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Method for Determination of Residual Organic Matter in PVC Paste Resin

A method of determination and technology of organic matter, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of high sensitivity, uniform distribution of peaks, and less time-consuming

Active Publication Date: 2017-04-26
山东朗晖石油化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are no relevant literature and reports on the determination method of residual organic matter in PVC paste resin

Method used

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  • Method for Determination of Residual Organic Matter in PVC Paste Resin
  • Method for Determination of Residual Organic Matter in PVC Paste Resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The determination method of residual organic matter in PVC paste resin is as follows:

[0030] Extraction and distillation of PVC paste resin samples:

[0031] Weigh 12±0.05g sample, accurate to 0.001g, the Soxhlet extractor has a capacity of 100mL and a 250mL single-neck flask; wrap the sample with filter paper, put a layer of absorbent cotton at the bottom of the extractor, and then wrap the filter paper Add 3-4 pieces of clean zeolite to the cleaned flask, then add 200mL of absolute ethanol, connect the flask to the extractor and place it on an electric heating mantle for heating; start the extraction and adjust the reflux speed to make the extraction cylinder The collected ethanol is discharged at least six times per hour, start timing after the first discharge of the extract, extract to 6h±10min, pour the ethanol in the extractor into the flask, connect the flask to the distillation device for distillation, and distill to the flask About 10 mL of ethanol remained ...

Embodiment 2

[0033] Chromatographic analysis was used to determine the residual organic content:

[0034] 1. Instruments and reagents

[0035] Gas Chromatograph: Agilent 7820A.

[0036] Chromatographic column: OV-17 capillary column; length 30m, diameter 0.32mm, film thickness 0.33μm;

[0037] Carrier gas: 99.99% high-purity hydrogen, 99.99% high-purity nitrogen;

[0038] Injector: temperature 250℃;

[0039] Detector: hydrogen flame detector FID, the temperature is 300 ℃;

[0040] Injection volume: 0.4 μL;

[0041] Column temperature program heating: the initial temperature is 120 °C for 1 min, the temperature is increased to 270 °C at a rate of 6 °C / min, and the temperature is maintained for 20 min; the column temperature is 270 °C;

[0042] Split ratio: 10:1;

[0043] Chromatographic gas flow: hydrogen flow: 40ml / min; nitrogen flow: 10ml / min; makeup flow: 25ml / min; air flow: 300ml / min.

[0044] 2. Quantitative and qualitative method: Because the main substances in the sample are a...

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Abstract

The invention relates to a determination method for residual organic matter of PVC paste resin, and belongs to the technical field of chemical content determination methods. The determination method comprises the steps that extraction and distillation are performed on a PVC paste resin sample to obtain the residual organic matter, and then the content of the residual organic matter is determined by adopting chromatographic analysis. The chromatographic conditions are as follows: a chromatographic column serves as a chromatographic column; 99.99% high-purity hydrogen and 99.99% high-purity nitrogen serve as carrier gas; the temperature of a sample injector is set as 250 DEG C; a hydrogen flame detector serves as a detector, and the temperature of the hydrogen flame detector is set as 300 DEG C; the injection volume is 0.4 microliter; temperature programming is performed on the column temperature, wherein the initial temperature is set as 120 DEG C and maintained for 20 min, and the temperature rises to 270 DEG C at the rate of 6 DEG C / min and maintained for 20 min; the split ration is 10:1; chromatographic gas flow is set, wherein the hydrogen flow is set as 40 ml / min, the nitrogen flow is set as 10 ml / min, the tail blowing flow is set as 25 ml / min, and the air flow is set as 300 ml / min. According to the determination method, the advantages of being high in efficiency, good in selectiveness, high in sensitivity, easy to operate, even in peak distribution, good in effect and short in time are achieved, and the components of PVC paste resin emulsifiers of different brands can be analyzed quantitatively.

Description

technical field [0001] The invention relates to a method for measuring the residual organic matter of PVC paste resin, and belongs to the technical field of chemical content measuring methods. Background technique [0002] There are many different grades of PVC paste resin in the prior art, and different grades of PVC paste resin are developed to meet the different needs of customers, and their products have different properties and have a greater impact on PVC production. Therefore, studying the composition of different grades of PVC paste resin has guiding significance for production. [0003] The main substances of the emulsifier in the PVC paste resin sample are alcohols with different alkyl groups. By processing the PVC paste resin sample, residual organic substances can be obtained, and then the composition of the emulsifier can be determined. The composition of emulsifier is also the main core technology of PVC paste resin production. Therefore, it is very important...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 李艳申洪达褚秀娟
Owner 山东朗晖石油化学股份有限公司