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Method for quickly detecting low-molecular chlorinated organic compounds in papermaking white water, and application

A technology for chlorinated organic matter and white water for papermaking, which is applied in measurement devices, material separation, and analysis of materials, etc., can solve the problems of large interference of white water matrix, cumbersome and time-consuming operation, large solvent consumption, etc., and achieves low detection limit and rapid analysis. , the effect of easy operation

Active Publication Date: 2018-12-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the content of low-molecular chlorinated organics in papermaking white water is generally low, and the white water matrix interferes greatly, traditional liquid-liquid extraction, solid-phase extraction and other methods need to be enriched and concentrated with large volumes of white water (500-1000ml) to ensure When the detection limit is reached, there is a large amount of solvent consumption in the pretreatment process (100-300ml organic reagent is required for liquid-liquid extraction), and the operation is cumbersome and time-consuming (it takes about 8 hours for each sample to go through extraction, enrichment, concentration and other steps). Greatly restricts the development of related testing and research work

Method used

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  • Method for quickly detecting low-molecular chlorinated organic compounds in papermaking white water, and application
  • Method for quickly detecting low-molecular chlorinated organic compounds in papermaking white water, and application
  • Method for quickly detecting low-molecular chlorinated organic compounds in papermaking white water, and application

Examples

Experimental program
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Effect test

Embodiment 1

[0047]A rapid assay method for low-molecular chlorinated organics in papermaking white water, comprising the following steps:

[0048] (1) Pretreatment of samples to be tested

[0049] The paper-making white water to be tested was filtered with medium-speed qualitative filter paper to remove suspended matter, and then 5 grams of paper-making white water and 2.1 g of NaCl were accurately weighed in a 20ml headspace bottle at 40°C for 1 hour.

[0050] (2) Solid phase microextraction (SPME)

[0051] Perform aging treatment on the solid-phase microextraction fiber head: place the 85 μm polyacrylate (Polyacrylate) extraction head in the GC (gas chromatography) inlet for aging for 15 minutes at a temperature of 250 ° C to remove surface residues; then step (1) Insert the well-balanced sample into the headspace bottle with the aged solid-phase microextraction fiber head (polyacrylate extraction head), and push out the headspace extraction sample of the solid-phase microextraction fi...

Embodiment 2

[0067] Detect according to the method of Example 1, the difference is: the time of solid phase microextraction (SPME) in step (2) is 10, 20, 30, 40, 50, 60min. Its detection signal is as Figure 4 shown. In the SPME process, the extraction time is generally increased to ensure the maximum volatilization of volatile substances into the headspace to improve the detection sensitivity, but by Figure 4 It can be seen that after 40 minutes, the sensitivity of 1,2,3-trichloropropane decreased significantly, while DCP gradually increased, which is the performance of adsorption competition. In order to ensure the accurate detection of the two substances, the optimal extraction time was 40 minutes.

Embodiment 3

[0069] Detect according to the method of Example 1, the difference is: the quality of NaCl added during the pretreatment of the sample to be tested in step (1) is 0.3, 0.6, 0.9, 1.2, 1.5, 1.8, 2.1 grams. Its detection signal is as Figure 5 shown. The ionic effect will reduce the solubility of substances in water, and the addition of salts containing chlorine will increase the volatility of chlorinated organic compounds. Depend on Figure 5 It can be seen that the addition of NaCl significantly increases the sensitivity of the two substances to be detected, therefore, the detection sensitivity of low-molecular chlorinated organic compounds in white water can be improved by adding NaCl.

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Abstract

The invention discloses a method for quickly detecting low-molecular chlorinated organic compounds in papermaking white water, and application. The method comprises the following steps that: (1) the preprocessing of a sample to be detected: filtering papermaking white water of a water sample to be detected, and adding chloride salt to obtain a sample to be tested; (2) standard solution preparation: adding 1,3-dichloro-2-propyl alcohol and 1,2,3-trichloropropane into the papermaking white water to prepare standard solutions of at least five concentrations; and (3) solid phase microextraction-gas chromatography-mass spectrometry detection: independently adopting a headspace solid-phase microextraction way to extract the sample to be detected and the standard solutions in the (2), inserting an extraction head into the sample introduction hole of gas chromatography-mass spectrometry to carry out desorption, and carrying out gas chromatography-mass spectrometry measurement to calculate thecontents of 1,3-dichloro-2-propyl alcohol and 1,2,3-trichloropropane in the sample. The method disclosed by the invention has the advantages of being simple, efficient and sensitive in operation, highin recovery rate and low in cost and is suitable for analyzing volatile chlorinated organic compounds in the papermaking white water.

Description

technical field [0001] The invention belongs to the field of detection of toxic substances in papermaking chemicals, in particular to a method and application for rapidly detecting low-molecular chlorinated organic substances in papermaking white water. Background technique [0002] Polyamide epichlorohydrin resin (referred to as PAE resin) as a humidifying agent has the advantages of good humidifying effect, no formaldehyde, less dosage, suitable for medium-alkaline papermaking, etc., and is widely used in the paper industry. With the improvement of people's living standards, the demand for high wet strength paper is becoming stronger and stronger, so PAE resin is widely used in the papermaking process. However, in the current existing technology, some by-products will be produced in the process of producing PAE, and these by-products are produced by the hydrolysis of epichlorohydrin to generate small molecule chlorinated organic compounds. When PAEs are used in the paperm...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 武书彬魏琪陈春霞赵媛媛马浩宋飞宇
Owner SOUTH CHINA UNIV OF TECH
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