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Bis(cyclohexanone)oxalydihydrazone spectrophotometric method for determining high content copper in alloy

A bicyclohexanone oxalyldihydrazone, high-content technology, applied in the field of casting, can solve the problems that are not suitable for fast and simple analysis work, cannot measure high-content Cu, and the operation of electrolytic gravimetric method is complicated, etc., and achieves short time consumption , simple steps, overcome the effect of complex operation

Inactive Publication Date: 2015-05-13
青岛齐力铸钢有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the electrolytic gravimetric method is complicated to operate and takes a long time, which is not suitable for fast and simple analysis work, and the measurement range of the latter two analysis methods is ≤5.0%, that is, it cannot measure high-content Cu

Method used

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Embodiment

[0014] The dicyclohexanone oxalyldihydrazone photometric method of the determination of high-content copper in the alloy of the present embodiment includes the following contents:

[0015] (1) Main instruments and reagents: T6 New Century UV-Vis Spectrophotometer (Beijing Puxi General Analytical Instrument Co., Ltd.); concentrated hydrochloric acid: ρ about 1.18g / mL; concentrated nitric acid: ρ about 1.4g / mL; ammonia water: ρ is about 0.90g / L; ammonium citrate: 500g / L; ammonium chloride-ammonia water buffer solution (pH9.2): weigh 54g ammonium chloride, dissolve in 500mL water, add 63mL ammonia water, dilute to 1000mL; BCO solution : 1g / L, weigh about 1g of BCO, add 40mL of absolute ethanol (1+1) to slightly heat to dissolve, dilute to 1000mL with water; Cu standard stock solution: 1g / L, accurately weigh 0.1000g of metal copper (99.99%) , with 20mLHNO 3 (1+1) Dissolve by heating at low temperature, cool to room temperature, transfer to a 1000mL volumetric flask, and dilute to...

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Abstract

The invention discloses a bis(cyclohexanone)oxalydihydrazone spectrophotometric method for determining high content copper in an alloy. The bis(cyclohexanone)oxalydihydrazone (BCO) spectrophotometric method is adopted to rapidly determine the high content copper in the alloy, and optimum chromogenic conditions are discussed. A result shows that copper and the BCO form a blue complex in an ammonia water-ammonium chloride buffer solution with the pH value of 8.5-11.0, and the maximum absorption wavelength of the complex is 600nm; the concentration of the BCO is 0.1g / L; the chromogenic temperature is 20DEG C; the chromogenic time is 10min, and the use amount of ammonium citrate is 1mL. Copper in a range of 0.4-4.0[mu]g / mL accords with Beer's law, and the apparent molar absorption coefficient epsilon is 1.6*10<4>L.mol<-1>.cm<-1>. The method can be used to determine high content copper in high temperature alloy and copper alloy standard samples, the obtained measured value is consistent with a certified value, the relative error is smaller than 1.0%, and the relative standard deviation is smaller than 6.5%.

Description

[0001] technical field [0002] The invention belongs to the technical field of casting, and in particular relates to a dicyclohexanone oxalyldihydrazone photometric method for determining high-content copper in alloys. [0003] Background technique [0004] At present, the chemical methods for the determination of Cu mainly include electrolytic gravimetry, sodium thiosulfate separation-iodometric method (measurement range: 0.10% to 5.00%) and neocuproine-chloroform extraction photometry (measurement range: 0.010% ~1.00%). Among them, the electrolytic gravimetric method is complicated to operate and takes a long time, which is not suitable for fast and simple analysis work, and the measurement range of the latter two analysis methods is ≤5.0%, that is, it cannot measure high-content Cu. Therefore, it is necessary to explore an accurate and convenient analytical method for the determination of high-content Cu. [0005] Contents of the invention [0006] In order to ...

Claims

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Application Information

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IPC IPC(8): G01N21/31
Inventor 刘占向
Owner 青岛齐力铸钢有限公司