Determination of Ti, V, Zr, Nb, Mo and Ta in High-Purity Iron Using Cupferron Co-Precipitation Separation by Axially Viewed ICP-AES with Ultrasonic Nebulization System and a Long Torch

Abstract

An analytical method was established for the determination of trace amounts of refractory metal elements (Ti, V, Zr, Nb, Mo and Ta) in high-purity iron samples by axially viewed inductively coupled plasma atomic emission spectroscopy (ICP-AES). We investigated the analytical method of a trace amount of refractory metal elements in high-purity iron matrix using cupferron coprecipitation separation procedure and by axially viewed ICP-AES with ultrasonic nebulization system and a long torch. The established analytical procedure was as follows. A 1.0 g of high-purity iron sample was decomposed with 150 cm 3 of hydrochloric acid (1 + 4) by heating on a hot plate at 453 K. After cooling the sample solution to room temperature, we added 10 cm 3 of ascorbic acid solution and cupferron solution to it, and then separated analyte elements. After filtration, the precipitate and residue were decomposed with 10 cm 3 of nitric acid and 10 cm 3 of perchloric acid, and evaporated to dryness. After leaving cool, salts were dissolved with nitric acid. The sample solution was determined by axially viewed ICP-AES with ultrasonic nebulization system and a long torch. For the controlled matrix concentration, the good precisions and accuracy were obtained by using matrixmatched standard solutions for calibration curves to the ultrasonic nebulization system method. The limit of determination is considerably low in the ultrasonic nebulization system method, which thus demonstrating the effectiveness of the ultrasonic nebulization system method. The recoveries of added six elements were 100% for Ti, Nb and Mo, and 101% for V and Zr, 102% for Ta; the limits of detection were 0.03 ng cm −3 for Ti and Zr to 1.00 ng cm −3 for Ta. (Received February 18, 2002; Accepted April 30, 2002) Keywords: inductively coupled plasma atomic emission spectroscopy, ultrasonic nebulization system, axially viewed inductively coupled plasma atomic emission spectroscopy (ICP-AES), long torch, determination of titanium-vanadium-zirconium-niobiummodybdenum and tantalum, cupferron coprecipitation separation, high-purity iron sample

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

“…It is obvious that low detection limits of trace-elements in the matrices with multilinear spectra (d-and f-elements) require the sample matrix to be separated. The use of ultrasonic nebulisers, instruments with an axial observation of plasma 65 , and ETA also reduces the detection limits.…”

“…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.…”

Estudo da matéria orgânica e composição elementar de solos arenosos de regiões próximas a São Gabriel da Cachoeira no Amazonas

“…Esta técnica analítica possibilita a determinação rápida de vários elementos em diferentes faixas de concentração, baseada no espectro de emissão dos mesmos (Vandecasteele;Block, 1997 (Ide;Nakamura, 2002;Trevizan et al, 2003). A amostra pode ser introduzida no plasma na forma gasosa, líquida ou suspensão.…”

Determination of the Trace Refractory Elements V, Nb and Ta in Environmental Samples by ICP-MS After Separation and Preconcentration with Nanometre-Sized Alumina Microcolumns Following Chemical Modification by Gallic Acid

“…Nowadays, many separation/preconcentration techniques for metal ions have been developed for this purpose, and these include liquid-liquid extraction (LLE) (Agrawal 2002, Agulyansky et al 2004, cloud point extraction (CPE) (Paleologos et al 2001), co-precipitation (Ide and Nakamura 2002), solid phase extraction (SPE) (Pyrzynska and Wierzbicki 2004), high performance liquid chromatography (HPLC) (Li et al 2004) and capillary electrophoresis (CE) (Liu et al 2001), and so on. Of all these methods, SPE is used widely in online flow injection separation and preconcentration systems.…”