Measurement method for content of magnesium and content of aluminium in main component of pyrotechnic composition for fireworks and crackers

A technology of fireworks and firecrackers and measurement methods, which is applied in the field of analysis and testing, can solve problems such as cumbersome operation steps, insufficient operation proficiency, and long detection cycle, and achieve the effect of low requirements for operators, low labor intensity, and short detection cycle

Active Publication Date: 2014-07-02
广西出入境检验检疫局危险品检测技术中心
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  • Description
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Problems solved by technology

However, the method described in this standard has the following disadvantages: (1) The detection period is long
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 more cumbersome
(3) The titration process is easily interfered by other metal ions or compounds, which will affect the titration results
In recent years, there has also been an application of the ICP method to the detection of various components in the pyrotechnics used in fireworks and firecrackers in the prior art. Metrology 2010 No. 05), this document discloses the characteristic spectral lines and methods of 16 elements such as Mg and Al in fireworks and firecrackers determined by ICP-AES method, but adopts the characteristic spectral lines and methods disclosed in this document to detect Mg, The accuracy is not high enough for the Al element, where the Mg recovery is only 93.4% and the Al recovery is 113.3%, in addition, their precision is not good enough

Method used

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  • Measurement method for content of magnesium and content of aluminium in main component of pyrotechnic composition for fireworks and crackers
  • Measurement method for content of magnesium and content of aluminium in main component of pyrotechnic composition for fireworks and crackers
  • Measurement method for content of magnesium and content of aluminium in main component of pyrotechnic composition for fireworks and crackers

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Draw a calibration curve

[0035] 1) Prepare several parts of magnesium-aluminum working solution (the mass concentration of Mg in the obtained magnesium-aluminum working solution is required to be 20-160 mg / L, and the mass concentration of Al is 20-160 mg / L):

[0036] The specific preparation method is as follows:

[0037] Prepare 6 parts of magnesium-aluminum working solution: respectively pipette 0 mL, 2 mL, 4 mL, 8 mL, 12 mL and 16 mL of magnesium single standard solution and aluminum single standard solution with a mass concentration of 1000 mg / L and place them in six 100 mL volumetric flasks respectively. Use 2% mass of hydrochloric acid solution to set the volume to the scale, and number them respectively as Work 1, Work 2, Work 3, Work 4, Work 5 and Work 6. The concentrations of Mg and Al in them are shown in Table 1 respectively;

[0038] 2) Draw a calibration curve:

[0039] 2a) Using an inductively coupled plasma emission spectrometer (produced b...

Embodiment 2

[0049] Embodiment 2: adopting the method of the present invention to carry out the recovery test of addition of high-purity magnesium powder and high-purity aluminum powder with the actual pyrotechnic powder as the matrix

[0050] Contain magnesium, aluminum high-purity elemental pyrotechnic powder sample listed in Table 5 to carry out standard addition recovery test, wherein the Mg and Al nominal content of the pyrotechnic powder that is added with high-purity magnesium powder and high-purity aluminum powder are as shown in Table 5; Adopt When the method of the present invention is measured, the magnesium and aluminum content determination is carried out after the standard substance prepares the sample solution according to the following method.

[0051] 1) Preparation of sample solution:

[0052]Prepare the sample liquid with the pyrotechnic powder added with high-purity magnesium powder and high-purity aluminum powder of No. 1 as the sample, weigh 3 parts of 390-410 mg samp...

Embodiment 3

[0064] Embodiment 3: Adopt the method of the present invention to the precision test of the detection result of aluminum-marked pyrotechnic powder

[0065] In this embodiment, the aluminum-marked pyrotechnic powders numbered 1, 2, 3 and 4 in Table 5 were used as samples for testing.

[0066] 1) Preparation of sample solution:

[0067] Prepare the sample liquid with the pyrotechnic powder with high-purity magnesium powder and high-purity aluminum powder No. 1 as the sample, weigh 4 parts of 390-410 mg samples, and the accuracy of weighing is 0.1 mg, and put the first sample in a beaker Inside, add acetone (C 3 h 6 O content is 99% by mass), add absolute ethanol in the amount of 40mL / g sample to fully dissolve (to separate the organic binder in the pyrotechnic powder), filter, add hydrochloric acid in the amount of 20mL / g sample to the filter residue (HCl content is 36% by mass) to completely dissolve the filter residue, filter, add water to the filtrate to 1L to obtain the f...

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Abstract

The invention discloses a measurement method for the content of magnesium and the content of aluminium in a main component of pyrotechnic composition for fireworks and crackers. The measurement method comprises the following steps: (1) taking inductively-coupled plasma emission spectrometer as a detecting instrument, selecting 279.0nm as a characteristic spectral line for detecting Mg element, and selecting 256.7nm or 237.3nm as a characteristic spectral line for detecting Al element; respectively making a Mg-element calibration curve and a Al-element calibration curve; and (2) preparing pyrotechnic composition sample liquid, detecting on a computer, displaying the characteristic spectral intensity on a recording instrument, reading a mass concentration value corresponding to Mg or Al according to the determined calibration curve by the characteristic spectral intensity; and calculating the mass percent concentration of elementary magnesium or aluminium according to the specific formula. The measurement method disclosed by the invention has the advantages that method is simple and the detection period is short; and the characteristic spectral line is adopted for detection by combination with the sample treatment method, the recovery rate is high (99.85%-103.07%) and the precision is high,.

Description

technical field [0001] The invention relates to a method for determining magnesium and aluminum contents in main components of pyrotechnic powder for fireworks and firecrackers, and belongs to the technical field of analysis and testing. Background technique [0002] In the prior art, the detection methods of magnesium and aluminum content in the pyrotechnic powder used for fireworks and firecrackers are all based on the traditional chemical analysis method of EDTA complexometric titration, wherein: [0003] The commonly used methods and standards for aluminum content are: "Determination of Aluminum Content in Fireworks and Pyrotechnic Powder" (GB / T20615-2006). The basic principle of this standard method: use sodium hydroxide solution to precipitate ionic components that may be used in pyrotechnic powder at PH13, such as: Bi 3+ 、Cu 2+ , Fe 3+ , Mg 2+ 、Ti 4+ etc., put Al 3+ The mixed ions are separated. Then, through Na 2 SO 4 solution to mask the possible presence o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
Inventor 吴俊逸肖焕新
Owner 广西出入境检验检疫局危险品检测技术中心
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