Method for determining content of chromium in pyrotechnic composition for fireworks and crackers

A pyrotechnic agent, fireworks and firecrackers technology, applied in the field of analysis and testing, can solve the problems of insufficient operation proficiency, cumbersome operation steps, and inability to use energy, etc., and achieve the effect of low labor intensity, simple operation, and good accuracy

Inactive Publication Date: 2017-01-18
吴俊逸
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 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 cumbersome. After the sample is washed with absolute ethanol and acetone for many times, it has been dissolved in hot water, filtered, washed, suction filtered, transferred, precipitated, precipitated and enriched, filter residue dissolved, washed, transferred, fixed. volume and titration
There are complex matrix effects (including inter-element absorption-enhancement effects and physical-chemical effects) among the elements of pyrotechnic agents, and energy dispersive X-ray fluorescence spectrometry (EDXRF) cannot be used to directly measure the matrix background by powder compression method and melting method Complex and changeable solid powder samples
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.
So far, there is no public literature report on the detection of chromium content in pyrotechnic agents used in fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry

Method used

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  • Method for determining content of chromium in pyrotechnic composition for fireworks and crackers
  • Method for determining content of chromium in pyrotechnic composition for fireworks and crackers
  • Method for determining content of chromium in pyrotechnic composition for fireworks and crackers

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Experimental program
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Embodiment 1

[0035] Embodiment 1: make standard curve

[0036] 1) Prepare multiple chromium working solutions (the mass concentration of Cr in the obtained chromium working solution is required to be 0.03g / L~0.58g / L):

[0037] The specific preparation method is as follows:

[0038] Accurately weigh 2.0g of potassium dichromate reference substance (accurate to 0.1mg), put it in a 300mL beaker, add 100mL~150mL of water, place the beaker on an electric furnace and heat for 10min~15min, and transfer the solution to 500mL after cooling to room temperature Volumetric flask, add 10mL ~ 30mL nitric acid and add water to make up to the mark; wherein, the nitric acid is HNO 3 Nitric acid with a content of 10% to 30% by mass.

[0039] Prepare 10 parts of chromium working solution: pipette 5mL, 10mL, 15mL, 20mL, 30mL, 40mL, 50mL, 60mL, 70mL and 80mL of the above-mentioned chromium working solution after constant volume into a group of 100mL volumetric flasks, add water to dilute to the mark, Mix ev...

Embodiment 2

[0051] Embodiment 2: Adopt the method described in the present invention to carry out the control experiment that pyrotechnic agent reference substance and chromium standard solution are measured

[0052] Test with pyrotechnic agent reference substance and chromium standard solution listed in table 3, wherein the chromium nominal content of pyrotechnic agent reference substance and chromium standard solution is as shown in table 3; When adopting the method of the present invention to measure, pyrotechnic agent The reference substance shall be prepared as the sample solution according to the following method, and then the chromium content shall be determined.

[0053] 1) Preparation of sample solution:

[0054] Use the reference substance No. 1 as the sample to prepare the sample solution, weigh 3 parts of 1.9g ~ 2.1g sample, and weigh to an accuracy of 0.1mg, put the first sample in a 300mL beaker, add 100mL of water, and place Heat it on an electric furnace for 10 minutes, u...

Embodiment 3

[0066] Embodiment 3: Adopt the method of the present invention to the precision test of the detection result of pyrotechnic agent reference substance

[0067] In this embodiment, the pyrotechnic agent reference substances numbered 4, 5 and 6 in Table 3 were used as samples for testing.

[0068] 1) Preparation of sample solution:

[0069] Use the reference substance No. 1 as the sample to prepare the sample solution, weigh 4 parts of 1.9g ~ 2.1g sample, and weigh to an accuracy of 0.1mg, put the first sample in a 300mL beaker, add 100mL of water, and place Heat it on an electric furnace for 10 minutes, use filter paper to filter it into a 500mL volumetric flask while it is hot, rinse it repeatedly with water, and after the filtrate is cooled to room temperature, add 5mL-10mL of nitric acid with a concentration of 10%-30%, and then dilute it to 500mL with water to obtain The first sample solution; repeat the above method to obtain 4 sample solutions of No. 4 reference substance...

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Abstract

The invention discloses a method for determining the content of chromium in pyrotechnic composition for fireworks and crackers. The method comprises the following steps: preparing a plurality of parts of chromium working fluid with different concentrations, taking an energy dispersion X-ray fluorescence spectrophotometer as a detecting instrument, assuming a certain sample size, establishing an analysis method through an intensity calibration mathematical calibration method to convert the mass concentrations of Cr in the plurality of parts of prepared Cr working fluid into mass percent concentrations of Cr, recording the fluorescence intensity of Cr element injected each time, and establishing a calibration curve; preparing the pyrotechnic composition to be tested into sample fluid, recording the fluorescence intensity corresponding to Cr element, reading out the mass percent concentration value of Cr corresponding to the fluorescence intensity of Cr element according to the determined calibration curve, and computing the content of chromium in a sample. According to the method, matrix effects can be eliminated or basically eliminated by optimizing sample dissolving conditions and all parameter conditions of the X-ray fluorescence spectrophotometer, and the method is simple to operate, short in detection period and high in precision.

Description

technical field [0001] The invention relates to the technical field of analysis and testing, in particular to a method for measuring chromium content in pyrotechnic agents for fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry. Background technique [0002] In the prior art, the detection method of chromium content in the pyrotechnic agent for fireworks and firecrackers is based on the traditional chemical analysis method, and the method standard commonly used at present is "The pyrotechnic agent for fireworks and firecrackers Part 2: Determination of dichromate content" (SN / T1732.2-2014). The basic principle of this standard method: After the sample is pretreated, it is dissolved in hot water and filtered, the filtrate is eliminated with interference ions, the filter residue is dissolved with sodium hydroxide and EDTA, and then the content of dichromate in the sample is determined by iodometric method. . [0003] The method described in this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223
CPCG01N23/223G01N2223/076G01N2223/1016
Inventor 吴俊逸
Owner 吴俊逸
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