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Method for analyzing trace boron in steel by using microwave digestion ICP-AES method

An ICP-AES and microwave digestion technology, applied in the field of iron and steel, can solve the problems of complicated operation process and long analysis process, and achieve the effect of large environmental pollution, simple operation and small pollution

Inactive Publication Date: 2019-01-25
NANJING IRON & STEEL CO LTD
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Problems solved by technology

[0003] Inductively Coupled Plasma Atomic Emission Spectrometry, referred to as ICP-AES method, at present, my country has not formulated the relevant national standard analysis method, the Japanese Industrial Standard has boron quantitative method - trimethyl borate distillation separation method, the standard number is JIS G1258-7 : 2007, using the ICP-AES analysis method, which can quantitatively analyze boron in the range of 0.0001%-0.010% mass fraction in steel. Although the method has high sensitivity, the whole process needs to use quartz vessels for distillation and separation, and the operation process is complicated. Analysis process is long

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  • Method for analyzing trace boron in steel by using microwave digestion ICP-AES method
  • Method for analyzing trace boron in steel by using microwave digestion ICP-AES method
  • Method for analyzing trace boron in steel by using microwave digestion ICP-AES method

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Effect test

Embodiment 1

[0055] 1.1 Experimental part

[0056] 1.1.1 Instruments and reagents

[0057] Microwave digestion system: MARS closed microwave digestion system produced by CEM;

[0058] Full-spectrum direct-reading ICP-AES spectrometer: iCAP 6300 produced by Thermoelectricity in the United States; hydrofluoric acid-resistant solution atomization sampling system;

[0059] Dilute hydrochloric acid-nitric acid mixed acid: both hydrochloric acid and nitric acid are of superior grade, hydrochloric acid+nitric acid+water=1+1+2;

[0060] Phosphoric acid: superior grade;

[0061] Hydrofluoric acid: superior grade;

[0062] Boron standard solution: 100μg / ml, prepared with boric acid, diluted when used;

[0063] Standard sample of boron-free steel: It is known that the mass percentage of boron is less than 0.00005%;

[0064] Steel standards containing trace amounts of boron.

[0065] 1.1.2 Working conditions of the instrument

[0066] Table 1 Working conditions of iCAP-6300 spectrometer

[006...

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Abstract

The invention discloses a method for analyzing and measuring trace boron in steel by applying a microwave digestion inductively coupled plasma atomic emission spectrometry method. The method comprisesthe steps that only a small amount of hydrochloric acid, nitric acid, hydrofluoric acid and phosphoric acid are applied, complete decomposition of boron in the steel is achieved, and meanwhile boronloss does not exist. The whole sample digestion process is conducted completely in a closed environment, operation is easy, and pollution to the environment is small. A small amount of phosphoric acidis added in digestion acid, and volatilization of boron is inhibited, so that the recovery rate of boron is improved, and the precision and accuracy of analysis are improved.

Description

technical field [0001] The invention belongs to the technical field of iron and steel, and relates to an analysis method of iron and steel components, in particular to a method for determining trace boron in iron and steel (mainly for the mass fraction of 0.0002%-0.0005%). Background technique [0002] There are many analysis methods for trace boron in steel, and the current national standard analysis methods mainly include three: methanol distillation-curcumin photometry, referred to as photometry (GB / T223.75-2008); spark discharge atomic emission spectrometry, referred to as spark Source-OES method (GB / T4336-2016); microwave digestion-inductively coupled plasma mass spectrometry, referred to as ICP-MS method (GB / T 223.81-2007). Among these three methods, only GB / T223.81-2007 can meet the technical requirements of some special steel grades in terms of analysis range and analysis accuracy, that is, it can analyze the mass fraction of boron in the range of 0.0002%-0.0005%, wh...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/44
CPCG01N1/44G01N21/73
Inventor 程坚高兵汪五一杜志忠杨建平刘素祥
Owner NANJING IRON & STEEL CO LTD
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