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User Benefits Application News Introduction Steel materials are widely used in a diverse range of industries, including construction, transportation, and machinery manufacturing, and are indispensable in modern society. Steel contains various elements, and the types and concentrations of these elements significantly influence its properties. Accordingly, elemental analysis is essential for quality assurance and performance control. The elements in steel range from trace constituents to major components, with concentrations spanning a broad range from mg/L levels to percentage levels. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is well suited to the analysis of elements across such a wide concentration range. It enables highly accurate quantitative analysis from trace elements to major components. This Application News presents an analysis example of a stainless-steel certified reference material using the Shimadzu ICPE-9820 multi-type ICP atomic emission spectrometer (Fig. 1). The ICPE-9820 enables analysis across a wide concentration range, from trace to major elements in steel. Using a torch for high-salt samples and a water bubbler can suppress salt deposition when analyzing high-salt samples. The use of a vacuum spectrometer enables rapid startup and quick analysis in the vacuum ultraviolet region (wavelengths below 190 nm). Analysis of Trace and Major Elements in Steel by ICP-AES Jiajie Du and Susumu Hashimoto Inductively Coupled Plasma Atomic Emission Spectrometer Instrument Configuration Measurements were performed using the Shimadzu ICPE-9820. For the analysis of trace elements at low dilution ratios, a torch for high-concentration salt solution samples and a water bubbler were used to prevent sensitivity loss from salt deposition. In addition, the plasma torch is positioned vertically in the ICPE-9820, which helps reduce potential memory effects (Application News No. J112). The chamber was equipped with a Twister spray chamber (Fig. 2), which enables finer particle-size selection and improves analytical accuracy for high-salt samples. Details of the instrument configuration are provided in Table 1. Fig. 1 ICPE-9820 Sample Stainless-steel certified reference material NSTM SUS570-1 (Nippon Steel Technology Co., Ltd.) Sample Pretreatment One gram of the sample was weighed and dissolved by heating in 60 mL of mixed acid (hydrochloric acid: nitric acid: water = 3 : 1 : 4). The resulting solution was made up to 100 mL and used as the stock solution for measurement. As a parallel preparation test, the same pretreatment procedure was repeated three times. Sample for Major Element Analysis The stock solution obtained during sample preparation was diluted 25-fold with dilute hydrochloric acid solution. Yttrium (Y) was added as an internal standard element to achieve a concentration of 20 mg/L in the measurement solution. Sample for Trace Element Analysis The stock solution obtained during sample preparation was diluted twofold with purified water. During dilution, the elements to be analyzed were added to prepare standard addition sample solutions. Fig. 2 Twister Spray Chamber Table 1 Instrument Configuration Instrument: ICPE-9820 Nebulizer: Nebulizer, 10UES Chamber: Twister Spray Chamber, HE Torch: Torch for High-concentration Salt Solution Samples Auto Sampler: AS-10 Other Accessories: Water Bubbler Analysis Conditions The ICPE-9820 enables simultaneous analysis using two view orientations: axial view (AX), which offers higher sensitivity, and radial view (RD), which is suitable for high-concentration analysis. For major element analysis, quantification was performed using the calibration curve method with the internal standard method. For trace element analysis, quantification was performed using the standard addition method. The analysis conditions are listed in Table 2. Table 2 Analysis Conditions RF Power: 1.40 kW Plasma Gas Flowrate: 15.0 L/min Auxiliary Gas Flowrate: 1.20 L/min Carrier Gas Flowrate: 0.70 L/min (0.65 L/min*) Observation Mode: AX, RD * Carrier gas flowrate used for trace element analysis
Application News www.shimadzu.com/an/ Shimadzu Corporation © Shimadzu Corporation, 2026 For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. See https://www.shimadzu.com/about/trademarks/index.html for details. Third party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “”. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. Calibration Standards For Major Element Analysis Commercial single-element standard solutions were diluted and mixed to prepare calibration standards. The concentrations of the analytes contained in the calibration standards for major element analysis are listed in Table 3. First Edition: Sep. 2026 01-01072-EN Related Applications 1. Simultaneous Analysis of Trace and Major Elements in Iron and Steel by ICPE-9820, Application News No. J112 2. Trace Element Analysis of Steel Using ICP-MS, Application News No. 01-01207-en Table 4 Standard Addition Samples for Trace Elements Elem. STD1 (mg/L) STD2 (mg/L) STD3 (mg/L) STD4 (mg/L) Cu 0 5 10 - P 0 5 10 - Sn 0 1 2 - Si 0 - - 50 Elem. Wavelength (nm) View Solid Conc. (%) SD σ (%) Rep. (%) Cert. Values (%) Cr 267.716 RD 18.17 0.02 0.1 18.14 ± 0.04 Mn 257.610 RD 1.96 0.002 0.1 1.95 ± 0.01 Mo 202.030 RD 2.58 0.004 0.2 2.59 ± 0.02 Ni 231.604 RD 8.21 0.007 0.08 8.21 ± 0.02 * 1 Solid Detection Limit (Solid DL): 3 × σ(standard deviation of STD-1) × slope of calibration curve × dilution factor * 2 Si was subjected to pretreatment with mixed acid; however, due to its limited long-term stability, it is listed here as a reference value. Table 5 Quantitative Results for Major Elements Elem. Wavelength (nm) View Solid DL (%)* 1 Solid Conc. (%) SD σ (%) Rep. (%) Cert. Values (%) Cu 324.754 AX 0.0002 0.0509 0.0003 0.6 0.0515 ± 0.0008 P 178.287 AX 0.0005 0.0421 0.0004 0.9 0.0423 ± 0.0005 Sn 189.989 AX 0.0001 0.0097 0.0001 1.0 0.00976 ± 0.00024 Si* 2 251.611 AX 0.009 0.530 0.005 1.0 0.515 ± 0.005 Table 6 Quantitative Results for Trace Elements Table 3 Calibration Standards for Major Elements Elem. STD1 (mg/L) STD2 (mg/L) STD3 (mg/L) STD4 (mg/L) STD5 (mg/L) Cr 0 10 25 50 100 Mn 0 1 2.5 5 10 Mo 0 2 5 10 20 Ni 0 5 12.5 25 50 Y 20 mg/L Fe 250 mg/L Nitric Acid 0.3 v/v% Hydrochloric Acid 2.0 v/v% For Trace Element Analysis Standard addition samples were prepared as shown in Table 4. Fig. 3 shows an example of manganese (Mn) calibration curves. For the same element, calibration curves covering different concentration ranges can be prepared by changing the view orientation or measurement wavelength. This allows the software to automatically select the appropriate calibration curve for each sample according to the element concentration, thereby reducing post-analysis data evaluation time and minimizing evaluation errors. Fig. 3 Mn Calibration Curves (a) Mn 257.610nm RD (0.625–2.5 wt%) (b) Mn 260.569nm AX (0–0.625 wt%) Results For the quantitative analysis, samples prepared in triplicate during sample pretreatment were analyzed. The three sample solutions prepared during pretreatment were each measured three times within a single analytical run (N = 3), yielding a total of nine analytical results. Table 5 shows the mean solid concentration (Solid Conc.), standard deviation (SD), and repeatability (Rep.) for each element. Quantitative results for the major elements are presented in Table 5, and those for the trace elements are presented in Table 6. For many elements, good agreement with the certified values (Cert. Values) was obtained. The parallel tests also demonstrated good reproducibility. Conclusion In this Application News, trace and major elements in a stainless-steel certified reference material were analyzed using the ICPE-9820. The measured values showed good agreement with the certified values. The sample introduction system, consisting of a torch for high- concentration salt solution samples and a water bubbler, effectively prevented sensitivity loss from salt deposition. At the same time, the use of a Twister spray chamber enabled finer particle-size selection, thereby improving analytical accuracy for high-salt samples. In addition, the ICPE-9820 employs a vacuum spectrometer, enabling rapid startup and fast analysis in the vacuum ultraviolet region (wavelengths below 190 nm).
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