Method for determining content of Cu in CuO for fireworks and firecrackers

A technology for fireworks and firecrackers and copper oxide, which is applied in the field of analysis and testing, can solve the problems of insufficient operation proficiency, high requirements for experimental personnel, and complicated operation steps, and achieves the effects of low labor intensity, high absolute sensitivity, and simple operation.

Inactive Publication Date: 2017-01-11
吴俊逸
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 the sample is dissolved with dilute nitric acid, filtered, and fixed to volume, different methods must be used to measure the total amount of copper ions and iron ions and the individual amount of iron ions. The total amount minus the amount of iron ions amount to get the amount of copper ions
(3) The method has high requirements for experimenters, and the operation steps often involve pipetting, pH adjustment, titration, etc., which are easy to introduce uncertainties. Operators must be extra careful and meticulous in each test, otherwise it is very easy to introduce artificial errors. uncertainty
There are complex matrix effects (including inter-element absorption-enhancement effects and physical-chemical effects) among elements in copper oxide raw materials, which cannot be directly determined by powder compression method and melting method by energy dispersive X-ray fluorescence spectrometry (EDXRF) Solid powder samples with complex and changeable matrix background
So far, there is no public literature report on the detection of copper content in copper oxide for fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry

Method used

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  • Method for determining content of Cu in CuO for fireworks and firecrackers
  • Method for determining content of Cu in CuO for fireworks and firecrackers
  • Method for determining content of Cu in CuO for fireworks and firecrackers

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Experimental program
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Effect test

Embodiment 1

[0042] Embodiment 1: Make calibration curve

[0043] 1) Prepare multiple copper working solutions (the mass concentration of Cu element in the obtained copper working solution is required to be 0.19g / L~0.84g / L):

[0044] The specific preparation method is as follows:

[0045] Accurately weigh 2.50g of high-purity copper oxide (accurate to 0.1mg), put it in a 300mL beaker, add 50mL~80mL of dilute nitric acid, place the beaker on an electric furnace and heat for 25min~35min, and transfer the solution to a 500mL capacity after cooling to room temperature. bottle, add water to make it up to the mark; wherein, the mass percent concentration of nitric acid is 10% to 30% by mass.

[0046] Prepare 11 copies of copper working solution: Pipette 5mL, 10mL, 15mL, 20mL, 25mL, 30mL, 35mL and 40mL of the above-mentioned copper working solution after constant volume into a group of 100mL volumetric flasks, add water to dilute to the mark, mix well, and respectively The numbers are Work 1, W...

Embodiment 2

[0058] Embodiment 2: adopt the method described in the present invention to measure the control test of copper oxide reference material for fireworks and firecrackers

[0059] Test with the copper oxide reference substance listed in table 3, wherein the copper oxide nominal content of reference substance is as shown in table 3; Then the copper content was measured.

[0060] 1) Preparation of sample solution:

[0061] Use the reference substance No. 1 as the sample to prepare the sample solution, weigh 3 parts of 0.49g ~ 0.51g sample, and the weighing is accurate to 0.1mg. The first sample is placed in a 300mL beaker, and weighed at 40mL / g Add nitric acid to an amount of ~50mL / g sample, the mass percentage concentration of nitric acid is 40%~60%, place it on an electric furnace and heat it to a slight boil for 30min, filter it with filter paper while it is hot, collect the filtrate into a 500mL volumetric flask, and wait for the After the solution is cooled to room temperatur...

Embodiment 3

[0072] Embodiment 3: adopt the method for the present invention to the precision test of the detection result of copper oxide reference substance

[0073] In this embodiment, three copper oxide reference substances for fireworks and firecrackers with different copper contents were used as samples for testing, numbered 1, 2 and 3.

[0074] 1) Preparation of sample solution:

[0075] Use the reference substance No. 1 as the sample to prepare the sample solution, weigh 4 parts of 0.49g ~ 0.51g sample, when weighing, the accuracy is 0.1mg, put the first sample in a 300mL beaker, and weigh 40mL / g Add nitric acid to an amount of ~50mL / g sample, the mass percentage concentration of nitric acid is 40%~60%, place it on an electric furnace and heat it to a slight boil for 30min, filter it with filter paper while it is hot, collect the filtrate into a 500mL volumetric flask, and wait for the After the solution is cooled to room temperature, add water to make up to the mark to obtain the...

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Abstract

A method for determining the content of Cu in CuO for fireworks and firecrackers comprises the following steps: dissolving high-purity CuO in dilute nitric acid as a solvent, preparing multiple Cu standard solutions, and determining the fluorescence intensity of the standard solutions by an energy dispersion type X-ray fluorescence spectrophotometer; drawing a calibration curve with mass percent concentration of CuO as a horizontal axis and fluorescence intensity of the Cu standard solution with the corresponding concentration (or calculated mass percent concentration of CuO) as a vertical axis; dissolving a CuO specimen with dilute nitric acid, determining the fluorescence intensity of Cu in a specimen solution by the energy dispersion type X-ray fluorescence spectrophotometer, analyzing CuO quantitively based on the calibration curve and calculating the content of Cu in the CuO specimen. According to the method, a matrix effect between elements in the specimen can be eliminated or basically eliminated by optimizing specimen dissolving conditions and parameter conditions of the X-ray fluorescence spectrophotometer. The method is simple to operate, short in detection cycle, good in detection result accuracy and high in precision.

Description

technical field [0001] The invention relates to a method for measuring copper content in copper oxide used for fireworks and firecrackers by energy dispersive X-ray fluorescence spectrometry, and belongs to the technical field of analysis and testing. Background technique [0002] In the prior art, the detection method of copper content in copper oxide for fireworks and firecrackers is a traditional chemical analysis method based on EDTA complexometric titration. -2006). The basic principle of this standard method: after the sample is dissolved in nitric acid, the EDTA complexometric titration method is used to use PAN as the indicator solution under the condition of pH 10.0, and the copper sulfate standard titration solution is used to titrate the test solution from yellow to blue, which is the end point. Measure the sum of the content of copper ions and iron ions in the test solution, and subtract the amount of iron to obtain the amount of copper. [0003] The method des...

Claims

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Application Information

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IPC IPC(8): G01N21/64G01N1/38
CPCG01N1/38G01N21/64
Inventor 吴俊逸
Owner 吴俊逸
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