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Method for measuring content of barium in barium nitrate for fireworks and crackers

A technology for fireworks and firecrackers and barium nitrate, which is applied in the field of analysis and testing, can solve the problems of insufficient operation proficiency, complicated operation steps, error in measurement results, etc., and achieves the effects of low labor intensity, simple operation, and short detection period.

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

[0003] The method described in this standard has the following disadvantages: (1) The detection cycle is long, and generally skilled technicians need 2 to 3 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, and the amount of I must be measured through sample dissolution, heating and boiling, precipitation, filtration and titration with sodium thiosulfate standard titration solution, and then indirectly calculate the amount of Ba
So far, there is no public literature report on the detection of barium content in barium nitrate for fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry based on matrix effect targeted control technology (solution method)

Method used

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  • Method for measuring content of barium in barium nitrate for fireworks and crackers

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Embodiment 1

[0033] Embodiment 1: Make calibration curve

[0034] 1) Prepare several parts of barium working solution (the mass concentration of Ba in the obtained barium nitrate working solution is required to be 0.15g / L~0.73g / L):

[0035] The specific preparation method is as follows:

[0036] Accurately weigh 3.0g of high-purity barium nitrate (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, filter it with filter paper while it is hot, and filter the filtrate to a capacity of 500mL bottle, add 10mL ~ 30mL nitric acid, after the solution in the volumetric flask is cooled to room temperature, add water to make it up to the mark; wherein, the nitric acid is HNO 3 Nitric acid with a content of 10% to 30% by mass.

[0037] Prepare 8 parts of barium nitrate working solution: pipette 5mL, 10mL, 13mL, 15mL, 20mL, 23mL, 25mL and 30mL of the above-mentioned barium nitrate working solution after constant vo...

Embodiment 2

[0048] Embodiment 2: adopt method of the present invention to measure the control experiment of barium nitrate reference substance and barium standard solution

[0049] Test with barium nitrate reference material and barium standard solution listed in table 3, wherein the barium nominal content of barium nitrate reference material and barium standard solution is as shown in table 3; When adopting the method for the present invention to measure, barium nitrate The reference substance is prepared in the following way to prepare the sample solution, and then the barium content is determined.

[0050] 1) Preparation of sample solution:

[0051] Use the reference substance No. 1 as the sample to prepare the sample solution, weigh 3 parts of 0.4g ~ 0.6g sample, and the weighing is accurate to 0.1mg, put the first sample in a 300mL beaker, add 100mL ~ 150mL of water , put the beaker on the electric furnace and heat it for 10min~15min, filter it with filter paper while it is hot, fil...

Embodiment 3

[0063] Embodiment 3: Adopt the precision test of the detection result of barium nitrate reference substance by method of the present invention

[0064] In this embodiment, three barium nitrate reference substances for fireworks and firecrackers with different main contents were taken as samples for testing, and the numbers were 4, 5 and 6 respectively.

[0065] 1) Preparation of sample solution:

[0066] Use the reference substance No. 4 as the sample to prepare the sample solution, weigh 4 parts of 0.4g ~ 0.6g sample, and weigh it accurately to 0.1mg, put the first sample in a 300mL beaker, add 100mL ~ 150mL of water , put the beaker on the electric furnace and heat it for 10min~15min, filter it with filter paper while it is hot, filter the filtrate into a 500mL volumetric flask, add 10mL~30mL of nitric acid with a concentration of 10%~30%, and add water after the solution in the volumetric flask cools to room temperature Dilute to the mark to obtain the first sample solutio...

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Abstract

The invention relates to a method for measuring the content of barium in barium nitrate for fireworks and crackers. The method comprises the following steps: preparing multiple barium nitrate working solutions with different concentrations, establishing an analysis method by adopting a mathematic correction method for intensity correction through taking an energy dispersion type X-ray fluorescence spectrophotometer as a detecting instrument and supposing a certain sample size, converting mass concentrations of Ba in multiple prepared barium nitrate working solutions into mass percentage concentrations of Ba, recording the fluorescence intensity of each sample feeding, and drawing a calibration curve; preparing a sample solution from a barium nitrate raw material for to-be-measured fireworks and crackers, recording the fluorescence intensity of Ba displayed on an instrument, recording a mass percentage concentration value of corresponding Ba according to the determined calibration curve according to the fluorescence intensity, and calculating the content of Ba in the sample. According to the method, by optimizing dissolving conditions of the sample and parameter conditions of the X-ray fluorescence spectrophotometer, the matrix effect among elements of the sample can be eliminated or basically eliminated; and the operation is simple, the detection period is short, the accuracy is good, and the precision is high.

Description

technical field [0001] The invention relates to the technical field of analysis and testing, in particular to a method for measuring barium content in barium nitrate used for fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry. Background technique [0002] In the prior art, the detection method of the main component barium content in barium nitrate for fireworks and firecrackers is based on traditional chemical analysis methods, and the method standard commonly used at present is "the determination of key indicators of chemical raw materials for fireworks and firecrackers Part 12: barium nitrate" ( SN / T 3056.12-2011). The basic steps of this standard method: weigh about a certain amount of sample, put it in a 500mL beaker, add 100mL of water to dissolve it. Add acetic acid-sodium acetate buffer solution, heat to boiling, add potassium dichromate solution while stirring, cover with a watch glass and boil for 10-15 minutes, cool to room temperatur...

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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