Detection method of lead content in triacetin

A technology of glycerol acetate and a determination method, applied in the field of determination of lead content in triacetin, can solve problems such as physical harm to operators, low sensitivity, and complicated operation procedures, and achieves less interference in the measurement process, reduction of process losses, The effect of accurate detection results

Inactive Publication Date: 2013-07-10
CHINA TOBACCO GUANGXI IND
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  • Abstract
  • Description
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Problems solved by technology

[0003] The detection of lead content in triacetin in my country generally adopts the national recommended standard: GB / T 5009.75 Determination of lead in food additives. This method has cumbersome operating procedures and low sensitivity, and is not suitable for the determination of lead in batch samples. Chloroform and other reagents are highly toxic and harmful to operators

Method used

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  • Detection method of lead content in triacetin
  • Detection method of lead content in triacetin
  • Detection method of lead content in triacetin

Examples

Experimental program
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preparation example Construction

[0029] (3) Preparation of standard curve

[0030] Draw up 20 μL each of the standard blank solution and the prepared standard working solution of different concentrations, and automatically add 10 μl of glycerol triacetate sample diluent, and inject 5 μL of palladium nitrate solution into the graphite furnace. Under the instrument operating conditions in Table 1, measure the absorbance, and draw the standard curve according to the standard addition method.

[0031] (4) Determination of sample lead content

[0032] Place the processed sample on the sample plate, and measure under the same conditions as the standard curve preparation. A sample volume of 20 μl was injected, and the reagent blank was determined simultaneously.

[0033] (5) detection limit of the inventive method

[0034] Prepare 10 blank solutions at the same time, measure 10 blank samples with atomic absorption spectrometer, calculate the deviation, take 3 times of the deviation value as the detection limit of...

example 1

[0052] 1. Instruments and reagents: PTFE volumetric flask, 50mL. Analytical balance, the sensitivity is 0.0001g. Teflon beaker, 100mL. Graphite Furnace Atomic Absorption Spectrometer. Water, ultrapure water or double distilled water of equivalent purity. Absolute ethanol (excellent grade pure), palladium nitrate solution concentration is 2.0g / L, lead standard solution.

[0053] 2. Sample treatment: Accurately weigh 1.0g of glycerol triacetate sample A, put it into a 50ml polytetrafluoroethylene volumetric flask, then dilute to 50ml with absolute ethanol, shake well for testing.

[0054] 3. Determination method: draw standard blank solution, prepared concentration of 1.0μg / L, 5.0μg / L, 20μg / L, 40μg / L lead standard solution and 20μL each of the sample after digestion, blank, standard solution and sample 5 μ L of palladium nitrate solution was added into the graphite furnace for measurement, and the lead in the sample was measured to be 0.36 mg / kg.

example 2

[0056] As described in Example 1, a glycerol triacetate sample from manufacturer B was selected, and the lead in the sample was measured to be 0.21 mg / kg.

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Abstract

The invention discloses a detection method of lead content in triacetin. The detection method is characterized in that a sample is diluted through absolute ethyl alcohol at the pre-processing stage, a standard adding method is adopted, and an air oxidation step is added between the drying step and the ashing step in the atomic absorption spectrometer heating process, thus the sample can be directly fed and detected, and the content of lead in triacetin can be quickly and accurately detected. Compared with the conventional electric hot plate digesting and microwave digestion pre-processing, the detection method disclosed by the invention has the advantages that little loss of the element to be detected is caused during direct feeding, the operation is easy, and poisonous and harmful chemicals are not used in the experimental process, so nearly no harm is brought to an operator. According to the detection method of the lead content in triacetin, after detection adopting the optimized related heating processes, ashing temperature and atomizing temperature of the atomic absorption spectrometry based on the characteristics of the triacetin material, a matrix modifier is adopted and used for eliminating the interference, thus high recovery rate is realized, and the detection result is accurate.

Description

Technical field: [0001] The invention belongs to the technical field of physical and chemical testing, and in particular relates to a method for determining the lead content in glycerol triacetate. Background technique: [0002] Glyceryl triacetate is a widely used organic industrial raw material, often used as a plasticizer for vinyl polymers, copolymers and cellulose resins. It is used as a carrier and solvent in the pharmaceutical industry. It is often used as a fragrance and perfume, a fixative for cosmetics, and a lubricating matrix in daily necessities. With the increasing awareness of environmental protection and the concern about the harm of chemicals to human health, the quality and safety of glycerol triacetate has received more and more attention from all aspects. As we all know, lead is a chronic and cumulative poison. Lead is a potential carcinogen to the human body, and its toxicity is mainly manifested in the inhibition of hemoglobin synthesis and its hemolys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
Inventor 徐雪芹田兆福李小兰陈志燕周芸许蔼飞曾德芬蒋宏霖
Owner CHINA TOBACCO GUANGXI IND
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