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Method for quickly and semiquantitatively detecting mercury content in firework propellant blind sample for firework

A semi-quantitative detection, fireworks technology, applied in the field of analysis and testing, can solve problems such as unseen, and achieve the effect of short detection cycle, high precision and high detection efficiency

Inactive Publication Date: 2018-04-24
吴俊逸
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no public literature report on the rapid semi-quantitative detection of mercury content in pyrotechnics used in fireworks and firecrackers based on energy dispersive X-ray fluorescence spectroscopy.

Method used

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  • Method for quickly and semiquantitatively detecting mercury content in firework propellant blind sample for firework
  • Method for quickly and semiquantitatively detecting mercury content in firework propellant blind sample for firework
  • Method for quickly and semiquantitatively detecting mercury content in firework propellant blind sample for firework

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0031] Since it is impossible to find pyrotechnic powder reference materials with accurate determination of mercury content in the market, and because the physical form of pyrotechnic powder is similar to that of black powder powder, it is possible to configure pyrotechnic powder reference materials with different mercury contents on the basis of black powder, and measure the pyrotechnic The general correspondence between the fluorescence intensity value of the characteristic line corresponding to mercury in the pharmaceutical reference material and its corresponding content. The energy dispersive X-ray fluorescence spectrometer is used as the detection instrument, and the parameters of the detection instrument are set as follows: use the intensity method to establish the analysis method, the apert...

Embodiment 2

[0035] Embodiment 2: the repeatability test of method (mercury content is 0.1%)

[0036] The purpose of the method repeatability test is to further confirm the fluorescence intensity values ​​of the corresponding mercury element characteristic lines when the mass percentage of mercury in different types of pyrotechnic agents is 0.1%. Different types of pyrotechnic powders were used as substrates, and pyrotechnic powder reference material samples with a mercury content of 0.1% were used for determination. The 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, the filter is set to thick Pd, the voltage is 28kV, the analysis time is 50s, 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...

Embodiment 3

[0040] Example 3: Semi-quantitative rapid detection of mercury 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. After drying, place in a desiccator to cool to room temperature.

[0042] (2) Establish the detection method: use the energy dispersive X-ray fluorescence spectrometer as the detection instrument, and use the intensity method of the X-ray fluorescence spectrometry to establish the analysis method; the parameters of the detection instrument are set as follows: the aperture of the collimator is 8.8mm, and the filter is set to Thick Pd, voltage is 30 KV, analysis time is 40s, energy range is 40keV, cou...

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Abstract

The invention discloses a method for quickly and semiquantitatively detecting the mercury content in a firework propellant blind sample for a firework, and belongs to the technical field of analysis testing. A firework propellant sample is dissected from a firework product, grinded, screened, dried and cooled to room temperature, an energy dispersive X-ray fluorescence spectrophotometer is used asa detection instrument, a strength method is adopted to build an analysis method, the sample is loaded into an instrument sample cup, then the sample to be detected is placed into a detection instrument testing cabin, the fluorescence strength value of a mercury element characteristic spectral line displayed on the instrument is recorded, the content of the mercury element in the sample in estimated, and then an appropriate analysis instrument is selected to accurately analyze the mercury content in the firework propellant blind sample for the firework. By adopting the method to semiquantitatively analyze the mercury content, the operation is simple, the efficiency is high, the mercury content in the estimated sample is slightly different from the actual mercury content, and a data basiscan be further effectively provided for selecting the method for accurately and quantitatively analyzing the mercury 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 mercury 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 mercury content in blind samples of pyrotechnic powder used in fireworks and firecrackers based on energy dispersive X-ray fluorescence spectroscopy has been found, only methods for measuring mercury content in other fields, such as: Determination of Arsenic, Chromium, Cadmium, Lead and Mercury Contents Inductively Coupled Plasma Mass Spectrometry (ICP-MS)" (GB / T 6730.72-2016), "Determination of Mercury Content in Chromium Ore Direct Determination of Solid Sample Injection" (GB / T T 31948-2015) and "General Method for Determination of Mercu...

Claims

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Application Information

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IPC IPC(8): G01N23/223
CPCG01N23/223
Inventor 吴俊逸
Owner 吴俊逸
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