CN104535681A - Method for measuring short chain chlorinated paraffin in high polymer material - Google Patents
Method for measuring short chain chlorinated paraffin in high polymer material Download PDFInfo
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- CN104535681A CN104535681A CN201410824636.8A CN201410824636A CN104535681A CN 104535681 A CN104535681 A CN 104535681A CN 201410824636 A CN201410824636 A CN 201410824636A CN 104535681 A CN104535681 A CN 104535681A
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Abstract
The present invention relates to the field of measurement of short chain chlorinated paraffin and particularly relates to a method for measuring short chain chlorinated paraffin in a high polymer material. The method comprises the following steps: dedusting the high polymer material; shearing the dedusted high polymer material into pieces, putting the pieces in a round-bottom flask, and heating the pieces to a molten state; pouring the molten high polymer material into a first reaction container, adding cyclohexanone in twice, oscillating and filtering; adding mixed liquor of ethyl acetate and amyl acetate into a second reactor, oscillating and filtering; adding mixed liquor of acetone/normal hexane/ dichloromethane with a volume ratio of 1:2:1, and oscillating and concentrating the mixed liquor in an ultrasonic oscillator; spraying the concentrated solution onto a chromatographic column, leaching and receiving eluant; feeding the eluant into a chromatographic column from the sample feed opening of a metastable atom bombardment high-resolution mass spectrometer to realize mass spectrometric detection. According to the invention, the main components and the added components in the high polymer material are fully separated to improve the detection efficiency and accuracy of the short chain chlorinated paraffin.
Description
Technical field
The present invention relates to the mensuration field of short chain chlorinated paraffin, particularly relate to the assay method of short chain chlorinated paraffin in a kind of macromolecular material.
Background technology
Chlorinated paraffin is a kind of long-chain normal paraffin of many chloros, and chain length can change from C10 to C30, and chlorinty is between 30wt%-70wt%.According to the difference of chain length, chlorinated paraffin can be divided into short chain (C10-C13), medium chain (C14-C17) and long-chain (C18-C30) chlorinated paraffin.Short chain chlorinated paraffin, also claims short chain chlorination n-alkane, is again kelene, chloralkane, chlorinated paraffin.Short chain chlorinated paraffin is positive paraffin, and its carbon chain lengths is 10 ~ 13 carbon atoms, and by weight, chlorination degree is about 16% ~ 78%, and its molecular formula is CxH (2x-y+2) Cly, wherein, and x=10 ~ 13, y=1 ~ 13.Molecular weight is 320 ~ 500.Short chain chlorinated paraffin is the organism that a class has persistence, bioconcentration, toxicity and remote transfer ability, has harmfulness to environmental and human health impacts, and its ecological risk has in the environment caused the attention of the World Health Organization (WHO) and Environmental Studies person.The use in the cable of short chain chlorinated paraffin is the most extensive, is also usually used in manufacturing water pipe, floor, film, leatheret, macromolecular material and commodity etc.The short chain chlorinated paraffin of 65 ~ 70% is mainly used as fire retardant, used in combination in tygon, polystyrene with antimony oxide.In addition, short chain chlorinated paraffin is also used as the plasticiser of textile, rubber and flame retardant of plastic agent, leather treatment, paint and other coating, and intermetallic composite coating oil additive.
Analytical approach at present for short chain chlorinated paraffin has a lot, as high-resolution gas chromatography and high/low Resolution Mass Spectrometry coupling technique, comprehensive two dimensional gas chromatography-rapid scanning level Four bar mass spectrum, high performance liquid chromatography-chlorine strengthen Atmosphere Pressure Chemical Ionization (APCI) ion trap mass spectrometry, but because in macromolecular material, short chain chlorinated paraffin just accounts for little part, and principal ingredient tygon, Polyvinylchloride and other adjuvants are as not thorough because process in early stage is separated in stabilizing agent, lubricant etc. in macromolecular material, the analysis of short chain chlorinated paraffin can be disturbed in late detection process.
Summary of the invention
For above-mentioned technical matters, the present invention has designed and developed the assay method of short chain chlorinated paraffin in a kind of macromolecular material, and object is fully to be separated the principal ingredient in macromolecular material and adding ingredient, improves detection efficiency and the accuracy of short chain chlorinated paraffin.
Technical scheme provided by the invention is:
An assay method for short chain chlorinated paraffin in macromolecular material, comprising:
Step one, dedusting is carried out to macromolecular material, to remove the dirt of polymer surface;
Step 2, the macromolecular material after dedusting is cut into area is 0.2 ~ 0.5cm
2small pieces, take 2 ~ 3g small pieces and be placed in round-bottomed flask, be heated to molten condition, be conducive to dissolving each other with solvent; The macromolecular material of melting is poured in the first reaction vessel, add the cyclohexanone of 20 ~ 30mL, described first reaction vessel is put the 10 ~ 15min that vibrates on the oscillator, by the first extract by after filter paper that anhydrous sodium sulfate is housed, extract once with the cyclohexanone of 10 ~ 15mL and be filled in the second reaction vessel again, twice cyclohexanone dissolution extraction, makes the Polyvinylchloride in macromolecular material dissolve, and vibration accelerates the rate of dissolution of Polyvinylchloride; The volume ratio adding 10 ~ 15mL in described second reaction vessel is ethyl acetate and the pentyl acetate mixed liquor of 1: 2, described second reaction vessel is put the 20 ~ 30min that vibrates on the oscillator, by the second extract by being equipped with the filter paper of anhydrous sodium sulfate, be filled in flat bottom flask, stabilizing agent stearate, epoxy resin and lubricant stearic acid in macromolecular material and calcium magnesium salts thereof are by acetic acid ethyl dissolution, and tygon is dissolved by pentyl acetate; Mixed liquor 100 ~ 120mL that volume ratio is the acetone/normal hexane/methylene chloride of 1: 2: 1 is added in described flat bottom flask, and be placed in supersonic oscillations instrument vibration 60 ~ 70min, filtrate is concentrated into 5 ~ 8mL with Rotary Evaporators, and the mixing extraction agent of acetone/normal hexane/methylene chloride is more conducive to the abundant dissolving of chlorinated paraffin;
Step 3, by the concentrate through step 2 process by being filled with the chromatographic column of alkali alumina, neutral silica gel, acidic silica gel and anhydrous sodium sulfate from top to bottom successively, first use 30mL eluent methylene chloride, then the drip washing of 40mL normal hexane is used, by volume ratio be the mixed liquor 80mL drip washing of the acetone/normal hexane/methylene chloride of 1: 1: 1 again and access eluent, in concentrate, remaining other compositions a small amount of are fully adsorbed through chromatographic column;
Step 4, the injection port of the eluent of step 3 through metastable atom bombardment high-resolution mass spectrometer is entered in chromatographic column and carry out Mass Spectrometer Method, obtain the content of each concrete material in short chain chlorinated paraffin in macromolecular material.
Preferably, in described macromolecular material short chain chlorinated paraffin assay method in, the testing conditions of the metastable atom bombardment high-resolution mass spectrometer adopted in described step 4 is: injector temperature 150 ~ 180 DEG C, flow rate of carrier gas is 3 ~ 5mL/min, and interface temperature is 200 ~ 220 DEG C.
Preferably, in described macromolecular material short chain chlorinated paraffin assay method in, after described sample enters chromatographic column from injection port, carry out temperature programme, 120 ~ 130 DEG C keep 10 ~ 15min, are warming up to 200 ~ 220 DEG C with the speed of 15 ~ 20 DEG C/min, keep 5 ~ 8min; Then be warming up to 280 ~ 300 DEG C with the speed of 25 ~ 30 DEG C/min, keep 20 ~ 30min, adopt gradient increased temperature to be more conducive to the separation of each composition in macromolecular material.
Preferably, in described macromolecular material short chain chlorinated paraffin assay method in, in described step one, macromolecular material is placed in clear water and soaks 20 ~ 40min, and with the dust of polymer surface described in hairbrush outwash and dirt, avoid contaminating impurity.
Preferably, in described macromolecular material short chain chlorinated paraffin assay method in, the macromolecular material in described step 2 after dedusting is heated to 150 ~ 180 DEG C in molten condition, and high temperature is conducive to dissolving each other of macromolecular material and solvent.
Preferably, in described macromolecular material short chain chlorinated paraffin assay method in, be filled with 20 ~ 30g alkali alumina, 10 ~ 12g neutral silica gel, 25 ~ 35g acidic silica gel and 2 ~ 5g anhydrous sodium sulfate in described step 3 chromatographic column, the composition in concentrate is by adsorptive separation successively.
Preferably, in described macromolecular material short chain chlorinated paraffin assay method in, be filled with 25g alkali alumina, 12g neutral silica gel, 30g acidic silica gel and 3g anhydrous sodium sulfate in described step 3 chromatographic column.
Preferably, in described macromolecular material short chain chlorinated paraffin assay method in, described macromolecular material is plastics, rubber or textile material.
In macromolecular material of the present invention short chain chlorinated paraffin assay method in, be heated to molten condition by the macromolecular material after dedusting, to be conducive to various composition in macromolecular material and organic solvent fully dissolves each other.First in fused solution, cyclohexanone is added at twice, so that the principal ingredient Polyvinylchloride in macromolecular material is fully dissolved, then in filtered fluid, add the mixed liquor of ethyl acetate and pentyl acetate, stabilizing agent in macromolecular material and lubricant are by acetic acid ethyl dissolution, tygon is dissolved by pentyl acetate, most of composition in such macromolecular material except chlorinated paraffin is all dissolved, again with the mixed liquor extraction chlorinated paraffin of acetone/normal hexane/methylene chloride, effectively avoid being mixed into of other compositions, improve the percentage extraction of chlorinated paraffin, thus be conducive to follow-up analysis detection.And be separated through chromatographic column again before detected liquid sample introduction, the mixed liquor drip washing respectively of methylene chloride, normal hexane and acetone/normal hexane/methylene chloride, eliminates other compositions in eluent further, avoids the interference of the close composition of late detection middle-molecular-weihydroxyethyl.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the assay method of short chain chlorinated paraffin in macromolecular material of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail, can implement according to this with reference to instructions word to make those skilled in the art.
Embodiment 1
The invention provides the assay method of short chain chlorinated paraffin in a kind of macromolecular material, comprising:
Step one, dedusting is carried out to plastics to be detected, plastics to be detected are placed in clear water and soak 20min, and with the dust of frosting to be detected described in hairbrush outwash and dirt.
Step 2, the plastics to be detected after dedusting are cut into area is 0.2cm
2small pieces, take 2g small pieces and be placed in round-bottomed flask, be heated to 150 DEG C in molten condition; The plastics to be detected of melting are poured in the first reaction vessel, add the cyclohexanone of 20mL, described first reaction vessel is put the 10min that vibrates on the oscillator, by the first extract by after filter paper that anhydrous sodium sulfate is housed, then with the cyclohexanone extraction of 10mL once and be filled in the second reaction vessel; The volume ratio adding 10mL in described second reaction vessel is ethyl acetate and the pentyl acetate mixed liquor of 1: 2, described second reaction vessel is put the 20min that vibrates on the oscillator, by the second extract by being equipped with the filter paper of anhydrous sodium sulfate, be filled in flat bottom flask; In described flat bottom flask, add the mixed liquor 100mL that volume ratio is the acetone/normal hexane/methylene chloride of 1: 2: 1, and be placed in supersonic oscillations instrument and vibrate 60min, filtrate is concentrated into 5mL with Rotary Evaporators.
Step 3, by the concentrate through step 2 process by being filled with the chromatographic column of 25g alkali alumina, 12g neutral silica gel, 30g acidic silica gel and 3g anhydrous sodium sulfate from top to bottom successively, first use 30mL eluent methylene chloride, then use the drip washing of 40mL normal hexane, then by volume ratio be 1: 1: 1 acetone/normal hexane/methylene chloride mixed liquor 80mL drip washing and access eluent.
Step 4, the injection port of the eluent of step 3 through metastable atom bombardment high-resolution mass spectrometer is entered in chromatographic column and carry out Mass Spectrometer Method.Testing conditions is: injector temperature 150 DEG C, and flow rate of carrier gas is 3mL/min, and interface temperature is 200 DEG C, after described sample enters chromatographic column from injection port, carries out temperature programme, and 120 DEG C keep 10min, are warming up to 200 DEG C with the speed of 15 DEG C/min, keep 5min; Then be warming up to 280 DEG C with the speed of 25 DEG C/min, keep 20min.
The content (unit ng/g) of each concrete material in short chain chlorinated paraffin in the plastics that table 1 is to be detected
| C 10H 17Cl 5 | 0.01 | C 11H 19Cl 5 | 0.05 | C 12H 21Cl 5 | 0.02 | C 13H 23Cl 5 | 0.21 |
| C 10H 16Cl 6 | 0.08 | C 11H 18Cl 6 | 0.69 | C 12H 20Cl 6 | 0.57 | C 13H 22Cl 6 | 0.47 |
| C 10H 15Cl 7 | 0.99 | C 11H 17Cl 7 | 6.26 | C 12H 19Cl 7 | 5.31 | C 13H 21Cl 7 | 2.98 |
| C 10H 14Cl 8 | 1.67 | C 11H 16Cl 8 | 12.84 | C 12H 18Cl 8 | 13.76 | C 13H 20Cl 8 | 8.39 |
| C 10H 13Cl 9 | 0.73 | C 11H 15Cl 9 | 6.75 | C 12H 17Cl 9 | 7.25 | C 13H 19Cl 9 | 11.76 |
| C 10H 12Cl 10 | 0.61 | C 11H 14Cl 10 | 2.17 | C 12H 16Cl 10 | 3.62 | C 13H 18Cl 10 | 8.71 |
Embodiment 2
The invention provides the assay method of short chain chlorinated paraffin in a kind of macromolecular material, comprising:
Step one, dedusting is carried out to rubber to be detected, rubber to be detected is placed in clear water and soaks 40min, and with the dust of rubber surface to be detected described in hairbrush outwash and dirt.
Step 2, the rubber to be detected after dedusting is cut into area is 0.5cm
2small pieces, take 3g small pieces and be placed in round-bottomed flask, be heated to 180 DEG C in molten condition; The rubber to be detected of melting is poured in the first reaction vessel, add the cyclohexanone of 30mL, described first reaction vessel is put the 15min that vibrates on the oscillator, by the first extract by after filter paper that anhydrous sodium sulfate is housed, then with the cyclohexanone extraction of 15mL once and be filled in the second reaction vessel; The volume ratio adding 15mL in described second reaction vessel is ethyl acetate and the pentyl acetate mixed liquor of 1: 2, described second reaction vessel is put the 30min that vibrates on the oscillator, by the second extract by being equipped with the filter paper of anhydrous sodium sulfate, be filled in flat bottom flask; In described flat bottom flask, add the mixed liquor 120mL that volume ratio is the acetone/normal hexane/methylene chloride of 1: 2: 1, and be placed in supersonic oscillations instrument and vibrate 70min, filtrate is concentrated into 8mL with Rotary Evaporators.
Step 3, by the concentrate through step 2 process by being filled with the chromatographic column of 30g alkali alumina, 10g neutral silica gel, 35g acidic silica gel and 5g anhydrous sodium sulfate from top to bottom successively, first use 30mL eluent methylene chloride, then use the drip washing of 40mL normal hexane, then by volume ratio be 1: 1: 1 acetone/normal hexane/methylene chloride mixed liquor 80mL drip washing and access eluent.
Step 4, the injection port of the eluent of step 3 through metastable atom bombardment high-resolution mass spectrometer is entered in chromatographic column and carry out Mass Spectrometer Method.Testing conditions is: injector temperature 180 DEG C, and flow rate of carrier gas is 5mL/min, and interface temperature is 220 DEG C, after described sample enters chromatographic column from injection port, carries out temperature programme, and 130 DEG C keep 15min, are warming up to 220 DEG C with the speed of 20 DEG C/min, keep 8min; Then be warming up to 300 DEG C with the speed of 30 DEG C/min, keep 30min.
The content (unit ng/g) of each concrete material in short chain chlorinated paraffin in the rubber that table 2 is to be detected
| C 10H 17Cl 5 | 0.02 | C 11H 19Cl 5 | 0.06 | C 12H 21Cl 5 | 0.01 | C 13H 23C1 5 | 0.22 |
| C 10H 16Cl 6 | 0.09 | C 11H 18Cl 6 | 0.67 | C 12H 20Cl 6 | 0.63 | C 13H 22Cl 6 | 0.45 |
| C 10H 15Cl 7 | 0.87 | C 11H 17Cl 7 | 6.38 | C 12H 19Cl 7 | 5.29 | C 13H 21Cl 7 | 2.87 |
| C 10H 14Cl 8 | 1.91 | C 11H 16Cl 8 | 12.89 | C 12H 18Cl 8 | 13.84 | C 13H 20Cl 8 | 8.44 |
| C 10H 13Cl 9 | 0.68 | C 11H 15Cl 9 | 6.74 | C 12H 17Cl 9 | 7.43 | C 13H 19Cl 9 | 11.89 |
| C 10H 12Cl 10 | 0.64 | C 11H 14Cl 10 | 2.15 | C 12H 16Cl 10 | 3.57 | C 13H 18Cl 10 | 8.73 |
Although embodiment of the present invention are open as above, but it is not restricted to listed in instructions and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (8)
1. the assay method of short chain chlorinated paraffin in macromolecular material, is characterized in that, comprising:
Step one, dedusting is carried out to macromolecular material;
Step 2, the macromolecular material after dedusting is cut into area is 0.2 ~ 0.5cm
2small pieces, take 2 ~ 3g small pieces and be placed in round-bottomed flask, be heated to molten condition; The macromolecular material of melting is poured in the first reaction vessel, add the cyclohexanone of 20 ~ 30mL, described first reaction vessel is put the 10 ~ 15min that vibrates on the oscillator, by the first extract by after filter paper that anhydrous sodium sulfate is housed, then with the cyclohexanone extraction of 10 ~ 15mL once and be filled in the second reaction vessel; The volume ratio adding 10 ~ 15mL in described second reaction vessel is ethyl acetate and the pentyl acetate mixed liquor of 1: 2, described second reaction vessel is put the 20 ~ 30min that vibrates on the oscillator, by the second extract by being equipped with the filter paper of anhydrous sodium sulfate, be filled in flat bottom flask; In described flat bottom flask, add mixed liquor 100 ~ 120mL that volume ratio is the acetone/normal hexane/methylene chloride of 1: 2: 1, and be placed in supersonic oscillations instrument vibration 60 ~ 70min, filtrate is concentrated into 5 ~ 8mL with Rotary Evaporators;
Step 3, by the concentrate through step 2 process by being filled with the chromatographic column of alkali alumina, neutral silica gel, acidic silica gel and anhydrous sodium sulfate from top to bottom successively, first use 30mL eluent methylene chloride, then use the drip washing of 40mL normal hexane, then by volume ratio be 1: 1: 1 acetone/normal hexane/methylene chloride mixed liquor 80mL drip washing and access eluent;
Step 4, the injection port of the eluent of step 3 through metastable atom bombardment high-resolution mass spectrometer is entered in chromatographic column and carry out Mass Spectrometer Method.
2. the assay method of short chain chlorinated paraffin in macromolecular material as claimed in claim 1, it is characterized in that, the testing conditions of the metastable atom bombardment high-resolution mass spectrometer adopted in described step 4 is: injector temperature 150 ~ 180 DEG C, flow rate of carrier gas is 3 ~ 5mL/min, and interface temperature is 200 ~ 220 DEG C.
3. the assay method of short chain chlorinated paraffin in macromolecular material as claimed in claim 2, it is characterized in that, after described sample enters chromatographic column from injection port, carry out temperature programme, 120 ~ 130 DEG C keep 10 ~ 15min, be warming up to 200 ~ 220 DEG C with the speed of 15 ~ 20 DEG C/min, keep 5 ~ 8min; Then be warming up to 280 ~ 300 DEG C with the speed of 25 ~ 30 DEG C/min, keep 20 ~ 30min.
4. the assay method of short chain chlorinated paraffin in macromolecular material as claimed in claim 1, is characterized in that, in described step one, macromolecular material is placed in clear water and soaks 20 ~ 40min, and with the dust of polymer surface described in hairbrush outwash and dirt.
5. the assay method of short chain chlorinated paraffin in macromolecular material as claimed in claim 1, it is characterized in that, the macromolecular material in described step 2 after dedusting is heated to 150 ~ 180 DEG C in molten condition.
6. the assay method of short chain chlorinated paraffin in macromolecular material as claimed in claim 1, is characterized in that, be filled with 20 ~ 30g alkali alumina, 10 ~ 12g neutral silica gel, 25 ~ 35g acidic silica gel and 2 ~ 5g anhydrous sodium sulfate in described step 3 chromatographic column.
7. the assay method of short chain chlorinated paraffin in macromolecular material as claimed in claim 6, is characterized in that, be filled with 25g alkali alumina, 12g neutral silica gel, 30g acidic silica gel and 3g anhydrous sodium sulfate in described step 3 chromatographic column.
8. the as described in claim 1 assay method of short chain chlorinated paraffin in macromolecular material, it is characterized in that, described macromolecular material is plastics, rubber or textile material.
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| CN105588889A (en) * | 2015-06-19 | 2016-05-18 | 上海英格尔认证有限公司 | Detection and analysis method of short-chain chlorinated paraffin |
| CN106645515A (en) * | 2016-12-29 | 2017-05-10 | 嘉兴学院 | Detection method for content of short-chain chlorinated paraffin in leather |
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| CN108254474A (en) * | 2018-02-02 | 2018-07-06 | 通标标准技术服务（天津）有限公司 | The assay method of short chain chlorinated paraffin in high molecular material |
| CN110372018A (en) * | 2019-07-31 | 2019-10-25 | 中国环境科学研究院 | A method of inactivation aluminum oxide and preparation method thereof, the short chain chlorinated paraffin of qualitative quantitative analysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105588889A (en) * | 2015-06-19 | 2016-05-18 | 上海英格尔认证有限公司 | Detection and analysis method of short-chain chlorinated paraffin |
| CN106799195A (en) * | 2015-11-25 | 2017-06-06 | 衡阳市骏杰化工有限公司 | It is a kind of to determine the carbon skeleton reaction bushing pipe that chlorinated paraffin content is used |
| CN106645515A (en) * | 2016-12-29 | 2017-05-10 | 嘉兴学院 | Detection method for content of short-chain chlorinated paraffin in leather |
| CN107884493A (en) * | 2017-11-08 | 2018-04-06 | 国家地质实验测试中心 | The method of short chain chlorinated paraffin in comprehensive two dimensional gas chromatography flying time mass spectrum analysis environmental sample |
| CN107884493B (en) * | 2017-11-08 | 2020-11-24 | 国家地质实验测试中心 | Method for analyzing short-chain chlorinated paraffin in environmental sample by using full-two-dimensional gas chromatography-time-of-flight mass spectrometry |
| CN108254474A (en) * | 2018-02-02 | 2018-07-06 | 通标标准技术服务（天津）有限公司 | The assay method of short chain chlorinated paraffin in high molecular material |
| CN110372018A (en) * | 2019-07-31 | 2019-10-25 | 中国环境科学研究院 | A method of inactivation aluminum oxide and preparation method thereof, the short chain chlorinated paraffin of qualitative quantitative analysis |
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