Measurement of Inclusion Size by Laser Ablation ICP Mass Spectrometry

Abstract

By using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), the measurement of particle size has been made for one component oxide (Al 2 O 3 and MgO) and multicomponent oxide (12CaO · 7Al 2 O 3 and CaO-Al 2 O 3 -MgO) located on surface of iron or glass sample. The method of particle size estimation by LA-ICP-MS has been developed coupled with a new method of making samples with particles. The size calibration lines for Al 2 O 3 , MgO and CaO particles have been obtained. The results of particle size measurement by LA-ICP-MS are compared with those by SEM and single-particle optical sensing (SPOS) methods. It was confirmed that LA-ICP-MS has the perspective to be used for the quick measurement of inclusion composition and size in metal and other materials. The size frequency distributions of Al 2 O 3 particles measured by LA-ICP-MS in iron samples with particles agree reasonably well with those by SEM and SPOS in the range of particle diameter from 2 to 20 mm. The size of Al 2 O 3 , MgO and complex oxide (12CaO · 7Al 2 O 3 and CaO-Al 2 O 3 -MgO) particles measured by LA-ICP-MS is in good agreement with that by SEM in the range of particle diameter from 10 to 40 mm.KEY WORDS: quantitative analysis; metal; particle size; laser ablation ICP mass spectrometry.

Analysis of Composition and Size Distribution of Inclusions in Fe-10Mass%Ni Alloy Deoxidized by Al and Mg Using Laser Ablation ICP Mass Spectrometry

“…Detailed explanation and some characteristics of LA-ICP-MS system are already given in previous article. 1,3) The standard samples and metal samples were ablated and analyzed by using the following parameters; laser scan rate of 0.01 mm/s, laser energy of 2.0 mJ/shot, frequency of laser shots of 20 Hz, defocus of laser beam of 0 mm, and integration time of 0.1 or 0.01 s. The width and depth of laser track on metal surface were on the average 25 and 50 mm, respectively at given ablation parameters. Total ablated area was 0.7 to 1.0 and 0.2 to 0.4 mm 2 for the samples in Exp.…”

“…The analysis of standard samples was made every 1 h since the slope of calibration line changes with ablation time. 1,3) …”

“…Then, the sample was dissolved in the mixture of 10 cm 3 of hot HCl (1ϩ1) and 5 cm 3 of HNO 3 (1ϩ1). For the estimation of soluble Mg and Al, the solution after filtration was vaporized with 30 cm 3 of HCl (1ϩ1), followed by dissolution in the mixture of 10 cm 3 of hot HCl (1ϩ1) and 5 cm 3 of HNO 3 (1ϩ1). The soluble and insoluble Al and Mg contents were determined by using inductively coupled plasma (ICP) emission spectrometry.…”

“…In previous works, [1][2][3][4][5] it has been demonstrated that the composition and size of oxide particles in metal and other materials can be measured by using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The precision and accuracy of the LA-ICP-MS analysis is found to be 2 to 5 % for Al 2 O 3 , MgO and CaO content in synthetic particles of CaO-Al 2 O 3 , CaO-Al 2 O 3 -MgO and MgO-Al 2 O 3 systems.…”

“…1,2) The difference between the size of synthetic particles in the range of 10Յd V Յ40 mm obtained by LA-ICP-MS and that by SEM is on the average 1.7 mm by using Al 2 O 3 calibration line and 2.4 mm by using MgO calibration line. 3) In this study, the LA-ICP-MS has been used for the determination of the inclusion composition and size distribution of oxide particles with d V Ͻ10 mm in an Fe-10mass%Ni alloy deoxidized by Al followed by Mg and Mg followed by Al addition. The composition, number and size of inclusions on metal surface are analyzed as a function of holding time at 1 600°C.…”