Inductively coupled plasma mass spectrometry used for determining trace aluminum molybdenum vanadium titanium niobium in silicon steel

An inductive coupling, plasma technology, applied in the field of plasma mass spectrometry, can solve the problems of many interference factors, difficult magnetization of silicon steel sheets, damage to product performance, etc., to overcome many interference factors, fast multi-element analysis, wide linear dynamic range Effect

Inactive Publication Date: 2015-05-13
QINGDAO TIANHENG MACHINERY
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Problems solved by technology

Molybdenum, vanadium, titanium, niobium and other impurity elements in silicon steel are easy to form inclusion particles such as nitrides, carbides and carbonitrides during the smelting process, which will not only inhibit the growth of grains in silicon steel, make it difficult to magnetize silicon steel sheets, and cause iron loss. Increase, it will also make it difficult to decarburize the steel, increase the coe

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Embodiment

[0017] The inductively coupled plasma mass spectrometry for the determination of trace amounts of aluminum, molybdenum, vanadium, titanium and niobium in silicon steel in this embodiment includes the following:

[0018] (1) Main instruments: Xseries Ⅱ type inductively coupled plasma mass spectrometer (Thermo Fisher Scientific, USA); BSB-939-IR acid purifier (BERGHOF, Germany);

[0019] (2) Working conditions: ICP-MS working conditions: plasma power, 1400W; atomization pressure, 0.2MPa; atomization chamber temperature, 2℃; cooling air pressure, 0.6MPa; sample lift, 1.0mL / min; quality Resolution, 0.7amu; residence time, 25ms; 1 measurement channel; initial sensitivity of 10ng / mL In is about 5×10 5 cps, Ba 2+ / Ba + Less than 2%, CeO / Ce less than 2%;

[0020] (3) Reagents: Al, Mo, V, Ti, Nb standard solution: 50μg / mL, respectively prepared with metals or oxides with a mass fraction greater than 99.95%, and then gradually diluted to obtain; Al, Mo, V, Ti, Nb Mixed standard solution: 1μg / ...

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Abstract

The invention discloses an inductively coupled plasma mass spectrometry used for determining trace aluminum molybdenum vanadium titanium niobium in silicon steel, and simultaneous determination of trace aluminum, molybdenum, vanadium, titanium, and niobium in silicon steel via inductively coupled plasma mass spectrometry (ICP-MS) is discussed. Determination parameters are optimized via condition experiments, and it is determined that RF power is 1400W, pump speed is 30rpm, sampling depth is 140, and atomization pressure is 0.90. Sample decomposition is realized using nitric acid, Be and Y mixed inner standard method is used for correcting signal drift caused by high matrix in measuring processes. Isotope 27Al, 98Mo, 51V, 47Ti, and 93Nb are taken as measuring isotopes based on mass spectrum interference conditions in determination; and at the same time, yield of double charged ions and oxide ions is adjusted to be lowest by adjusting instrument parameters so as to reduce influences. Calibration solutions are prepared via matrix matching, working curve is established via standard addition method, and reagent blank is deducted. Determination lower limit of the elements reaches 1<mu>g/g, and element RSD is less than 5.2% when the inductively coupled plasma mass spectrometry is used for determining silicon steel standard samples.

Description

[0001] Technical field [0002] The invention belongs to the technical field of casting, and specifically relates to an inductively coupled plasma mass spectrometry method for determining trace amounts of aluminum, molybdenum, vanadium, titanium and niobium in silicon steel. [0003] Background technique [0004] Silicon steel sheet is an indispensable and important magnetic material in the power, telecommunications and instrument industries. With the in-depth development of the manufacturing industry, people have put forward higher requirements for the electromagnetic properties of silicon steel, prompting steel companies to continue to develop new silicon steel products. At present, a hot spot in the research and development of new silicon steel is the development of high-performance pure silicon steel with extremely low residual impurity elements. Impurity elements such as molybdenum, vanadium, titanium, and niobium in silicon steel are easy to form nitrides, carbides, carbo...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N27/626
Inventor 刘升迁
Owner QINGDAO TIANHENG MACHINERY
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