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Determination method for short-chain chlorinated paraffin in high molecular material

A technology of short-chain chlorinated paraffin and polymer materials, which is applied in the directions of analysis materials, material separation, measuring devices, etc., can solve the problems of inaccurate detection, incomplete separation, interference analysis, etc., and achieves high detection accuracy and improved accuracy. The effect of improving the extraction yield

Inactive Publication Date: 2018-07-06
通标标准技术服务(天津)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many analytical methods for short-chain chlorinated paraffins, such as high-resolution gas chromatography and high / low-resolution mass spectrometry, comprehensive two-dimensional gas chromatography-fast scanning quadrupole mass spectrometry, high performance liquid chromatography-chlorine enhanced atmospheric pressure chemistry Ionization ion trap mass spectrometry, but because the short-chain chlorinated paraffins in the polymer materials only account for a small part, and the main components of the polymer materials are polyethylene, polyvinyl chloride and other additives such as stabilizers, lubricants, etc. due to pre-treatment separation Incomplete, it will interfere with the analysis of short-chain chlorinated paraffins in the later detection process, making the detection inaccurate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Determination methods for short-chain chlorinated paraffins in polymer materials, including:

[0032] Step 1. Soak 0.5g of polymer material in the cleaning solution, place it together with the cleaning solution in an ultrasonic wave with a frequency of 120KHz for 40min, then take out the polymer material and rinse it with pure water for 1min, wherein the cleaning solution is composed of 0.05g of alkyl Prepared by mixing sodium benzenesulfonate, 0.1g sodium fatty alcohol sulfate, 2g apple juice, 0.05g sodium tripolyphosphate, and 10g pure water;

[0033] Step 2. Melt the polymer material treated in step 1, then add 10mL of n-hexane, and irradiate it under ultraviolet light for 10 minutes, then place it in a water bath constant temperature oscillator and shake it at 50°C and 150rpm for 60min, then place it at 40°C Under the condition of water bath for 30min, perform the first centrifugation to take the supernatant and precipitate, add 10mL n-hexane to the precipitate, and...

Embodiment 2

[0048] Determination methods for short-chain chlorinated paraffins in polymer materials, including:

[0049] Step 1. Soak 2g of the polymer material in the cleaning solution, and place it together with the cleaning solution in an ultrasonic wave with a frequency of 120KHz for 40min, then take out the polymer material and rinse it with pure water for 1min, wherein the cleaning solution consists of 0.05g of alkylbenzene Sodium sulfonate, 0.1g fatty alcohol sodium sulfate, 2g apple juice, 0.05g sodium tripolyphosphate, and 10g pure water are uniformly mixed;

[0050] Step 2. Melt the polymer material treated in step 1, then add 30mL of n-hexane, and irradiate it under ultraviolet light for 10 minutes, then place it in a water bath constant temperature oscillator and shake it at 50°C and 150rpm for 60min, then place it at 40°C Under the condition of water bath for 30min, perform the first centrifugation to take the supernatant and precipitate, add 30mL of n-hexane to the precipita...

Embodiment 3

[0065] Determination methods for short-chain chlorinated paraffins in polymer materials, including:

[0066] Step 1. Soak 1g of the polymer material in the cleaning solution, place it together with the cleaning solution in an ultrasonic wave with a frequency of 120KHz for 40min, then take out the polymer material and rinse it with pure water for 1min, wherein the cleaning solution is made of 0.05g of alkylbenzene Sodium sulfonate, 0.1g fatty alcohol sodium sulfate, 2g apple juice, 0.05g sodium tripolyphosphate, and 10g pure water are uniformly mixed;

[0067] Step 2. Melt the polymer material treated in step 1, then add 20mL of n-hexane, and irradiate it under ultraviolet light for 10 minutes, then place it in a water bath constant temperature oscillator and vibrate for 60 minutes at 50°C and 150rpm, and then oscillate at 40°C Under the condition of water bath for 30min, perform the first centrifugation to take the supernatant and precipitate, add 20mL n-hexane to the precipit...

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Abstract

The invention discloses a determination method for short-chain chlorinated paraffin in a high molecular material. The determination method comprises the following steps: step 1, immersing the high molecular material in a cleaning solution and carrying out ultrasonic treatment and washing in sequence, wherein the cleaning solution is prepared by mixing sodium alkyl benzene sulfonate, sodium aliphatic alcohol sulfate, apple juice, sodium tripolyphosphate and pure water; step 2, smelting the high molecular material and adding n-hexane; carrying out ultraviolet irradiation, oscillation, water-bathtreatment and centrifuging in sequence; taking supernatant and carrying out blowing drying by adopting nitrogen gas to obtain powder; step 3, carrying out magnetic field treatment and infrared irradiation on the powder; then adding the n-hexane for dissolving and making the volume constant; adding into a filtering column and eluting with an eluting agent; collecting an eluting solution; step 4, carrying out the blowing drying on the eluting solution to obtain powder; dissolving the powder with the n-hexane and making the volume constant; then feeding into a chromatographic column from a sample inlet of a metastable-state atomic bombardment high-resolution mass spectrometer and carrying out mass spectrometric detection. The determination method disclosed by the invention has the beneficialeffects of high detection accuracy and wide detection range.

Description

technical field [0001] The invention relates to the field of determination of short-chain chlorinated paraffins. More specifically, the present invention relates to a method for determining short-chain chlorinated paraffins in polymer materials. Background technique [0002] Chlorinated paraffin is a polychlorinated long-chain normal alkanes, the chain length can vary from C10 to C30, and the chlorine content is between 30wt% and 70wt%. Short-chain chlorinated paraffins are a class of organic substances with persistence, bioaccumulation, toxicity and long-distance migration, which are harmful to the environment and human health. Their ecological risks in the environment have attracted the attention of the World Health Organization and Environmental Research attention. SCCPs are commonly used as flame retardants for textiles, rubber and plastics, leather treatments, plasticizers for paints and other coatings, and metalworking oil additives. [0003] At present, there are m...

Claims

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Application Information

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IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/062
Inventor 刘潇
Owner 通标标准技术服务(天津)有限公司
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