A Simultaneous Rapid Determination of Ethyl Acetate and Seven Residual Monomers in Adhesives
A technology based on ethyl acetate and residual monomers, which is applied in the detection field of cigarette adhesives, can solve the problems of gas chromatography with weak qualitative ability and easy interference of false positive samples, and achieve simple sample pretreatment, wide automation and wide application range Effect
Active Publication Date: 2015-12-02
CHINA TOBACCO ZHEJIANG IND
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Problems solved by technology
[0003] Tobacco industry standard "YC / T267—2008 Determination of Vinyl Acetate in White Latex for Tobacco by Headspace Gas Chromatography" uses headspace gas chromatography to determine vinyl acetate in adhesives, but the qualitative ability of gas chromatography is weak and is easily caused by interference. false positive samples
At present, there is no report on the simultaneous determination of ethyl acetate, vinyl acetate and six residual monomers of acrylates (methyl methacrylate, ethyl methacrylate, butyl methacrylate, methyl acrylate, ethyl acrylate, etc.) in adhesives. esters, butyl acrylate) research
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[0027] The following examples are intended to further illustrate the present invention, rather than limit the present invention.
[0028] A method for rapidly determining ethyl acetate and seven residual monomers in an adhesive simultaneously, wherein the seven residual monomers are vinyl acetate, methyl methacrylate, ethyl methacrylate, butyl methacrylate, Methyl acrylate, ethyl acrylate and butyl acrylate, the method comprises the following steps:
[0029] 1) Sample pretreatment: Weigh 0.1g (accurate to 0.1mg) adhesive sample, place it in a 20mL headspace bottle, add 1.0mL internal standard solution with a concentration of 2μg / mL (accurately weigh 0.1g of 2-hexanone in 50mL volumetric flask, dilute with N,N-dimethylformamide to constant volume), seal the cap and inject the sample.
[0030] 2) Prepare internal standard solution, mixed standard stock solution, and mixed standard working solution: accurately weigh 0.1g of 2-hexanone into a 50mL volumetric flask, dilute with DM...
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The invention relates to a method for simultaneously measuring ethyl acetate and seven residual monomers in adhesive quickly, which comprises the following steps: 1) preparing an inner standard solution, a mixed standard stock solution and a mixed standard working solution; 2) pretreatment of a sample: weighing 0.1g of adhesive sample, placing the sample in a 20 mL of headspace bottle, adding the inner standard solution and adding the sample after gland seal; 3) headspace-gas chromatographic test; and 4)determining the nature and quantity: determining the nature by using a standard retention time of the sample and a single standard sample introduction, wherein the chromatogram of the standard solution is as shown in Fig . 1, and determining the quantity by an internal standard method and drawing a standard working curve by using the peak area ratio y and concentration ratio x of an analyte to the internal standard to obtain the corresponding retention time, linear equation, limit of detection and limit of quantitation. According to the invention, headspace sampling is adopted, and the pretreatment of sample is simple and easy to automate. The method has the advantages of simplicity, quickness, accuracy, automation, wide application scope and the like.
Description
technical field [0001] The invention relates to a detection method for cigarette adhesives, in particular to a method for simultaneously determining ethyl acetate and seven residual monomers (vinyl acetate, methyl methacrylate, ethyl methacrylate, butyl methacrylate, acrylic acid) in adhesives. Methyl acrylate, ethyl acrylate, butyl acrylate) analysis method. Background technique [0002] Adhesive is an important smoking material, and its safety has attracted much attention. Vinyl acetate and acrylate monomers are commonly used raw materials. Due to incomplete conversion, they remain in the adhesive. Ethyl acetate is a residual impurity accompanying vinyl acetate. These residues will affect the quality and safety of cigarettes ("Tobacco Science and Technology" Magazine, No. 8, p. 35 (2009)). In recent years, gas chromatography and high performance liquid chromatography have been widely used in the determination of monomers in adhesives, but the pretreatment is more complic...
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IPC IPC(8): G01N30/02G01N30/88
Inventor 游金清张艳
Owner CHINA TOBACCO ZHEJIANG IND