Quantitative chemical analysis of pickling solutions by x‐ray fluorescence spectrometry

Abstract

A quantitative analytical method of chlorine and iron in hydrochloric pickling solutions by x‐ray spectrometry in atmospheric He mode is proposed. This work is concerned with the replacement of the wet chemical analyses of pickling solutions with rapid and reproducible quantification by an x‐ray fluorescence spectrometer. An in‐depth investigation was performed to identify the species present in real pickling solutions. X‐ray diffraction patterns and semiquantitative results for the pickling solutions provided synthetic standards based on the compositional range of solutions by analyzing the pickling solutions obtained in real processes. Twenty‐seven liquid calibration standards were prepared by diluting standard solutions certified by wet chemical analyses for the x‐ray fluorescence spectrometry (XRF) calibration curves for Cl and Fe. The suggested method showed satisfactory precision and accuracy in the analysis of pickling solutions. It is possible to estimate the acidities of pickling acid solutions on the basis of the correlation between the HCl concentrations calculated from a simple XRF measurement of total Cl and Fe concentrations and those measured by acid‐base titration methods. Copyright © 2007 John Wiley & Sons, Ltd.

Atomic spectrometry update. X-ray fluorescence spectrometry

“…Specifically, the determination of Mg and S was affected by a matrix effect from phosphorous, whilst different C/H ratios did not cause significant differences. Jung et al [259][260][261] devised three quantitative analytical methods using XRF. The first paper presented the determination of Cl and Fe in hydrochloric pickling solutions, whilst the second contribution described the determination of Cl, Fe and Zn in electroplating solutions.…”

Chemical Analysis of Zinc Electroplating Solutions by X-ray Fluorescence Spectrometry

“…The second mode, atmospheric He mode, is selected for the measurement of volatile elements in solutions where reproducible measurement should be required for acid-based solutions. The previous research 10) convey that the precision RSD values of the volatile element like chlorine measured in atmospheric He mode were significantly smaller than those in He mode. This might indicate that the X-ray radiation has an influence on the heating of acid-based solutions and on the rapid decrease of solution acidity with time.…”

Development of a Concentration Measurement System for Pickling Line Control

“…Ultrasonic velocity changes due to acid concentration. 0.0000000e+000 a 5 -4.7305890e+000 a 6 0.0000000e+000 a 7 0.0000000e+000 a 8 2.0413212e+000 a 9 0.0000000e+000 a 10 2.0413212e+000 a 11 4.9006009e-002 a 12 7.1304870e-003 a 13 -1.7665033e-003 Accuracy +-0.7 g/l…”