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: 2015-03-11
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°C, and add 0.01mol NaNO dropwise 2 Aqueous solution, kept at 0°C and fully stirred until the diazotization reaction is complete, checked with starch-potassium iodide test paper until the diazotization is complete, and the diazonium salt is obtained; add 0.01moL of 8-aminoquinaldine to the diazonium salt, Keep at 0°C, add sodium hydroxide to adjust the pH value of the reaction system to 5, react for 1.5 hours, then adjust the pH value of the reaction system to 8, check the complete diazotization with starch-potassium iodide test paper until the diazonium salt coupling reaction Completely, the product a was obtained; the product a was suction filtered, washed once with water and 60% ethanol, dried at 30°C at low temperature to obtain a crude compound, and the crude product was recrystallized twice by ethanol to obtain the pure compound product with a yield of 34%.

Embodiment 2

[0054] Mix and stir according to the ratio of 0.01mol p-acetylaniline and 5ml concentrated hydrochloric acid, cool to 5°C, and dropwise add 0.01mol NaNO 2 Aqueous solution, kept at 5°C and fully stirred until the diazotization reaction is complete, detected with starch-potassium iodide test paper until the diazotization is complete, and the diazonium salt is obtained; add 0.01moL of 8-aminoquinaldine to the diazonium salt, Keep at 5°C, 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, monitor with starch-potassium iodide test paper until the diazonium salt coupling reaction is complete, and the product is obtained a: Suction filter the product a, wash it once with water and 50% ethanol, dry it at 40°C with vacuum drying equipment at low temperature to obtain the crude compound, recrystallize the crude product through ethanol three times, and obtain the pure product of th...

Embodiment 3

[0056] Mix and stir according to the ratio of 0.01mol p-acetylaniline and 5ml hydrobromic acid, cool to 10°C, and dropwise add 0.01mol NaNO 2 Aqueous solution, kept at 10°C and fully stirred until the diazotization reaction is complete, checked with starch-potassium iodide test paper until the diazotization is complete, and the diazonium salt is obtained; add 0.01moL of 8-aminoquinaldine to the diazonium salt, Keeping at 10°C, adding ammonia water to adjust the pH value of the reaction system to 5, and after reacting for 2 hours, adjust the pH value of the reaction system to 7, and check the completion of diazotization with starch-potassium iodide test paper until the coupling reaction of diazonium salt is complete to obtain Product a: the product a was suction filtered, washed once with water and 25% ethanol, dried at 60°C at low temperature to obtain a crude product of the compound, and the crude product was recrystallized 3 times with ethanol to obtain the pure product of th...

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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 in particular relates to a triazene compound with good selectivity, which can improve the sensitivity and accuracy of spectrophotometric detection of cadmium content, a preparation method and a method for measuring cadmium content. Background technique [0002] Cadmium is an important heavy metal element in tobacco. Tobacco is a cadmium-rich plant, and its cadmium content is higher than that of ordinary plant samples. Therefore, it is of great significance to determine the cadmium content in tobacco. The methods for measuring cadmium content in the prior art 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 easy-to-promote method. At present, there are many reports on the photometric deter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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