CN104215719A - Purge and trap method for measuring migration volume of particular volatile and semi-volatile substances of paper and paperboards by using water as mimetic - Google Patents
Purge and trap method for measuring migration volume of particular volatile and semi-volatile substances of paper and paperboards by using water as mimetic Download PDFInfo
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Abstract
The invention provides a method for measuring the migration volume of particular volatile and semi-volatile substances of paper and paperboards. The purge and trap-gas chromatography/mass spectrometry method is used for measuring migrated volatile and semi-volatile compounds by using water as a mimetic. The method includes the steps of cutting for preparing a sample, adding a certain amount of distilled water in the sample as a mimic, soaking at required temperature for required time, absorbing a certain amount of the soaking solution, and analyzing through the purge and trap-gas chromatography/mass spectrometry to obtain the migration volume. The method for measuring the migration volume of the particular volatile and semi-volatile substances of the paper and paperboards can be effectively used for measuring the migration volume of the particular volatile and semi-volatile substances from the paper and paperboards to water, is feasible and easy to operate, omits pre-treatment of the soaking solution and the use of organic solvents, and has the advantages of simple and rapid operation, accuracy, high sensitivity, good recovery and the like.
Description
Technical field
The present invention relates to a kind of method measuring specific volatilization and half volatile substance migration amount in paper and paperboard, be specifically related to adopt water as analogies, purge and trap-gas chromatography/mass spectrometry method measures volatilization and half volatile compound of migration.
Background technology
Paper wrapper is as the important wrappage of a class, be widely used, but the body material body paper of packaging Paper or cardboard, and in packages printing process, use ink, solvent and the auxiliary material etc. that may contain harmful composition, there is the potential risk of the contaminating impurity such as volatility and semi-volatile organic matter.These materials, due to its volatility, easily migrate in food, also can be discharged in environment, all can cause harm to a certain degree to human health and environment.
Evaluate the safe and sanitary quality of packaging Paper or cardboard, mainly investigate whether its material composition contained moves, whether the amount of moving reaches the level jeopardizing human health.Domestic and international wrappage relevant laws and regulations carry out strict, detailed regulation to the Special migration of objectionable constituent, and have formulated the specific transfer weight testing method of a series of restricted substances, normally choose suitable analogies and set up migration models, obtain migration amount.At present both at home and abroad, the analogies for aqueous food contact material are all choose water, but using water as analogies, measure the method also existing defects of volatility and the semi-volatile organic matter moved in water.
Current mensuration moves to the mensuration of volatile organic matter in water and adopts Head space, liquid-liquid extraction method to be combined with gas chromatography or gas chromatography mass spectrometry method more.But Head space take water as matrix, can heat the temperature reached low, the recovery of method is low, and sensitivity is low, and precision is poor, and large quantity of moisture can enter chromatographic column in addition, all causes larger damage to chromatographic column and instrument.As for liquid-liquid extraction method, as being that extractant carries out liquid-liquid extraction with glyceryl triacetate, low for alcohol soluble substance extraction efficiency, the recovery is low.Above method is to the equal Shortcomings of the mensuration moving to multiple volatilization and semi-volatile organic matter in water.
Using water as analogies, in conjunction with purge and trap-gas chromatography/mass spectrometry method, set up that to measure in paper and paperboard the method moving to volatility in water and semi-volatile organic matter very meaningful.
Summary of the invention
There is the problems such as the recovery is low, sensitivity is low, precision is poor, instrument is fragile for overcoming prior art, the invention provides a kind of method measuring specific volatilization and half volatile substance migration amount in paper and paperboard, the method adopts water as analogies, and purge and trap-gas chromatography/mass spectrometry method measures the migration amount of volatilization and half volatile compound moved in water.
The object of the invention is to be achieved through the following technical solutions: a kind of method measuring specific volatilization and half volatile substance migration amount in paper and paperboard, through following each step:
(1) Paper or cardboard to be measured is cut into 0.2 ~ 2 dm
2sample;
(2) step (1) gained sample is pressed every dm
2sample add 100 mL distilled water, at 5 ~ 100 DEG C, in distilled water, soak 5 min ~ 240 h;
(3) soak solution 5 mL of aspiration step (2), adopt Puffing and trapping-gas chromatography/mass spectrometry method analysis to obtain the quota ion peak area of volatilization and Semi-volatile organism in soak solution, instrument condition is as follows:
The condition of Puffing and trapping process is for purging temperature: 40 DEG C; Purge flow velocity: 40 mL/min; Purge time: 11 min; Dry purge time: 1 min; Pre-desorption temperature: 180 DEG C; Desorption temperature: 190 DEG C; Desorption time: 2 min; Baking temperature: 200 DEG C; Baking time: 6 min;
The condition of gas chromatography is injector temperature: 220 DEG C; Input mode: split sampling (split ratio 30:1); Temperature programme: 35 DEG C (5 min) → 2.5 DEG C/min → 120 DEG C → 5 DEG C/min → 220 DEG C (2 min); Carrier gas: helium; Flow: 1.0 mL/min;
Mass spectrographic condition is ion gun: EI source; Ion source temperature: 230 DEG C; Ionization energy: 70eV; Scan mode: full scan and Selective ion mode scanning (SIM); Sweep limit: m/z 35 ~ 270 amu; Solvent delay: 2.0 min; Interface temperature: 280 DEG C;
(4) take ultrapure water as the series standard solution that solvent prepares volatilization and Semi-volatile organism, each series standard solution at least prepares 5 grades, its concentration range should cover the content of determinand in sample, concentration range is 0 ~ 100 μ g/L, each standard solution 5 mL is accurately drawn with purge and trap injector, gas chromatograph-mass spectrometer (GCMS) analysis is carried out to series standard solution, quota ion peak area according to each volatilization and Semi-volatile organism is ordinate, with each volatilization and Semi-volatile organism unit area migration amount, (namely concentration of standard solution is multiplied by multiple 100, unit is μ g/dm
2) be horizontal ordinate, working curve forced initial point, made the typical curve of each volatilization and Semi-volatile organism,
(5) according to step (4) gained typical curve, by the ion peak areas of volatilization and Semi-volatile organism in step (3) gained soak solution, the migration amount that typical curve calculates volatilization and semi-volatile organic matter in soak solution is brought into.
The soaking conditions employing table 1 of described step (2) and the time conditions of table 2 and temperature conditions control:
Table 1 soaks the time conditions of migration test
Table 2 soaks the temperature conditions of migration test
The specific volatilization of described step (3) and Semi-volatile organism comprise methyl alcohol, ethanol, isopropyl alcohol, acetone, n-propanol, butanone, ethyl acetate, isopropyl acetate, normal butyl alcohol, benzene, 1-methoxy-2-propanol, n-propyl acetate, 4-methyl-2 pentanone, 1-ethoxy-2-propyl alcohol, toluene, n-butyl acetate, ethylbenzene, dimethylbenzene, styrene and cyclohexanone.
The mass spectrographic ion Selection parameter of described step (3) is in table 3:
The quota ion of table 3 volatilization and semi-volatile organic matter
Outstanding advantages of the present invention is: the step and method provided can be effective to measure the specific volatilization that moves to from paper and paperboard in water and half volatile substance migration amount, method is feasible, soak solution is without the need to pre-treatment, simple to operate, method is accurate, highly sensitive, the recovery is good, has application value.Existing Head space and extraction can be avoided as defects such as the recovery are low in conjunction with Puffing and trapping, and without the need to an organic solvent, have fast easy and simple to handle, recovery advantages of higher, be more suitable for mensuration and move to multiple volatilization and semi-volatile organic matter in water.
Accompanying drawing explanation
Fig. 1 is the total ions chromatogram adopting volatilization and Semi-volatile organism in Puffing and trapping-gas chromatography/mass spectrometry method analytical standard solution in embodiment 1 step (4).
Wherein, 1, methyl alcohol (6.63 min); 2, ethanol (9.74 min); 3, acetone (11.60 min); 4, isopropyl alcohol (12.64 min); 5, n-propanol (19.77); 6, butanone (22.79 min); 7, ethyl acetate (23.18 min); 8, benzene (28.52 min); 9, isopropyl acetate (30.36 min); 10,1-methoxy-2-propanol (propylene glycol monomethyl ether) (34.09 min); 11, normal butyl alcohol (34.69 min); 12, n-propyl acetate (37.12 min); 13,4-methyl-2 pentanone (41.00 min); 14, toluene (41.40 min); 15,1-ethoxy-2-propyl alcohol (propylene-glycol ethyl ether) (41.63 min); 16, n-butyl acetate (45.82 min); 17, ethylbenzene (48.84 min); 18, P-xylene (49.40 min); 19, o-xylene (51.25 min); 20, cyclohexanone (53.21 min); 21, styrene (56.57 min).
Embodiment
The present invention is further described below with reference to embodiment, but does not limit the present invention.
The embodiment of the present invention adopts following instrument and reagent:
Instrument: Eclipse 4660 purge and trap instrument (O.I. Analytical, the U.S.); Clarus 600 gas chromatograph (GC) (PerkinElmer, the U.S.); Clarus 600T mass spectrometer (MS) (PerkinElmer, the U.S.).
Agents useful for same and material: ultrapure water (through the purification of MILLI-Q ultrapure water system); Tenax adsorbent, 60/80 order (CNW Technologies GmbH, Germany).
Embodiment 1
(1) art paper to be measured is cut into 0.6 dm
2sample;
(2) step (1) gained sample is added 60 mL distilled water, at 40 DEG C, in distilled water, soak 24 h; Time conditions and the temperature conditions of soaking conditions employing table 1 and table 2 control:
Table 1 soaks the time conditions of migration test
Table 2 soaks the temperature conditions of migration test
(3) soak solution 5 mL of aspiration step (2), adopt Puffing and trapping-gas chromatography/mass spectrometry method analysis to obtain the ion peak areas of volatilization and Semi-volatile organism in soak solution, instrument condition is as follows:
The condition of Puffing and trapping process is for purging temperature: 40 DEG C; Purge flow velocity: 40 mL/min; Purge time: 11 min; Dry purge time: 1 min; Pre-desorption temperature: 180 DEG C; Desorption temperature: 190 DEG C; Desorption time: 2 min; Baking temperature: 200 DEG C; Baking time: 6 min;
The condition of gas chromatography is injector temperature: 220 DEG C; Input mode: split sampling (split ratio 30:1); Temperature programme: 35 DEG C (5 min) → 2.5 DEG C/min → 120 DEG C → 5 DEG C/min → 220 DEG C (2 min); Carrier gas: helium; Flow: 1.0 mL/min;
Mass spectrographic condition is ion gun: EI source; Ion source temperature: 230 DEG C; Ionization energy: 70eV; Scan mode: full scan and Selective ion mode scanning (SIM); Sweep limit: m/z 35 ~ 270 amu; Solvent delay: 2.0min; Interface temperature: 280 DEG C;
Mass spectrographic ion Selection parameter is in table 3:
The quota ion of table 3 volatilization and semi-volatile organic matter
(4) take ultrapure water as the series standard solution that solvent prepares volatilization and Semi-volatile organism, each series standard solution preparation 5 grades, concentration range is 0 ~ 100 μ g/L, each standard solution 5 mL is accurately drawn with purge and trap injector, gas chromatograph-mass spectrometer (GCMS) analysis is carried out to series standard solution, the total ions chromatogram of standard solution as shown in Figure 1, quota ion peak area according to each volatilization and Semi-volatile organism is ordinate, with each volatilization and Semi-volatile organism unit area migration amount, (namely concentration of standard solution is multiplied by multiple 100, unit is μ g/dm
2) be horizontal ordinate, working curve forced initial point, made the typical curve of each volatilization and Semi-volatile organism, the results are shown in Table 4,
The typical curve of table 4 standard solution and the migration amount obtained after measuring
Note: in table, "-" representative does not detect.
(5) according to step (4) gained typical curve, by the ion peak areas of volatilization and Semi-volatile organism in step (3) gained soak solution, the migration amount that typical curve calculates volatilization and semi-volatile organic matter in soak solution is brought into.
The migration amount moving to volatility and semi-volatile organic matter in water recorded is in table 4.
According to the method described above, do 3 parallel determinations, its relative standard deviation is 6.8 ~ 9.8%; Illustrate that this method measures volatility and the half volatile standard substance reliable results of migration, precision is good.
Embodiment 2
(1) art post paperboard to be measured is cut into 1 dm
2sample;
(2) step (1) gained sample is added 100 mL distilled water, at 20 DEG C, in distilled water, soak 240 h; Time conditions and the temperature conditions of soaking conditions employing table 1 and table 2 control;
(3) soak solution 5 mL of aspiration step (2), arranges specific volatilization and Semi-volatile organism, and adopt Puffing and trapping-gas chromatography/mass spectrometry method analysis to obtain the ion peak areas of volatilization and Semi-volatile organism in soak solution, instrument condition is with embodiment 1;
(4) Specification Curve of Increasing is with embodiment 1;
(5) according to step (4) gained typical curve, by the ion peak areas of volatilization and Semi-volatile organism in step (3) gained soak solution, the migration amount that typical curve calculates volatilization and semi-volatile organic matter in soak solution is brought into.
Move to volatility and the semi-volatile organic matter in water that record are methyl alcohol 1.21 μ g/dm
2, ethanol 2.16 μ g/dm
2, acetone 2.98 μ g/dm
2, ethyl acetate 3.13 μ g/dm
2, cyclohexanone 2.67 μ g/dm
2, all the other detection material do not detect.
According to the method that technique scheme of the present invention is recorded, the relative standard deviation of 3 parallel determinations is 5.2 ~ 9.7 %.
Embodiment 3
(1) template to be measured is cut into 2 dm
2sample;
(2) step (1) gained sample is added 200 mL distilled water, at 100 DEG C, in distilled water, soak 5 min; Time conditions and the temperature conditions of soaking conditions employing table 1 and table 2 control;
(3) soak solution 5 mL of aspiration step (2), arranges specific volatilization and Semi-volatile organism, and adopt Puffing and trapping-gas chromatography/mass spectrometry method analysis to obtain the ion peak areas of volatilization and Semi-volatile organism in soak solution, instrument condition is with embodiment 1;
(4) Specification Curve of Increasing is with embodiment 1;
(5) according to step (4) gained typical curve, by the ion peak areas of volatilization and Semi-volatile organism in step (3) gained soak solution, the migration amount that typical curve calculates volatilization and semi-volatile organic matter in soak solution is brought into.
Move to volatility and the semi-volatile organic matter in water that record are methyl alcohol 1.11 μ g/dm
2, ethanol 1.21 μ g/dm
2, acetone 1.31 μ g/dm
2, butanone 0.97 μ g/dm
2, ethyl acetate 1.56 μ g/dm
2, n-propyl acetate 1.23 μ g/dm
2, all the other detection material do not detect.
According to the method that technique scheme of the present invention is recorded, the relative standard deviation of 3 parallel determinations is 7.6 ~ 9.8 %.
Embodiment 4
(1) be 0.2 dm by Paperboard cutting to be measured
2sample;
(2) by step (1) gained sample 20 mL distilled water, at 5 DEG C, in distilled water, 240 h are soaked; Time conditions and the temperature conditions of soaking conditions employing table 1 and table 2 control;
(3) soak solution 5 mL of aspiration step (2), arranges specific volatilization and Semi-volatile organism, and adopt Puffing and trapping-gas chromatography/mass spectrometry method analysis to obtain the ion peak areas of volatilization and Semi-volatile organism in soak solution, instrument condition is with embodiment 1;
(4) Specification Curve of Increasing is with embodiment 1;
(5) according to step (4) gained typical curve, by the ion peak areas of volatilization and Semi-volatile organism in step (3) gained soak solution, the migration amount that typical curve calculates volatilization and semi-volatile organic matter in soak solution is brought into.
Move to volatility and the semi-volatile organic matter in water that record are methyl alcohol 0.99 μ g/dm
2, ethanol 1.07 μ g/dm
2, acetone 1.21 μ g/dm
2, all the other detection material do not detect.
According to the method that technique scheme of the present invention is recorded, the relative standard deviation of 3 parallel determinations is 7.1 ~ 9.9 %.
Claims (2)
1. measure a method for specific volatilization and half volatile substance migration amount in paper and paperboard, it is characterized in that through following each step:
(1) Paper or cardboard to be measured is cut into 0.2 ~ 2 dm
2sample;
(2) step (1) gained sample is pressed every dm
2sample add 100 mL distilled water, at 5 ~ 100 DEG C, in distilled water, soak 5 min ~ 240 h;
(3) soak solution 5 mL of aspiration step (2), adopt Puffing and trapping-gas chromatography/mass spectrometry method analysis to obtain the quota ion peak area of volatilization and Semi-volatile organism in soak solution, instrument condition is as follows:
The condition of Puffing and trapping process is for purging temperature: 40 DEG C; Purge flow velocity: 40 mL/min; Purge time: 11 min; Dry purge time: 1 min; Pre-desorption temperature: 180 DEG C; Desorption temperature: 190 DEG C; Desorption time: 2 min; Baking temperature: 200 DEG C; Baking time: 6 min;
The condition of gas chromatography is injector temperature: 220 DEG C; Input mode: split sampling (split ratio 30:1); Temperature programme: 35 DEG C (5 min) → 2.5 DEG C/min → 120 DEG C → 5 DEG C/min → 220 DEG C (2 min); Carrier gas: helium; Flow: 1.0 mL/min;
Mass spectrographic condition is ion gun: EI source; Ion source temperature: 230 DEG C; Ionization energy: 70eV; Scan mode: full scan and Selective ion mode scanning (SIM); Sweep limit: m/z 35 ~ 270 amu; Solvent delay: 2.0 min; Interface temperature: 280 DEG C;
(4) take ultrapure water as the series standard solution that solvent prepares volatilization and Semi-volatile organism, each series standard solution at least prepares 5 grades, concentration range is 0 ~ 100 μ g/L, each standard solution 5 mL is accurately drawn with purge and trap injector, gas chromatograph-mass spectrometer (GCMS) analysis is carried out to series standard solution, quota ion peak area according to each volatilization and Semi-volatile organism is ordinate, with the unit area migration amount of each volatilization and Semi-volatile organism for horizontal ordinate, working curve forced initial point, made the typical curve of each volatilization and Semi-volatile organism;
(5) according to step (4) gained typical curve, by the ion peak areas of volatilization and Semi-volatile organism in step (3) gained soak solution, the migration amount that typical curve calculates volatilization and semi-volatile organic matter in soak solution is brought into.
2. the method for specific volatilization and half volatile substance migration amount in mensuration paper and paperboard according to claim 1, is characterized in that: the specific volatilization of described step (3) and Semi-volatile organism comprise methyl alcohol, ethanol, isopropyl alcohol, acetone, n-propanol, butanone, ethyl acetate, isopropyl acetate, normal butyl alcohol, benzene, 1-methoxy-2-propanol, n-propyl acetate, 4-methyl-2 pentanone, 1-ethoxy-2-propyl alcohol, toluene, n-butyl acetate, ethylbenzene, dimethylbenzene, styrene and cyclohexanone.
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| CN109668973A (en) * | 2017-10-17 | 2019-04-23 | 中国石油化工股份有限公司 | The measuring method of gas station underground water pollutant |
| CN110780000A (en) * | 2019-11-01 | 2020-02-11 | 上海烟草集团有限责任公司 | Method for detecting migration amount of volatile organic compounds in paper packaging material to dry simulant |
| CN111239307A (en) * | 2020-03-10 | 2020-06-05 | 浙江格临检测股份有限公司 | Method for measuring butyl acetate and cyclohexanone in water and soil |
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| CN112730663A (en) * | 2020-12-22 | 2021-04-30 | 华测检测认证集团湖北有限责任公司 | Method for rapidly and accurately measuring volatile nitrosamine in food |
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| 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 |
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| CN112730663A (en) * | 2020-12-22 | 2021-04-30 | 华测检测认证集团湖北有限责任公司 | Method for rapidly and accurately measuring volatile nitrosamine in food |
| CN112858502A (en) * | 2021-01-06 | 2021-05-28 | 徐州市质量技术监督综合检验检测中心(徐州市标准化研究中心) | Method for detecting migration quantity of volatile organic compounds in food contact material and product in oil-based simulant |
| CN113504333A (en) * | 2021-08-20 | 2021-10-15 | 上海烟草集团有限责任公司 | Method for detecting organic matter migration amount in paper packaging material |
| CN113504333B (en) * | 2021-08-20 | 2023-03-14 | 上海烟草集团有限责任公司 | Method for detecting organic matter migration amount in paper packaging material |
| CN115166069A (en) * | 2022-06-13 | 2022-10-11 | 徐州市检验检测中心 | Method for detecting migration volume of volatile organic compounds in water toy and application |
| CN115166069B (en) * | 2022-06-13 | 2024-04-19 | 徐州市检验检测中心 | Detection method and application of migration quantity of volatile organic compounds in water toy |
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