A Powder Sample Preparation Method for X Fluorescence Analysis

A fluorescence analysis and powder technology, applied in the field of chemical analysis, can solve the problems of analysis equipment damage, easy cracking, corrosion of X-fluorescence spectroscopic crystals, etc., and achieve the effects of improved accuracy, good quality and use effect, and simple sample preparation methods

Active Publication Date: 2019-06-07
铜陵有色金属集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the samples rely on binders such as boric acid to be pressed into shape. When the samples enter the near-vacuum X-ray fluorescence analysis environment, the surface of the samples is easy to crack, and the samples disintegrate and fall, which will pollute the analysis chamber; Acid gas will volatilize under ray irradiation, corrode the X-ray fluorescence spectroscopic crystal, and cause fatal damage to the analysis equipment

Method used

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  • A Powder Sample Preparation Method for X Fluorescence Analysis
  • A Powder Sample Preparation Method for X Fluorescence Analysis
  • A Powder Sample Preparation Method for X Fluorescence Analysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: Smelting slag sample

[0020] Smelting slag is an important product of the pyrometallurgical smelting process in copper smelters. The chemical composition of the smelting slag can be used to judge the quality of the furnace indirectly. At the same time, the smelting slag is also the direct raw material for the mineral processing system of the copper smelter (slag beneficiation raw ore). The smelting slag contains about 2% copper, about 40% iron, and about 30% silicon dioxide, and its viscosity is relatively poor. It is difficult to obtain ideal samples by direct powder pressing method, and the surface of the samples is easy to fall off powder. Sometimes it cracks.

[0021] Tablet the smelt slag sample as follows:

[0022] (1) On the pressure-bearing tray 10, lay a layer of XRF discs with a thickness of 3.6 μm and a diameter of 63.5 mm to test the Mylar film 20;

[0023] (2) On the XRF disc test Mylar film 20, put a pressure sample with an outer diameter ...

Embodiment 2

[0043] Embodiment 2: slag separation tailings sample

[0044] The smelting slag leaves tailings after beneficiation, the copper grade is low, and the powder viscosity is poor. The direct sample pressing method cannot obtain qualified samples. The surface of the samples is easy to crack, and the powder will fall off during analysis. In a scattered state.

[0045] The powder sample is changed to a slag beneficiation tailings sample, and the tableting method is the same as that in Example 1 to obtain a slag beneficiation tailings sample.

[0046] Performance test experiment:

[0047] Test 1: Control group: The slag beneficiation tailings samples were pressed into tablets using the conventional powder pressing method, specifically: the slag beneficiation tailings samples were directly pressed with an aluminum cover as the base, the obtained samples were subjected to X-ray fluorescence analysis, and the samples were taken out , to check the usage, see Table 4 for the results, and...

Embodiment 3

[0060] Example 3: Soot sample

[0061] A large amount of soot is produced during the copper smelting process. The composition of the soot returned to the furnace needs to be quickly analyzed by X-ray fluorescence. Since the soot sample contains a lot of acid, it is difficult to bake out all the acidic substances. If the soot is directly pressed into a tablet for X-ray fluorescence analysis, the soot sample will volatilize acidic substances under the irradiation of X-ray fluorescence, which will not only greatly corrode the X-ray fluorescence spectroscopic crystal, but also increase the vacuum degree of the vacuum chamber and increase the difficulty of analysis. .

[0062] The powder sample is changed to a soot sample, and the tableting method is the same as in Example 1 to obtain a soot sample.

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Abstract

The invention relates to the technical field of chemical analysis, and in particular to a powder sampling method for X-fluorescence analysis. The powder sampling method comprises the following steps: (1) covering a working tray with an XRF Mayra film, placing a plastic ring on the XRF Mayra film, and enabling the working tray to hold the plastic ring completely; (2) adding a powder sample into the plastic ring, flattening, and compacting to enable powder to be parallel to the opening of the plastic ring so as to obtain a product to be manufactured; and (3) pressing the product to be manufactured on a sample pressing machine, molding, removing the working tray, and tightly sealing one side directly contacting air, of a sample piece, by using a transparent adhesive tape, thereby obtaining a finished product. The powder sampling method provided by the invention is simple, convenient and rapid to operate, the prepared sample piece is good in quality and use effect, surface flatness and smoothness can be stilled maintained under X-ray radiation and an environment approximate to vacuum environments, and cracking can be avoided in the actual analysis process, so that an analysis cavity can be prevented from being polluted, light splitting crystal can be prevented from corrosion in analysis, and the sample analysis accuracy and the X-fluorescence use security can be greatly improved.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a powder sample preparation method for X-ray fluorescence analysis. Background technique [0002] X-ray fluorescence analysis technology, also known as X-ray secondary emission spectroscopy analysis technology, is a method for qualitative and quantitative analysis of the type and content of substances based on the intensity of characteristic X-rays generated by the analyzed sample under primary X-rays. During the use of X-ray fluorescence analysis technology, it is necessary to make the sample to be tested into a ring cake sample for accurate analysis. [0003] When preparing samples for powders with poor viscosity, the fast and simple powder compression method is often used in production. During the specific operation, it is necessary to add boric acid, polyethylene, etc. as a binder to the sample to bond the powder, and then press it into shape. However, the samples...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N1/36G01N23/223
CPCG01N1/28G01N1/36G01N23/223G01N2001/366
Inventor 钱庆长李长春谢鹏
Owner 铜陵有色金属集团股份有限公司
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