Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion
High carbon-chrome iron samples can be decomposed using strong oxidizing acid, mixed acid or by the alkali fusion method under high temperature. These chemical procedures are complex, especially the alkali fusion method, which introduces a large amount of interfering ions such as Na+. Microwave dige...
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Science Press, PR China
2014-03-01
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Online Access: | http://www.ykcs.ac.cn/cn/article/id/2a661f20-2ec0-406b-bb7d-f52f0ef23709 |
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author | HU De-xin XIAO Ku WANG Xiang-dong WANG Zhen-kun LIU Min LI Quan-bin |
author_facet | HU De-xin XIAO Ku WANG Xiang-dong WANG Zhen-kun LIU Min LI Quan-bin |
author_sort | HU De-xin |
collection | DOAJ |
description | High carbon-chrome iron samples can be decomposed using strong oxidizing acid, mixed acid or by the alkali fusion method under high temperature. These chemical procedures are complex, especially the alkali fusion method, which introduces a large amount of interfering ions such as Na+. Microwave digestion technology is widely used in the pretreatment process of insoluble samples. This pretreatment method combined with Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) has been reported to determine Fe in high carbon-chrome iron. Based on previous studies, a method for the simultaneous determination of silicon, manganese and phosphorus has been established in this study. HNO3 is conducted to digest easy decomposition components in high carbon-chrome iron. HClO4 and HF are then loaded to digest carbides and silicides. Since there is a reduction in the volume of HClO4, the process is stable and safe. Using high carbon-chrome iron standard materials to set up the calibration curve, and Y, In and Bi as internal standard elements, the detection limits of silicon manganese and phosphorus were 0.0017%, 0.0025% and 0.0033%, respectively. Precision and accuracy of this method were verified by using high carbon-chrome iron standard materials of GSB 03-1562—2003, GSB 03-1058—1999 and GSB 03-1059—1999. The results were consistent with the certified values. The relative standard deviations (RSD) are in the range 0.8%-6.0% (n=11), and the relative deviations (RE) are from 0.044% to 0.227%. This method has the advantage of digesting the sample completely, is safe and has a simple operation process and a high degree of accuracy, which can also be used for the determination of several elements in high carbon-chrome iron. |
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spelling | doaj.art-0c56a04f8d6e498fbcdf7f2ba0891a592023-02-09T07:06:31ZengScience Press, PR ChinaYankuang ceshi0254-53572014-03-01332208211ykcs-33-2-208Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave DigestionHU De-xin0XIAO Ku1WANG Xiang-dong2WANG Zhen-kun3LIU Min4LI Quan-bin5Minerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, ChinaMinerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, ChinaTianjin Inspection and Test Development Service Co., LTD, Tianjin 300457, ChinaMinerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, ChinaMinerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, ChinaMinerals and Metallic Materials Inspection Center, Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, ChinaHigh carbon-chrome iron samples can be decomposed using strong oxidizing acid, mixed acid or by the alkali fusion method under high temperature. These chemical procedures are complex, especially the alkali fusion method, which introduces a large amount of interfering ions such as Na+. Microwave digestion technology is widely used in the pretreatment process of insoluble samples. This pretreatment method combined with Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) has been reported to determine Fe in high carbon-chrome iron. Based on previous studies, a method for the simultaneous determination of silicon, manganese and phosphorus has been established in this study. HNO3 is conducted to digest easy decomposition components in high carbon-chrome iron. HClO4 and HF are then loaded to digest carbides and silicides. Since there is a reduction in the volume of HClO4, the process is stable and safe. Using high carbon-chrome iron standard materials to set up the calibration curve, and Y, In and Bi as internal standard elements, the detection limits of silicon manganese and phosphorus were 0.0017%, 0.0025% and 0.0033%, respectively. Precision and accuracy of this method were verified by using high carbon-chrome iron standard materials of GSB 03-1562—2003, GSB 03-1058—1999 and GSB 03-1059—1999. The results were consistent with the certified values. The relative standard deviations (RSD) are in the range 0.8%-6.0% (n=11), and the relative deviations (RE) are from 0.044% to 0.227%. This method has the advantage of digesting the sample completely, is safe and has a simple operation process and a high degree of accuracy, which can also be used for the determination of several elements in high carbon-chrome iron.http://www.ykcs.ac.cn/cn/article/id/2a661f20-2ec0-406b-bb7d-f52f0ef23709high carbon-chrome ironsiliconmanganesephosphorusmicrowave digestioninductively coupled plasma-atomic emission spectrometry |
spellingShingle | HU De-xin XIAO Ku WANG Xiang-dong WANG Zhen-kun LIU Min LI Quan-bin Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion Yankuang ceshi high carbon-chrome iron silicon manganese phosphorus microwave digestion inductively coupled plasma-atomic emission spectrometry |
title | Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion |
title_full | Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion |
title_fullStr | Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion |
title_full_unstemmed | Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion |
title_short | Determination of Silicon Manganese and Phosphorus in High Carbon-chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion |
title_sort | determination of silicon manganese and phosphorus in high carbon chrome iron by inductively coupled plasma atomic emission spectrometry after microwave digestion |
topic | high carbon-chrome iron silicon manganese phosphorus microwave digestion inductively coupled plasma-atomic emission spectrometry |
url | http://www.ykcs.ac.cn/cn/article/id/2a661f20-2ec0-406b-bb7d-f52f0ef23709 |
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