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Triazene compound, preparation method, and method for determination of cadmium content

A triazene and compound technology, applied in the field of analytical chemistry, can solve the problems of poor cadmium selectivity and unsatisfactory sensitivity, and achieve the effects of high sensitivity, guaranteed sensitivity and safe operation

Active Publication Date: 2013-05-01
YUNNAN ACAD OF TOBACCO AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many reports on the photometric determination of cadmium with heterocyclic azo reagents, but the selectivity of heterocyclic azo reagents to cadmium is poor, and for some samples with low cadmium content, the sensitivity of ordinary photometric methods cannot meet the requirements of cadmium determination.

Method used

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  • Triazene compound, preparation method, and method for determination of cadmium content
  • Triazene compound, preparation method, and method for determination of cadmium content
  • Triazene compound, preparation method, and method for determination of cadmium content

Examples

Experimental program
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Effect test

Embodiment 1

[0052] Mix and stir according to the ratio of 0.01mol p-acetylaniline and 5ml hydrofluoric acid, cool to 0℃, add 0.01mol NaNO dropwise 2 Keep the aqueous solution at 0°C and stir well until the diazotization reaction is complete. Use starch-potassium iodide test paper to test until the diazotization is complete to obtain the diazonium salt; add 0.01moL of 8-aminoquinaldine to the diazonium salt, Keep at 0℃, add sodium hydroxide to adjust the pH value of the reaction system to 5, after 1.5 hours of reaction, adjust the pH value of the reaction system to 8, and use starch-potassium iodide test paper to check the complete diazotization until the diazonium salt coupling reaction Complete, obtain product a; product a is suction filtered, washed with water and 60% ethanol each, dried at a low temperature at 30°C to obtain a crude compound, and the crude product is recrystallized from ethanol twice to obtain the pure compound The yield is 34%.

Embodiment 2

[0054] Mix and stir according to the ratio of 0.01mol p-acetylaniline and 5ml concentrated hydrochloric acid, cool to 5℃, add 0.01mol NaNO dropwise 2 Keep the aqueous solution at 5°C and stir well until the diazotization reaction is complete. Use starch-potassium iodide test paper to test until the diazonium is complete to obtain the diazonium salt; add 0.01moL of 8-aminoquinaldine to the diazonium salt, Keep at 5℃, add saturated sodium acetate to adjust the pH value of the reaction system to 4, after 1.5 hours of reaction, adjust the pH value of the reaction system to 7, and monitor with starch-potassium iodide test paper until the diazonium salt coupling reaction is complete to obtain the product a; The product a is suction filtered, washed once with water and 50% ethanol, dried at a low temperature with a vacuum drying equipment at 40°C to obtain a crude compound, and the crude product is recrystallized from ethanol three times to obtain the pure compound , The yield is 36%. ...

Embodiment 3

[0056] Mix and stir according to the ratio of 0.01mol p-acetylaniline and 5ml hydrobromic acid, cool to 10℃, add 0.01mol NaNO dropwise 2 Keep the aqueous solution at 10°C and stir well until the diazotization reaction is complete. Use starch-potassium iodide test paper to test until the diazotide is complete, and the diazonium salt is obtained; 0.01moL of 8-aminoquinaldine is added to the diazonium salt, Keep at 10°C, add ammonia water to adjust the pH of the reaction system to 5, after 2 hours of reaction, adjust the pH of the reaction system to 7, and use starch-potassium iodide test paper to check the complete diazotization until the diazonium salt coupling reaction is complete. Product a; product a is suction filtered, washed with water and 25% ethanol each, dried at a low temperature at 60°C to obtain a crude compound, and the crude product is recrystallized from ethanol three times to obtain the pure compound. The rate is 35.6%.

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Abstract

The invention discloses a triazene compound, a preparation method, and a method for determination of a cadmium content. A structural formula of the triazene compound is as shown in the specification, wherein the name of the triazene compound is 1-(p-acetylbenzole)-3-(quinaldine)-triazene. The preparation method comprises the steps of diazonium salt synthesis, diazonium salt coupling and product purification. The method for the determination of the cadmium content comprises the steps of sample digestion, cadmium enrichment, complex reaction and absorbance determination. The triazene compound is a new compound synthesized for the first time; for the determination of the cadmium content, solid phase extraction is adopted to enrich cadmium, a lower cadmium content in a sample can be tested, interfering ions are few, and the contrast of absorption positions of a cadmium ion complex and a reagent blank is large, so that the sensitivity of spectrophotometric determination is ensured. The method for the determination of the cadmium content with the triazene compound has the characteristics that a reaction system develops colors rapidly, the system is stable, the use amount of an organic solvent is small, the operation is safer, and the pollution to an environment is small.

Description

Technical field [0001] The invention belongs to the technical field of analytical chemistry, and specifically relates to a triazene compound with good selectivity and capable of improving the sensitivity and accuracy of spectrophotometric detection of cadmium content, a preparation method and a method for determining cadmium content. Background technique [0002] Cadmium is an important heavy metal element in tobacco. Tobacco is a cadmium-rich plant. The content of cadmium is higher than that of ordinary plant samples. Therefore, the determination of cadmium in tobacco is of great significance. The prior art methods for determining cadmium content include: spectrophotometry, atomic absorption method, atomic fluorescence method, plasma emission spectrometry and plasma mass spectrometry. Due to the simple equipment and low cost of analysis, spectrophotometry is the most commonly used and easily promoted method. At present, there are many reports on the spectrophotometric determina...

Claims

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Application Information

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IPC IPC(8): C07D215/40G01N21/31
Inventor 吴玉萍卢秀萍夏振远胡秋芬王丙武李文正
Owner YUNNAN ACAD OF TOBACCO AGRI SCI
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