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: 2013-11-13
安徽科测检测有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 to make it The loss of boron oxide and the generation of hard-to-dissociate boron carbide, so it is necessary to add a matrix modifier and coat the graphite tube. The existing modifier Ca-Mg, such as "Boron's Atomic Absorption Spectrometry Determination" (rock Mine test, Jiang Yongqing Yao Jinyu, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences), using this improver, although its test sensitivity is high, the measurement repeatability is poor, and the accuracy is not good

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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Embodiment 1

[0018] Embodiment 1: the sample processing method of measuring boron in industrial silicon by graphite furnace atomic absorption spectrometry comprises 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 wash 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 electric heating plate and heat until the water is about to evaporate to dryness, remove the beaker, add 9-11mL of hydrofluoric acid, shake the beaker gently to make the silicon powder and hydrofluoric acid fully contact, use a dropper to absorb nitric acid ( HNO 3 :H 2 (0=1:1), drip into the beaker drop by drop, add about 0.6mL and stop adding to wait for the reaction. If the reaction is relatively gentle, you can continue to drop in nitric acid, about 5mL;

[0021] (3) Heat the beaker on a 100-150°C electric heating p...

Embodiment 2

[0025] Embodiment 2: concrete 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), pyrolytically coated graphite tube ( Jilin Tianbao).

[0028] 1.2 Reagents and solutions

[0029] (1) Nitric acid, super pure, 68-70%, product of Beijing Chemical Factory; (2) Hydrofluoric acid, super pure, 40%, product of Beijing Chemical Factory; (3) High-purity deionized water. Resistivity ≥ 18MΩ.cm; (4) Ba standard solution: 1000μg / mL, Beijing General Institute of Nonferrous Metals; (5) Zirconium oxychloride analytically pure, ≥99.0% Sinopharm reagent; (6) B standard solution: 1000μg / mL , Beijing General Institute of Nonferrous Metals; (7) Barium Hydroxide Superior Pure Chinese Medicine Reagent.

[0030] 1.3 Standard solu...

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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 measuring 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 physical properties required by 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 limit. As boron and phosphorus have the greatest impact on the performance of industrial silicon, boron, as a common element in nature, is widely distributed in soil, and there are relatively few determinations of boron in silicon in previous literatures. Activation method, ICP-OES, atomic absorption, atomic fluorescence, e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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