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Analysis method of antimony trisulfide in mixed agent for firecracker

A technology of antimony trisulfide and mixed reagents is used in material analysis by observing the influence on chemical indicators, analysis by chemical reaction of materials, preparation of samples for testing, etc., to achieve high measurement accuracy and application. Extensive, simple and easy-to-operate effects

Inactive Publication Date: 2011-05-25
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After retrieval, there is no report on the analysis method of antimony sulfide content in firecrackers mixed agent. Therefore, the establishment of this method can effectively monitor the amount of antimony sulfide in firecracker agent in real time, and provide powerful support for relevant inspection departments to strictly control the safety of fireworks and firecrackers. s method

Method used

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  • Analysis method of antimony trisulfide in mixed agent for firecracker
  • Analysis method of antimony trisulfide in mixed agent for firecracker

Examples

Experimental program
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Effect test

Embodiment 1

[0031]Disassemble the firecrackers in a dry environment, separate the mixed agent, and store it in a ground glass bottle. Use a small number of times to grind repeatedly with an agate mortar, and sieve with a 120-mesh sieve. A small amount of ingredients that cannot be ground are directly mixed into the sample, mixed evenly, put into an oven and baked at 50°C±2°C for 3 hours, then transferred to a desiccator to cool down at room temperature for testing.

[0032] Weigh 0.6g of the sample to be tested (accurate to 0.0001g), put it in a 50mL beaker, add 3mL of hot water to dissolve it, filter it on a piece of medium-speed filter paper with constant weight by decanting method, and wash it repeatedly 20 times in this way. After volatilizing a large amount of water, place it in an oven to dry at 50°C±2°C for 1h. Wash the sulfur in the sample with 5mL of slightly hot carbon disulfide, shake the funnel gently to dissolve the sulfur in the residue completely and filter it down, wash i...

Embodiment 2

[0037] Disassemble the firecrackers in a dry environment, separate the mixed agent, and store it in a ground glass bottle. Use a small number of times to grind repeatedly with an agate mortar, and sieve with a 120-mesh sieve. A small amount of ingredients that cannot be ground are directly mixed into the sample, mixed evenly, put into an oven and baked at 50°C±2°C for 3 hours, then transferred to a desiccator to cool down at room temperature for testing.

[0038] Weigh 0.4g of the sample to be tested (accurate to 0.0001g), put it in a 50mL beaker, add 3mL of hot water to dissolve it, filter it on a piece of medium-speed filter paper with constant weight by decanting method, and wash it repeatedly 18 times in this way. After volatilizing a large amount of water, place it in an oven to dry at 50°C±2°C for 1h. Wash the sulfur in the sample with 4mL of slightly hot carbon disulfide, shake the funnel gently to dissolve the sulfur in the residue completely and filter it down, wash ...

Embodiment 3

[0043] Disassemble the firecrackers in a dry environment, separate the mixed agent, and store it in a ground glass bottle. Use a small number of times to grind repeatedly with an agate mortar, and sieve with a 120-mesh sieve. A small amount of ingredients that cannot be ground are directly mixed into the sample, mixed evenly, put into an oven and baked at 50°C±2°C for 3 hours, then transferred to a desiccator to cool down at room temperature for testing.

[0044] Weigh 0.3g of the sample to be tested (accurate to 0.0001g), put it in a 50mL beaker, add 3mL of hot water to dissolve it, filter it on a piece of medium-speed filter paper with constant weight by decanting method, and wash it repeatedly 15 times in this way. After volatilizing a large amount of water, place it in an oven to dry at 50°C±2°C for 1h. Wash the sulfur in the sample with 3mL of slightly hot carbon disulfide, shake the funnel gently to dissolve the sulfur in the residue completely and filter it down, wash ...

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Abstract

The invention discloses an analysis method for measuring Sb2S3 in a mixed agent for firecracker. The analysis method comprises the steps of: with civil firecracker as a raw material, forming the best measuring conditions by detaching the firecracker for sampling in a dry environment, grinding, screening with a sieve of 120 meshes, and drying; weighing a sample, washing potassium perchlorate, sulphur and organic binder components in the sample by respectively using hot water, carbon bisulfide and acetone, and drying for later use; weighing a sample, adding 12ml of hydrochloric acid and 5ml of phosphoric acid, covering a watch glass, slowly heating the sample on an electric furnace by shaking simultaneously until the solution boils slightly, removing the watch glass, and keeping the solution boiling slightly until the color of the solution becomes yellowish and transparent; adding 30-35ml of boiling water, shaking uniformly, dripping two drops of methyl orange indicator, titrating the solution with a potassium bromate standard solution until the solution becomes reddish, adding one drop of the indicator, and titrating until the solution fades. The method has the advantages of less interference and high accuracy, and can meet the requirements in industrial production. The method can also be used for measuring the content of chemical agents, stibnite, and antimony trisulfide used as an additive in industry, thereby having a broad application prospect.

Description

technical field [0001] The invention relates to an analysis method of antimony trisulfide, more particularly, relates to an analysis method of antimony trisulfide in a firecracker mixed agent. The method includes five parts: sampling, sample preparation, sample washing, sample dissolution and potassium bromate titration. Background technique [0002] Commonly used oxidants for firecrackers include perchlorate and nitrate. Common combustibles are charcoal, sulfur, etc. At present, antimony trisulfide is used in firecrackers to replace part of sulfur as combustion accelerant and reducing agent. Its mixture with potassium chlorate and potassium perchlorate is highly sensitive, slightly more stable than the mixture of sulfur, potassium chlorate and potassium perchlorate, and is already the main component. . Antimony sulfide (Sb 2 S 3 ) black solid powder, amphoteric sulfide. Insoluble in water and acetic acid, slowly soluble in hot concentrated sulfuric acid, soluble in co...

Claims

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Application Information

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IPC IPC(8): G01N21/79G01N1/28
Inventor 刘淑萍闫路省
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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