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Method for determining dimethyl sulfate and diethyl sulfate in electronic and electric products

A technology of dimethyl sulfate and diethyl sulfate, applied in measuring devices, instruments, scientific instruments, etc., can solve the problem of no method for measuring dimethyl sulfate and diethyl sulfate, so as to meet the requirements of research and production, exclusive Strong and accurate effect

Inactive Publication Date: 2014-02-19
青岛谱尼测试有限公司
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Problems solved by technology

However, there is no method for the determination of dimethyl sulfate and diethyl sulfate in electrical and electronic products

Method used

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Embodiment Construction

[0017] The present invention will be described in further detail below in conjunction with specific examples, but the present invention is not limited to the specific examples.

[0018] The detection of dimethyl sulfate and diethyl sulfate content in the plastic case of embodiment

[0019] 1. Sample pretreatment

[0020] Take 1g of the pulverized solid plastic casing sample to be tested (accurately weighed to 0.001g), put it in a 25mL colorimetric tube, add 10mL of acetone, and ultrasonically extract for 30min; take it out and cool it to room temperature, take 2mL into a 25mL colorimetric tube, Add 400 mg of p-nitrophenol, 8 mL of 12 g / L sodium hydroxide solution, and mix well. Derivatize in a water bath at 40°C for 1 h, take it out, cool to room temperature, add 10 mL of diethyl ether to shake and extract, and let stand to separate layers. Take the upper ether phase and filter it through an organic filter membrane, then carry out liquid chromatography analysis.

[0021] 2....

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Abstract

The invention discloses a method for determining dimethyl sulfate and diethyl sulfate in electronic and electric products. The method comprises the following steps: adding a certain amount of acetone into a prepared sample, carrying out ultrasonic extraction to obtain the target compounds, deriving the target compounds with p-nitrophenol under alkaline conditions, extracting the derivation products with diethyl ether, and separating and detecting the ethyl ether extraction solution with a high performance liquid chromatography (HPLC) system. The chromatographic column uses an octadecyl bonded silica gel as the filler; the detector is a diode array detector; the mobile phase is a mixed solvent composed of 40-60 vol% of methanol and 60-40 vol% of water; the detection wavelength is 305nm; the column temperature is 40-60 DEG C; and the sample injection volume is 5-20 muL. After the systemic comparative studies, the invention establishes an HPLC method for determining contents of dimethyl sulfate and diethyl sulfate in electronic and electric products for the first time; and the method has the technical characteristics of favorable separating effect, high determination accuracy, high sensitivity, high specificity, simple and quick analysis and the like.

Description

technical field [0001] The invention relates to a method for determining dimethyl sulfate and diethyl sulfate in electrical and electronic products, in particular to a method for determining the content of dimethyl sulfate and diethyl sulfate in electrical and electronic products through high performance liquid chromatography . Background technique [0002] Dimethyl sulfate (CAS: 77-78-1), English name dimethyl sulfate, chemical formula C 2 h 6 o 4 S, with a relative molecular mass of 126.13, is a colorless or light yellow oily flammable liquid with a slight onion smell. It is easily hydrolyzed into sulfuric acid and methanol at 50°C or in alkaline water. Soluble in ethanol, ether, dioxane, acetone and aromatic hydrocarbons, slightly soluble in carbon disulfide and aliphatic hydrocarbons. Dimethyl sulfate is a highly toxic reagent. Possibly carcinogenic, corrosive, and combustible when exposed to heat, open flame or oxidizing agents. Dimethyl sulfate is a reagent that ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 宋薇
Owner 青岛谱尼测试有限公司
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