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Method for detecting phthalate ester plasticizer in plastic

A technology of phthalic acid and ester plasticizers, which can be used in measurement devices, analytical materials, solid solvent extraction, etc. The effect of fast measurement speed, reduced inspection investment and low operating cost

Inactive Publication Date: 2010-10-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

①The widespread existence of PAEs makes the measured matrix complex and diverse, which brings certain difficulties to the pretreatment of samples. Therefore, the sample pretreatment process is still the "bottleneck" step in the analysis of PAEs
② The separation and detection of isomer mixtures with a large number of carbon atoms is still a difficult point in the analysis of PAEs. The need for detection of compounds with multiple isomers

Method used

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  • Method for detecting phthalate ester plasticizer in plastic
  • Method for detecting phthalate ester plasticizer in plastic
  • Method for detecting phthalate ester plasticizer in plastic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In order to realize the rapid and sensitive detection of plasticizers in plastic products, the present invention uses ion mobility spectrometry as an analysis method, which is combined with the simple sample pretreatment technology of solvent extraction.

[0029]This method has low requirements for sample pretreatment, and can be extracted with organic solvent methanol. The specific steps are as follows: Accurately weigh 0.5g of plastic sample and place it in a test tube, add 10mL of analytically pure organic solvent methanol to extract for 0.1-2min (special material plastic products take longer), the extract can be directly used for detection and analysis.

[0030] The process of using ion mobility spectrometer to detect phthalates is as follows: extract 20-50 μL of the above extract, drop it on a clean PTFE sheet, evaporate methanol, and then insert it into the sample inlet of the instrument. The sample containing phthalates is quickly vaporized by a built-in thermal ...

Embodiment 2

[0035] Different plasticizers (phthalates) have different peak times, which can be used for qualitative analysis. Moreover, when the sample contains two or more phthalate plasticizers, it can be detected by ion mobility spectrometer at the same time, and the analysis and test method is the same as in Example 1.

[0036] image 3 Shown is the control migration spectrum of different phthalates detected by ion mobility spectrometer. The three esters shown in the figure are well detected, the characteristic peak of dibutyl phthalate is at 9.6ms, while the characteristic peak of dinonyl phthalate is at 13.1ms, and the characteristic peak of didecyl phthalate is The characteristic peak is at 13.5ms.

[0037] Figure 4 Shown is the migration spectrum of an experiment separating two phthalates. For phthalate plasticizers with different peak times, they can be detected and separated at the same time.

Embodiment 3

[0039] In life, people tend to use plastic and water more often. Therefore, the dissolution and detection of plasticizers under this condition were studied.

[0040] In life, if plastic lasts for a certain period of time in boiling water or certain plastic products are used in a microwave oven. The plasticizers in its plastic are oozing out.

[0041] The difference from Example 1 is that the sample pretreatment steps are as follows: Accurately weigh 1g of plastic sample (cut into small pieces, about 0.5mm*0.5mm in size), soak in water (10mL), heat and boil for more than 5min or Microwave treatment for 0.5-2min (or longer) to dissolve the phthalate plasticizer in the plastic sample in water, and then use an organic solvent (dichloromethane) for liquid-liquid extraction; take 20-50μL for extraction The final organic solvent is put into the injector of the ion mobility spectrometer rapid detector, and can be directly used for detection;

[0042] Figure 5 shows the plasticizer ...

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Abstract

The invention discloses a simple, fast and sensitive method for detecting a plasticizer (phthalate ester) in plastic, which is based on ion mobility spectrometry and detects phthalate ester in an extracting solution using a fast ion mobility spectrometry detector in combination with a simple organic solvent extraction pretreatment method. The measurement method is simple, fast and reliable. The analysis time of the method is only 0.5min, the requirement on a sample pretreatment is low, the detection time is short, the sensitivity is high, and the detection limit can be up to 1ppb.

Description

technical field [0001] The present invention relates to the detection method of plasticizer (being phthalates) in plastics, specifically a kind of new quick, the method for sensitive detection phthalates, this method uses ion mobility spectrometry technology Based on this, using the ion mobility spectrometer fast detector as the analysis method, and adopting simple (low requirement) sample pretreatment and extraction technology, the detection limit can reach 1ppb. The speed is fast, the analysis time is only 0.5min, and the test operation is simple, no special professional background personnel are required to operate. Background technique [0002] Phthalic acid esters (Phthalic Acid Esters, referred to as PAEs, alias phthalates) is an important class of organic compounds. Generally, it is a colorless and transparent oily liquid, insoluble in water but easily soluble in methanol and ethanol. The common ones are dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl p...

Claims

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Application Information

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IPC IPC(8): G01N27/62B01D11/02G01N27/622
Inventor 李海洋王新仓怀文王卫国侯可勇李林鞠帮玉王海龙王祯鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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