Method for measuring potassium content in potassium hydrogen terephthalate for fireworks and crackers

A technology of potassium hydrogen terephthalate and fireworks is applied in the field of analysis and testing to achieve the effects of short detection period, good accuracy and simple operation

Inactive Publication Date: 2017-02-01
广西出入境检验检疫局危险品检测技术中心
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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 detection of potassium content in potassium hydrogen terephthalate used in fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry based on collective effect targeted control technology (solution method)

Method used

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  • Method for measuring potassium content in potassium hydrogen terephthalate for fireworks and crackers
  • Method for measuring potassium content in potassium hydrogen terephthalate for fireworks and crackers
  • Method for measuring potassium content in potassium hydrogen terephthalate for fireworks and crackers

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Make a calibration curve:

[0037] 1) Prepare multiple parts of potassium chloride working solution (the mass concentration of K in the obtained potassium chloride working solution is required to be 0.16g / L~0.99g / L, and the mass concentration of Cl is 0.18g / L~1.10g / L) :

[0038] The specific preparation method is as follows:

[0039] Accurately weigh 3.5g of potassium chloride 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 a capacity of 500mL after cooling to room temperature bottle, add 10mL of dilute nitric acid, and dilute to the mark with water; wherein, the mass percent concentration of nitric acid is 10% to 30%.

[0040] Prepare 6 parts of potassium chloride working solution: pipette 5mL, 10mL, 15mL, 20mL, 25mL and 30mL of the above-mentioned potassium chloride working solution after constant volume into a group of 100mL vo...

Embodiment 2

[0051] Embodiment 2: adopt the method for the present invention to measure the control test of reference substance or standard solution

[0052] Test with potassium hydrogen terephthalate reference substance and potassium standard solution listed in table 3, wherein the potassium nominal content of reference substance and potassium standard solution is as shown in table 3; When adopting the method of the present invention to measure, The reference substance is prepared in the following way to prepare the sample solution, and then the potassium content is 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 1.4g ~ 1.6g 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 the electric furnace for 10 minutes, filter it into a volumetric flask with filter paper while it is hot, and rinse it repeatedly w...

Embodiment 3

[0068] Adopt the precision test of the detection result of method of the present invention to potassium hydrogen terephthalate reference substance:

[0069] In this embodiment, another potassium hydrogen terephthalate reference substance with three quality main contents was taken as a sample for testing, and the numbers were 4, 5 and 6 respectively.

[0070] 1) Preparation of sample solution:

[0071] Use the reference substance No. 4 as the sample to prepare the sample solution, weigh 4 parts of 1.4g ~ 1.6g 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 the electric furnace for 10 minutes, filter it into a volumetric flask with filter paper while it is hot, and rinse it repeatedly with water for several times. After the filtrate is cooled to room temperature, add 10 mL of nitric acid. 1st sample solution. Repeat the above method to obtain 4 sample solutions of No. 4 reference substance.

[0072] 2...

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Abstract

The invention discloses a method for measuring the potassium content in potassium hydrogen terephthalate for fireworks and crackers. The method includes the following steps that 1, a calibration curve is drawn, wherein multiple parts of potassium chloride working solutions are prepared, the mass concentration of K in the potassium chloride working solutions is converted into the mass percent concentration of K, an energy chromatic dispersion type X-ray fluorescence spectrometer is adopted as a detection instrument, the mass percent concentration of K in the potassium chloride working solutions serves as transverse coordinates, fluorescence intensity corresponding to the mass percent concentration of K serves as longitudinal coordinates, and the calibration curve is drawn; 2, the potassium content in potassium hydrogen terephthalate for the fireworks and crackers is measured, wherein a sample solution is prepared, the fluorescence intensity, displayed on the instrument, of K is recorded according to detection conditions in the steps 1 and 2, the mass percent concentration value, corresponding to the fluorescence intensity, of K is read out according to the determined calibration curve, and the mass percent concentration of potassium in a sample is calculated according to the formula. The method for measuring the potassium content is easy to operate, short in detection period, good in detection result accuracy and high in precision degree.

Description

technical field [0001] The invention belongs to the technical field of analysis and testing, and in particular relates to a method for measuring potassium content in potassium hydrogen terephthalate used for fireworks and firecrackers. [0002] technical background [0003] In the prior art, the detection method of potassium hydrogen terephthalate content, the main component of potassium hydrogen terephthalate used in fireworks and firecrackers, has not yet been found, usually referring to the chemical analysis method of potassium hydrogen phthalate——"Working Standard Reagent Potassium hydrogen phthalate" (GB 1257-2007), the principle of the standard method is: Weigh a certain amount of standard substance potassium hydrogen phthalate that has been dried to constant weight, dissolve it in water, and use a 231-type glass electrode as an indicating electrode , use 232-type saturated calomel electrode as reference electrode, titrate with sodium hydroxide standard titration soluti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223
CPCG01N23/223G01N2223/303
Inventor 吴俊逸肖焕新李宁涛王华熊中强
Owner 广西出入境检验检疫局危险品检测技术中心
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