CN108693015A - A kind of PET film digestion procedure - Google Patents
A kind of PET film digestion procedure Download PDFInfo
- Publication number
- CN108693015A CN108693015A CN201810274705.0A CN201810274705A CN108693015A CN 108693015 A CN108693015 A CN 108693015A CN 201810274705 A CN201810274705 A CN 201810274705A CN 108693015 A CN108693015 A CN 108693015A
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- Prior art keywords
- pet film
- digestion
- solution
- digestion procedure
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The present invention discloses a kind of PET film digestion procedure, including:S11, the PET film is crushed, the distance of any two points of the diaphragm after crushing is not more than 1mm;S12, the PET film after crushing is placed in micro-wave diminishing pot, and concentrated nitric acid is added;S13, the micro-wave diminishing pot is placed in microwave dissolver and is cleared up, obtain digestion solution;S14, the digestion solution is diluted to faintly acid with non-sulfur-bearing solvent;S15, the measurement that element sulphur is carried out to obtained weakly acidic solution.PET film by being first crushed to small diaphragm by the present invention, it is cleared up simultaneously using the nitric acid of not sulfur-bearing, it improves the resolution degree of PET film and obtains the digestion solution without containing external element sulphur, so as to accurately measure the content of element sulphur, lower limit of quantitation can reach 2ppm (mg/kg), far below present 30ppm (mg/kg), the rate of recovery is stablized between 80%~120%.
Description
Technical field
The present invention relates to optical film field more particularly to a kind of PET film digestion procedures.
Background technology
PET film is a kind of basement membrane for being difficult to clear up, the method used at present be with 65% nitric acid and 95% sulfuric acid with
1:1 is blended under high-temperature and high-pressure conditions more than reaction 30min clocks, this influences not the measurement of PET class optical film metallic elements
Greatly, however because the presence of sulfuric acid, this method are not suitable for the test of sulfur content in PET class optical films.But if not adding
Add sulfuric acid, according to current method, PET class optical films resolution degree is low, and the resolution degree of PET class optical films is to sulfur content
The accuracy of measurement has vital influence, to seriously affect the accuracy of element sulphur test.
Invention content
It is an object of the invention in view of the above problems and insufficient, a kind of digestion procedure of PET film is provided, is passed through
The mode for not adding element sulphur improves the resolution degree of PET film, to solve the above problems.
The technical proposal of the invention is realized in this way:
The present invention provides a kind of PET film digestion procedure, including:
S11, the PET film is crushed, the distance of any two points of the diaphragm after crushing is not more than 1mm;
S12, the PET film after crushing is placed in micro-wave diminishing pot, and concentrated nitric acid is added;
S13, the micro-wave diminishing pot is placed in microwave dissolver and is cleared up, obtain digestion solution;
S14, the digestion solution is diluted to faintly acid with non-sulfur-bearing solvent;
S15, the measurement that element sulphur is carried out to obtained weakly acidic solution.
Preferably, Freezing smashing mode is used in the S11.
Preferably, the micro-wave diminishing pot is polytetrafluoro micro-wave diminishing pot.
Preferably, a concentration of 65-68% of the concentrated nitric acid.
Preferably, it is cleared up using gradual heating mode in the step S13.
Preferably, the digestion solution is clear digestion solution.
Preferably, it measures element sulphur by plasma inductance coupling firing graticule S180.672 in the step S15 and contains
Amount.
Preferably, the volume of the concentrated nitric acid and the volume ratio of weakly acidic solution are 1:5-1:20, preferably 1:8-1:
10。
Preferably, 10-20gPET films, preferably 15-17g are put into every 100ml concentrated nitric acids.
Preferably,
The step S13 includes:
The temperature of microwave dissolver is set in 160 °, maximum pressure 50bar, rotating speed 10r/min, microwave energy 80%,
Keep 10min;
It is warming up to 200 °, maximum pressure 50bar, rotating speed 5r/min later, microwave energy 80% keeps 5min;
It is warming up to 250 °, maximum pressure 50bar, rotating speed 5r/min later, microwave energy 100% keeps 5min.
Advantageous effect:
PET film, is first crushed to small diaphragm by PET film digestion procedure provided by the invention, and wantonly 2 points of distance is little
It is cleared up in 1mm, while using the nitric acid of not sulfur-bearing, improve the resolution degree of PET film and obtains not containing external element sulphur
Digestion solution, so as to accurately measure the content of element sulphur, lower limit of quantitation can reach 2ppm (mg/kg), far below present
30ppm (mg/kg), the rate of recovery stablize between 80%-120%.
Description of the drawings
The accompanying drawings which form a part of this application are used to provide further understanding of the present invention, and of the invention shows
Meaning property embodiment and its explanation do not constitute improper limitations of the present invention, in the accompanying drawings for explaining the present invention:
Fig. 1 is the step schematic diagram of the present invention.
Specific implementation mode
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The application is described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
For ease of description, herein can with use space relative terms, as " ... on ", " in ... top ",
" ... upper surface ", " above " etc., for describing such as a device shown in the figure or feature and other devices or spy
The spatial relation of sign.It should be understood that spatially relative term is intended to comprising the orientation in addition to device described in figure
Except different direction in use or operation.For example, if the device in attached drawing is squeezed, it is described as " in other devices
It will be positioned as " under other devices or construction after part or construction top " or the device of " on other devices or construction "
Side " or " under other devices or construction ".Thus, exemplary term " ... top " may include " ... top " and
" in ... lower section " two kinds of orientation.The device can also other different modes positioning (be rotated by 90 ° or be in other orientation), and
And respective explanations are made to the opposite description in space used herein above.
According to the description of background technology, if only with nitric acid, PET can be caused to clear up incomplete problem.It is attempting
After numerous modes, inventor has found, if it is that the distance of any two points is not more than the diaphragm of 1mm that PET, which is crushed, to improving
The resolution of PET has very great help.This discovery makes the attention of inventor be first focused in the crushing of PET film.But it uses
The mode of existing rotating shredder, if rotating speed increases, PET film can be sticked to machine sidewalls, can not further crush and reach
It is required that if rotating speed reduces, it can not also be crushed to the diaphragm of very little.For this purpose, inventor has attempted the mode crushed after freezing, film
Become fragile, to be easy to be crushed to small diaphragm.Certainly, the present invention can also select other modes, be cut such as artificial.But ice
It is another inventive point of the present invention that agar is broken.
Diaphragm after crushing is placed after weighing in high-temperature and high-presure resistent micro-wave diminishing pot, and concentrated nitric acid is added, and concentration is excellent
It is selected in 65-68%.To avoid introducing external element sulphur in either step, the present invention uses the counteracting tank without element sulphur, such as
Polytetrafluoro micro-wave diminishing pot.
Micro-wave diminishing pot is placed in microwave dissolver later and is cleared up.The temperature of microwave dissolver, energy, rotating speed,
Pressure and digestion time have an impact resolution degree.In the digestion process, inventor's test of many times is found, if directly will
Microwave dissolver is located at higher temperature, and higher microwave energy, since quick-fried tank can occur for high temperature and pressure, and it is low to clear up degree.If
Using gradual heating, the mode of microwave energy is stepped up, quick-fried tank does not occur not only, further improves resolution degree.
Optimal mode is as described below:
The temperature of microwave dissolver is set in 160 °, maximum pressure 50bar, rotating speed 10r/min, microwave energy 80%,
Keep 10min;
It is warming up to 200 °, maximum pressure 50bar, rotating speed 5r/min later, microwave energy 80% keeps 5min;
It is warming up to 250 °, maximum pressure 50bar, rotating speed 5r/min later, microwave energy 100% keeps 5min.
It is found through experiment and comparison is repeated several times, using the heating step of top, resolution degree can be improved to the greatest extent.
If resolution can obtain transparent clear solution completely.It can carry out diluting work in next step when observing this solution
Make.
Solution after resolution is diluted using solvent.The solvent is free of element sulphur, can be water or low concentration
It is weakly acidic to be diluted to a certain concentration by the nitric acid of nitric acid such as 2% for solution.
By weakly acidic solution by plasma inductance coupling firing spectrum sample introduction, suitable element sulphur spectral line is selected, with mark
Line S180.672 is the first spectral line, measures sulfur content in optical film.
In this way, the present invention provides a kind of digestion procedures of PET classes film, as shown in Figure 1, including the following steps:
S11, the PET film is crushed, the distance of any two points of the diaphragm after crushing is not more than 1mm;
S12, the PET film after crushing is placed in micro-wave diminishing pot, and concentrated nitric acid is added;
S13, the micro-wave diminishing pot is placed in microwave dissolver and is cleared up, obtain digestion solution;
S14, the digestion solution is diluted to faintly acid with non-sulfur-bearing solvent;
S15, the measurement that element sulphur is carried out to obtained weakly acidic solution.
It should be noted that the weight of PET film to be cleared up in the present invention, the volume of concentrated nitric acid and the soft acid after dilution
Property solution measurer have certain proportionate relationship, it is abundant so could so that the reaction was complete.As the concentrated nitric acid volume with it is weak
The volume ratio of acid solution is 1:5-1:20, preferably 1:8-1:10.10-20gPET films are put into per 100ml concentrated nitric acids, it is excellent
Choosing is 15-17g.
It is compared below by way of specific embodiment, is known to the sulfur content of PET in each embodiment and comparative example
A, following rate of recovery are the sulfur content measured and the percentage of A.
Embodiment 1
Optical film is crushed to 1mm*1mm sizes;
The optical film products of precise 0.5g (being accurate to 0.1mg) are placed in polytetrafluoro micro-wave diminishing pot, are added 6ml's
65% concentrated nitric acid;
Micro-wave diminishing pot is placed in microwave dissolver, temperature program in setting such as following table is slowly added using temperature programming
Heat so that the digestion solution of gained is the solution of clear;
The solution of gained is diluted to 50ml faintly acids using 2% nitric acid;
By weakly acidic solution by plasma inductance coupling firing spectrum sample introduction, select suitable element sulphur spectral line with graticule
S180.672 is the first spectral line, measures sulfur content in optical film, and the sulfur content accuracy of measurement reaches 2ppm (mg/
kg)。
Embodiment 2
Optical film is crushed to 1mm*1mm sizes;
The optical film products of precise 0.5g (being accurate to 0.1mg) are placed in polytetrafluoro micro-wave diminishing pot, are added 6ml's
65% concentrated nitric acid;
Micro-wave diminishing pot is placed in microwave dissolver, temperature program in setting such as following table is slowly added using temperature programming
Heat so that the digestion solution of gained is the solution of clear;
The solution of gained is diluted to 50ml faintly acids using 2% nitric acid;
By weakly acidic solution by plasma inductance coupling firing spectrum sample introduction, select suitable element sulphur spectral line with graticule
S180.672 is the first spectral line, measures sulfur content in optical film, and the sulfur content accuracy of measurement reaches 2ppm (mg/
kg)。
Embodiment 3
Optical film is crushed to 0.5mm*0.7mm sizes;
The optical film products of precise 0.5g (being accurate to 0.1mg) are placed in polytetrafluoro micro-wave diminishing pot, are added 6ml's
65% concentrated nitric acid;
Micro-wave diminishing pot is placed in microwave dissolver, temperature program in setting such as following table is slowly added using temperature programming
Heat so that the digestion solution of gained is the solution of clear;
The solution of gained is diluted to 50ml faintly acids using 2% nitric acid;
By weakly acidic solution by plasma inductance coupling firing spectrum sample introduction, select suitable element sulphur spectral line with graticule
S180.672 is the first spectral line, measures sulfur content in optical film.
Comparative example 1
Optical film is crushed to 2mm*2mm sizes;
The optical film products of precise 0.5g (being accurate to 0.1mg) are placed in polytetrafluoro micro-wave diminishing pot, are added 6ml's
65% concentrated nitric acid;
Micro-wave diminishing pot is placed in microwave dissolver, temperature program in setting such as following table is slowly added using temperature programming
Heat so that the digestion solution of gained is the solution of clear;
The solution of gained is diluted to 50ml faintly acids using 2% nitric acid;
By weakly acidic solution by plasma inductance coupling firing spectrum sample introduction, select suitable element sulphur spectral line with graticule
S180.672 is the first spectral line, measures sulfur content in optical film.
Comparative example 2
Optical film is crushed to 2mm*2mm sizes;
The optical film products of precise 0.5g (being accurate to 0.1mg) are placed in polytetrafluoro micro-wave diminishing pot, are added 6ml's
65% concentrated nitric acid;
Micro-wave diminishing pot is placed in microwave dissolver, temperature program in setting such as following table is slowly added using temperature programming
Heat so that the digestion solution of gained is the solution of clear;
The solution of gained is diluted to 50ml faintly acids using 2% nitric acid;
By weakly acidic solution by plasma inductance coupling firing spectrum sample introduction, select suitable element sulphur spectral line with graticule
S180.672 is the first spectral line, measures sulfur content in optical film.
Following table is the sulfur content test data of embodiment 1-3 and comparative example 1-2.
From the comparison of embodiment 1 and embodiment 2, comparative example 2, comparative example 1 and the comparison of comparative example 2 can be seen that microwave
The temperature program of resolution instrument has measurement result important influence.
From the comparison of embodiment 1 and embodiment 3, comparative example 1, it can be seen that PET is crushed smaller, and measurement result is more accurate
Really.
The present invention is described by embodiment, but is not limited the invention, with reference to description of the invention, institute
Other variations of disclosed embodiment, are such as readily apparent that the professional person of this field, such variation should belong to
Within the scope of the claims in the present invention limit.
Claims (10)
1. a kind of PET film digestion procedure, which is characterized in that including:
S11, the PET film is crushed, the distance of any two points of the diaphragm after crushing is not more than 1mm;
S12, the PET film after crushing is placed in micro-wave diminishing pot, and concentrated nitric acid is added;
S13, the micro-wave diminishing pot is placed in microwave dissolver and is cleared up, obtain digestion solution;
S14, the digestion solution is diluted to faintly acid with non-sulfur-bearing solvent;
S15, the measurement that element sulphur is carried out to obtained weakly acidic solution.
2. PET film digestion procedure as described in claim 1, which is characterized in that use Freezing smashing mode in the S11.
3. PET film digestion procedure as described in claim 1, which is characterized in that the micro-wave diminishing pot is that polytetrafluoro microwave disappears
Solve tank.
4. PET film digestion procedure as described in claim 1, which is characterized in that a concentration of 65-68% of the concentrated nitric acid.
5. PET film digestion procedure as described in claim 1, which is characterized in that use gradual heating mode in the step S13
It is cleared up.
6. PET film digestion procedure as described in claim 1, which is characterized in that the digestion solution is clear digestion solution.
7. PET film digestion procedure as described in claim 1, which is characterized in that pass through plasma inductance coupling in the step S15
Transmitting graticule S180.672 is closed, sulfur content is measured.
8. PET film digestion procedure as described in claim 1, which is characterized in that the volume and weakly acidic solution of the concentrated nitric acid
Volume ratio be 1:5-1:20, preferably 1:8-1:10.
9. PET film digestion procedure as described in claim 1, which is characterized in that be put into 10-20gPET in per 100ml concentrated nitric acids
Film, preferably 15-17g.
10. PET film digestion procedure as described in claim 1, which is characterized in that
The step S13 includes:
The temperature of microwave dissolver is set in 160 °, maximum pressure 50bar, rotating speed 10r/min, microwave energy 80% is kept
10min;
It is warming up to 200 °, maximum pressure 50bar, rotating speed 5r/min later, microwave energy 80% keeps 5min;
It is warming up to 250 °, maximum pressure 50bar, rotating speed 5r/min later, microwave energy 100% keeps 5min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810274705.0A CN108693015A (en) | 2018-03-30 | 2018-03-30 | A kind of PET film digestion procedure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810274705.0A CN108693015A (en) | 2018-03-30 | 2018-03-30 | A kind of PET film digestion procedure |
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| Publication Number | Publication Date |
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| CN108693015A true CN108693015A (en) | 2018-10-23 |
Family
ID=63844678
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|---|---|---|---|
| CN201810274705.0A Withdrawn CN108693015A (en) | 2018-03-30 | 2018-03-30 | A kind of PET film digestion procedure |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102348772A (en) * | 2009-01-21 | 2012-02-08 | 生物圈工业有限责任公司 | Moisture resistant coating |
| CN104181147A (en) * | 2014-07-20 | 2014-12-03 | 中国人民解放军第五七一九工厂 | Test method for determining content of sulfur in lubrication oil |
| CN104297100A (en) * | 2014-10-27 | 2015-01-21 | 中国汽车技术研究中心 | Detection method for vanadium trace amount evaporation rate of vanadium-based selective catalyst |
| CN106404513A (en) * | 2015-07-24 | 2017-02-15 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for treating sample by using microwave digestion technology, and detection method using the same |
| KR101785958B1 (en) * | 2017-05-19 | 2017-10-17 | 서기찬 | Manufacturing method of microwave feed using the sweet potato and meat or fish for pet animal and the microwave feed from prepared therefrom |
-
2018
- 2018-03-30 CN CN201810274705.0A patent/CN108693015A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102348772A (en) * | 2009-01-21 | 2012-02-08 | 生物圈工业有限责任公司 | Moisture resistant coating |
| CN104181147A (en) * | 2014-07-20 | 2014-12-03 | 中国人民解放军第五七一九工厂 | Test method for determining content of sulfur in lubrication oil |
| CN104297100A (en) * | 2014-10-27 | 2015-01-21 | 中国汽车技术研究中心 | Detection method for vanadium trace amount evaporation rate of vanadium-based selective catalyst |
| CN106404513A (en) * | 2015-07-24 | 2017-02-15 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for treating sample by using microwave digestion technology, and detection method using the same |
| KR101785958B1 (en) * | 2017-05-19 | 2017-10-17 | 서기찬 | Manufacturing method of microwave feed using the sweet potato and meat or fish for pet animal and the microwave feed from prepared therefrom |
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Application publication date: 20181023 |