective precipitation followed by ICP-MS determination was developed. On the basis of an extreme difference in the solubilities of the chlorides of silver and the other accompanying trace elements, silver can be separated completely through the addition of hydrochloric acid. The sample of silver was at first dissolved in 7 M nitric acid followed by addition of hydrochloric acid to remove the silver matrix by formation of a silver chloride precipitate, while leaving the trace element impurities in the solution, which was subsequently analysed by ICP-MS. Eleven elements (Al, Au, Cd, Co, Cu, Fe, Mg, Mn, Ni, Pb and Sn) were determined with good accuracy and precision. The limits of detection (based on the 3 sigma criterion) of these elements were 10(-1)-10(-3) ng g-1. The proposed method was successfully applied to the determination of metal impurities in high-purity silver samples (EM9465 and EM 9343) and validated by the analysis of NIST SRM 8171 (Fine Silver FS 14).

Analysis of high-purity solids by atomic emission spectroscopy and mass spectrometry with atom excitation and ionisation in inductively coupled plasma

“…Unfortunately, their list for the high-purity substances is short. Standards of the SARM, BCR and NIST series (SRM 1635, SRM 1630a, SRM 1632b and SRM 1633b) are used for the ICP-MS analysis of coal and ash, 9,17,19 NIST (SRM 8171) for the analysis of silver, 63 65 and silicate glasses NIST (SRM 610-615) for the analysis of oxide crystals. 66 ± 68 According to the results of the inter-laboratory measurements, these glasses contain *50 elements as impurities in the 1610 74 mass % ± 5610 72 mass % concentration range.…”

Determination of trace elements in the Pb–Bi-eutectic system by inductively coupled plasma-quadrupole mass spectrometry after sequential removal of the matrix by precipitation

“…A number of methods such as solvent extraction, [10][11][12] ionexchange 13 or selective precipitation [14][15][16] may be employed to remove the matrix. Extraction of Bi(III) from acid or highly acidic solutions of HCl, HBr, HNO 3 and/or H 2 SO 4 using Cyanex® 925, Cyanex® 921, 2-bromoalkanoic acid and Cyanex® 302 as extractants has been proposed.…”

Estimation of Metal Impurities in High-Purity Nitric Acids Used for Metal Analysis by Inductively Coupled Plasma-Mass Spectrometry

“…The preconcentration methods, such as evaporation, 1 solvent extraction, 2 precipitation, 3 and ion-exchange, 4 for trace metals in high-purity reagents, are infeasible because possible contaminations from experimental environment and vessels are often very serious. In this work, an evaluation for metal impurities in nitric acid was directly accomplished by measuring diluted nitric acid by ICP-MS.…”