CN105510481A - Detection method for 2,6-di-tert-butyl-4-methylphenol in hot melt adhesive - Google Patents
Detection method for 2,6-di-tert-butyl-4-methylphenol in hot melt adhesive Download PDFInfo
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- CN105510481A CN105510481A CN201610051646.1A CN201610051646A CN105510481A CN 105510481 A CN105510481 A CN 105510481A CN 201610051646 A CN201610051646 A CN 201610051646A CN 105510481 A CN105510481 A CN 105510481A
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- 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
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Abstract
The invention relates to a detection method for 2,6-di-tert-butyl-4-methylphenol in hot melt adhesive, and belongs to the technical field of analytical chemistry. 2,6-di-tert-butyl-4-methylphenol in the hot melt adhesive is measured through a gas chromatography-mass spectrometry method. The detection method includes the steps that 0.05-0.1 g of the hot melt adhesive cut into pieces is added into a centrifugal tube, 10-15 ml of normal hexane is added to conduct ultrasonic extraction for 10-20 min, after centrifugation is carried out, 1-2 ml of supernatant liquor is taken and analyzed through a gas chromatography-mass spectrometry instrument, and an external standard method is used for quantifying. The detection method can be used for detecting the content of 2,6-di-tert-butyl-4-methylphenol in the hot melt adhesive, has the advantages that sample pretreatment is simple, operation is convenient, quantification is accurate, and the detection method is easy to apply and popularize.
Description
Technical field
The invention belongs to technical field of analytical chemistry, be specifically related to the detection method that one is exclusively used in 2,6-di-tert-butyl-4-methy phenols in hot melt adhesive.
Background technology
2,6-di-tert-butyl-4-methy phenol is a kind of antioxidant, has industrial use widely, is mainly used in the grease field of food, increases the shelf life of grease.2, the 6-di-tert-butyl-4-methy phenol major parts that wherein German Yang Ying group produces are used in edible oil product ink and rubber plastic industry.
Hot melt adhesive, as one of smoking material, cigarette filter rod and packing box all has application, may produce directly contact with consumer.Although hot melt adhesive proportion in the composition of cigarette material is relatively little, but there is maximum use quantitative limitation to 2,6-di-tert-butyl-4-methy phenols in hot melt adhesive in tobacco business at present, therefore, be necessary to study it, formulate corresponding detection method and control.
At present bibliographical information is had no to the detection method of 2,6-di-tert-butyl-4-methy phenols in hot melt adhesive.Therefore, the detection method developing 2,6-di-tert-butyl-4-methy phenols in simple, the easy and simple to handle and quantitative hot melt adhesive accurately of sample pre-treatments is very urgent.
Summary of the invention
The object of the invention is to in current hot melt adhesive 2, the detection method of 6-di-tert-butyl-4-methy phenol has no the present situation of bibliographical information, to there is provided in a kind of hot melt adhesive 2, the detection method of 6-di-tert-butyl-4-methy phenol, the method has the advantages such as sample pre-treatments is simple, easy and simple to handle and quantitatively accurate.
For achieving the above object, the technical solution used in the present invention is as follows:
The detection method of 2,6-di-tert-butyl-4-methy phenols in a kind of hot melt adhesive, comprises the following steps:
Take 0.05 ~ 0.1g and shred hot melt adhesive to grain of rice size in centrifuge tube, after adding 10 ~ 15mL normal hexane, ultrasonic extraction 10 ~ 20min, then centrifugal, get 1 ~ 2mL supernatant liquor through gas chromatograph-mass spectrometer (GCMS) analysis, according to component peaks area quantitative.
Described GC conditions is as follows: chromatographic column is HP-INNOWax chromatographic column or equivalent post, and length × internal diameter × thickness is 30m × 0.25mm × 0.25 μm; Carrier gas is helium (He); Injector temperature is 185 ~ 200 DEG C; Constant current mode, post flow 1.5 ~ 2.0mL/min, split ratio 5:1 ~ 10:1; Heating schedule is keep 10 ~ 12min at 60 ~ 70 DEG C, then with ramp to 230 ~ 260 DEG C of 8 ~ 10 DEG C/min, keeps 15 ~ 20min.
Described Mass Spectrometry Conditions is as follows: ionization mode is electron bombardment ionization source (EI), and ion source temperature is 200 ~ 240 DEG C, and ionizing energy is 65 ~ 75eV, and quadrupole rod temperature is 160 ~ 170 DEG C.Salbutamol Selected Ion Monitoring pattern, ion Selection parameter is in table 1.
Table 1 ion Selection parameter
| Material title | Quota ion | Qualitative ion |
| 2,6-di-tert-butyl-4-methy phenol | 205 | 57 or 145 |
Compared with prior art, its beneficial effect is in the present invention:
(1); Detection method of the present invention can be used for the content detecting 2,6-di-tert-butyl-4-methy phenols in hot melt adhesive, and pre-treatment step is 1. by the ultrasonic extraction of sample normal hexane, 2. centrifugal, 3. gets supernatant liquor through instrumental analysis, has the simple feature of sample pre-treatments;
(2) detection method of the present invention is easy and simple to handle, and quantitatively accurately, the relative standard deviation adopting detection method 5 parallel determinations is between 2.16 ~ 4.21%.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 measures 2,6-di-tert-butyl-4-methy phenol gas chromatogram.
Wherein, retention time is that the chromatographic peak of 10.95min represents 2,6-di-tert-butyl-4-methy phenol.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by buying the conventional products obtained.
In the present invention indication shred to the grain of rice in grain of rice size be traditional large grain of rice size, without particular restriction.
Embodiment 1
Take 0.05g and shred hot melt adhesive to grain of rice size in centrifuge tube, add 10mL normal hexane ultrasonic extraction 10min, after centrifugal, get 1mL supernatant liquor through gas chromatograph-mass spectrometer (GCMS) analysis, according to component peaks area quantitative (quantified by external standard method).
GC conditions is as follows:
Chromatographic column is HP-INNOWax chromatographic column or equivalent post, and length × internal diameter × thickness is 30m × 0.25mm × 0.25 μm; Carrier gas is helium (He); Injector temperature is 185 DEG C; Constant current mode, post flow 1.5mL/min, split ratio 5:1; Temperature programme is 60 DEG C, keeps 10min, and with the ramp to 230 DEG C of 8 DEG C/min, keep 15min, the chromatogram obtained as shown in Figure 1.
Mass Spectrometry Conditions is as follows:
Ionization mode is electron bombardment ionization source (EI), and ion source temperature is 200 DEG C, and ionizing energy is 65eV, quadrupole rod temperature is 160 DEG C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: 2,6-di-tert-butyl-4-methy phenol quota ion 205, qualitative ion 57.
According to the method described above, the mean value of 5 parallel determinations is 38.54 μ g/g, and relative standard deviation is 1.26%, and illustrate that this method detects 2,6-di-tert-butyl-4-methy phenol reliable results in hot melt adhesive, precision is good.
Embodiment 2
Take 0.07g and shred hot melt adhesive to grain of rice size in centrifuge tube, add 12mL normal hexane ultrasonic extraction 13min, after centrifugal, get 1.2mL supernatant liquor through gas chromatograph-mass spectrometer (GCMS) analysis, according to component peaks area quantitative (quantified by external standard method).
GC conditions is as follows:
Chromatographic column is HP-INNOWax chromatographic column or equivalent post, and length × internal diameter × thickness is 30m × 0.25mm × 0.25 μm; Carrier gas is helium (He); Injector temperature is 190 DEG C; Constant current mode, post flow 1.6mL/min, split ratio 6:1; Temperature programme is 65 DEG C, keeps 11min, with the ramp to 240 DEG C of 9 DEG C/min, keeps 16min.
Mass Spectrometry Conditions is as follows:
Ionization mode is electron bombardment ionization source (EI), and ion source temperature is 210 DEG C, and ionizing energy is 70eV, quadrupole rod temperature is 165 DEG C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: 2,6-di-tert-butyl-4-methy phenol quota ion 205, qualitative ion 145.
According to the method described above, the mean value of 5 parallel determinations is 35.25 μ g/g, and relative standard deviation is 4.21%.
Embodiment 3
Take 0.07g shred after hot melt adhesive in centrifuge tube, add 13mL normal hexane ultrasonic extraction 14min, after centrifugal, get 1.3mL supernatant liquor through gas chromatograph-mass spectrometer (GCMS) analysis, according to component peaks area quantitative (quantified by external standard method).
GC conditions is as follows:
Chromatographic column is HP-INNOWax chromatographic column or equivalent post, and length × internal diameter × thickness is 30m × 0.25mm × 0.25 μm; Carrier gas is helium (He); Injector temperature is 195 DEG C; Constant current mode, post flow 1.7mL/min, split ratio 7:1; Temperature programme is 67 DEG C, keeps 12min, with the ramp to 250 DEG C of 10 DEG C/min, keeps 17min.
Mass Spectrometry Conditions is as follows:
Ionization mode is electron bombardment ionization source (EI), and ion source temperature is 220 DEG C, and ionizing energy is 72eV, quadrupole rod temperature is 167 DEG C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: 2,6-di-tert-butyl-4-methy phenol quota ion 205, qualitative ion 57.
According to the method described above, the mean value of 5 parallel determinations is 264.12 μ g/g, and relative standard deviation is 2.16%.
Embodiment 4
Take 0.1g and shred hot melt adhesive to grain of rice size in centrifuge tube, add 15mL normal hexane ultrasonic extraction 20min, after centrifugal, get 2mL supernatant liquor through gas chromatograph-mass spectrometer (GCMS) analysis, according to component peaks area quantitative (quantified by external standard method).
GC conditions is as follows:
Chromatographic column is HP-INNOWax chromatographic column or equivalent post, and length × internal diameter × thickness is 30m × 0.25mm × 0.25 μm; Carrier gas is helium (He); Injector temperature is 200 DEG C; Constant current mode, post flow 2.0mL/min, split ratio 10:1; Temperature programme is 70 DEG C, keeps 12min, with the ramp to 260 DEG C of 10 DEG C/min, keeps 20min.
Mass Spectrometry Conditions is as follows:
Ionization mode is electron bombardment ionization source (EI), and ion source temperature is 240 DEG C, and ionizing energy is 75eV, quadrupole rod temperature is 170 DEG C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: 2,6-di-tert-butyl-4-methy phenol quota ion 205, qualitative ion 145.
According to the method described above, the mean value of 5 parallel determinations is 135.14 μ g/g, and relative standard deviation is 3.47%.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and instructions just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (3)
1. in a hot melt adhesive 2, the detection method of 6-di-tert-butyl-4-methy phenol, it is characterized in that: take 0.05 ~ 0.1g and shred hot melt adhesive to grain of rice size in centrifuge tube, after adding 10 ~ 15mL normal hexane, ultrasonic extraction 10 ~ 20min, then centrifugal, get 1 ~ 2mL supernatant liquor through gas chromatograph-mass spectrometer (GCMS) analysis, according to component peaks area quantitative.
2. 2,6-di-tert-butyl-4-methy phenol detection methods in hot melt adhesive according to claim 1, it is characterized in that, GC conditions is as follows:
Chromatographic column is HP-INNOWax chromatographic column or equivalent post, and length × internal diameter × thickness is 30m × 0.25mm × 0.25 μm; Carrier gas is helium; Injector temperature is 185 ~ 200 DEG C; Constant current mode, post flow 1.5 ~ 2.0mL/min, split ratio 5:1 ~ 10:1; Heating schedule is keep 10 ~ 12min at 60 ~ 70 DEG C, then with ramp to 230 ~ 260 DEG C of 8 ~ 10 DEG C/min, keeps 15 ~ 20min.
3. 2,6-di-tert-butyl-4-methy phenol detection methods in hot melt adhesive according to claim 1, it is characterized in that, Mass Spectrometry Conditions is as follows:
Ionization mode is electron bombardment ionization source, and ion source temperature is 200 ~ 240 DEG C, and ionizing energy is 65 ~ 75eV, quadrupole rod temperature is 160 ~ 170 DEG C, Salbutamol Selected Ion Monitoring pattern, ion Selection parameter: 2,6-di-tert-butyl-4-methy phenol quota ion 205, qualitative ion is 57 or 145.
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| CN201610051646.1A CN105510481A (en) | 2016-01-26 | 2016-01-26 | Detection method for 2,6-di-tert-butyl-4-methylphenol in hot melt adhesive |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568883A (en) * | 2016-10-21 | 2017-04-19 | 云南中烟工业有限责任公司 | Method for simultaneously measuring phenol and BHT in hot melt adhesive |
| CN107367559A (en) * | 2017-07-19 | 2017-11-21 | 云南电网有限责任公司电力科学研究院 | The detection method of oxidation preventive content in a kind of insulating oil |
| CN111077237A (en) * | 2018-10-22 | 2020-04-28 | 山东省医疗器械产品质量检验中心 | Gas chromatography detection method for medicine compatibility of medicinal butyl rubber plug |
| CN118294569A (en) * | 2024-05-14 | 2024-07-05 | 广州海关技术中心 | Method for measuring free phenol content in friction layer of brake pad |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198605A (en) * | 2014-09-09 | 2014-12-10 | 中国烟草总公司郑州烟草研究院 | Method for determining content of phenolic antioxidant for tobacco hot melt adhesive |
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2016
- 2016-01-26 CN CN201610051646.1A patent/CN105510481A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198605A (en) * | 2014-09-09 | 2014-12-10 | 中国烟草总公司郑州烟草研究院 | Method for determining content of phenolic antioxidant for tobacco hot melt adhesive |
Non-Patent Citations (2)
| Title |
|---|
| 蔡德玲: "气质联用仪测定EVA材料中BHT和BHA", 《化工技术与开发》 * |
| 陈皖芳: "GC-MS 快速测定塑胶包装材料中的BHT", 《广东化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568883A (en) * | 2016-10-21 | 2017-04-19 | 云南中烟工业有限责任公司 | Method for simultaneously measuring phenol and BHT in hot melt adhesive |
| CN107367559A (en) * | 2017-07-19 | 2017-11-21 | 云南电网有限责任公司电力科学研究院 | The detection method of oxidation preventive content in a kind of insulating oil |
| CN107367559B (en) * | 2017-07-19 | 2019-10-01 | 云南电网有限责任公司电力科学研究院 | The detection method of oxidation preventive content in a kind of insulating oil |
| CN111077237A (en) * | 2018-10-22 | 2020-04-28 | 山东省医疗器械产品质量检验中心 | Gas chromatography detection method for medicine compatibility of medicinal butyl rubber plug |
| CN118294569A (en) * | 2024-05-14 | 2024-07-05 | 广州海关技术中心 | Method for measuring free phenol content in friction layer of brake pad |
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