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Method for purifying bisphenol compound in surface water sample extraction liquid

A technology of surface water and extraction liquid, which is applied in the preparation of test samples, etc., can solve the problems of bisphenol compounds affecting the water body matrix, and achieve the effects of reducing inhibition effect, shortening time, and saving time

Inactive Publication Date: 2016-01-20
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims to solve the problem that the bisphenol compounds in the current surface water samples are easily affected by the water matrix during the analysis and detection process, and proposes a method for purifying the bisphenol compounds in the surface water sample extract

Method used

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  • Method for purifying bisphenol compound in surface water sample extraction liquid
  • Method for purifying bisphenol compound in surface water sample extraction liquid
  • Method for purifying bisphenol compound in surface water sample extraction liquid

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specific Embodiment approach 1

[0020] Specific implementation mode one: as figure 1 As shown, a method for purifying bisphenols in the surface water sample extract comprises the following steps:

[0021] Step 1: Obtain the surface water sample extract by extracting the surface water sample;

[0022] Step 2: preparation of composite chromatographic column;

[0023] Take an all-glass chromatography column with a PTFE joint door at the bottom, and fill in the glass wool layer, the first anhydrous sodium sulfate layer, the florisil layer, the neutral silica layer, the acid silica layer and the The second anhydrous sodium sulfate layer;

[0024] Using the sulfonation of sulfuric acid, the acidic silica gel is placed on the upper layer to remove most of the matrix effect first, which is helpful for the purification of the lower column chromatography. The lower layer of Florisil can better separate bisphenols and water. Humic acid and pigments in environmental samples;

[0025] Step 3: pre-washing the composit...

specific Embodiment approach 2

[0029] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the specific process of the extraction of the surface water sample in the step one is:

[0030] (1) Take a surface water sample, adjust pH=4, take a WatersOasisHLB solid phase extraction column, use an automatic solid phase extraction instrument, activate the solid phase extraction column with ethyl acetate, methanol, and pure water in sequence, and use WatersOasisHLB as the solid phase extraction column model;

[0031] (2) Take the water sample after adjusting the pH value and pass through the solid phase extraction column at a flow rate of 2-5mL / min;

[0032] (3) After loading the sample, use ultrapure water as the eluent to rinse the solid-phase extraction column to remove impurities;

[0033] (4) After the solid-phase extraction column is dried under high-purity nitrogen, it is eluted twice with ethyl acetate. The mixed solution was redissolved and purified.

specific Embodiment approach 3

[0034] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that in the step 2, the all-glass chromatography column with a PTFE joint at the bottom has a column length of 45 cm and an inner diameter of 3 cm.

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Abstract

The invention relates to a method for purifying a bisphenol compound in a surface water sample extraction liquid and aims to solve the problem that the current analysis detection process of the bisphenol compound in the surface water sample extraction liquid is easily affected by a water matrix. The method comprises the steps that a composite chromatographic column is prepared, fillers of the composite chromatographic column comprise glass wool, anhydrous sodium sulfate, magnesiumtrisilicate, neutral silicone and anhydrous sodium sulfate sequentially from bottom to top, after the extraction liquid is added to a pre-leached chromatographic column, leaching is performed with a normal hexane and dichloromethane mixed solution, then eluting is performed with an acetone and dichloromethane solution, and a fully purified effect is finally realized. According to the method, the purifying treatment time can be shortened, the use amount of an elution solvent is reduced, and the cost is saved. The method is applied to the field of surface water sample purifying.

Description

technical field [0001] The invention relates to a method for purifying bisphenol compounds in surface water sample extracts. Background technique [0002] Bisphenols, (Bisphenols, BPs), are a class of substances with two hydroxyphenyl structures, and are important chemical raw materials. Bisphenol A is a precursor substance for the manufacture of polycarbonate and epoxy resin, and is mostly used in dyes, medical equipment, food packaging and lining materials. Bisphenol S (BPS) and bisphenol C (BPC) are mainly used as color fixing agent and resin flame retardant. Bisphenol B (BPB) can be used for resin coating. Bisphenol AF (BPAF) is used as a crosslinking agent for fluororubbers, and is widely used in microelectronics, optics, and space technology. Tetrabromobisphenol A (TBBPA) is a reactive flame retardant, which can be used as a flame retardant treatment agent for paper and fiber. [0003] With the increasing use of bisphenol materials, their fat solubility, bioaccumul...

Claims

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Application Information

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IPC IPC(8): G01N1/34
Inventor 陈忠林尹航
Owner HARBIN INST OF TECH
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