Method for measuring graphite oven atomic absorption spectrum of arsenic element in steel

A technology of graphite furnace atomic and absorption spectroscopy, which is applied in the detection field of raw materials and finished products, can solve the problems of poor quantitative analysis accuracy, background interference, chemical interference, etc., and achieve the effect of improving stability and ensuring accuracy

Inactive Publication Date: 2010-06-16
CHINA FIRST HEAVY IND +1
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Problems solved by technology

Due to the different samples to be analyzed, the temperature required for instantaneous vaporization-atomization is different, generally ranging from several hundred degrees to thousands of degrees. To achieve this purpose, low voltage 12V and high current 400A are usually used. It is feasible in practice, but many instruments cannot complete this work in actual operation, mainly because the content

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  • Method for measuring graphite oven atomic absorption spectrum of arsenic element in steel
  • Method for measuring graphite oven atomic absorption spectrum of arsenic element in steel
  • Method for measuring graphite oven atomic absorption spectrum of arsenic element in steel

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Embodiment

[0040]1. Experimental conditions. Use a Zeeman graphite furnace atomic absorption spectrometer, an electrodeless discharge lamp as a light source, a platform graphite tube, and nitric acid to be prepared in a weight ratio of concentrated nitric acid: water=1:3.

[0041] 2. Sampling. Weigh 0.1000 g of chip steel sample.

[0042] 3. The sample dissolves. Weigh 0.1000 g of steel sample and put it into a 100 ℃ quartz beaker, add 5.00 ml of nitric acid of this concentration, heat to dissolve at a low temperature less than 300°C, remove nitrogen oxides in the steel sample, and wait until the sample is completely dissolved Afterwards, remove and cool to room temperature; transfer the dissolved sample to a 100ml volumetric flask, add deionized water to dilute to the mark, shake well, and wait for the test.

[0043] 4. Dissolve the standard sample series according to the above analysis steps (determined according to the concentration of arsenic, such as 0.0038%, 0.0064%, 0.0080% and...

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Abstract

The invention relates to a method for measuring the graphite oven atomic absorption spectrum of an arsenic element in steel, which comprises the following steps: setting the atomization condition of a graphite oven atomic absorption spectrophotometer and constructing an analytical standard curve, wherein the atomization working condition of the graphite oven atomic absorption spectrophotometer is as follows: in the drying condition of a steel sample to be measured, the temperature is firstly raised from the room temperature to the temperature of 100+/-2 DEG C, is kept for several seconds, then is raised to the temperature of 120-150 DEG C within several seconds and is kept for several seconds, and the flow rate of carrier gas is 250+/-10mL/min; in the incineration condition of the steel sample to be measured, the temperature is raised to the temperature of 1200+/-10 DEG C within several seconds and is kept for several seconds, and the flow rate of the carrier gas is 250+/-10mL/min; in the atomization condition of the steel sample to be measured, the temperature is instantaneously raised to the temperature of 2300+/-10 DEG C and is kept for several seconds, and the carrier gas is closed; the idle-burning washing temperature is 2450+/-10 DEG C, the slope time is several seconds and is kept for several seconds, and the flow rate of the carrier gas is 250+/-10mL/min; the current of an electrodeless discharge lamp is 350-400mA, and the wavelength is 180-200nm; the slit width is 0.5-1nm; and the method also comprises the step of carrying out coating treatment on a graphite pipe of the graphite oven atomic absorption spectrophotometer.

Description

technical field [0001] The invention relates to a detection method for raw materials and finished products, in particular to a graphite furnace atomic absorption spectrometry method for measuring arsenic in iron and steel through a graphite furnace atomization method. Background technique [0002] Arsenic in iron and steel is brought in by smelting materials and is one of the five harmful elements in iron and steel. It is mainly dissolved in Fe in iron and steel. 3 Among the compounds such as C, some of them are based on Fe 2 As, Fe 3 As 2 , FeAs exists in the form, arsenic is difficult to remove in the smelting process. Since arsenic has a great influence on the performance of steel, it is necessary to strictly control its content in high-quality steel and high-temperature alloys in steel materials, especially for pressure vessel products, which have stricter requirements on arsenic content. [0003] In the past, the measurement methods of arsenic in iron and steel main...

Claims

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Application Information

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IPC IPC(8): G01N21/31
Inventor 刘志民王志成郑承平刘怀丽李超
Owner CHINA FIRST HEAVY IND
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