Sample processing method for detecting boron in industrial silicon with graphite furnace atomic absorption spectrometry

A graphite furnace atomic absorption spectrometry technique is applied in the field of sample processing for the determination of boron in industrial silicon by graphite furnace atomic absorption spectrometry. The effect of low cost, improved sensitivity and fast analysis

Active Publication Date: 2012-03-28
安徽科测检测有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

Their shortcomings: 1 pair of operating conditions, high requirements on environmental conditions, many interfering ions, and poor reproducibility
[0005] There is also a small amount of application in the determination of graphite furnace atomic absorption method, but because the memory effect is serious when measuring boron, and boron is a high-temperature element, its atomization temperature is very high, which will seriously affect the service life of the graphite tube, and it is also easy t

Method used

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  • Sample processing method for detecting boron in industrial silicon with graphite furnace atomic absorption spectrometry
  • Sample processing method for detecting boron in industrial silicon with graphite furnace atomic absorption spectrometry
  • Sample processing method for detecting boron in industrial silicon with graphite furnace atomic absorption spectrometry

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Experimental program
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Effect test

Embodiment 1

[0018] Example 1: The sample processing method for the determination of boron in industrial silicon by graphite furnace atomic absorption spectrometry includes the following steps:

[0019] (1) Weigh 0.995-1.005 grams of silicon powder crushed to more than 100 mesh into a 280-320mL polytetrafluoroethylene beaker, and flush a small amount of silicon powder attached to the inner wall of the cup to the bottom of the cup with pure water;

[0020] (2) Put the beaker on the hot plate and heat it until the water is about to evaporate. Remove the beaker, add 9-11mL of hydrofluoric acid, gently shake the beaker to make the silicon powder and hydrofluoric acid fully contact, and suck the nitric acid with a dropper ( HNO 3 : H 2 O=1:1), drop by drop into the beaker, add about 0.6mL, stop adding and wait for the reaction, if the reaction is relatively gentle, continue to drip nitric acid, and drop about 5mL;

[0021] (3) Put the beaker on a 100-150℃ electric hot plate to heat, continue heating u...

Embodiment 2

[0025] Example 2: Specific experimental test of the present invention:

[0026] 1.1 Instruments and equipment

[0027] WYS2200 atomic absorption spectrometer (Anhui Wanyi Technology), adjustable electric heating plate, WY802-II ultrapure water machine (Anhui Wanyi Technology), boron hollow cathode lamp (Beijing Nonferrous Metals General Institute), pyrolytic coating graphite tube ( Jilin Tianbao).

[0028] 1.2 Reagents and solutions

[0029] (1) Nitric acid, pure superior grade, 68-70%, products of Beijing Chemical Plant; (2) Hydrofluoric acid, pure superior grade, 40%, products of Beijing Chemical Plant; (3) High-purity deionized water. Resistivity ≥18MΩ.cm; (4) Ba standard solution: 1000μg / mL, Beijing Nonferrous Metals Institute; (5) Zirconium oxychloride analytically pure, ≥99.0% Sinopharm reagent; (6) B standard solution: 1000μg / mL , Beijing Nonferrous Metals General Institute; (7) Barium hydroxide premium grade pure Chinese medicine reagent.

[0030] 1.3 Standard solution prepar...

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PUM

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Abstract

The invention discloses a sample processing method for detecting boron in industrial silicon with graphite furnace atomic absorption spectrometry. The method comprises the following steps: weighing proper sample silicon powder; selecting proper acid to digest and dissolve the sample; heating to volatilize the silicon, and separating the residue; and filtering to obtain a clear solution and adding Zr-Ba serving as a proper matrix modifier to suppress the interference of a matrix. The method disclosed by the invention can be used for increasing the measurement sensitivity of the graphite furnace atomic absorption spectrometry and improving precision, is high in measurement speed, small in interference, high in accuracy and low in measurement cost, and is especially suitable for the quality detection in an industrial silicon production enterprise.

Description

Technical field [0001] The invention relates to element detection of chemical raw materials, in particular to a sample processing method for determining boron in industrial silicon by graphite furnace atomic absorption spectrometry. Background technique [0002] With the development of the electronics industry, industrial silicon as a raw material is widely used in the field of semiconductor manufacturing. Based on the required physical properties of its semiconductor materials, the requirements for impurity elements in industrial silicon materials are very strict, so the detection of its impurities is very strict, and there are strict requirements for its limits. As boron and phosphorus have the greatest impact on the performance of industrial silicon, boron, as a common element in nature, is generally distributed in the soil. In the past, the determination of boron in silicon is relatively rare. The analysis method is mainly ultraviolet absorption method and neutron Activation...

Claims

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Application Information

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IPC IPC(8): G01N21/33G01N1/44
Inventor 李涛王国东
Owner 安徽科测检测有限公司
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