CN108037223A - The detection method of bisphenol-A in a kind of paint - Google Patents
The detection method of bisphenol-A in a kind of paint Download PDFInfo
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- CN108037223A CN108037223A CN201711328847.2A CN201711328847A CN108037223A CN 108037223 A CN108037223 A CN 108037223A CN 201711328847 A CN201711328847 A CN 201711328847A CN 108037223 A CN108037223 A CN 108037223A
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of detection method of bisphenol-A in paint, its key points of the technical solution are that：Specifically comprise the following steps：The detection method of bisphenol-A, specifically comprises the following steps in a kind of paint：Step 1：Weigh the paint reagent to be measured after 60~120 DEG C of drying to add in sample bottle, lid is tightened after adding extractant；Step 2：Sample bottle is placed on water temperature under the conditions of 15~35 DEG C, ultrasonic extraction is carried out using ultrasonic extraction instrument to solution；Step 3：The sample bottle after ultrasound is taken out, precipitating reagent is added into sample bottle and is shaken up；Step 4：Above-mentioned solution is transferred to centrifugal treating in centrifuge tube, condition 2000~5000rpm, 5~10min；Step 5：The solution after centrifugation is taken into test tube, is blown to using nitrogen evaporator nitrogen and closely done, organic solvent is added and is redissolved with water, use the organic system membrane filtration in 0.45um or following apertures；Step 6：Filter out aqueous solution to mix with methanol, quantitative analysis is carried out by liquid chromatograph testing result.
Description
【Technical field】
The present invention relates to coating detection technique field, and in particular to the detection method of bisphenol-A in a kind of paint.
【Background technology】
As requirement of the people to toy safety gradually steps up, since the U.S. in 2009 begins to focus on bisphenol-A, trigger complete
Ball is discussed warmly, and various countries one after another carry out bisphenol-A risk assessment, and carry out regulation limitation to bisphenol-A again and again.European Union, the U.S., China etc.
Bisphenol-A in articles for children is contacted to food to disable.The GB 9685-2008 standards of revision renewal in 2008《Food holds
Device, packaging material use sanitary standard with additive》Middle regulation, when bisphenol-A is used for food contact plastics, coating, adhesive, its
Special migration should be no more than 0.6mg/kg.
Bisphenol-A is industrially used to the materials such as polycarbonate synthesis (PC) and epoxy resin, is in the world using most wide
One of general industrial compound, is widely used in packaging material for food, medical instrument, feeding bottle, water bottle, ophthalmic len and other is hundreds of
The manufacturing process of kind daily necessities.After heated, BPA is likely to move in food and drink from container or packaging material.
Many studies have shown that contact BPA, may influence whether the function of nervous function development and immune system, it is especially right
For infant.BPA can also simulate female sex hormone, upset internal system, may trigger fertility Issue, sex premature, influence
Breast development and reproductive function, even result in the various and relevant cancer of hormone, therefore are more paid close attention to.
Chinese national standard GB14942-94, GB13116-1991 and GB/T5009.99-2003 test phenols (containing bisphenol-A)
The amount of migration is soaked for n-hexane or distilled water reflux, EU criteria EN71-10:2009 are extracted using pure water.Due to these standards
Method is that test object is extracted using solution and tests its bisphenol-A the amount of migration, using bisphenol-A the amount of migration result to inspection
Survey object accordance to be judged, and ignore and the content of bisphenol A that test object contains is tested.
Conventional test method time length, it is complex, and the bisphenol-A that can only be directed to gas phase volatilization is analyzed, it is impossible to
Bisphenol-A total content in coating is accurately detected, has been difficult to tackle detection demand.
【The content of the invention】
The present invention provides a kind of detection method of bisphenol-A in paint, can it is simple and efficient, accurately to bisphenol-A in paint
Carry out total content quantitatively detect.
The present invention is achieved by the following technical solutions：
The detection method of bisphenol-A, specifically comprises the following steps in a kind of paint：
The detection method of bisphenol-A, specifically comprises the following steps in a kind of paint：
Step 1：Weigh the paint reagent to be measured after 60~120 DEG C of drying to add in sample bottle, tightened after adding extractant
Lid；
Step 2：Sample bottle is placed on water temperature under the conditions of 15~35 DEG C, ultrasound is carried out using ultrasonic extraction instrument to solution
Extraction；
Step 3：The sample bottle after ultrasound is taken out, precipitating reagent is added into sample bottle and is shaken up；
Step 4：Above-mentioned solution is transferred to centrifugal treating in centrifuge tube, condition 2000~5000rpm, 5~10min；
Step 5：The solution after centrifugation is taken into test tube, is blown to using nitrogen evaporator nitrogen and closely done, organic solvent is added and is answered with water
It is molten, use the organic system membrane filtration in 0.45um or following apertures；
Step 6：Filter out aqueous solution to mix with methanol, quantitative analysis is carried out by liquid chromatograph testing result.
Preferably, extractant is that one or both of tetrahydrofuran, butanone, dichloromethane, acetone are mixed in the step 1
Close.Choose and carry out ultrasonic extraction for painting the solvents tetrahydrofurane with strong solubility, butanone, dichloromethane, acetone etc.,
Its main theoretical basis of the reform of Chinese economic structure is under ul-trasonic irradiation, paint can be dissolved by dichloromethane etc., destroys the resin in paint
The polymer architecture formed with auxiliary agent, makes bisphenol-A be discharged into dichloromethane, and reaction process is stablized completely, is adapted to qualitative or fixed
Amount analysis.
Preferably, in the step 3 precipitating reagent be methanol, n-hexane, one kind in acetonitrile.Resin and auxiliary agent in paint
After the polymer architecture of formation is extracted agent destruction, the precipitating reagents such as methanol, n-hexane, acetonitrile are added, make destroyed polymerization
Thing forms precipitation, is taken out by centrifugally operated, obtains settled solution, blows concentration by nitrogen, reuses acetonitrile and water redissolves, so as to
The sample solution of liquid chromatograph test can be entered by obtaining.
Preferably, paint sample quality (unit in the step 1：G) volume (Unit/mL) with extractant is than being 1：20
~40.Paint moisture to be measured after drying is reduced, and paint sample can be fully dissolved among extractant, promote bisphenol-A abundant
Release.
Preferably, the condition of ultrasonic extraction process is 300W~600W, 30~120min of time in the step 2.It is super
Sound wave extraction be a kind of strong cavitation produced using Ultrasonic Radiation pressure answer effect, mechanical oscillation, disturbance effect, it is high plus
Speed, emulsification, spread, smash and worn with the multistage effect such as stirring action, increase molecular motion of material frequency and speed, increase solvent
Saturating power, so as to accelerate target component to enter solvent, promotes the progress of extraction, applicant by test condition for 300W~
When 600W, 30~120min of time, the polymer architecture that the resin in paint is formed with auxiliary agent can be effectively facilitated and be destroyed, made
Bisphenol-A is discharged completely.
Preferably, 10~50% that precipitating reagent volume is extractant volume are added in the step 3 into sample bottle.
Preferably, the organic system membrane filtration in 0.22um apertures is used in the step 5.
Preferably, liquid chromatograph test condition is in the step 6：Mobile phase is methanol and aqueous solution mixed solution,
Flow velocity is 0.5 to 1.5mL/min；Sampling volume is 5-40uL；Liquid-phase chromatographic column is reversed-phase liquid chromatography column；Column oven temperature is set
Put 10 DEG C higher than room temperature；Fluorescence detector temperature is 10 DEG C higher than column oven temperature；Fluorescence detector parameter is arranged to excitation wavelength
275nm, launch wavelength 313nm.
Compared with prior art, the invention has the advantages that：
1. the detection method of bisphenol-A in a kind of paint of the present invention, with reference to ultrasonic extraction, using dichloromethane etc. as
Extractant, after solvent switch, bisphenol-A, which is dissolved in, to be analyzed into liquid chromatograph, and this test method advantage is,
First, the equipment of ultrasonic extraction is relatively cheap, and more other extracting process such as microwave abstracting needs to buy expensive microwave
Abstraction instrument；Secondly, the sweetening agent that ultrasonic extraction uses is few, reduces the pollution to environment and the injury to personnel；3rd, surpass
The time of sound wave extraction is shorter, compared to traditional soxhlet extraction method, require more than 24 it is small when, greatly shorten the pre-treatment time, use
Ultrasonic extraction is detected with liquid chromatography for bisphenol-A in the paint of complicated component, and equipment cost is low, pretreatment process
Simple and fast, as a result accurately, and in being painted bisphenol-A total content data, it is more objective compared to conventional test data
It is accurate to see；
2. the present invention a kind of paint in bisphenol-A detection method, it is that this method obtains as a result, the rate of recovery 85% to
115% scope, and in order to improve the accuracy of detection method, Taguchi's method is selected from numerous experimental data optimization method and is come pair
The important parameter for influencing testing result optimizes, and Taguchi's method is a kind of low cost, the quality engineering method of high benefit, it is strong
The raising for adjusting product quality be not by examining, but by design and optimal conditions, from field oral examination test, can be with statistical method
Optimal example weight, the volume of extractant, ultrasonic time, ultrasonic temperature are obtained, is made to bisphenol-A test experience knot in paint
Fruit value is more accurate.
【Brief description of the drawings】
Fig. 1 is the A factor trend figures that field cause for gossip is tested in the embodiment of the present invention 1；
Fig. 2 is the Factor B tendency chart that field cause for gossip is tested in the embodiment of the present invention 1；
Fig. 3 is the C factor tendency chart that field cause for gossip is tested in the embodiment of the present invention 1；
Fig. 4 is the D factor trend figures that field cause for gossip is tested in the embodiment of the present invention 1；
Fig. 5 is the A factor trend figures that field cause for gossip is tested in the embodiment of the present invention 2；
Fig. 6 is the Factor B tendency chart that field cause for gossip is tested in the embodiment of the present invention 2；
Fig. 7 is the C factor tendency chart that field cause for gossip is tested in the embodiment of the present invention 2；
Fig. 8 is the D factor trend figures that field cause for gossip is tested in the embodiment of the present invention 2；
Fig. 9 is the A factor trend figures that field cause for gossip is tested in the embodiment of the present invention 3；
Figure 10 is the Factor B tendency chart that field cause for gossip is tested in the embodiment of the present invention 3；
Figure 11 is the C factor tendency chart that field cause for gossip is tested in the embodiment of the present invention 3；
Figure 12 is the D factor trend figures that field cause for gossip is tested in the embodiment of the present invention 3.
【Embodiment】
1-3 illustrates the detection method of bisphenol-A in a kind of paint of the invention in conjunction with specific embodiments：
Embodiment 1：
Step 1：Weigh the paint reagent to be measured after 60 DEG C of drying to add in sample bottle, add dichloromethane as extractant
After tighten lid；
Step 2：Sample bottle is put in a water bath, ultrasonic extraction, ultrasonic extraction are carried out using ultrasonic extraction instrument to solution
Condition is 300W；
Step 3：The sample bottle after ultrasound is taken out, acetonitrile is added into sample bottle and is shaken up as precipitating reagent；
Step 4：Above-mentioned solution is transferred to centrifugal treating in centrifuge tube, condition 5000rpm, 5min；
Step 5：The solution after centrifugation is taken into test tube, is blown to using nitrogen evaporator nitrogen and closely done, organic solvent is added and is answered with water
It is molten, use the organic system membrane filtration in 0.22um or following apertures；
Step 6：Filter out aqueous solution to mix with methanol, quantitative analysis, liquid phase color are carried out by liquid chromatograph testing result
Spectrometer test condition is：Mobile phase is methanol and aqueous solution mixed solution, flow velocity 1.5mL/min；Sampling volume is 40uL；Liquid
Phase chromatographic column is reversed-phase liquid chromatography column；Column oven temperature setting is 30 DEG C (20 DEG C of room temperatures)；Fluorescence detector temperature is 40 DEG C；
Fluorescence detector parameter is arranged to excitation wavelength 275nm, launch wavelength 313nm.
The present inventor has found in the course of the research, and during using head space auto injection, maximum parameter is influenced on quantitative result
Tested for A (example weight), B (extraction liquor capacity), C (ultrasonic time) and D (ultrasonic temperature) using field cause for gossip to above-mentioned each ginseng
Number is verified that four controlling elements, three levels of each correspondence, each controlling elements use three levels, used three water
Standard is that the data of the present invention can be achieved, as shown in table 1：
Table 1：Controlling elements and its corresponding three levels
| Controlling elements | Explanation | Lever 1 | Lever 2 | Lever 3 |
| A | Example weight (g) | 0.15 | 0.3 | 0.6 |
| B | Extract liquor capacity (ml) | 5 | 7 | 15 |
| C | Ultrasonic time | 30min | 60min | 120min |
| D | Ultrasonic temperature | 15℃ | 25℃ | 35℃ |
Paint for detection is AG-100, orthogonal table L9 (34) experimental program to this toy paint using three levels
Tested, totally 9 groups of experiments, this 9 groups of experiments are detected using high performance liquid chromatography, and the standard liquid in each experiment is prepared, examination
Sample preparation, the parameter of blank preparation and ultrasonic extraction, parameter of chromatography etc., in addition to changing four conditions in table 1,
Other conditions are consistent.
Table 2：Each sample is carried out at the same time 5 Duplicate Samples tests, obtains tests below result
In above-mentioned table 2, rate of recovery calculation formula：
Table 3：The rate of recovery average value of field mouthful orthogonal table L9 (34) experimental programs and result of the test
Above-mentioned result of the test and result of calculation are obtained into tendency chart 1~4 using the Tian Kou mapping softwares of mintab softwares.
Embodiment 2：
Step 1：Weigh the paint reagent to be measured after 85 DEG C of drying to add in sample bottle, add butanone and acetone as extraction
Lid is tightened after agent；
Step 2：Sample bottle is put in a water bath, ultrasonic extraction, ultrasonic extraction are carried out using ultrasonic extraction instrument to solution
Condition is 600W；
Step 3：The sample bottle after ultrasound is taken out, methanol is added into sample bottle and is shaken up as precipitating reagent；
Step 4：Above-mentioned solution is transferred to centrifugal treating in centrifuge tube, condition 3500rpm, 8min；
Step 5：The solution after centrifugation is taken into test tube, is blown to using nitrogen evaporator nitrogen and closely done, organic solvent is added and is answered with water
It is molten, use the organic system membrane filtration in 0.35um or following apertures；
Step 6：Filter out aqueous solution to mix with methanol, quantitative analysis, liquid phase color are carried out by liquid chromatograph testing result
Spectrometer test condition is：Mobile phase is methanol and aqueous solution mixed solution, flow velocity 1mL/min；Sampling volume is 25uL；Liquid phase
Chromatographic column is reversed-phase liquid chromatography column；Column oven temperature setting is 35 DEG C (25 DEG C of room temperatures)；Fluorescence detector temperature is 45 DEG C；It is glimmering
Photodetector parameter is arranged to excitation wavelength 275nm, launch wavelength 313nm.
The present inventor has found in the course of the research, and during using head space auto injection, maximum parameter is influenced on quantitative result
Tested for A (example weight), B (extraction liquor capacity), C (ultrasonic time) and D (ultrasonic temperature) using field cause for gossip to above-mentioned each ginseng
Number is verified that four controlling elements, three levels of each correspondence, each controlling elements use three levels, used three water
Standard is that the data of the present invention can be achieved, as shown in table 4：
Table 4：Controlling elements and its corresponding three levels
| Controlling elements | Explanation | Lever 1 | Lever 2 | Lever 3 |
| A | Example weight (g) | 0.1 | 0.2 | 0.5 |
| B | Extract liquor capacity (mL) | 4 | 8 | 12 |
| C | Ultrasonic time | 25min | 50min | 100min |
| D | Ultrasonic temperature | 10℃ | 20℃ | 40℃ |
Paint for detection is PPS-100, orthogonal table L9 (34) experiment side to this toy paint using three levels
Case is tested, totally 9 groups of experiments, this 9 groups of experiments are detected using high performance liquid chromatography, the standard liquid in each experiment prepares,
Sample preparation, the parameter of blank preparation and ultrasonic extraction, parameter of chromatography etc., except changing four conditions in table 1
Outside, other conditions are consistent.
Table 5：Each sample is carried out at the same time 5 Duplicate Samples tests, obtains tests below result
In above-mentioned table 5, rate of recovery calculation formula：
Table 6：The rate of recovery average value of field mouthful orthogonal table L9 (34) experimental programs and result of the test
Above-mentioned result of the test and result of calculation are obtained into tendency chart 5~8 using the Tian Kou mapping softwares of mintab softwares.
Embodiment 3：
Step 1：Weigh the paint reagent to be measured after 120 DEG C of drying to add in sample bottle, add tetrahydrofuran as extraction
Lid is tightened after agent；
Step 2：Sample bottle is put in a water bath, ultrasonic extraction, ultrasonic extraction are carried out using ultrasonic extraction instrument to solution
Condition is 450W；
Step 3：The sample bottle after ultrasound is taken out, n-hexane is added into sample bottle and is shaken up as precipitating reagent；
Step 4：Above-mentioned solution is transferred to centrifugal treating in centrifuge tube, condition 2000rpm, 10min；
Step 5：The solution after centrifugation is taken into test tube, is blown to using nitrogen evaporator nitrogen and closely done, organic solvent is added and is answered with water
It is molten, use the organic system membrane filtration in 0.45um or following apertures；
Step 6：Filter out aqueous solution to mix with methanol, quantitative analysis, liquid phase color are carried out by liquid chromatograph testing result
Spectrometer test condition is：Mobile phase is methanol and aqueous solution mixed solution, flow velocity 0.5mL/min；Sampling volume is 5uL；Liquid
Phase chromatographic column is reversed-phase liquid chromatography column；Column oven temperature setting is 38 DEG C (28 DEG C of room temperatures)；Fluorescence detector temperature is 48 DEG C；
Fluorescence detector parameter is arranged to excitation wavelength 275nm, launch wavelength 313nm.
The present inventor has found in the course of the research, and during using head space auto injection, maximum parameter is influenced on quantitative result
Tested for A (example weight), B (extraction liquor capacity), C (ultrasonic time) and D (ultrasonic temperature) using field cause for gossip to above-mentioned each ginseng
Number is verified that four controlling elements, three levels of each correspondence, each controlling elements use three levels, used three water
Standard is that the data of the present invention can be achieved, as shown in table 7：
Table 7：Controlling elements and its corresponding three levels
Paint for detection is SSA-100, orthogonal table L9 (34) experiment side to this toy paint using three levels
Case is tested, totally 9 groups of experiments, this 9 groups of experiments are detected using high performance liquid chromatography, the standard liquid in each experiment prepares,
Sample preparation, the parameter of blank preparation and ultrasonic extraction, parameter of chromatography etc., except changing four conditions in table 1
Outside, other conditions are consistent.
Table 8：Each sample is carried out at the same time 5 Duplicate Samples tests, obtains tests below result
In above-mentioned table 8, rate of recovery calculation formula：
Table 9：The rate of recovery average value of field mouthful orthogonal table L9 (34) experimental programs and result of the test
Above-mentioned result of the test and result of calculation are obtained into tendency chart 9~12 using the Tian Kou mapping softwares of mintab softwares.
Embodiment 1-3 uses high performance liquid chromatography, and combines four Optimal Parameters, to the bisphenol-A material in paint into
Row detection, respectively to adding oil made of bisphenol-A standard substance using paint PPS-100, paint AG-100 and paint SSA-100
Sample tests analysis is painted, is tested by liquid chromatography, the results are shown in Table 10.
Table 10：Liquid-phase chromatographic analysis result
As can be seen from Table 10, this method obtain as a result, the rate of recovery in 85% to 115% scope, thus explanation this
The detection method of invention can actually accomplish the total content of bisphenol-A in accurately detection paint, and the detection method of the present invention, behaviour
Make simple and fast, and it is of low cost.
Claims (8)
- A kind of 1. detection method of bisphenol-A in paint, it is characterised in that：Specifically comprise the following steps：Step 1：Weigh the paint reagent to be measured after 60~120 DEG C of drying to add in sample bottle, lid is tightened after adding extractant；Step 2：Sample bottle is placed on water temperature under the conditions of 15~35 DEG C, ultrasonic extraction is carried out using ultrasonic extraction instrument to solution Take；Step 3：The sample bottle after ultrasound is taken out, precipitating reagent is added into sample bottle and is shaken up；Step 4：Above-mentioned solution is transferred to centrifugal treating in centrifuge tube, condition 2000~5000rpm, 5~10min；Step 5：The solution after centrifugation is taken into test tube, is blown to using nitrogen evaporator nitrogen and closely done, organic solvent is added and is redissolved with water, made With the organic system membrane filtration in 0.45um or following apertures；Step 6：Filter out aqueous solution to mix with methanol, quantitative analysis is carried out by liquid chromatograph testing result.
- 2. the detection method of bisphenol-A in a kind of paint according to claim 1, it is characterised in that：Extracted in the step 1 Agent is the mixing of one or both of tetrahydrofuran, butanone, dichloromethane, acetone.
- 3. the detection method of bisphenol-A in a kind of paint according to claim 1, it is characterised in that：Precipitated in the step 3 Agent is methanol, one kind in n-hexane, acetonitrile.
- 4. the detection method of bisphenol-A in a kind of paint according to claim 1, it is characterised in that：Painted in the step 1 Sample quality (unit：G) volume (Unit/mL) with extractant is than being 1：20~40.
- 5. the detection method of bisphenol-A in a kind of paint according to claim 1, it is characterised in that：It is ultrasonic in the step 2 The condition of ripple extraction process is 300W~600W, 25~140min of time.
- 6. the detection method of bisphenol-A in a kind of paint according to claim 1, it is characterised in that：To sample in the step 3 10~50% that precipitating reagent volume is extractant volume are added in product bottle.
- 7. the detection method of bisphenol-A in a kind of paint according to claim 1, it is characterised in that：Used in the step 5 The organic system membrane filtration in 0.22um apertures.
- 8. the detection method of bisphenol-A in a kind of paint according to claim 1, it is characterised in that：Liquid phase in the step 6 Chromatograph test condition is：Mobile phase is methanol and aqueous solution mixed solution, and flow velocity is 0.5 to 1.5mL/min；Sampling volume is 5-40uL；Liquid-phase chromatographic column is reversed-phase liquid chromatography column；Column oven temperature setting is 10 DEG C higher than room temperature；Fluorescence detector temperature ratio Column oven temperature is 10 DEG C high；Fluorescence detector parameter is arranged to excitation wavelength 275nm, launch wavelength 313nm.
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