Method for performing rapid semi-quantitative determination on aluminum content in pyrotechnic composite blind samples for fireworks and crackers

A semi-quantitative detection, fireworks technology, applied in the field of analysis and testing, can solve problems such as insufficient operation proficiency, error in measurement results, cumbersome operation steps, etc., and achieve the effect of low labor intensity, high precision and high detection efficiency

Inactive Publication Date: 2018-05-04
吴俊逸
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method described in this standard has the following deficiencies: (1) The detection cycle is long, and generally skilled technicians need 2 working days to complete a detection
In addition, in the specific test process, it is easy to introduce the uncertainty of the measurement result error due to the lack of proficiency of the test personnel.
(2) The operation steps are relatively cumbersome. After washing the sample several times with absolute ethanol and acetone, dissolve it with dilute nitric acid, filter, transfer, and collect the filter residue, then fully dissolve the filter residue with sulfuric acid, and then undergo filtration, washing, and pH adjustment. , add a precipitant to separate the aluminum ions, and finally measure the aluminum content in the solution by the differential method
So far, there is no public literature report on the rapid semi-quantitative detection of aluminum content in pyrotechnics used in fireworks and firecrackers based on energy dispersive X-ray fluorescence spectroscopy.

Method used

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  • Method for performing rapid semi-quantitative determination on aluminum content in pyrotechnic composite blind samples for fireworks and crackers
  • Method for performing rapid semi-quantitative determination on aluminum content in pyrotechnic composite blind samples for fireworks and crackers
  • Method for performing rapid semi-quantitative determination on aluminum content in pyrotechnic composite blind samples for fireworks and crackers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: Comparison of the aluminum element content in the pyrotechnic powder and the fluorescence intensity value of the characteristic spectral line of the aluminum element

[0031] Since it is impossible to find pyrotechnic powder standard materials with accurate aluminum content in the market, and because the physical form of black powder is similar to that of pyrotechnic powder, reference materials of pyrotechnic powders with different aluminum contents based on black powder are formulated with aluminum powder standard materials. Substances are tested. By detecting the corresponding relationship between the aluminum content in different pyrotechnic drug reference materials and the corresponding characteristic line fluorescence intensity values, the general corresponding relationship between the aluminum content in pyrotechnic agents and the corresponding characteristic line fluorescence intensity is deduced. The energy dispersive X-ray fluorescence spectrometer i...

Embodiment 2

[0035] Embodiment 2: the repeatability test of method (aluminum content is 10%)

[0036] The purpose of the method repeatability test is to further confirm the corresponding aluminum element characteristic line fluorescence intensity values ​​when the mass percentage of aluminum in different types of pyrotechnic agents is 10%. Different types of pyrotechnic agents were used as substrates, and pyrotechnic drug reference material samples with an aluminum content of 10% were configured for determination. Energy dispersive X-ray fluorescence spectrometer was used as the detection instrument. The parameters of the detection instrument were set as follows: use the intensity method to establish the analysis method, The aperture of the collimator is 8.8mm, no filter is set, the voltage is 20kV, the analysis time is 30s, the energy range is 0-40keV, the count rate is medium, the gas environment is air, the current is automatic and the peak spectrum observation line is K line , to semi-...

Embodiment 3

[0040] Example 3: Semi-quantitative rapid detection of aluminum content in pyrotechnic powder blind samples and selection of further accurate quantitative analysis methods

[0041] (1) Dissect the pyrotechnic powder sample from the fireworks and firecracker products, take 5g of the sample in a copper mortar, grind it carefully with a copper rod, pass through a 40-mesh sieve, and place the sample powder in an explosion-proof Dry in an oven for 4 hours at a drying temperature of 50°C, and place in a desiccator to cool to room temperature after drying.

[0042] (2) Establish the detection method: use the energy dispersive X-ray fluorescence spectrometer as the detection instrument, and use the intensity method to establish the analysis method; the parameters of the detection instrument are set as follows: the aperture of the collimator is 8.8mm, no filter is set, and the voltage is 20 KV , the analysis time is 40s, the energy range is 40keV, the count rate is medium, the gas envi...

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Abstract

The invention discloses a method for performing rapid semi-quantitative determination on aluminum content in pyrotechnic composite blind samples for fireworks and crackers and belongs to the technicalfield of analytical tests. The method comprises the following steps: separating pyrotechnic composite samples from firework and cracker products, grinding, screening, drying, and cooling to a room temperature; taking an energy dispersion type X-ray fluorescence spectrometer as a detection instrument, adopting an analytical method by a strength method, filling the samples into instrument sample cups, placing a to-be-detected sample into a test chamber of the detection instrument, recording a fluorescence intensity level of an aluminum element characteristic spectral line displayed on the instrument, and estimating the content of the aluminum element in the samples; further selecting an appropriate analytical instrument to perform accurate quantitative analysis on the pyrotechnic compositesfor fireworks and crackers. The method disclosed by the invention is adopted for performing semi-quantitative analysis on the aluminum content and is simple in operation and high in efficiency, and the estimated aluminum content in the sample is slightly different from the actual content. Moreover, a data basis can be effectively provided for further selecting a method for accurately and quantitatively analyzing the aluminum content in the sample.

Description

technical field [0001] The invention relates to the technical field of analysis and testing, in particular to a method for rapidly and semi-quantitatively detecting aluminum content in a blind sample of pyrotechnic powder for fireworks and firecrackers by using an energy dispersive X-ray fluorescence spectrometer and adopting an intensity method. Background technique [0002] In the prior art, no rapid semi-quantitative detection method for aluminum content in blind samples of pyrotechnic powder for fireworks and firecrackers based on energy dispersive X-ray fluorescence spectroscopy has been found, only a quantitative detection method for aluminum content. The detection method of aluminum content in pyrotechnic agents for fireworks and firecrackers is based on traditional chemical analysis methods. The current determination method for aluminum content in pyrotechnic agents for fireworks and firecrackers (GB / T 20615-2006 "Determination of Aluminum Content in Fireworks and Fir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223
CPCG01N23/223G01N2223/076
Inventor 吴俊逸
Owner 吴俊逸
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