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Method for determining volatile components in polyvinyl alcohol in full-evaporation headspace gas chromatography

A headspace gas chromatography and polyvinyl alcohol technology, applied in the field of instrument analysis, can solve problems such as poor repeatability, difficult work, and low stability, and achieve good reproducibility of analysis data, accuracy and reliability of analysis data, and work high efficiency effect

Inactive Publication Date: 2012-06-27
HUNAN XIANGWEI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. Each measurement needs to add a solvent or a reference to the sample, which is complicated to operate
[0007] 2. Due to the addition of the solvent, it will cause some interference to the analysis, the stability is not high, and the repeatability is not good
[0008] 3. In static headspace gas chromatography, due to the presence of a solvent (or reference substance), the work of the distribution coefficient of the component i to be measured in the concentrated phase (L) and the gas phase (G) is very difficult.

Method used

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  • Method for determining volatile components in polyvinyl alcohol in full-evaporation headspace gas chromatography
  • Method for determining volatile components in polyvinyl alcohol in full-evaporation headspace gas chromatography
  • Method for determining volatile components in polyvinyl alcohol in full-evaporation headspace gas chromatography

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Effect test

Embodiment 1

[0034] The assay method of methyl alcohol in polyvinyl alcohol (PVA) resin material of the present invention

[0035] Put 0.1g to 0.5g of polyvinyl alcohol (PVA) resin material into a headspace sampler with a 20ml headspace bottle, and heat it at 120°C for 90 minutes to completely evaporate volatile components such as methanol. Analyze by gas chromatography, record the spectrum of volatile components such as methanol, and calculate the content of volatile components such as methanol by standard regression curve method.

[0036] 1. The operating conditions of the instrument are gas chromatograph: Agilent 6890 gas chromatograph (Agilent Technologies); DB-1 chromatographic column (J&W Scientific, 30m×0.45mm×2.55μm, 100% dimethyl polysiloxane); DK- Model 3001A headspace sampler (Beijing Zhongxing Institute of Analytical Instrument Technology); XS105 dual-range electronic analytical balance (METTLER TOLEDO); 20 ml headspace vials (Agilent Technologies); methanol, acetone, and methy...

Embodiment 2

[0075] Weigh 0.2235 g of the sample, accurate to 0.1 mg, place it in a 20 ml headspace vial and seal it, heat it in a headspace sampler at 120 ° C for 85 minutes, DB-1 type chromatographic column, column length 30 meters, column temperature 40 °C, FID detector, measured under the above chromatographic conditions, the peak area is 56233.6 area units. Calculated by the formula in Example 1, the methanol content in polyvinyl alcohol represented by mass percent w is 1.2498%.

Embodiment 3

[0077] Weigh 0.3936 g of the sample, accurate to 0.1 mg, place it in a 20 ml headspace vial and seal it, heat it in a headspace sampler at 115 °C for 95 minutes, DB-1 type chromatographic column, column length 30 meters, column temperature 40 °C, FID detector, measured under the above chromatographic conditions, the peak area is 76263.9 area units. Calculated by the formula in Example 1, the methanol content in polyvinyl alcohol represented by mass percent w is 1.6743%.

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Abstract

The invention relates to a method for determining volatile components in substances like polyvinyl alcohol resin, which adopts a full-evaporation headspace gas chromatography for analyzing and includes the following steps: sealing 0.1g-0.5g polyvinyl alcohol resin in a 20ml headspace bottle, placing the bottle in a headspace sample injector, heating at temperature of 115 DEG C to 125 DEG C for 85min to 95min to lead the volatile components to be evaporated totally, adopting gas chromatography for analyzing, recording a spectrogram of the volatile components, and calculating content of the volatile components through a standard regression curve. The analysis condition is that: adopting a DB-1 type chromatographic column, adopting a flame ionization detector (FID) detector with the column temperature at 40 DEG C, the detector temperature at 200 DEG C and the sampler temperature at 150 DEG C. The method is good in data repeatability and accurate and reliable in data analysis and has the advantages of being easy and convenient to operate, fast in analysis and high in sensitivity, and the volatile components in samples are good in separation effect.

Description

technical field [0001] The invention belongs to the field of instrument analysis, and relates to a method for measuring the content of volatile components in polyvinyl alcohol (PVA) resins by using the method, in particular to measuring the content of volatile components in polyvinyl alcohol (PVA). Background technique [0002] Polyvinyl Alcohol (Polyvinyl Alcohol) is a high-molecular organic compound, which is obtained by alkali-catalyzed alcoholysis of polyvinyl acetate with methanol as a solvent. It is non-toxic to the human body, has no side effects, and is non-irritating to the skin. With good water solubility and biocompatibility, it has become the world's largest water-soluble polymer with a wide range of applications. Since the solvent methanol is a poisonous and harmful substance, the residual methanol in polyvinyl alcohol affects its use, especially the export products have strict requirements on methanol content. Establish a method for the determination of methano...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/16
Inventor 曾卫国唐松乔张艳君尹飞奇李自启张艳
Owner HUNAN XIANGWEI
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