CN111595965A - Method for detecting transport amount of isoprene in packaging material - Google Patents
Method for detecting transport amount of isoprene in packaging material Download PDFInfo
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- CN111595965A CN111595965A CN202010390046.4A CN202010390046A CN111595965A CN 111595965 A CN111595965 A CN 111595965A CN 202010390046 A CN202010390046 A CN 202010390046A CN 111595965 A CN111595965 A CN 111595965A
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- Prior art keywords
- isoprene
- temperature
- sample
- packaging material
- headspace
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- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000005022 packaging material Substances 0.000 title claims abstract description 14
- 238000013508 migration Methods 0.000 claims abstract description 31
- 230000005012 migration Effects 0.000 claims abstract description 31
- 238000001514 detection method Methods 0.000 claims abstract description 18
- 239000012488 sample solution Substances 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 4
- 238000004817 gas chromatography Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000523 sample Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000012546 transfer Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 239000011550 stock solution Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 238000013461 design Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000002791 soaking Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000088 plastic resin Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The invention relates to a method for detecting the migration quantity of isoprene in a packaging material, which is characterized by comprising the following steps: the method comprises the following steps: 1) preparing a sample solution; 2) gas chromatography analysis; 3) and (4) calculating the migration quantity. The invention has scientific and reasonable structural design, can accurately detect the transference amount of the isoprene, and has quick detection and high detection precision.
Description
Technical Field
The invention belongs to the technical field of material detection, relates to packaging material detection, and particularly relates to a method for detecting the migration amount of isoprene in a packaging material.
Background
Isoprene is an important chemical raw material and is widely applied to the fields of medicines, plastics, resins, fine chemicals, rubber and the like at present. Isoprene is colorless transparent liquid at normal temperature, has a boiling point of 34 ℃, is insoluble in water and soluble in ethanol, has conjugated double bonds in molecules, is easy to generate polymerization reaction, is easy to generate oxidation and polymerization in the storage process, and is often added with a small amount of stabilizer.
Isoprene is a 2B-type carcinogen published by the International cancer research institute of the world health organization, and GB4806.6-2016 (national food safety Standard for food contact Plastic resin) and GB9685-2016 (national food safety Standard for food contact Material and use of additives for products) require that the limit of the migration amount is not detected (detection limit is 0.01 mg/kg).
Under the existing national standard system, the chemical migration test of the food contact material generally refers to GB 31604.1-2016 (general rules for food safety national standard food contact material and product migration test) and GB5009.156-2016 (general rules for food safety national standard food contact material and product migration test pretreatment method) to carry out sample soaking treatment, but at present, no national standard method for detecting isoprene is available, and the stability of a soaking solution is not researched and specified.
Disclosure of Invention
The invention aims to provide a method for detecting the migration amount of isoprene in a packaging material, aiming at the defects and shortcomings of the prior art, so that isoprene can be accurately detected, the detection is rapid, and the detection precision is high.
The technical problem to be solved by the invention is realized by the following technical scheme:
a method for detecting the transport volume of isoprene in a packaging material is characterized by comprising the following steps: the method comprises the following steps:
1) preparation of a sample solution: cutting a 6cm multiplied by 10cm PS hard sheet, dripping 5 mu LN, N-dimethylformamide and a proper amount of isoprene standard stock solution with the purity of 98.8% on the surface of the PS hard sheet in sequence, completely immersing the PS hard sheet in 100mL of transfer liquid, preparing the PS hard sheet to the concentration required by detection to obtain a sample solution, and placing the sample solution into an oven for constant-temperature storage for 10 days;
2) gas chromatographic analysis: transferring a small amount of the sample solution obtained in the step 1) into a headspace bottle, sealing the headspace bottle by using a spacer and an aluminum cover, adding 10 mu LN, N-dimethylformamide into the headspace bottle by using a liquid transfer device, uniformly mixing, and injecting the mixed solution into a gas chromatograph by using a headspace sample injector for gas chromatography analysis;
3) calculating the migration quantity: the isoprene concentration was calculated by software and mapped.
Further, the migration liquid in the step 1) is acetic acid or ethanol having a purity of 99%.
And, the headspace conditions of the headspace sampler are: the balance time is 30min, the headspace bottle temperature is 80 ℃, and the transmission line temperature is 85 ℃.
Moreover, the chromatographic conditions of the gas chromatograph are as follows:
a chromatographic column: capillary chromatography column DB-WAX 30m × 0.32mm × 0.50 μm;
sample injection and carrier gas: high-purity nitrogen;
and (3) sample introduction mode: split-flow sample injection, the split-flow ratio is 20: 1, the flow rate is 3.0 mL/min;
sample inlet temperature: 220 ℃;
temperature programming: keeping the temperature at 80 ℃ for 12min, then heating to 120 ℃ at the speed of 10 ℃/min, and keeping the temperature for 10 min;
FID detector, detection temperature 250 ℃.
The invention has the advantages and beneficial effects that:
1. the method for detecting the transport amount of isoprene in the packaging material determines the transport amount detection method of isoprene, and makes up for the vacancy of the national standard for detecting isoprene at present.
2. According to the method for detecting the migration amount of the isoprene in the packaging material, the migration liquid is alcohol, and when the migration temperature is lower, the migration of the isoprene is more thorough, and the detection result of the migration amount is more accurate.
3. The invention has scientific and reasonable structural design, can accurately detect the transference amount of the isoprene, and has quick detection and high detection precision.
Drawings
FIG. 1 is a gas chromatogram of a sample solution according to the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
A detection method for the transport volume of isoprene in a packaging material is innovative in that: the method comprises the following steps:
1) preparation of a sample solution: sample preparation: a PS hard sheet; specification and model number: the material is as follows: PS; description of the samples: sealing and packaging the sample; the test contents are as follows: testing the food contact material for changes in concentration during isoprene migration;
a. influence of migration liquid: cutting two 6cm × 10cm PS hard sheets, respectively and uniformly dripping 5 μ LN, N-dimethylformamide and a proper amount of isoprene standard stock solution with the purity of 98.8% on the surfaces of the two hard sheets, respectively immersing the two hard sheets in 100mL of 4% acetic acid and 50% ethanol to ensure that the concentration of the obtained solution is 5mg/L, obtaining a sample solution, and placing the sample solution into a 40 ℃ oven to keep the temperature for 10 days;
b. influence of migration temperature: cutting four PS hard sheets of 6cm multiplied by 10cm, respectively and uniformly dripping 5 mu LN, N-dimethylformamide and a proper amount of isoprene standard stock solution with the purity of 98.8% on the surfaces of the PS hard sheets, respectively immersing two sheets of the PS hard sheets in 100mL of 4% acetic acid, respectively immersing the other two sheets of the PS hard sheets in 50% ethanol, respectively, so that the concentration of the obtained solutions is 5mg/L, regarding one part of 4% acetic acid migration solution and one part of 50% migration solution as a group of samples, obtaining sample solutions, and respectively putting the sample solutions into a 40 ℃ oven and a 60 ℃ oven to keep the temperature for 10 days;
c. influence of initial concentration: cutting four PS hard sheets of 6cm multiplied by 10cm, uniformly dripping 5 mu LN, N-dimethylformamide and a proper amount of isoprene standard stock solution with the purity of 98.8% on the surfaces of two sheets, and respectively immersing the two sheets in 100mL of 4% acetic acid and 50% ethanol to ensure that the concentration of the obtained solution is 5 mg/L; uniformly dripping 5 mu LN, N-dimethylformamide and a proper amount of isoprene standard stock solution with the purity of 98.8 percent on the surfaces of the other two sheets, respectively completely immersing the two sheets in 100mL of 4 percent acetic acid and 50 percent ethanol to ensure that the concentration of the obtained solution is 10mg/L to obtain a sample solution, and placing the sample solution into a 40 ℃ oven to keep the temperature for 10 days;
different factor tests in the step 1) can show that the concentration of isoprene is reduced along with the increase of time in the process of the migration test, and the attenuation of the migration liquid in 50% ethanol is slower than that of the migration liquid in 4% acetic acid; the temperature has a remarkable influence on the decay speed of the migration liquid no matter which migration liquid is used, and the higher the temperature is, the faster the decay is; when other conditions are uniform, the attenuation degree of isoprene has no obvious correlation with the initial concentration; in the migration experiment, the alcohol migration solution and the lower soaking temperature are preferably considered, and if the 4% acetic acid migration is required, the standing time of the migration solution needs to be shortened to 48 hours for detection so as to obtain a more accurate result.
2) Gas chromatographic analysis: transferring 1mL of the sample solution obtained in the step 1) into a headspace bottle, sealing the headspace bottle by using a spacer and an aluminum cover, adding 10 mu LN, N-dimethylformamide into the headspace bottle by using a liquid transfer device, uniformly mixing, and injecting the mixed solution into a gas chromatograph by using a headspace sampler for gas chromatography analysis, wherein the mixed solution is shown in figure 1;
3) calculating the migration quantity: the isoprene concentration was calculated by software and mapped.
The headspace conditions for the headspace sampler were: the balance time is 30min, the headspace bottle temperature is 80 ℃, and the transmission line temperature is 85 ℃.
The chromatographic conditions of the gas chromatograph are as follows:
a chromatographic column: capillary chromatography column DB-WAX 30m × 0.32mm × 0.50 μm;
sample injection and carrier gas: high-purity nitrogen;
and (3) sample introduction mode: split-flow sample injection, the split-flow ratio is 20: 1, the flow rate is 3.0 mL/min;
sample inlet temperature: 220 ℃;
temperature programming: keeping the temperature at 80 ℃ for 12min, then heating to 120 ℃ at the speed of 10 ℃/min, and keeping the temperature for 10 min;
FID detector, detection temperature 250 ℃.
Although the embodiments of the present invention and the accompanying drawings are disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments and the accompanying drawings.
Claims (4)
1. A method for detecting the transport volume of isoprene in a packaging material is characterized by comprising the following steps: the method comprises the following steps:
1) preparation of a sample solution: cutting a 6cm multiplied by 10cm PS hard sheet, dripping 5 mu LN, N-dimethylformamide and a proper amount of isoprene standard stock solution with the purity of 98.8% on the surface of the PS hard sheet in sequence, completely immersing the PS hard sheet in 100mL of transfer liquid, preparing the PS hard sheet to the concentration required by detection to obtain a sample solution, and placing the sample solution into an oven for constant-temperature storage for 10 days;
2) gas chromatographic analysis: transferring a small amount of the sample solution obtained in the step 1) into a headspace bottle, sealing the headspace bottle by using a spacer and an aluminum cover, adding 10 mu LN, N-dimethylformamide into the headspace bottle by using a liquid transfer device, uniformly mixing, and injecting the mixed solution into a gas chromatograph by using a headspace sample injector for gas chromatography analysis;
3) calculating the migration quantity: the isoprene concentration was calculated by software and mapped.
2. The method for detecting the transfer amount of isoprene in a packaging material according to claim 1, wherein: the transfer liquid in the step 1) is acetic acid or ethanol with the purity of 99%.
3. The method for detecting the transfer amount of isoprene in a packaging material according to claim 1, wherein: the headspace conditions of the headspace sampler are: the balance time is 30min, the headspace bottle temperature is 80 ℃, and the transmission line temperature is 85 ℃.
4. The method for detecting the transfer amount of isoprene in a packaging material according to claim 1, wherein: the chromatographic conditions of the gas chromatograph are as follows:
a chromatographic column: capillary chromatography column DB-WAX 30m × 0.32mm × 0.50 μm;
sample injection and carrier gas: high-purity nitrogen;
and (3) sample introduction mode: split-flow sample injection, the split-flow ratio is 20: 1, the flow rate is 3.0 mL/min;
sample inlet temperature: 220 ℃;
temperature programming: keeping the temperature at 80 ℃ for 12min, then heating to 120 ℃ at the speed of 10 ℃/min, and keeping the temperature for 10 min;
FID detector, detection temperature 250 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010390046.4A CN111595965A (en) | 2020-05-11 | 2020-05-11 | Method for detecting transport amount of isoprene in packaging material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010390046.4A CN111595965A (en) | 2020-05-11 | 2020-05-11 | Method for detecting transport amount of isoprene in packaging material |
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| CN111595965A true CN111595965A (en) | 2020-08-28 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362971A (en) * | 2000-02-15 | 2002-08-07 | 阿托费纳化学股份有限公司 | Fluoropolymer resins containing ionic or ionizable groups and products containing the same |
| CN102590457A (en) * | 2012-02-21 | 2012-07-18 | 四川农业大学 | Method for identifying stable carbon isotope composition of isoprene in atmosphere |
| US20140130399A1 (en) * | 2012-11-09 | 2014-05-15 | Westham Ltd | Devices and methods for a durable insect bait station |
| CN107515264A (en) * | 2017-08-31 | 2017-12-26 | 中国检验检疫科学研究院 | Benzene homologues migrate quantity measuring method in food processing electrical appliance based on Dynamic headspace |
| CN110376299A (en) * | 2019-06-24 | 2019-10-25 | 杭州市质量技术监督检测院 | The measuring method of diisopropyl naphthalene the amount of migration in silicone oil paper |
| EP3594301A1 (en) * | 2017-03-07 | 2020-01-15 | Kao Corporation | Film comprising hydrophobized cellulose fibers and oil |
-
2020
- 2020-05-11 CN CN202010390046.4A patent/CN111595965A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362971A (en) * | 2000-02-15 | 2002-08-07 | 阿托费纳化学股份有限公司 | Fluoropolymer resins containing ionic or ionizable groups and products containing the same |
| CN102590457A (en) * | 2012-02-21 | 2012-07-18 | 四川农业大学 | Method for identifying stable carbon isotope composition of isoprene in atmosphere |
| US20140130399A1 (en) * | 2012-11-09 | 2014-05-15 | Westham Ltd | Devices and methods for a durable insect bait station |
| EP3594301A1 (en) * | 2017-03-07 | 2020-01-15 | Kao Corporation | Film comprising hydrophobized cellulose fibers and oil |
| CN107515264A (en) * | 2017-08-31 | 2017-12-26 | 中国检验检疫科学研究院 | Benzene homologues migrate quantity measuring method in food processing electrical appliance based on Dynamic headspace |
| CN110376299A (en) * | 2019-06-24 | 2019-10-25 | 杭州市质量技术监督检测院 | The measuring method of diisopropyl naphthalene the amount of migration in silicone oil paper |
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| Title |
|---|
| BARISIC DAMIR等: "Pentadienyl migration and abstraction in yttrium aluminabenzene complexes including a single-component catalyst for isoprene polymerization", 《CHEMICAL COMMUNICATIONS》 * |
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Application publication date: 20200828 |