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Method for measuring potassium content of black powder

A technology of potassium content and black powder, applied in the field of analysis and testing, can solve the problems of long detection cycle, insufficient operation proficiency, and measurement error, etc., and achieve the effect of short detection cycle, low labor intensity and high precision

Inactive Publication Date: 2017-02-15
吴俊逸
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  • Abstract
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  • Claims
  • Application Information

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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 relatively cumbersome. After washing the sample with absolute ethanol and acetone for many times, dissolve it in water, filter, transfer, and constant volume, then take a certain sample solution and add phenolphthalein, formaldehyde, EDTA, and NaOH, etc. Then, potassium ions were precipitated with tetraphenylborate sodium ethanol solution, then filtered and washed several times, and finally weighed after drying and constant weight.
[0005] Black powder is generally composed of potassium nitrate, carbon powder and sulfur. It is often used as propellant and bud opening powder for fireworks and firecrackers. Due to the complex matrix effect (including inter-element absorption-enhancement effect and physical- chemical effects), it is impossible to use energy dispersive X-ray fluorescence spectrometry (EDXRF) to directly measure solid powder samples with complex and changeable matrix background by powder pressing method and melting method
Furthermore, due to the flammable and explosive characteristics of black powder, it is difficult to pre-treat it by tableting or melting
So far, there is no public literature report on the detection of potassium content in black powder by energy dispersive X-ray fluorescence spectrometry

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  • Method for measuring potassium content of black powder
  • Method for measuring potassium content of black powder
  • Method for measuring potassium content of black powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: Make calibration curve

[0036] 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) :

[0037] The specific preparation method is as follows:

[0038] 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 5mL-10mL nitric acid, and dilute to the mark with water; wherein, the nitric acid is HNO 3 Nitric acid with a content of 10% to 30% by mass.

[0039] 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...

Embodiment 2

[0050] Embodiment 2: adopt method of the present invention to carry out the control test that black powder reference substance and potassium standard solution are measured

[0051] Test with black powder reference substance and potassium standard solution listed in table 3, wherein the potassium nominal content of black powder reference substance and potassium standard solution is as shown in table 3; When adopting the method of the present invention to measure, black powder The reference substance is prepared in the following way to prepare the sample solution, and then the potassium content is determined.

[0052] 1) Preparation of sample solution:

[0053] 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 an electric furnace for 10 minutes, filter it into a 500mL volumetric flask while it is h...

Embodiment 3

[0065] Embodiment 3: adopt the method for the present invention to the precision test of the detection result of black powder reference material

[0066] In this embodiment, the reference substances numbered 4, 5 and 6 in Table 3 were used as samples for testing.

[0067] 1) Preparation of sample solution:

[0068] Use the reference substance No. 1 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 an electric furnace for 10 minutes, filter it into a 500mL volumetric flask while it is hot, rinse it with water several times, and add 5mL to 10mL of nitric acid after the filtrate is cooled to room temperature (in this step, HNO 3 Nitric acid with a content of 10% to 30% by mass), then dilute to 500mL with water to obtain the first sample solution; repeat the above method to obtain 4 sample solutions of No. 1 reference substance.

[...

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Abstract

The invention discloses a method for measuring the potassium content of black powder. The method comprises the following steps: preparing multiple potassium chloride working solutions with different concentrations, taking an energy dispersion type X-ray fluorescence spectrometer as the detection instrument, assuming a certain amount of samples, adopting a mathematical intensity correction method to establish an analysis method, converting the potassium (K) mass concentrations of prepared potassium chloride working solutions into potassium (K) mass percentage concentrations; recording the fluorescence strength of K for each sample injection, drawing a calibration curve; preparing a sample solution from black powder to be detected, recording the fluorescence strength of K displayed on the instrument, reading the value of mass percentage concentration of K on the calibration curve corresponding to the fluorescence strength, and calculating the content of K. By optimizing the dissolution conditions and parameters of the X-ray fluorescence spectrometer, the matrix effect among elements in the sample can be eliminated or basically eliminated. The provided method has the advantages of simple operation, short detection period, good accuracy, and high precision.

Description

technical field [0001] The invention relates to the technical field of analysis and testing, in particular to a method for measuring potassium content in black powder by energy dispersive X-ray fluorescence spectrometry. Background technique [0002] In the prior art, there is no standard method for the detection of potassium content in black powder. You can refer to "Pyrotechnic Agents for Fireworks and Firecrackers Part 11: Determination of Potassium Content" (SN / T 1732.11-2014). Quantitative traditional chemical analysis methods. The basic principle of this standard method: After the sample is properly pretreated, it is filtered with hot water, and the experimental solution containing potassium ions is in a weakly alkaline medium to form potassium tetraphenylborate precipitation with sodium tetraphenylborate, and the sample is determined by gravimetric method. content of potassium. [0003] The method described in this standard has the following deficiencies: (1) the de...

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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