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Detection method for content of short-chain chlorinated paraffin in leather

A short-chain chlorinated paraffin and detection method technology, applied in the field of analysis and testing, can solve the problems of high detection cost, expensive instruments with mass spectrometers, and inability to eliminate serious interference, and achieve the effect of simple quantification and elimination of interference

Inactive Publication Date: 2017-05-10
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

While these methods have individual applicability due to differences in sample matrices, they are not universal
Moreover, instruments with mass spectrometers are more expensive, resulting in higher detection costs
The more important problem is that the above method cannot eliminate the serious interference of the sample matrix and medium-chain chlorinated paraffin (MCCP) on SCCP during instrumental analysis, especially for the analysis of leather samples with complex matrix, it is difficult to obtain accurate detection results

Method used

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  • Detection method for content of short-chain chlorinated paraffin in leather

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Embodiment 1

[0030] Embodiment 1: the detection of short-chain chlorinated paraffin content in leather

[0031] (1) Sample extraction

[0032] Accurately weigh 2g of shredded (about 2mm×2mm) leather samples, mix with about 2g of anhydrous sodium sulfate, add to a 100ml stoppered conical flask, add 25ml of chromatographically pure hexane; At ~45°C, carry out ultrasonic extraction (40Hz), the extraction time is more than 30min; wash the residue with 2×10ml n-hexane, combine the n-hexane extract, and filter it into a 100ml pear-shaped flask with a 0.45μm filter membrane, and then put The solution was concentrated by rotary evaporation to ~10 ml.

[0033] (2) Solid phase extraction purification

[0034] Inject the concentrated extract into a solid-phase extraction column (capacity is 6ml, the upper layer filler is florisil, the lower layer filler is silica gel, both are 500mg), the liquid flows out naturally, discards the effluent, and divides it with 10ml n-hexane Rinse the column twice, dis...

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Abstract

The invention discloses a detection method for a content of short-chain chlorinated paraffin in leather, which relates to the field of analysis and test. The detection method comprises the following steps: extracting a sample, solid-phase extracting and purifying, online catalyzing with palladium and detecting in a gas-phase chromatography, comparing with a standard working curve, and obtaining a concentration value of the short-chain chlorinated paraffin in the sample. Compared with the existing test method, the detection method is high in resistance to the interference of sample impurities, simple and convenient in operation and accurate in quantification, and can rapidly and accurately detect the content of the short-chain chlorinated paraffin in the leather without using an expensive mass spectrometer.

Description

[0001] 【Technical field】 [0002] The invention belongs to the field of analysis and testing, in particular to a detection method for short-chain chlorinated paraffins (English abbreviation is SCCP), especially for the detection of SCCP content in leather. [0003] 【Background technique】 [0004] SCCP is a by-product in the synthesis process of chlorinated paraffin, which exists with chlorinated paraffin, and it is currently impossible to separate it from chlorinated paraffin. In the leather industry, chlorinated paraffin is often used as a kind of oil. Because it has a function similar to "hoof oil fatliquor", which can give leather a good feel and performance, chlorinated paraffin is also called "synthetic hoof oil" and is widely used in leather making. This also results in SCCPs that may be present in the chlorinated paraffins remaining in the leather. [0005] Studies have confirmed that SCCP is refractory, bioaccumulative and biotoxic, and is identified as a persistent p...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14G01N30/68
CPCG01N30/06G01N30/14G01N30/68G01N2030/062
Inventor 马贺伟罗建勋
Owner JIAXING UNIV