CN106496857A - A kind of bisphenol-A measure standard substance and preparation method thereof - Google Patents
A kind of bisphenol-A measure standard substance and preparation method thereof Download PDFInfo
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- CN106496857A CN106496857A CN201610962903.7A CN201610962903A CN106496857A CN 106496857 A CN106496857 A CN 106496857A CN 201610962903 A CN201610962903 A CN 201610962903A CN 106496857 A CN106496857 A CN 106496857A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- G01N2001/2893—Preparing calibration standards
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Abstract
The present invention is applied to the compositions field of macromolecular compound, there is provided a kind of bisphenol-A measure standard substance and preparation method thereof.The component of the bisphenol-A measure standard substance that the present invention is provided includes bisphenol-A, Corvic, main plasticiser, heat stabilizer, lubricant and antioxidant.The composition designability of the bisphenol-A measure standard substance is strong, by adjusting each component content, makes the uniformity of the bisphenol-A measure standard substance of acquisition high, good stability.The bisphenol-A measure standard substance make the measure to bisphenol-A in PVC food contact materials more convenient, while improve the accuracy of its testing result.
Description
Technical field
The invention belongs to the compositions field of macromolecular compound, more particularly to a kind of bisphenol-A measure standard substance and its
Preparation method.
Background technology
Polrvinyl chloride (PVC) is one of utilization rate highest plastic packing bag, is often commonly used by people for packaging heating food,
Such as fritters of twisted dough, cake, meat and cooked food class etc. are containing the high food of oils and fatss.Bisphenol-A, scientific name 2,2- bis- (4- hydroxy phenyls) propane, letter
Claim diphenol propane, be one of most popular industrial compound in the world, be a kind of important organic intermediate, be synthesis
The important source material of Merlon, poly- vitriol resin, polyether-ketone, epoxy resin and poly- vitriol etc., is also commonly used for the interpolation of the plastics such as PVC
Agent, moulds mainly for the production of water bottle, canned food inner packing, tableware, packaging material for food, dental fillings, articles for babies etc.
Material industry.However, environment and the mankind are caused to endanger by a large amount of productions of bis-phenol and using it certainly will be made constantly to be transferred in environment
Evil.As most of food are wrapped inside dress or liner using plastic, bisphenol-A then may be from plastic packaging bag to food
Product, particularly contain fatty foods, migrate such as in milk, meat, the time that food store in plastic package material is longer, or use
In the plastic material of packaged food, content of bisphenol A is higher, can all increase the amount that bisphenol-A is migrated in food, i.e., to food
Pollution level is bigger.
China has strict regulation in terms of food packaging material, and such as GB 9685-2008 define food contact to be held
Bisphenol-A maximum magnitude used in device, material；GB 31604.10-2016 also specify the detection method of bisphenol-A.European Union
EC/1895/2005 regulations limit the Special migration of bisphenol-A in food or simulated foods should<3mg/kg, 2011 by repairing
The stripping quantity for ordering bisphenol-A in regulation plastic baby feeding bottle in the 2011/8/EU of 2002/72/EC standard formulations should be less than 0.6mg/
Kg (food or food simulants), U.S. FDA specify that the migration amount of bisphenol-A must not be higher than 0.05mg/kg.
Therefore, bisphenol-A measure standard substance are developed it is used for the comparison of bisphenol-A detection data, the accuracy of detection method and tests
Card, the quality control of the calibration of detecting instrument and test result and examination significant.
Content of the invention
The technical problem to be solved is to provide a kind of bisphenol-A measure standard substance and preparation method thereof, purport
In material is made, the detection of bisphenol-A is more convenient, while improving the accuracy of detection.
The present invention is achieved in that a kind of bisphenol-A measure standard substance, the bisphenol-A measure standard substance include with
The following components of percentage by weight meter：
Further, the main plasticiser be ATBC, trioctyl trimellitate (TOTM), epoxy soybean oil,
At least one in dioctyl adipate and triphenyl phosphite is described.
Further, the heat stabilizer be lead stearate, calcium stearate, zinc stearate, maleic acid dioctyltin and
At least one in the different monooctyl ester dioctyltin of two Thioglycolic acids.
Further, the lubricant is at least one in EBS, ACR, chlorinated paraffin and butyl stearate.
Further, the antioxidant be four [β-(3,5- di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester,
2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols), three [2.4- di-tert-butyl-phenyls] phosphite esters and triphenyl phosphite
In at least one.
Present invention also offers the preparation method of above-mentioned bisphenol-A measure standard substance, comprises the following steps：
Corvic, main plasticiser, heat stabilizer, lubricant and antioxidant is weighed, detection is sampled；
Above-mentioned each raw material is mixed with bisphenol-A, mixture is obtained；
The mixture is carried out melting extrusion by 25-55 rev/min of rate of feeding input double screw extruder, and is adopted
Hot cut method pelletize is used, micelle is obtained；
By the micelle mixed at high speed ,-extruding pelletization 4-7 time is melted repeatedly by above-mentioned steps, the bisphenol-A is obtained and is determined
Use standard substance.
Further, the temperature during mixing is 85-95 DEG C, and rotating speed is 1200 revs/min, mixes 60-120 minutes.
Further, the pan feeding section temperature of the melting extrusion is 130-150 DEG C, and compression section temperature is 140-160 DEG C,
It is 155-175 DEG C to change section temperature, and screw speed is 50-85 rev/min, and fervent rotating speed is 50-120 rev/min.
Further, the rotating speed of the mixed at high speed is 800 revs/min, and the time is 10-20 minutes.
Further, the content of bisphenol A in the bisphenol-A measure standard substance is 0.01～10.0mg/kg.
Compared with prior art, beneficial effect is the present invention：Bisphenol-A measure standard provided in an embodiment of the present invention
Product, composition designability are strong, by adjusting each component content, make the uniformity of the bisphenol-A measure standard substance of acquisition high, stable
Property is good.The bisphenol-A measure standard substance make the measure to bisphenol-A in PVC food contact materials more convenient, while improve
The accuracy of its testing result.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only in order to explain the present invention
Limit the present invention.
A kind of bisphenol-A measure standard substance are embodiments provided, the bisphenol-A measure standard substance are included with weight
The following components of amount percentages：
Bisphenol-A measure standard substance provided in an embodiment of the present invention, composition designability are strong, are contained by adjusting each composition
Amount, makes the uniformity of the bisphenol-A measure standard substance of acquisition high, good stability.By hydrogen bond and model between bisphenol-A and plastic molecules
De Huali connects, and retains each relatively independent chemical property each other, and bisphenol-A is easier to move in environment from plastics.Described
Bisphenol-A measure standard substance are measured to the content of bisphenol-A in PVC food contact materials, can make continuous mode more just
Victory, while improve the accuracy of its testing result.
Specifically, the Corvic can be with other plurality of raw materials, such as plasticizer, filler and other polymer phases
Hold.
The main plasticiser is that ATBC, trioctyl trimellitate (TOTM), epoxy soybean oil, adipic acid two are pungent
At least one in ester and triphenyl phosphite.
The heat stabilizer includes that lead stearate, calcium stearate, zinc stearate, maleic acid dioctyltin and two dredge base second
At least one in the different monooctyl ester dioctyltin of acid.The heat stabilizer is used as standard substance processing heat stability auxiliary agent.Polychlorostyrene second
The heat stability of olefine resin is poor, and the use of the additive such as main plasticiser, lubricant can change outside the physics of polrvinyl chloride (PVC)
See and operating characteristic, but the decomposition of polymer can not be prevented.(such as heat, radiation) and (oxygen, ozone) factor of chemistry in physics
Effect is lower to make each polymeric material of the standard substance gradually decompose, and the stabilizer can effectively be prevented, reduces or be stopped
The degraded of each polymeric material in the standard substance.
The lubricant includes at least one in EBS, ACR, chlorinated paraffin and butyl stearate.The lubricant conduct
Standard substance processing and lubrication auxiliary agent.High polymer after melting have higher viscosity, in process, the high polymer of melting
When by runners such as narrow slit, cast gates, polymer melt will produce friction with processing equipment surface, and some frictions are to polymer
Processing be very unfavorable, these frictions reduce fluidity of molten, while serious friction can make film surface become coarse,
Lack gloss or flow liner occur.The lubricant can improve lubricity, reduce friction, reduces Interface Adhesion performance.Additionally, institute
State lubricant and can improve mobility, play the effects such as melting accelerator, anti and antistatic agent, slipping agent.
The antioxidant includes four [β-(3,5- di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester (antioxidation
Agent 1010), 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols) (antioxidant 2246), three [2.4- di-tert-butyl-phenyls]
At least one in phosphite ester (antioxidant 168) and triphenyl phosphite.The antioxidant is anti-as standard substance processing
Oxidation promoter.In manufacture, processing, storage and application process, it is anti-that polymeric material therein oxidation to the standard substance can occur
Answer and cause material degradation or crosslinking, so as to change the performance of material.The oxidizing process of the polymeric material is free radical type
Chain reflex, the plastics antioxidant can capture reactive radical species, generate nonactive free radical, or can decompose
The polymer hydroperoxides produced in oxidizing process, terminate chain reflex, so as to delay the oxidation of the polymeric material
Process, enables polymeric material to be smoothed out processing, and increases the service life.
In bisphenol-A measure standard substance provided in an embodiment of the present invention, by optimizing concrete material used by each component, institute is made
State bisphenol-A measure standard substance stability high, with thermal ageing resistant performance high, meet melting extrusion technique needs repeatedly and each
The advantages of component is not separated out.
The embodiment of the present invention additionally provides the preparation method of above-mentioned bisphenol-A measure standard substance, comprises the following steps：
Corvic, main plasticiser, heat stabilizer, lubricant and antioxidant is weighed, detection is sampled, with true
Protect above-mentioned raw materials and do not contain target compound bisphenol-A；
Above-mentioned each raw material is mixed with bisphenol-A, mixture is obtained；
The mixture is carried out melting extrusion by 25-55 rev/min of rate of feeding input double screw extruder, and is adopted
Hot cut method pelletize is used, micelle is obtained；
By the micelle mixed at high speed ,-extruding pelletization 4-7 time is melted repeatedly by above-mentioned steps.
The preparation method of bisphenol-A measure standard substance provided in an embodiment of the present invention, using mixed at high speed, melts repeatedly and mixes
The mode that refining expressing technique combines, process are simple, make obtained standard sample uniformity height, good stability.Additionally, the system
Preparation Method overcomes traditional single melting extrusion technique and blowing is prepared in sample technique, is the uniformity for ensureing sample, must
Must give up extrusion finished product front 1/5 and rear 1/5 part, only stay mid portion product shortcoming.By the embodiment of the present invention
The bisphenol-A measure standard substance that preparation method is prepared be columned granule, wherein content of bisphenol A be 0.01～
10.0mg/kg.
Specifically, the temperature during mixing is 85-95 DEG C, and rotating speed is 1200 revs/min, mixes 60-120 minutes.
The pan feeding section temperature of the melting extrusion is 130-150 DEG C, and compression section temperature is 140-160 DEG C, homogenizing zone temperature
For 155-175 DEG C, screw speed is 50-85 rev/min, and fervent rotating speed is 50-120 rev/min.
The rotating speed of the mixed at high speed is 800 revs/min, and the time is 10-20 minutes.
The embodiment of the present invention makes the bisphenol-A standard for preparing by being optimized to each design parameter in preparation process
Sample has corresponding function.Bisphenol-A standard sample prepared by the present invention detects work containing bisphenol-A suitable for laboratory monitoring plastics
The quality evaluation of work, Laboratory Accreditation and proficiency testing, are also applied for measuring method evaluation, tester are examined and surveyed
Evaluation of amount uncertainty etc..
Embodiment
By taking the formula that gross weight is as 5kg, content of bisphenol A is as 10.0mg/kg as an example, a kind of bisphenol-A standard sample, its component
Including：
Corvic：3095.45g；
Calcium stearate：200.0g；
Zinc stearate：100.0g；
Butyl stearate：100.0kg；
Trioctyl trimellitate (TOTM)：1500.0g；
Antioxidant 1010：2.5g；
Antioxidant 168：2g；
Bisphenol-A 50.0mg.
The preparation method is as follows：
Weigh 3095.45g polrvinyl chloride and be added to high-speed mixer, then weigh calcium stearate 200.0g, zinc stearate
100.0g, butyl stearate 100.0g, trioctyl trimellitate (TOTM) 1500.0g, antioxidant 1010 2.5g and antioxidant 168
2g mixes 10 minutes with polrvinyl chloride by 50r/min；
Weigh bisphenol-A 50.0mg to put in high-speed mixer, open the heating of high-speed mixer chuck, temperature setting is
90 DEG C, mixed at high speed 120 minutes under 1200 revs/min of rotating speed；
The material powder feed machine of mix homogeneously is entered by 25-55 rev/min of rate of feeding input double screw extruder
Row melting extrusion, using hot cut method pelletize, technological parameter is as follows：Pan feeding section 130-150 DEG C, 140-160 DEG C of compression section, homogenizing zone
155-175 DEG C, 50-85 rev/min of screw speed, 50-120 rev/min of fervent rotating speed；
The micelle that produces is put in high-speed mixer, under 800 revs/min of rotating speed after mixed at high speed 10-20 minute
Press above-mentioned steps melting extrusion pelletize 6 times repeatedly, you can the uniform and stable standard sample of target compound bisphenol-A is obtained.
Uniformity testing is carried out to above standard sample：
(1) weigh at least 0.1g samples, be put in the flat screw socket bottle of 40mL browns.3mL normal hexane is added, is mixed, added
2mL methanol-water mixtures (1+1), ultrasound 60 minutes, stratification in supersonic cleaning machine.Lower floor is drawn with syringe water-soluble
Liquid, is tested for LC-MS after 0.2 μm of membrane filtration.
(2) LC-MS test conditions：
Chromatographic column：C18Post, column length 150mm, internal diameter 4.6mm, 5 μm of granularity, or the chromatographic column of equal performance；Mobile phase：First
Alcohol-water-ammonia water (70+30+0.1)；Flow velocity：0.5mL/min；Column temperature：Room temperature；Sample size：1μL；
Ionization mode：Electron spray ionisation negative ion mode (ESI-)；Scanning of the mass spectrum mode：Multiple-reaction monitoring (MRM)；Mist
Activating QI：207Pa；Spray voltage：500V；Capillary voltage：3500V；Air velocity：8L/min；Gas flow temperature：330℃；Sheath gas
(N2) flow velocity：11L/min；Sheath gas (N2) temperature：250℃；Fragmentation voltage：125V；Collision energy：20eV；Parent ion m/z
227；Quota ion m/z 211.9；Qualitative ion m/z 132.8.
(3) result of calculation：
According to known concentration of standard solution and response value Criterion working curve, LC-MS Chemstation software roots
Solution concentration result is calculated automatically according to the response value of sample, and computing formula is：Content of bisphenol A (mg/kg)=C × V × D/W,
Wherein C is the content (unit mg/L) of bisphenol-A in LC-MS Instrument measuring solution；V is that bisphenol-A extracts the total of pre-treatment addition water
Volume (Unit/mL)；D be LC-MS examination with computer dilution gfactors, D=1 if undiluted；Weight (unit gs) of the W for sample.
(4) calibration standard solution concentration
The preparation of standard solution is first pipetted the standard substance solution of 2.5mL, is settled to 25mL, is matched somebody with somebody using stepwise dilution method
The storing solution of 100mg/L is made, storing solution stepwise dilution concentration in table 1 is recycled, calibration curve is obtained.
1 calibration standard solution concentration of table
| Analytes | Standard1 | Standard2 | Standard3 | Standard4 | Standard5 |
| Bisphenol-A | 1mg/L | 2mg/L | 5mg/L | 10mg/L | 20mg/L |
Bisphenol-A mark sample tests：
Measurement result carries out data statistic analysis using variance statistic method.Through statistical computation, double in standard substance sample
The uniformity testing result of phenol A is as shown in table 4 below, in all standard substance samples the F values of bisphenol-A be respectively less than F0.05 (24,25)
=1.96, multinomial bisphenol-A has good uniformity in the standard substance sample, and uniformity testing method is sampled as 0.1g, final really
Standard substance minimum sample mass is determined for 0.1g.The detailed result of calculation of the uniformity testing of each bisphenol-A is shown in Table 2.
2 standard sample bisphenol-A uniformity testing result (mg/kg) of table
Presently preferred embodiments of the present invention is the foregoing is only, not in order to limit the present invention, all in essence of the invention
Any modification, equivalent and improvement that is made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of bisphenol-A measure standard substance, it is characterised in that the bisphenol-A measure standard substance are included with percentage by weight
The following components of meter：
2. bisphenol-A measure standard substance as claimed in claim 1, it is characterised in that the main plasticiser is acetyl tributyl citrate
At least one institute in tri-n-butyl, trioctyl trimellitate (TOTM), epoxy soybean oil, dioctyl adipate and triphenyl phosphite
State.
3. bisphenol-A measure standard substance as claimed in claim 1, it is characterised in that the heat stabilizer is lead stearate, hard
At least one in the different monooctyl ester dioctyltin of fat acid calcium, zinc stearate, maleic acid dioctyltin and two Thioglycolic acids.
4. bisphenol-A measure standard substance as claimed in claim 1, it is characterised in that the lubricant is EBS, ACR, chlorination
At least one in paraffin and butyl stearate.
5. bisphenol-A measure standard substance as claimed in claim 1, it is characterised in that the antioxidant is four [β-(3,5-
Di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester, 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols), three
At least one in [2.4- di-tert-butyl-phenyls] phosphite ester and triphenyl phosphite.
6. the preparation method of the bisphenol-A measure standard substance as described in claim 1 to 5 any one, it is characterised in that include
Following steps：
Corvic, main plasticiser, heat stabilizer, lubricant and antioxidant is weighed, detection is sampled；
Above-mentioned each raw material is mixed with bisphenol-A, mixture is obtained；
The mixture is carried out melting extrusion by 25-55 rev/min of rate of feeding input double screw extruder, and using heat
Pressure method pelletize, obtains micelle；
By the micelle mixed at high speed ,-extruding pelletization 4-7 time is melted repeatedly by above-mentioned steps, bisphenol-A measures is obtained and is marked
Quasi- product.
7. preparation method as claimed in claim 6, it is characterised in that the temperature during mixing is 85-95 DEG C, rotating speed is
1200 revs/min, mix 60-120 minutes.
8. preparation method as claimed in claim 6, it is characterised in that the pan feeding section temperature of the melting extrusion is 130-150
DEG C, compression section temperature is 140-160 DEG C, and homogenizing zone temperature is 155-175 DEG C, and screw speed is 50-85 rev/min, earnestly turns
Speed is 50-120 rev/min.
9. preparation method as claimed in claim 6, it is characterised in that the rotating speed of the mixed at high speed is 800 revs/min, when
Between be 10-20 minutes.
10. preparation method as claimed in claim 6, it is characterised in that the bisphenol-A in the bisphenol-A measure standard substance contains
Measure as 0.01～10.0mg/kg.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106916410A (en) * | 2017-04-11 | 2017-07-04 | 东莞出入境检验检疫局检验检疫综合技术中心 | Bisphenol-A and nonyl phenol standard sample and preparation method thereof in ABS plastic |
| CN108276648A (en) * | 2018-03-13 | 2018-07-13 | 宁波出入境检验检疫局检验检疫技术中心 | A kind of food packaging vinyon evaporation residue standard sample master batch particle and preparation method thereof |
| CN114196139A (en) * | 2021-12-27 | 2022-03-18 | 国高材高分子材料产业创新中心有限公司 | PVC matrix atomization standard substance and preparation method thereof |
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