CN113960123A - Ammonia-sensitive flexible intelligent package for detecting freshness of fish - Google Patents
Ammonia-sensitive flexible intelligent package for detecting freshness of fish Download PDFInfo
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- CN113960123A CN113960123A CN202111281112.5A CN202111281112A CN113960123A CN 113960123 A CN113960123 A CN 113960123A CN 202111281112 A CN202111281112 A CN 202111281112A CN 113960123 A CN113960123 A CN 113960123A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 34
- 241000251468 Actinopterygii Species 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 35
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000007650 screen-printing Methods 0.000 claims abstract description 7
- 238000007639 printing Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 24
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229920000144 PEDOT:PSS Polymers 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 235000013372 meat Nutrition 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- -1 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 229920000767 polyaniline Polymers 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 238000007790 scraping Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000012544 monitoring process Methods 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 21
- 238000004140 cleaning Methods 0.000 abstract description 10
- 238000009450 smart packaging Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 2
- 229920002457 flexible plastic Polymers 0.000 abstract 1
- 239000002985 plastic film Substances 0.000 abstract 1
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 9
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 235000013332 fish product Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 208000001953 Hypotension Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 208000024780 Urticaria Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036543 hypotension Effects 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
- 239000011970 polystyrene sulfonate Substances 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 230000026041 response to humidity Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/12—Stencil printing; Silk-screen printing
Abstract
An ammonia-sensitive flexible intelligent package for detecting freshness of fish belongs to the technical field of intelligent packaging. The flexible ammonia gas sensor comprises a flexible substrate, an interdigital electrode and an ammonia gas sensitive layer, and the preparation method comprises the following steps: (1) cleaning a flexible plastic film with ethanol and then drying the film to be used as a flexible substrate; (2) printing the conductive metal paste into an interdigital electrode on a flexible substrate by a screen printing technology; (3) mixing PEDOT, PSS and WS2Coating the substrate surface with the interdigital electrode by an ultrasonic mixed rear layer; drying to obtain a flexible ammonia gas sensor; (4) and combining the ammonia gas sensor with the NFC label to finish the preparation of the ammonia-sensitive intelligent package. The sensor has good stability, strong reliability, repeated use, low response value to humidity, good response to ammonia gas and wide application prospect in the aspect of intelligent packaging.
Description
Technical Field
The invention belongs to the technical field of flexible gas sensors, and particularly relates to an ammonia-sensitive sensor capable of being applied to intelligent fish packaging, wherein the ammonia-sensitive sensor is based on PEDOT (PEDOT: PSS/WS)2CompoundingA flexible ammonia gas sensor and a preparation method thereof.
Background
Fish food provides a variety of nutrients including high quality proteins, polyunsaturated fatty acids, and a variety of vitamins and minerals. However, fish products are subject to deterioration during production, storage and sale due to the large time span and the difficult control of environmental conditions. During the deterioration process, substances such as protein, fat, amino acid, urea and the like in the fish products are easy to generate NH under the action of bacteria3And other gases, which may cause harm to human health and seriously cause hypotension, edema, urticaria, diarrhea, vomiting and other symptoms, therefore, NH3Can be used as a marker for detecting the freshness of various fish foods. Reacting NH3The sensor is combined with intelligent packaging, the content of ammonia gas generated by fish food can be monitored in real time, and the sensor has vital practical significance to human health.
Researchers find that metal oxides, graphene, sulfides and conductive polymers can be applied to detection of ammonia gas, and the patent CN103076370A discloses that an ink-jet printing technology is used to prepare a flexible ammonia gas sensor compounded by carbon nanotubes and PABS, and the sensor has a high response to ammonia gas, but a high temperature treatment process is used in preparation. Patent CN 109632890A prepares a PAA/AgNPs composite flexible ammonia gas sensor, and patent CN 109470752A discloses a sensor based on poly (3, 4-ethylenedioxythiophene): the preparation method of the polystyrene sulfonate (PEDOT: PSS) flexible ammonia gas sensor has good response to ammonia gas at room temperature, but has high cost and certain response to humidity. Therefore, an ammonia gas sensor which is simple in process flow and has certain anti-interference capability on humidity needs to be developed, so that the sensor can be applied to intelligent packaging of fish food and has good response on ammonia gas at room temperature.
Disclosure of Invention
The invention aims to solve the technical problem of providing a PEDOT (PSS)/WS (WS) solution aiming at the defects of the prior art2The preparation method of the flexible ammonia gas sensor enables the sensor to be applied to an intelligent bagAnd (6) assembling. According to the invention, dimethyl sulfoxide is added into a PEDOT/PSS aqueous solution, so that the prepared ammonia gas sensor has low responsiveness to humidity, the sensor is simple in preparation process, can detect ammonia gases with different concentrations at room temperature, has a good response value to low-concentration ammonia gases, and can be widely used for fresh and intelligent packaging of meat.
The invention provides a flexible ammonia gas sensor, comprising: the device comprises a flexible substrate, interdigital electrodes and a sensitive layer. The technical scheme is as follows:
(1) preparing a flexible substrate, carrying out ultrasonic cleaning on the flexible substrate by adopting ethanol, acetone and deionized water in sequence, and then carrying out drying treatment, preferably drying at the temperature of 70 ℃;
(2) printing metal conductive paste on a flexible substrate in a screen printing mode, and then drying at the temperature of 40-100 ℃ to prepare a metal interdigital electrode on the flexible substrate;
(3) taking PEDOT: PSS water solution, adding dimethyl sulfoxide, stirring, ultrasonic dispersing, and mixing with WS2And (3) mixing the aqueous solution, and uniformly dispersing by using ultrasonic to obtain a mixture based on PEDOT: ammonia sensitive solutions of PSS;
(4) coating the ammonia-sensitive solution on the metal electrode by adopting a dropping coating, scraping coating or spraying mode and the like, and then drying at the temperature of 40-80 ℃ for 30-60 minutes to prepare a flexible ammonia gas sensor;
(5) and connecting the NFC label with the prepared ammonia gas sensor, and placing the NFC label inside the package to finish the preparation of the ammonia-sensitive intelligent package.
Preferably, the flexible substrate is one of polyethylene terephthalate, polyimide, polyurethane, polydimethylsiloxane, polymethyl methacrylate and polycarbonate.
PEDOT in step (3): the concentration of the PSS aqueous solution is 1.5 wt%; dimethylsulfoxide and PEDOT: the volume ratio of the PSS aqueous solution is 100: 5; PEDOT: aqueous solutions of PSS and WS2The volume ratio of the solution is 100 (1-5); WS2The concentration of the solution was 1 mg/ml.
Preferably, the sensitive layer mainly comprises PEDOT: PSS, WS2Or WS2Replacing one or more of MWCNTs, GO, PANI and PPy;
preferably, the width of the interdigital pair of the metal interdigital electrode is 100-1000 microns.
The PEDOT PSS/WS prepared by the invention2The flexible ammonia gas sensor has the following advantages:
1. according to the invention, the metal conductive electrode is printed on the flexible substrate by silk-screen printing and then the ammonia-sensitive mixture solution is coated, so that the use of complex equipment and process is avoided, the method has the advantages of simplicity, rapidness, low cost and the like, and the preparation of a large-area high-sensitivity flexible ammonia gas sensor can be realized;
2. the sensor prepared by the invention has low response value to humidity and has good response to ammonia gas;
3. the flexible ammonia gas sensor prepared by the invention has good stability and strong reliability, can be repeatedly used, and has good application prospect in the aspect of intelligent packaging.
Drawings
FIG. 1 is a schematic view of the structure of an ammonia gas level sensor;
FIG. 2 is a response recovery curve of the ammonia gas sensor in example 1 in an ammonia gas atmosphere having a concentration of 1000 ppm;
FIG. 3 is a response curve of the ammonia gas sensor in example 2 exposed to an atmosphere of ammonia gas of different concentrations;
fig. 4 is a graph comparing the response of the ammonia gas sensor in the humidity environment in the comparative example and the example 2.
Detailed Description
In order to better illustrate the present invention, specific embodiments of the present invention will be clearly and completely described with reference to the comparative examples and the accompanying drawings.
Comparative example 1
(1) Ultrasonically cleaning the flexible substrate for 15min by using absolute ethyl alcohol, ultrasonically cleaning the flexible substrate for 15min by using acetone, finally cleaning the flexible substrate by using deionized water, and drying the flexible substrate in a vacuum drying oven at 70 ℃.
(2) Printing conductive silver paste into an electrode on a flexible substrate in a screen printing mode, wherein the width of the electrode is 500 micrometers, and then drying the electrode at the temperature of 40-100 ℃ to prepare a silver interdigital electrode on the flexible substrate;
(3) taking 1000 microliter of PEDOT with a concentration of 1.5%: PSS aqueous solution, with 40. mu.l of 1mg/ml WS2Mixing the solutions, and carrying out ultrasonic oscillation at 60Hz for 1 hour to obtain an ammonia-sensitive solution;
(4) 200 microliter of ammonia-sensitive solution is coated on the silver electrode by adopting a dripping mode, and then is dried for 30 minutes at the temperature of 60 ℃ and is dried for 1 hour at room temperature to prepare PEDOT (PSS/WS)2The flexible ammonia gas sensor of (1).
Example 1
(1) Ultrasonically cleaning the flexible substrate for 15min by using absolute ethyl alcohol, ultrasonically cleaning the flexible substrate for 15min by using acetone, finally cleaning the flexible substrate by using deionized water, and drying the flexible substrate in a vacuum drying oven at 70 ℃;
(2) printing conductive silver paste into an electrode on a flexible substrate in a screen printing mode, wherein the width of the electrode is 1mm, and then drying the electrode at the temperature of 40-100 ℃ to prepare a silver interdigital electrode on the flexible substrate;
(3) taking 1000 microliter of PEDOT with a concentration of 1.5%: PSS aqueous solution, adding 50 microliters of dimethyl sulfoxide solution, mixing well with 10 microliters of 1mg/ml WS2Mixing the solutions, and carrying out ultrasonic oscillation at 60Hz for 1 hour to obtain an ammonia-sensitive solution;
(4) 300 microliter of ammonia-sensitive solution is coated on the silver electrode by adopting a dripping mode, and then is dried for 30 minutes at the temperature of 60 ℃ and is dried for 1 hour at room temperature to prepare PEDOT (PSS/WS) in the embodiment 12The flexible ammonia gas sensor of (1);
(5) the NFC tag was connected to the ammonia sensor in example 1 and placed inside the package to complete the preparation of the ammonia-sensitive smart package.
Example 2
(1) Ultrasonically cleaning the flexible substrate for 15min by using absolute ethyl alcohol, ultrasonically cleaning the flexible substrate for 15min by using acetone, finally cleaning the flexible substrate by using deionized water, and drying the flexible substrate in a vacuum drying oven at 70 ℃;
(2) printing conductive silver paste into an electrode on a flexible substrate in a screen printing mode, wherein the width of the electrode is 500 micrometers, and then drying the electrode at the temperature of 40-100 ℃ to prepare a silver interdigital electrode on the flexible substrate;
(3) taking 1000 microliter of PEDOT with a concentration of 1.5%: PSS aqueous solution, adding 50 microliters of dimethyl sulfoxide solution, mixing well with 40 microliters of 1mg/ml WS2Mixing the solutions, and carrying out ultrasonic oscillation at 60Hz for 1 hour to obtain an ammonia-sensitive solution;
(4) 200 microliter of ammonia-sensitive solution is coated on the silver electrode by adopting a dripping mode, and then is dried for 30 minutes at the temperature of 50 ℃ and is dried for 2 hours at room temperature to prepare PEDOT (PSS/WS) in the embodiment 22The flexible ammonia gas sensor of (1);
(5) the NFC tag was connected to the ammonia sensor in example 2 and placed inside the package to complete the preparation of the ammonia-sensitive intelligent package.
FIG. 1 shows PEDOT: PSS/WS2The flexible ammonia gas sensor of (1). Wherein reference numeral 1 denotes a flexible substrate, reference numeral 2 denotes a metal interdigital electrode, and reference numeral 3 denotes a sensitive layer.
FIG. 2 is a response recovery curve of the ammonia gas sensor in example 1 in an ammonia gas atmosphere having a concentration of 1000 ppm. As can be seen from the graph, the resistance of the sensor in an ammonia gas atmosphere tends to increase first and then decrease, and the response is good.
FIG. 3 is a fitted curve of the response of the sensor of example 2 to exposure to an atmosphere of varying concentrations of ammonia; the response value is represented by the letter S, S ═ Rg-Ra/Ra. Wherein, Ra is the initial resistance of sensor, and Rg is the corresponding resistance value when certain concentration target detection gas of sensing device contact. As can be seen from fig. 3, as the ammonia gas concentration increases, the response value of the sensor also increases. And the ammonia concentration and the response value have very good linear relation (R)2=0.98558)。
Fig. 4 is a graph showing the change in resistance of the comparative example and example 2 in a different humidity environment. As can be seen from fig. 3, the ammonia gas sensor in the comparative example showed a very clear response to a change in humidity. When the relative humidity exceeds 23%, the response value increases with the increase of the humidity, and when the humidity reaches 85%, the response value reaches 94%.
The ammonia gas sensor in example 2 has a response value between 1% and 3% in a low-humidity and high-humidity environment, and has no obvious change. These results show that the flexible ammonia gas sensor of PEDOT: PSS/WS2 has potential application in intelligent packaging of fish food.
Claims (9)
1. A preparation method of an ammonia-sensitive flexible intelligent package for detecting freshness of fish meat is characterized by comprising the following steps:
(1) preparing a flexible substrate, carrying out ultrasonic cleaning on the flexible substrate by adopting ethanol, acetone and deionized water in sequence, and then carrying out drying treatment, preferably drying at the temperature of 70 ℃;
(2) printing metal conductive paste on a flexible substrate in a screen printing mode, and then drying at the temperature of 40-100 ℃ to prepare a metal interdigital electrode on the flexible substrate;
(3) taking PEDOT: PSS water solution, adding dimethyl sulfoxide, stirring, ultrasonic dispersing, and mixing with WS2And (3) mixing the aqueous solution, and uniformly dispersing by using ultrasonic to obtain a mixture based on PEDOT: ammonia sensitive solutions of PSS;
(4) coating the ammonia-sensitive solution on the metal electrode by adopting a dropping coating, scraping coating or spraying mode and the like, and then drying at the temperature of 40-80 ℃ for 30-60 minutes to prepare a flexible ammonia gas sensor;
(5) and connecting the NFC label with the prepared ammonia gas sensor, and placing the NFC label inside the package to finish the preparation of the ammonia-sensitive intelligent package.
2. The method of claim 1, wherein the flexible substrate is one of polyethylene terephthalate, polyimide, polyurethane, polydimethylsiloxane, polymethylmethacrylate, and polycarbonate.
3. The method for preparing an ammonia-sensitive flexible smart package for detecting freshness of fish meat according to claim 1, wherein the ratio of PEDOT: the concentration of the aqueous PSS solution was 1.5 wt%.
4. The method for preparing an ammonia-sensitive flexible smart package for detecting freshness of fish meat according to claim 1, wherein the ratio of dimethylsulfoxide to PEDOT: volume ratio of PSS aqueous solution is 5: 100.
5. the method for preparing an ammonia-sensitive flexible smart package for detecting freshness of fish meat according to claim 1, wherein the ratio of PEDOT: aqueous solutions of PSS and WS2The volume ratio of the solution is 100 (1-5); WS2The concentration of the solution was 1 mg/ml.
6. The method of claim 1, wherein WS in the sensitive layer is selected from the group consisting of a liquid, a gel2Can be replaced by one or more of MWCNTs, GO, PANI and PPy.
7. The method for preparing an ammonia-sensitive flexible intelligent package for detecting the freshness of fish meat according to claim 1, wherein the width of the interdigital pair of the metal interdigital electrode is 100 to 1000 microns.
8. An ammonia-sensitive flexible smart package prepared according to the method of any one of claims 1 to 7.
9. An ammonia-sensitive flexible smart package prepared according to the method of any one of claims 1 to 7 for packaging and monitoring fish freshness.
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