Detection method for rapidly measuring micro trace quantity tin in ship hull steel by atomic fluorescence spectrometry

A rapid measurement technology of atomic fluorescence spectroscopy, which is applied in the field of special steel detection, can solve the problems of unapplicable and non-measurement of hull steel, etc.

Inactive Publication Date: 2008-12-17
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wait, the method of using ICP-AES to test trace tin in hull steel is much simpler than the national standard, but it cannot be applied to units that do not have inductively coupled plasma emission sp

Method used

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  • Detection method for rapidly measuring micro trace quantity tin in ship hull steel by atomic fluorescence spectrometry
  • Detection method for rapidly measuring micro trace quantity tin in ship hull steel by atomic fluorescence spectrometry
  • Detection method for rapidly measuring micro trace quantity tin in ship hull steel by atomic fluorescence spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0078] Weigh 0.1019g of the actual sample into a 100ml beaker, add 10ml of concentrated HCL, heat and dissolve on a hot plate, then add 2ml of concentrated HNO3, continue heating to a slight boiling state, evaporate until 1-2mL remains, remove and cool, Transfer to a 25ml volumetric flask, and dilute to the mark with 2% HCL. At the same time, make a sample blank. Under the working conditions selected by the instrument, measure the fluorescence intensity values ​​of the blank, tin standard solution and sample respectively.

[0079] The test conditions are: negative high voltage 330V lamp current 90mA atomization height 6mm carrier gas flow 400ml / min shielding gas flow 600ml / min potassium borohydride 2% tartaric acid 5%, thiourea and ascorbic acid 0.8%.

Embodiment 2

[0081] Weigh 0.1050g of the actual sample into a 100ml beaker, add 10ml of concentrated HCL, heat and dissolve on a hot plate, then add 2ml of concentrated HNO3, continue heating to a slight boiling state, evaporate until 1-2mL is left, then remove and cool. Transfer to a 25ml volumetric flask, and dilute to the mark with 3% HCL. At the same time, make a sample blank. Under the working conditions selected by the instrument, measure the fluorescence intensity values ​​of the blank, tin standard solution and sample respectively.

[0082] The test conditions are: negative high voltage 370V lamp current 50mA atomization height 8mm carrier gas flow 600ml / min shielding gas flow 900ml / min potassium borohydride 3.5% tartaric acid 3%, thiourea and ascorbic acid 2%.

Embodiment 3

[0084] Weigh 0.0990g of the real sample into a 100ml beaker, add 10ml of concentrated HCL, heat and dissolve on a hot plate, then add 2ml of concentrated HNO3, continue heating to a slight boiling state, evaporate until 1-2mL is left, remove and cool, Transfer to a 25ml volumetric flask, and dilute to the mark with 5% HCL. At the same time, make a sample blank. Under the working conditions selected by the instrument, measure the fluorescence intensity values ​​of the blank, tin standard solution and sample respectively.

[0085] The test conditions are: negative high voltage 360V lamp current 70mA atomization height 7mm carrier gas flow 500ml / min shielding gas flow 700ml / min potassium borohydride 3% tartaric acid 4%, thiourea and ascorbic acid 1%.

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Abstract

A method for rapidly detecting trace tin in the hull steel by adopting the atomic fluorescence spectrometry relates to the technology field of the special steel detection. Tartaric acid, thiourea and ascorbic acid are adopted as a masking agent so as to successfully eliminate the interference of the elements. The analysis time of one sample requires about 5 hours. The method is suitable for measuring the tin content with a mass fraction of 0.0001%-0.10%, a mark-on recovery rate of 98%-108% and detectability of 0.76ng/ml. The method has the advantages of lower interference, wide analytical range, high stability, high speed, etc., when detecting trace tin in the hull steel.

Description

technical field [0001] The invention relates to the technical field of detection of special steel materials, in particular to a detection method for rapid detection of micro-trace tin in ship hull steel by hydride generation-atomic fluorescence spectrometry. Background technique [0002] Tin is generally carried by steelmaking raw materials and remains in steel. It is one of the "five evils" we usually call. Its content in steel generally does not exceed 0.1%, and in most high-quality steels it does not exceed 0.01%. . Even the existence of a small amount of tin will have an adverse effect on the properties of the steel, and its main hazard is to reduce the impact value, strength and tensile capacity of the steel. Therefore, the accurate determination of tin in steel has a great effect on the research of the process performance of steel. [0003] Because the content of tin in steel is not high, it brings great difficulties to the chemical quantitative analysis of tin. The...

Claims

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Application Information

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IPC IPC(8): G01N21/62
Inventor 杜米芳李治亚高灵清
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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