Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry

A fluorescence spectrometry, energy dispersion technology, applied in measurement devices, material analysis using wave/particle radiation, instruments, etc., can solve the problems of insufficient operation proficiency, cumbersome operation steps, long detection period, etc., and achieve high absolute sensitivity. , The effect of low labor intensity and short detection cycle

Active Publication Date: 2013-10-23
广西出入境检验检疫局危险品检测技术中心
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Problems solved by technology

[0004] The method described in this standard has the following disadvantages: (1) the detection cycle is long (generally skilled technicians need about 2 working days to complete the detection); The introduction of uncertainty that causes errors in measurement results, and the determination of zinc concentrates containing different elements produced in different mining areas also brings uncertainty
(2) The operation steps are relatively cumbersome. Four strong acids such as hydrochloric acid, nitric acid, sulfuric acid, and perchloric acid are used continuously for sample dissolution, and then undergo multiple complex operations such as precipitation enrichment, transfer, dissolution, boiling, and concentration. A mixed solution containing zinc ions and other interfering ions to be determined
So far, there is no public literature report on the detection of zinc content in zinc concentrate by energy dispersive X-ray fluorescence spectrometry

Method used

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  • Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry
  • Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry
  • Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry

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Experimental program
Comparison scheme
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Embodiment 1

[0036] Embodiment 1: making working curve

[0037] 1) Prepare several parts of zinc-iron working solution (the mass concentration of Zn in the obtained zinc-iron working solution is required to be 0.05-0.40g / L, and the mass concentration of Fe is 0.01-0.09g / L):

[0038] The specific preparation method is as follows:

[0039] Accurately weigh 0.90g of zinc oxide reference material (accurate to 0.1mg) and 0.20g of iron (purity above 99.9%, accurate to 0.1mg when weighing) and place them in a 300mL beaker, add 100mL of water to the beaker and then add 50mL of concentrated nitric acid, heated for 15min until the reaction is complete, cooled to room temperature, transferred to a 500mL volumetric flask, and made to volume.

[0040] Prepare 11 parts of zinc-iron working solution: Pipette 5mL, 8mL, 10mL, 12mL, 14mL, 16mL, 18mL, 20mL, 22mL, 24mL and 26mL of the above-mentioned fixed-volume zinc-iron working solution into a group of 100mL volumetric flasks, add water Dilute to the sca...

Embodiment 2

[0051] Embodiment 2: adopt method of the present invention to measure the control test of national standard substance or standard solution

[0052] Test with the standard substance listed in the purchased table 3 and the zinc standard solution prepared by the method described in the relevant national standard with the zinc oxide standard substance, wherein the zinc nominal content of the standard substance and zinc standard solution is as shown in table 3; When adopting the method described in the present invention to measure, the standard substance is prepared the sample solution by the following method and then carries out zinc content determination.

[0053] 1) Preparation of sample solution:

[0054] Prepare the sample solution with the standard substance No. 1 as the sample, weigh 3 parts of 0.29 ~ 0.31g sample, and the accuracy of weighing is 0.1mg. The amount of dilute nitric acid (HNO 3 content of 44% by mass), and hydrofluoric acid (HF content of 40% by mass) was ad...

Embodiment 3

[0069] Embodiment 3: adopt method of the present invention to the precision test of the detection result of national standard substance

[0070] In this embodiment, the standard substances numbered 1, 2 and 3 in Table 3 were used as samples for testing.

[0071] 1) Preparation of sample solution:

[0072] Prepare the sample solution with the standard substance of No. 1 as the sample, weigh 4 parts of 0.29 ~ 0.31g sample, and the weighing is accurate to 0.1mg, put the first sample in the reaction tank, and test at 100mL / g. Dilute nitric acid (HNO3 content 43% by mass) was added to the sample amount, and hydrofluoric acid (HF content 40% by mass) was added in an amount of 18mL / g sample, and microwave digestion was carried out by using a microwave digestion instrument, and the heating method adopted a staged degree of heating , the specific parameters are shown in Table 4. After the sample is completely dissolved, transfer it, add water to make it up to 500mL, and filter it with...

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Abstract

The invention discloses a method for determining the content of zinc in the zinc concentrate through energy-dispersive X-ray fluorescence spectrometry. The method comprises the following steps: 1, preparing a plurality of zinc-iron working liquids, converting the mass concentrations of Zn in the operating liquids to Zn mass percentage concentrations, detecting the Zn mass percentage concentrations with an energy-dispersive X-ray fluorescence spectrometer as a detector, recording the fluorescence intensity during each time injection of a sample, and making a working curve; and 2, processing the zinc concentrate as a sample to prepare a sample solution, injecting the sample solution under detection conditions for making the working curve, recording the fluorescence intensity displayed on the detector, reading out the Zn mass percentage concentration corresponded to the fluorescence intensity according to the determined working curve, and calculating according to a specific formula to obtain the mass percentage concentration of simple substance zinc in the sample. The method utilizes a solution process to eliminate or basically eliminate the matrix effect, so the zinc content can be accurately determined; and the method has the advantages of simple operation, short detection period, good detection result accuracy and high precision.

Description

technical field [0001] The invention relates to a method for measuring zinc content in zinc concentrate by energy dispersive X-ray fluorescence spectrometry, and belongs to the technical field of analysis and testing. Background technique [0002] In the prior art, the detection method of zinc content in zinc concentrate is all based on the traditional chemical analysis method of EDTA complexometric titration, and the method standard commonly used at present has: [0003] 1. "Methods for Chemical Analysis of Zinc Concentrate Part 1: Determination of Zinc Quantity Precipitation and Separation of Na 2 EDTA titration and extraction to separate Na 2 EDTA Titration" (GB / T8151.1-2012). The basic principle of this standard method: the sample is dissolved with hydrochloric acid, nitric acid, sulfuric acid and perchloric acid, and the coexisting elements such as iron, manganese and lead are separated by precipitation. After several transfer, precipitation, dissolution, boiling and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223
Inventor 吴俊逸肖焕新商杰严春李一明
Owner 广西出入境检验检疫局危险品检测技术中心
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