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Method for determining copper content in pyrotechnic composition for fireworks and crackers

A technology of pyrotechnic agents, fireworks and firecrackers, which is applied in the field of analysis and testing, can solve the problems of high operation accuracy and requirements for experimenters, cumbersome operation steps, and error uncertainty, and achieve the effects of low labor intensity, simple operation, and high precision

Inactive Publication Date: 2016-11-09
吴俊逸
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) The detection cycle is long, and generally skilled technicians need 2 working days to complete a detection
[0005] (2) It is easy to cause errors. There are high requirements for the accuracy of the operation and the experimenters. Many operation steps involve washing, transfer, dissolution, filtration, titration, etc., which are easy to introduce uncertainties. The operator must be extra careful in each test and meticulous, otherwise it is very easy to introduce artificial error uncertainty
[0006] (3) The operation steps are relatively cumbersome. After washing the sample several times with absolute ethanol and acetone, dissolve it with nitric acid, filter and collect the filter residue, then fully dissolve the divalent copper ions in the filter residue with concentrated ammonia water, and then undergo washing and Constant volume, finally take a certain sample solution and add excess EDTA, with CuSO 4 Back titration excess EDTA, calculate the amount of copper
Furthermore, due to the flammable and explosive characteristics of the pyrotechnic agent used for fireworks and firecrackers, it is difficult to pre-treat it by tableting or melting.
Therefore, so far there is no public literature report on the detection of copper content in pyrotechnic agents for fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry

Method used

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  • Method for determining copper content in pyrotechnic composition for fireworks and crackers

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Embodiment 1

[0050] 1) Accurately weigh 1.31g of high-purity copper oxide powder (accurate to 0.1mg), put it in a 300mL beaker, add 50mL to 80mL of nitric acid with a concentration of 10% to 30%, and place the beaker on an electric furnace to heat for 25min to 35min. After the solution is cooled to room temperature, transfer it to a 500mL volumetric flask, and add water to make up to the mark;

[0051] 2) Prepare 8 parts of copper working solution: pipette 5mL, 10mL, 15mL, 20mL, 25mL, 30mL, 35mL and 40mL of the above-mentioned copper working solution after constant volume into a group of 100mL volumetric flasks, add water to dilute to the mark, and mix well , respectively numbered as Work 1, Work 2, Work 3, Work 4, Work 5, Work 6, Work 7 and Work 8, the concentration of Cu in them is shown in Table 1;

[0052] 3) Using an energy dispersive X-ray fluorescence spectrometer (produced by Thermo Electron Corporation (Thermo Electron Corporation), model QUANT'X EDXRY Analyzer) as a detection ins...

Embodiment 2

[0062] Embodiment 2: The control experiment that adopts the method of the present invention to measure the reference substance of pyrotechnic agent for fireworks and firecrackers

[0063] Test with the pyrotechnic agent reference substance listed in table 3, wherein the copper nominal content of reference substance is as shown in table 3; Carry out copper content determination.

[0064] 1) Preparation of sample solution:

[0065] Use the reference substance No. 1 as the sample to prepare the sample solution, weigh 3 parts of 1.9g ~ 2.1g sample, the weighing accuracy is 0.1mg, put the first sample in a 300mL beaker, add 50mL ~ 80mL water , heated to a slight boil for about 8 minutes, filtered while it was hot, washed with water several times, collected the filter residue into another beaker, and added nitric acid in an amount of 20mL / g~30mL / g sample, the mass percentage concentration of nitric acid was 40%~60 %, placed on an electric furnace and heated to a slight boil for 30...

Embodiment 3

[0076] Embodiment 3: Adopt the method of the present invention to the precision test of the detection result of pyrotechnic agent reference substance

[0077] In this embodiment, three pyrotechnic agent reference substances with different copper contents were used as samples for testing, numbered 1, 2 and 3.

[0078] 1) Preparation of sample solution:

[0079] Use the reference substance No. 1 as the sample to prepare the sample solution, weigh 4 parts of 1.9g~2.1g sample, and the weighing accuracy is 0.1mg, put the first sample in a 300mL beaker, add 50mL~80mL water , heated to a slight boil for about 8 minutes, filtered while it was hot, washed with water several times, collected the filter residue into another beaker, and added nitric acid in an amount of 20mL / g~30mL / g sample, the mass percentage concentration of nitric acid was 40%~60 %, placed on an electric furnace and heated to a slight boil for 30 minutes, filtered with filter paper while it was still hot, and collect...

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Abstract

The invention discloses a method for determining the copper content in a pyrotechnic composition for fireworks and crackers. The method comprises the steps that copper standard solutions with series of the concentration are prepared, an energy dispersion type X-ray fluorescence spectrophotometer is adopted as a detecting instrument, a certain sample size is assumed, an analysis method is established by adopting an intensity-correcting mathmetic correction method, the mass concentration of Cu in the copper standard solutions is converted into the mass percent concentration according to the assumed sample size of a sample material and the constant volume of a test solution, the Cu fluorescence intensity generated in each sample feeding is recorded, and a calibration curve for a Cu element is drawn; a test solution of the pyrotechnic composition to be determined is prepared, the Cu element fluorescence intensity displayed on the instrument is recorded, a Cu mass percent concentration value corresponding to the fluorescence intensity is read according to the calibration curve, and the copper content in the sample is calculated. According to the method, the matrix effect among all elements in the sample can be eliminated or basically eliminated by optimizing the sample dissolving condition and all parameter conditions of the X-ray fluorescence spectrophotometer. The method is easy to operate, short in detection period, good in accuracy and high in precision.

Description

technical field [0001] The invention relates to a method for measuring copper content in pyrotechnic agents for fireworks and firecrackers 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 copper content in pyrotechnic agent for fireworks and firecrackers is the traditional chemical analysis method based on EDTA complexometric titration, and the method standard commonly used at present is " pyrotechnic agent for fireworks and firecrackers Part 4: Determination of copper content " ( SN / T1732.4-2014). The basic principle of this standard method: After the sample is pretreated, it is fully dissolved with nitric acid, filtered, and the divalent copper ions in the test solution are separated by adjusting the pH value of the solution, adding a precipitant and concentrated ammonia water, and complexometric titration with EDTA The method uses PAN a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223
CPCG01N23/223
Inventor 吴俊逸
Owner 吴俊逸
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