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

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...

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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 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

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