X-ray fluorescence analysis of ferroalloys: development of methods for the preparation of test and calibration samples

Abstract

Methods were developed with a view to evaluating various sample preparation systems for use with X-ray fluorescence techniques in order to determine the major and minor components of ferroalloys, which are used as alloy-forming elements in steel making. The methods were compared in terms of simplicity and rapidity and these parameters were assessed in relation to the accuracy and precision of the results. The samples were prepared in three formats: metal samples, by dilution with iron and remelting in an induction furnace; pellets, by direct compaction of the ground material, and beads, by alkaline melting of the pre-oxidized sample. The tests used to optimize these methods were conducted with commercial ferroalloys, previously characterized by employing wet chemical and spectroscopic methods. Reproducibility and precision studies were conducted on samples obtained using each of the three sample preparation systems. The precisions (relative standard deviations) of major element determinations were <0.8, <1.0 and < O S % and those for minor elements were <5, <5 and <3% for metal samples, pellets and beads, respectively. The accuracy of the methods was checked by analysing reference materials of each type of ferroalloy.

Preconcentration and analysis of gold from cyanide solutions with the use of a microcolumn packed with the phosphine oxide Cyanex 921

“…used in the present work is a white solid. Its structure is R,PO, in which R represents the n-octyl chains, and its molecular weight is 386 [4]. The reagent was kindly supplied by Cyanamid Iberica S.A. and was used as obtained by the manufacturer.…”

“…Ref. [4]). The present work centres on the rapid preconcentration and determination by inductively-coupled plasma mass spectrometry (ICP-MS) of gold from 0039.914Oi96/$15.00 (0 1996 Elsevier Science B.V. All rights reserved SSDI 0039-9140(95)01753-4 cyanide solutions.…”

Novel sample treatment procedures for the determination of phosphorus in Cu‐based alloys using X‐ray fluorescence spectrometry to solve the microstructural effect issue

“…In the first method, the alloys were remelted and cast under controlled conditions to obtain fine‐grain samples. In the literature, remelting is described as a technique used for sample homogenization and shape standardization or for the production of test and calibration materials for ferroalloy analyses . Under certain conditions, remelting may be beneficial for material characteristics.…”

“…In the literature, remelting is described as a technique used for sample homogenization and shape standardization [6] or for the production of test and calibration materials for ferroalloy analyses. [7] Under certain conditions, remelting may be beneficial for material characteristics. For example, in SnPb alloys, rapid cooling resulted in the creation of small microstructures.…”

Analysis of Ferromanganese and Ferromanganese Slag by Means of Inductively Coupled Plasma Optical Emission Spectrometry

“…[2][3][4][5][6] The volumetric, spectrophotometric, and gravimetric procedures involve time-consuming and tedious m anipulations of samples. Although a number of papers were published regarding the analysis of ferroalloys [7][8][9][10][11] (including ferromanganese and ferromanganese nodules) by m eans of X-ray uorescence spectroscopy, the major dif culty with this technique is the well-known effects of absorption and/or enhancement related to the m ajor element composition of samples and standards, as well as the av ailability of suitable certi ed refere n ce m aterials (CRM s). Coedo and Dorado 11 recapitulate these two factors and add a third-namely, that ferroalloys are unsuitable for direct m easurement, and a preliminary treatment of the sample is necessary before it can be analyzed.…”