CN101876652A - Method for measuring benzene and benzene series in printing ink - Google Patents
Method for measuring benzene and benzene series in printing ink Download PDFInfo
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Abstract
The invention discloses a method for measuring benzene and benzene series in printing ink. In the method, fluorobenzene is used as an internal standard substance, and the benzene and benzene series content of the printing ink is measured by headspace gas chromatography-mass spectrometry. The measuring method has the advantages of simple sample pretreatment, high automation degree of the whole operation, high measurement sensitivity and repeatability, capability of realizing measurement continuity, and suitability for simultaneous, quick and accurate detection of the benzene and benzene series content of batch printing ink. The invention provides a method and scientific evidences for analyzing and controlling the benzene and benzene series content of the printing ink.
Description
Technical field
The invention belongs to chemical analysis detection technique field, be specifically related to benzene and Determination methods for benzene compounds in a kind of printing-ink.
Background technology
Printing-ink is applied to the packing of a large amount of food, medicine and cigarette, but it contains a large amount of toxic and harmful substances such as residual solvent, heavy metal and palycyclic aromatic, can pollute the packing content thing by chemical transport, wherein especially with the residual harm maximum of benzene and benzene series thing such as benzene, toluene, ethylbenzene, o-xylene, m-xylene, P-xylene to human body, even content is very low, also can have carcinogenic and teratogenesis.Compare with traditional solvent type ink, UV printing ink is as a kind of novel environmental protection printing ink, in the application of printing industry more and more widely in recent years.But find after deliberation, UV printing ink is not contain benzene and benzene series thing, and just the content of benzene and benzene series thing compare with traditional solvent type ink low, also discovery simultaneously, offset printing UV printing ink is uncured to detect benzene often, and solidifying that the back detects then is all to contain benzene in all offset printing UV printing ink.Do not see at present report relevant for the detection technique of benzene in the printing-ink and benzene series thing.
Summary of the invention
The purpose of this invention is to provide benzene and Determination methods for benzene compounds in a kind of printing-ink.
In order to realize above purpose, the technical solution adopted in the present invention is: benzene and Determination methods for benzene compounds in a kind of printing-ink are internal standard compound with the fluorobenzene, the content of benzene and benzene series thing in employing headspace gas chromatography-mass spectrometry method mensuration printing-ink.
Further, this assay method may further comprise the steps:
The preparation of standard operation solution, the drafting of detection and typical curve: the pure material that takes by weighing benzene and benzene series thing, be mixed with standard operation solution with concentration gradient more than 5 grades with inner mark solution, standard operation solution with concentration at different levels places the head space bottle to carry out the head space processing respectively, the head space composition that will contain benzene and benzene series thing afterwards is blown in the gas chromatograph with carrier gas and separates, utilize mass spectrometer to detect then, comparison corresponding standard working solution concentration mapping with the peak area of fluorobenzene in the benzene that obtains and benzene series thing and the inner mark solution, draw out typical curve, and calculate the regression equation of typical curve;
The preparation of testing sample reaches wherein benzene and benzene series thing Determination on content: printing-ink is injected head space bottle bottom, in the head space bottle, add inner mark solution again, carrying out head space afterwards handles, the head space composition that will contain benzene and benzene series thing then is blown in the gas chromatograph with carrier gas and separates, utilize mass spectrometer to detect then, obtain the peak area of benzene and benzene series thing and fluorobenzene, in the regression equation with benzene and benzene series thing and the peak area of fluorobenzene, obtain the content of benzene and benzene series thing in the printing-ink than substitution typical curve.
Wherein, described inner mark solution is the glyceryl triacetate solution of fluorobenzene, and its mass percent concentration is 0.30～0.60 μ g/mL.
Described standard operation solution has 6 grades of concentration gradients.
Described head space is treated to: with head space bottle sealing, put into the static head space instrument balance 30～40min that vibrates under 80～90 ℃ of temperature.
Described carrier gas is a helium.
The parameter of described gas chromatograph is: chromatographic column is the DB-624 capillary column, and the chromatographic column specification is 60m * 0.32mm * 1.8 μ m; Injector temperature is 150 ℃; Split ratio 10:1; Column flow rate 1mL/min; Adopt temperature programme: 40 ℃ of initial temperatures, keep 1min, the speed with 5 ℃/min rises to 160 ℃ afterwards, keeps 1min, and the speed with 20 ℃/min rises to 220 ℃ again, keeps 11min.
Described mass spectrometric parameter is: the transmission line temperature: 220 ℃; Ion source temperature: 200 ℃; Solvent delay 0 ~ 10min and 25 ~ 38min.
The present invention is internal standard compound with the fluorobenzene, the content of benzene and benzene series thing in employing headspace gas chromatography-mass spectrometry method mensuration printing-ink.The chemical property of internal standard compound fluorobenzene is stable, and its every performance is close with benzene and benzene series thing, the interference of suffered environment and matrix is little, and can with the target compound good separation, it is very suitable internal standard compound, the influence of printing-ink mesostroma and instrument fluctuation can be eliminated, the accuracy of mensuration can be improved greatly measuring.
In assay method of the present invention, at first testing sample being carried out head space handles, make benzene and benzene series thing in the sample in gas and liquid, reach partition equilibrium, the head space composition that contains benzene and benzene series thing after cooperating gas chromatography and mass spectrum to balance afterwards carried out separation detection, determined the content of benzene and benzene series thing in the printing-ink.Assay method sample pretreatment process provided by the invention is simple, whole operation automaticity height can be realized the continuity measured, and measure highly sensitive, good reproducibility is when being suitable in batches in the printing-ink benzene and benzene series thing content, fast, accurately detect.The present invention provides method and scientific basis for benzene in the printing-ink and benzene series thing analysis on Content and control.
Description of drawings
Fig. 1 is the chromatogram of benzene and benzene series thing standard operation solution.
Embodiment
Below assay method of the present invention is described further.
1, the preparation of solution
The preparation of A, inner mark solution: be solute with the fluorobenzene, be that solvent is made into the inner mark solution that mass percent concentration is 0.30～0.60 μ g/mL with the glyceryl triacetate;
The preparation of B, testing sample: inject 0.1g printing-ink sample to the bottom of 20mL head space bottle with the 1mL syringe, accurately in the head space bottle, add 200 μ L inner mark solutions with the liquid feeding rifle afterwards, sealing top empty bottle immediately, put into the static head space instrument balance 30～40min that under 80～90 ℃ of temperature, vibrates subsequently, to be measured afterwards;
The preparation of C, standard operation solution: accurately take by weighing benzene 8.1mg, toluene 8.6mg, ethylbenzene 8.6mg ,-dimethylbenzene (or right-dimethylbenzene) 7.7mg, ortho-xylene 8.4mg, place the 100mL volumetric flask, dilute constant volume with inner mark solution, as the mixed standard solution I; Get 5mL mixed standard solution I and place the 100mL volumetric flask, dilute constant volume with inner mark solution, as the mixed standard solution II; Pipette 1mL, 5mL, 10mL mixed standard solution II and mixed standard solution I respectively in the 50mL volumetric flask, dilute constant volume with inner mark solution, preparation 1 ~ 6 grade standard working solution, the concentration of concrete standard operation solution is shown in Table 1;
The standard operation solution concentration of table 1 benzene and benzene series thing
D, get 1 ~ 6 grade standard working solution, 200 μ L and add respectively in the 20ml head space bottle, put into the static head space instrument balance 30～40min that under 80～90 ℃ of temperature, vibrates after the sealing, to be measured afterwards.
2, instrument and condition
A, static head space instrument condition
Head space bottle pressing time: 1min; Transmission line temperature: 120 ℃; Sample introduction needle temperature: 100 ℃; Sample injection time: 0.2min; Sample introduction pattern: high pressure sample introduction; Pull out pin time: 0.5min; Chromatographic column pressure: 196.5kPa; Sample introduction pressure: 241.3kPa;
B, GC conditions
Chromatographic column: DB-624 capillary column, specification 60m * 0.32mm * 1.8 μ m; 150 ℃ of injector temperatures; Split ratio 10:1; Column flow rate 1mL/min; Temperature programme: 40 ℃ of initial temperatures, keep 1min, the speed with 5 ℃/min rises to 160 ℃ afterwards, keeps 1min, and the speed with 20 ℃/min rises to 220 ℃ again, keeps 11min;
C, mass spectrum condition
Transmission line temperature: 220 ℃; Ion source temperature: 200 ℃; Solvent delay 0 ~ 10min and 25 ~ 38min; Select ion mode SIM scanning, select ion to be shown in Table 2.
Table 2 benzene and benzene series thing characteristic ion are selected
Annotate: " * " is expressed as quota ion, and other ions are as auxiliary qualitative ion.
3, benzene and benzene series thing Determination on content in the printing-ink
The mensuration of standard operation solution and the drafting of typical curve: with helium as carrier gas, the head space composition that will contain benzene and benzene series thing is blown in the gas chromatograph and separates, utilize mass spectrometer to detect then, obtain the chromatogram of benzene and benzene series thing standard operation solution, see shown in Figure 1, comparison corresponding standard working solution concentration mapping with the peak area of fluorobenzene in the benzene that obtains and benzene series thing and the inner mark solution, draw out typical curve, and calculating the regression equation and the related coefficient of typical curve, regression equation and related coefficient are shown in Table 3;
Benzene and benzene series thing Determination on content in the testing sample: with helium as carrier gas, the head space composition that will contain benzene and benzene series thing is blown in the gas chromatograph with carrier gas and separates, utilize mass spectrometer to detect then, obtain the peak area of benzene and benzene series thing and fluorobenzene, in the regression equation with benzene and benzene series thing and the peak area of fluorobenzene, obtain the content of benzene and benzene series thing in the printing-ink than substitution typical curve.
Get least concentration standard operation solution, 10 parallel experiments, basis of calculation deviation, 3 times of standard deviations are qualitative detection limit, 10 times of standard deviations are the detection by quantitative limit, specifically are shown in Table 3.
Table 3 benzene and benzene series thing standard working curve and detectability
4, the recovery of assay method of the present invention and repeatability
The standard solution that in the printing-ink sample, adds high, medium and low variable concentrations level, every group of concentration level made 5 parts of mark-on samples, carrying out pre-treatment and GC/MS respectively analyzes, and calculate benzene and the recovery of benzene series thing composition and the relative standard deviation of measured value according to adding behind the scalar sum mark-on measured value, the results are shown in Table shown in 4.
The recovery of benzene and benzene series thing and repeatability in table 4 printing-ink (
n=5)
As can be seen from Table 4, on 3 mark-on levels, the average recovery rate of target compound all between 96%～103%, illustrates assay method accuracy height provided by the invention, and sample test result's average RSD＜6% illustrates the good reproducibility of assay method of the present invention.
Below adopt the above-mentioned assay method that further specifies that benzene in the concrete printing-ink sample and benzene series thing composition are measured.
Embodiment 1
In the assay method of present embodiment: choose a gravure and use red ink as sample A, inner mark solution is that mass percent concentration is the glyceryl triacetate solution of the fluorobenzene of 0.45 μ g/mL, head space treatment temperature to sample and standard specimen is 80 ℃, the vibration equilibration time is 30min, the results are shown in Table shown in 5 of mensuration.
Benzene and benzene series quality testing are surveyed the result among the table 5 printing-ink sample A
Embodiment 2
In the assay method of present embodiment: choose a gravure and use black ink as sample B, inner mark solution is that mass percent concentration is the glyceryl triacetate solution of the fluorobenzene of 0.30 μ g/mL, head space treatment temperature to sample and standard specimen is 85 ℃, the vibration equilibration time is 40min, the results are shown in Table shown in 6 of mensuration.
Benzene and benzene series quality testing are surveyed the result among the table 6 printing-ink sample B
Embodiment 3
In the assay method of present embodiment: choose a UV black ink as sample C, inner mark solution is that mass percent concentration is the glyceryl triacetate solution of the fluorobenzene of 0.45 μ g/mL, head space treatment temperature to sample and standard specimen is 80 ℃, the vibration equilibration time is 30min, the results are shown in Table shown in 7 of mensuration.
Benzene and benzene series quality testing are surveyed the result among the table 7 printing-ink sample C
Embodiment 4
In the assay method of present embodiment: choose a UV white ink as sample D, inner mark solution is that mass percent concentration is the glyceryl triacetate solution of the fluorobenzene of 0.60 μ g/mL, head space treatment temperature to sample and standard specimen is 90 ℃, the vibration equilibration time is 40min, the results are shown in Table shown in 8 of mensuration.
Benzene and benzene series quality testing are surveyed the result among the table 8 printing-ink sample D
Annotate: on behalf of target compound content, Trace be lower than the detection by quantitative limit, but is higher than qualitative detection limit.
Claims (8)
1. benzene and Determination methods for benzene compounds in the printing-ink is characterized in that: be internal standard compound with the fluorobenzene, adopt headspace gas chromatography-mass spectrometry method to measure the content of benzene and benzene series thing in the printing-ink.
2. benzene and Determination methods for benzene compounds in the printing-ink according to claim 1 is characterized in that: this assay method may further comprise the steps:
The preparation of standard operation solution, the drafting of detection and typical curve: the pure material that takes by weighing benzene and benzene series thing, be mixed with standard operation solution with concentration gradient more than 5 grades with inner mark solution, standard operation solution with concentration at different levels places the head space bottle to carry out the head space processing respectively, the head space composition that will contain benzene and benzene series thing afterwards is blown in the gas chromatograph with carrier gas and separates, utilize mass spectrometer to detect then, comparison corresponding standard working solution concentration mapping with the peak area of fluorobenzene in the benzene that obtains and benzene series thing and the inner mark solution, draw out typical curve, and calculate the regression equation of typical curve;
The preparation of testing sample reaches wherein benzene and benzene series thing Determination on content: printing-ink is injected head space bottle bottom, in the head space bottle, add inner mark solution again, carrying out head space afterwards handles, the head space composition that will contain benzene and benzene series thing then is blown in the gas chromatograph with carrier gas and separates, utilize mass spectrometer to detect then, obtain the peak area of benzene and benzene series thing and fluorobenzene, in the regression equation with benzene and benzene series thing and the peak area of fluorobenzene, obtain the content of benzene and benzene series thing in the printing-ink than substitution typical curve.
3. benzene and Determination methods for benzene compounds in the printing-ink according to claim 2 is characterized in that: described inner mark solution is the glyceryl triacetate solution of fluorobenzene, and its mass percent concentration is 0.30～0.60 μ g/mL.
4. benzene and Determination methods for benzene compounds in the printing-ink according to claim 2 is characterized in that: described standard operation solution has 6 grades of concentration gradients.
5. benzene and Determination methods for benzene compounds in the printing-ink according to claim 2 is characterized in that: described head space is treated to: with head space bottle sealing, put into the static head space instrument balance 30～40min that vibrates under 80～90 ℃ of temperature.
6. benzene and Determination methods for benzene compounds in the printing-ink according to claim 2 is characterized in that: described carrier gas is a helium.
7. benzene and Determination methods for benzene compounds in the printing-ink according to claim 2 is characterized in that: the parameter of described gas chromatograph is: chromatographic column is the DB-624 capillary column, and the chromatographic column specification is 60m * 0.32mm * 1.8 μ m; Injector temperature is 150 ℃; Split ratio 10:1; Column flow rate 1mL/min; Adopt temperature programme: 40 ℃ of initial temperatures, keep 1min, the speed with 5 ℃/min rises to 160 ℃ afterwards, keeps 1min, and the speed with 20 ℃/min rises to 220 ℃ again, keeps 11min.
8. benzene and Determination methods for benzene compounds in the printing-ink according to claim 2 is characterized in that: described mass spectrometric parameter is: the transmission line temperature: 220 ℃; Ion source temperature: 200 ℃; Solvent delay 0 ~ 10min and 25 ~ 38min.
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| CN102253140A (en) * | 2011-06-22 | 2011-11-23 | 红云红河烟草(集团)有限责任公司 | Method for testing content of benzene and benzene series in water base adhesive for tobaccos |
| CN102323364A (en) * | 2011-06-21 | 2012-01-18 | 红云红河烟草(集团)有限责任公司 | Method for measuring content of benzene and benzene series in hot melt glue |
| CN102393326A (en) * | 2011-08-08 | 2012-03-28 | 北京海岸鸿蒙标准物质技术有限责任公司 | Preparation method of benzene series mixed solution standard substance in carbon bisulfide |
| CN102486473A (en) * | 2010-12-06 | 2012-06-06 | 湖北中烟工业有限责任公司 | Method for measuring benzene series content in polypropylene tow filter rod and special extraction apparatus |
| CN102495144A (en) * | 2011-11-11 | 2012-06-13 | 深圳天祥质量技术服务有限公司 | Detecting method of Benzene content |
| CN103675134A (en) * | 2013-12-05 | 2014-03-26 | 上海金玺实验室有限公司 | Method for detecting benzene series pollutants in gas by using internal standard method |
| CN105467020A (en) * | 2014-08-29 | 2016-04-06 | 乐凯华光印刷科技有限公司 | Headspace gas chromatography determination method of residual solvent in PS plate |
| CN105675748A (en) * | 2016-01-15 | 2016-06-15 | 成都大学 | Method for determination of residual impurity propylene glycol in Cefatrizine by headspace gas chromatography |
| CN105823838A (en) * | 2016-03-15 | 2016-08-03 | 广东中烟工业有限责任公司 | Perfume component detection method taking glyceryl triacetate as solvent |
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| CN106950303A (en) * | 2017-03-21 | 2017-07-14 | 山西医科大学 | The assay method of benzene homologues in biological specimen blood |
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| CN102486473A (en) * | 2010-12-06 | 2012-06-06 | 湖北中烟工业有限责任公司 | Method for measuring benzene series content in polypropylene tow filter rod and special extraction apparatus |
| CN102486473B (en) * | 2010-12-06 | 2013-12-25 | 湖北中烟工业有限责任公司 | Method for measuring benzene series content in polypropylene tow filter rod |
| CN102323364A (en) * | 2011-06-21 | 2012-01-18 | 红云红河烟草(集团)有限责任公司 | Method for measuring content of benzene and benzene series in hot melt glue |
| CN102253140A (en) * | 2011-06-22 | 2011-11-23 | 红云红河烟草(集团)有限责任公司 | Method for testing content of benzene and benzene series in water base adhesive for tobaccos |
| CN102393326A (en) * | 2011-08-08 | 2012-03-28 | 北京海岸鸿蒙标准物质技术有限责任公司 | Preparation method of benzene series mixed solution standard substance in carbon bisulfide |
| CN102495144A (en) * | 2011-11-11 | 2012-06-13 | 深圳天祥质量技术服务有限公司 | Detecting method of Benzene content |
| CN103675134A (en) * | 2013-12-05 | 2014-03-26 | 上海金玺实验室有限公司 | Method for detecting benzene series pollutants in gas by using internal standard method |
| CN103675134B (en) * | 2013-12-05 | 2015-05-13 | 上海金玺实验室有限公司 | Method for detecting benzene series pollutants in gas by using internal standard method |
| CN105467020A (en) * | 2014-08-29 | 2016-04-06 | 乐凯华光印刷科技有限公司 | Headspace gas chromatography determination method of residual solvent in PS plate |
| CN105675748A (en) * | 2016-01-15 | 2016-06-15 | 成都大学 | Method for determination of residual impurity propylene glycol in Cefatrizine by headspace gas chromatography |
| CN105823838A (en) * | 2016-03-15 | 2016-08-03 | 广东中烟工业有限责任公司 | Perfume component detection method taking glyceryl triacetate as solvent |
| CN105974008A (en) * | 2016-04-27 | 2016-09-28 | 广东中烟工业有限责任公司 | Method for detecting spice ingredient in flavoring glyceryl triacetate |
| CN107860826A (en) * | 2016-09-22 | 2018-03-30 | 中美华世通生物医药科技（武汉）有限公司 | The method that residual solvent in Ezetimibe bulk drug is determined using headspace gas chromatography |
| CN107860826B (en) * | 2016-09-22 | 2021-06-22 | 中美华世通生物医药科技(武汉)股份有限公司 | Method for measuring residual solvent in ezetimibe bulk drug by using headspace gas chromatography |
| CN106950303A (en) * | 2017-03-21 | 2017-07-14 | 山西医科大学 | The assay method of benzene homologues in biological specimen blood |
| CN111537645A (en) * | 2020-05-25 | 2020-08-14 | 江南大学 | Method for determining content of benzene series in lubricating oil for food contact |
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