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Analytical reagent for detecting trace lead as well as preparation method and application thereof

A reagent and lead content technology, applied in the field of analytical chemistry, can solve the problems of not being able to meet the actual needs of production, the large amount of organic solvents used, and easy pollution of the environment, and achieve the effects of saving time, improving selectivity, and reducing environmental pollution

Inactive Publication Date: 2012-12-19
YUNNAN RES INST OF TOBACCO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, my country's national standard adopts dithizone extraction photometry, which needs to be extracted with chloroform, which is not only troublesome to operate, but also consumes a large amount of organic solvents, which is easy to pollute the environment and introduces many error factors.
In recent years, although other photometric methods have been reported for the determination of lead, due to the low lead content in the sample, it needs to be enriched before it can be accurately determined by photometric method, which cannot meet the actual needs of production and needs to be improved urgently.

Method used

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  • Analytical reagent for detecting trace lead as well as preparation method and application thereof
  • Analytical reagent for detecting trace lead as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] - Synthesis of analytical reagents

[0030] Dissolve 0.02mol of p-aminobenzenesulfonic acid in 400ml of absolute ethanol, add 2g of sodium amide, and heat to reflux in a water bath for 4 hours. Then add 8g of isoamyl nitrite, reflux for 30 minutes, and cool to obtain diazonium salt. Add 0.02mol of 8-aminoquinaldine and 2.5g of sodium carbonate to the diazonium salt solution, stir for 0.5 hour, place over the liquid, evaporate most of the ethanol off under reduced pressure, filter the precipitate to obtain the crude product, and weigh the crude product with ethanol The required analytical reagent can be obtained after crystallization for 2-3 times.

Embodiment 2

[0032] - Determination of lead in tobacco

[0033] Accurately weigh 0.2 g of tobacco into a polytetrafluoroethylene microwave digestion tank, add 1.5 mL of concentrated nitric acid and 2 mL of 30% H 2 o 2 , digested in a microwave digestion oven for 10min; after digestion, heated and evaporated on a hot plate until nearly dry, and washed with 20mL 5% H 2 SO 4 Dissolve the residue and transfer it to a 50mL colorimetric tube; then add 4mL of 0.1% 5-p-sulfophenylazo-8-aminoquinaldine solution, shake well, let it stand for 10min, and use the chromogenic solution at 10mL / min Flow rate through pre-activated Waters Sep-Pak-C 18 Solid-phase extraction column, dehydrate the column after enrichment, elute with 1.0mL ethanol at a flow rate of 5mL / min, adjust the volume of the eluent to 1.0mL accurately, use a reagent blank as a reference, use 1cm semi-micro cuvette, measure the absorbance at 610nm.

Embodiment 3

[0035] - Determination of lead in cigarette accessories

[0036] Accurately weigh 0.2 g of the cigarette auxiliary material sample into a polytetrafluoroethylene microwave digestion tank, add 1.5 mL of concentrated nitric acid and 2 mL of 30% H 2 o 2 , digested in a microwave digestion oven for 10min; after digestion, heated and evaporated on a hot plate until nearly dry, and washed with 20mL 5% H 2 SO 4 Dissolve the residue and transfer it to a 50mL colorimetric tube; then add 4mL of 0.1% 5-p-sulfophenylazo-8-aminoquinaldine solution, shake well, let it stand for 10min, and use the chromogenic solution at 10mL / min Flow rate through pre-activated WatersSep-Pak-C 18Solid-phase extraction column, dehydrate the column after enrichment, elute with 1.0mL ethanol at a flow rate of 5mL / min, adjust the volume of the eluent to 1.0mL accurately, use a reagent blank as a reference, use 1cm semi-micro cuvette, measure the absorbance at 610nm.

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Abstract

The invention discloses a new analytical reagent for detecting trace lead, which has the chemical structure represented by the general formula (I). The analytical reagent is synthesized by the following two steps of reaction: firstly, using sulfanilic acid to prepare diazonium salt; then, coupling with 8-azly quinaldine to obtain the analytical reagent. The invention provides a new method for detecting trace lead based on the newly synthesized analytical reagent, and the method is applied to analysis tests in the tobacco industry. The defect of relatively low sensitivity of absorption photometry is overcome, so that the common photometry can be used for detecting mug / g level lead. The detection results of the method are consistent with the results of the graphite furnace atomic absorptionmethod.

Description

technical field [0001] The invention relates to the field of analytical chemistry, more specifically, the invention relates to an analytical reagent for determining lead in tobacco and its additives. At the same time, the invention also relates to the preparation method of the agent and the application in the tobacco industry. Background technique [0002] Lead in tobacco is a harmful element. The determination of lead in tobacco, cigarette accessories and tobacco additives is of great significance to ensure the safety of cigarette products. In the prior art, methods for determining the lead content include spectrophotometry, atomic absorption method, atomic fluorescence method, plasma emission spectrometry, plasma mass spectrometry, and the like. Spectrophotometry is the most commonly used method because of its simple equipment and low cost. [0003] At present, my country's national standard adopts the dithizone extraction photometric method, which needs to be extracted ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D215/40G01N21/78
Inventor 杨光宇金永灿贺兵崔柱文孔维松刘巍
Owner YUNNAN RES INST OF TOBACCO SCI
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