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CN115651297B - High-tightness isotope sampling bottle and preparation method and application thereof - Google Patents

High-tightness isotope sampling bottle and preparation method and application thereof Download PDF

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Publication number
CN115651297B
CN115651297B CN202211307664.3A CN202211307664A CN115651297B CN 115651297 B CN115651297 B CN 115651297B CN 202211307664 A CN202211307664 A CN 202211307664A CN 115651297 B CN115651297 B CN 115651297B
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parts
bottle
sampling bottle
antioxidant
tightness
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CN115651297A (en
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郭华良
彭玉荣
徐家明
齐继祥
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Institute of Hydrogeology and Environmental Geology CAGS
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Institute of Hydrogeology and Environmental Geology CAGS
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Abstract

The invention belongs to the technical field of closed plastic bottles, and discloses a high-tightness isotope sampling bottle, a preparation method and application thereof. The sampling bottle comprises a bottle body, a bottle cap and a gasket, wherein the gasket is arranged in the bottle cap. The invention realizes high air-isolation and airtight performance by optimizing the raw material composition of the bottle body and setting the thickness of the bottle body to be 2-4 mm, so that the sampling bottle can meet the requirements of 14 The requirements of sampling, sample preparation and testing in the year C technology can be matched with the used equipment. The sampling bottle uses high-density polyethylene as a main material, is compounded with nylon 6 and intercalated montmorillonite to improve gas barrier property, and intercalation groups of the intercalated montmorillonite have certain interaction with the high-density polyethylene, so that the intercalated montmorillonite is uniformly dispersed in the high-density polyethylene, and the barrier property is improved through a lamellar structure of the intercalated montmorillonite. The use of the nano particles not only improves the mechanical property of the sampling bottle, but alsoThe sampling bottle has a certain antibacterial function, so that the sample can be stored in the bottle for a long time.

Description

High-tightness isotope sampling bottle and preparation method and application thereof
Technical Field
The invention relates to the technical field of closed plastic bottles, in particular to a high-tightness isotope sampling bottle and a preparation method and application thereof.
Background
14 The C year-round method is gradually applied to related researches and surveys of geology fourth century, groundwater and the like since the 80 s of the last century. With the development of the technology, 14 the year C method gradually forms a series of mature technologies, and the collected sample to be tested is isolated relative to the air no matter sampling or sample preparation and measurement is carried out, so that CO in the air is avoided 2 Which requires a sample bottle or sample bottle with high gas barrier properties and sealing properties. In actual sampling and measuring operations, the sampling bottle is usually used for sampling and then is matched with the carbon fourteen vacuum sample preparation system, so that the subsequent vacuumizing sample preparation and detection are carried out, and the sampling bottle is not replaced any more so as to eliminate the influence of carbon dioxide to the greatest extent. Therefore, the sampling bottle is required not only to have tightness, but also to be vacuumized and not deformed.
At present, although a common medicine bottle made of PE, PP, PET and other materials for storing chemical reagents has certain sealing performance, the chemical reagents still have the phenomena of caking or wetting after long-time storage, and the use requirements of solid or liquid reagents with higher sealing requirements cannot be met. Based on this, there is a study on improvement of the structure of a sample bottle, for example, patent 201710553929.0 discloses a sealed bottle for storing chemical reagents, which mainly comprises a bottle body, one or several containers having a certain volume, a conduit passing through the inner cavity of the container and the sealed end of the container, a sealing cap mounted on the top of the conduit, and a sealing material between the sealing cap and the inner cavity of the container. The sealed bottle has good tightness, but needs a certain time when being sealed again after being opened, and the bottle mouth is irregular and can not be matched with the bottle 14 The equipment in the year C technology is well matched.
Therefore, a sample bottle pair which has good tightness, can store isotope samples and is not deformed by vacuumizing is developed 14 The development of the technology for measuring the year is of great significance.
Disclosure of Invention
The invention aims to provide a high-tightness isotope sampling bottle, a preparation method and application thereof, and solves the technical problems existing in the existing sampling bottle.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a high-tightness isotope sampling bottle, which comprises a bottle body, a bottle cap and a gasket, wherein the gasket is arranged in the bottle cap;
the body of the sampling bottle is prepared from the following raw materials in parts by mass:
60-80 parts of high-density polyethylene, 10-30 parts of polyamide, 1-15 parts of polyolefin elastomer, 5-15 parts of filler, 1-10 parts of compatilizer, 1-5 parts of plasticizer, 3-8 parts of antioxidant and 10-15 parts of nano particles.
Preferably, in the high-tightness isotope sampling bottle, the polyamide is nylon 6; the polyolefin elastomer is POE.
Preferably, in the high-tightness isotope sampling bottle, the filler is a mixture of intercalated montmorillonite and attapulgite; the mass ratio of the intercalated montmorillonite to the attapulgite is 3-5: 1 to 3.
Preferably, in the high-tightness isotope sampling bottle, the intercalated montmorillonite is one of cetyl ammonium bromide, cetyl ammonium chloride or dodecyl trimethyl ammonium bromide.
Preferably, in the high-tightness isotope sampling bottle, the compatilizer is HDPE-g-MAH; the plasticizer is tributyl citrate or acetyl tributyl citrate; the antioxidant is one or more of antioxidant 1010, antioxidant 168, antioxidant MB and antioxidant BHT; the nano particles are any two of nano titanium dioxide, nano silicon dioxide and nano zinc oxide.
Preferably, in the high-tightness isotope sampling bottle, the thickness of the bottle body is 2-4 mm.
Preferably, in the high-tightness isotope sampling bottle, the bottle cap is prepared from the following raw materials in parts by weight: 60-80 parts of polypropylene, 620-30 parts of nylon, 1-10 parts of intercalated montmorillonite, 1-10 parts of compatilizer, 1-10 parts of plasticizer and 1-5 parts of antioxidant;
the gasket is made of polytetrafluoroethylene-silica gel composite gasket.
The invention also provides a preparation method of the high-tightness isotope sampling bottle, which comprises the following steps: mixing raw materials of the bottle body, and sequentially performing injection molding, blow molding and demolding to obtain the bottle body of the high-tightness isotope sampling bottle;
the preparation method of the bottle cap comprises the following steps: extruding, granulating and injection molding the raw materials of the bottle cap to obtain the bottle cap of the high-tightness isotope sampling bottle.
The invention also provides an application of the high-tightness isotope sampling bottle in a device for collecting underground water-dissolved inorganic carbon radioactive analysis samples, a device for acidolysis and sample preparation of liquid-flash carbon fourteen samples or an organic carbon high-temperature airtight combustion system.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention realizes high air-isolation and airtight performance by optimizing the raw material composition of the sampling bottle body and setting the thickness of the bottle body to be 2-4 mm, so that the sampling bottle can meet the requirements of 14 The requirements of sampling, sample preparation and testing in the year C technology can be matched with the used equipment.
(2) The sampling bottle of the invention uses high-density polyethylene as main material, and is compounded with nylon 6 and intercalated montmorillonite to improve gas barrier property, and the intercalated group of intercalated montmorillonite has certain interaction with the high-density polyethylene, so that the intercalated montmorillonite is uniformly dispersed in the high-density polyethylene, and the barrier property is improved through the lamellar structure of intercalated montmorillonite.
(3) The use of the nano particles not only improves the mechanical property of the sampling bottle, but also ensures that the sampling bottle has a certain antibacterial function, so that the collected sample can be stored in the bottle for a long time.
Detailed Description
The invention provides a high-tightness isotope sampling bottle, which comprises a bottle body, a bottle cap and a gasket, wherein the gasket is arranged in the bottle cap;
the body of the sampling bottle is prepared from the following raw materials in parts by mass:
60-80 parts of high-density polyethylene, 10-30 parts of polyamide, 1-15 parts of polyolefin elastomer, 5-15 parts of filler, 1-10 parts of compatilizer, 1-5 parts of plasticizer, 3-8 parts of antioxidant and 10-15 parts of nano particles.
In the invention, the bottle body is preferably prepared from the following raw materials in parts by weight: 62-78 parts of high-density polyethylene, 13-29 parts of polyamide, 4-14 parts of polyolefin elastomer, 7-13 parts of filler, 2-8 parts of compatilizer, 1.5-4.5 parts of plasticizer, 4-7 parts of antioxidant and 11-14 parts of nano particles; the preparation method is further preferably prepared from the following raw materials in parts by weight: 66-75 parts of high-density polyethylene, 18-24 parts of polyamide, 7-11 parts of polyolefin elastomer, 8-12 parts of filler, 3-6 parts of compatilizer, 2.2-3.5 parts of plasticizer, 5-6 parts of antioxidant and 12-13 parts of nano particles; more preferably, the material is prepared from the following raw materials in parts by weight: 69 parts of high-density polyethylene, 19 parts of polyamide, 10 parts of polyolefin elastomer, 11 parts of filler, 5 parts of compatilizer, 2.5 parts of plasticizer, 5.6 parts of antioxidant and 12.6 parts of nano particles.
In the present invention, the polyamide is preferably nylon 6; the polyolefin elastomer is preferably POE.
In the invention, the filler is preferably a mixture of intercalated montmorillonite and attapulgite; the mass ratio of the intercalated montmorillonite to the attapulgite is preferably 3-5: 1 to 3, more preferably 3.3 to 4.6:1.2 to 2.8, more preferably 4.2: 2.3.
In the present invention, the intercalated montmorillonite is preferably one of cetyl ammonium bromide, cetyl ammonium chloride or dodecyl trimethyl ammonium bromide.
In the invention, the preparation method of the intercalated montmorillonite comprises the following steps: mixing sodium montmorillonite and water to obtain montmorillonite solution; mixing an intercalation agent with water by taking one of hexadecyl ammonium bromide, hexadecyl ammonium chloride or dodecyl trimethyl ammonium bromide as the intercalation agent to obtain an intercalation agent solution; mixing the intercalation agent solution and the montmorillonite solution, stirring for a certain time, and standing for layering; washing the precipitate obtained by standing and layering with water until no precipitate is generated by dropwise adding silver nitrate solution into the supernatant, thereby obtaining the intercalated montmorillonite.
In the present invention, the compatibilizer is preferably HDPE-g-MAH; the plasticizer is preferably tributyl citrate or acetyl tributyl citrate, and more preferably acetyl tributyl citrate; the antioxidant is preferably one or more of antioxidant 1010, antioxidant 168, antioxidant MB and antioxidant BHT, more preferably one or more of antioxidant 1010, antioxidant MB and antioxidant BHT, and even more preferably an oxidizing agent MB; the nanoparticle is preferably any two of nano titanium dioxide, nano silicon dioxide and nano zinc oxide, more preferably a mixture of nano titanium dioxide and nano silicon dioxide or a mixture of nano zinc oxide and nano titanium dioxide, and even more preferably a mixture of nano zinc oxide and nano titanium dioxide; the particle diameter of the nanoparticle is preferably 10 to 300nm, more preferably 30 to 220nm, and even more preferably 160nm.
In the present invention, the thickness of the body is preferably 2 to 4mm, more preferably 2.3 to 3.7mm, and still more preferably 3.1mm.
In the invention, the bottle cap is prepared from the following raw materials in parts by weight:
60-80 parts of polypropylene, 620-30 parts of nylon, 1-10 parts of intercalated montmorillonite, 1-10 parts of compatilizer, 1-10 parts of plasticizer and 1-5 parts of antioxidant.
In the invention, the bottle cap is preferably prepared from the following raw materials in parts by weight: 61-76 parts of polypropylene, 621-28 parts of nylon, 2-9 parts of intercalated montmorillonite, 3-9 parts of compatilizer, 3-8 parts of plasticizer and 1.6-4.2 parts of antioxidant; the preparation method is further preferably prepared from the following raw materials in parts by weight: 66-73 parts of polypropylene, 624-27 parts of nylon, 3-8 parts of intercalated montmorillonite, 4-8 parts of compatilizer, 4-7 parts of plasticizer and 2.6-3.7 parts of antioxidant; more preferably, the material is prepared from the following raw materials in parts by weight: 68 parts of polypropylene, 626 parts of nylon, 6 parts of intercalated montmorillonite, 7 parts of compatilizer, 5 parts of plasticizer and 2.9 parts of antioxidant.
In the invention, the intercalated montmorillonite in the raw material of the bottle cap is preferably cetyl ammonium bromide intercalated modified sodium montmorillonite; the compatilizer is preferably PP-g-MAH; the plasticizer is preferably tributyl citrate or acetyl tributyl citrate, and more preferably tributyl citrate; the antioxidant is preferably one or more of antioxidant 1010, antioxidant 168 and antioxidant BHT, more preferably antioxidant 1010 or antioxidant 168, and even more preferably antioxidant 168.
In the invention, the gasket is preferably made of polytetrafluoroethylene-silica gel composite gasket; the gasket is a commercial product and is purchased from Nantong cloud range experimental equipment Co., ltd; the preparation method of the gasket is not limited, and the polytetrafluoroethylene-silica gel composite gasket can be purchased by a person skilled in the art. In the invention, one side of the polytetrafluoroethylene material of the gasket is contacted with the bottle mouth of the bottle body, and one side of the silica gel material is contacted with the bottle cap.
The invention also provides a preparation method of the high-tightness isotope sampling bottle, which comprises the following steps: mixing raw materials of the bottle body, and sequentially performing injection molding, blow molding and demolding to obtain the bottle body of the high-tightness isotope sampling bottle;
the preparation method of the bottle cap comprises the following steps: extruding, granulating and injection molding the raw materials of the bottle cap to obtain the bottle cap of the high-tightness isotope sampling bottle.
In the invention, an injection molding machine is used for injection molding in the preparation method of the bottle body and the bottle cap; the temperature of the front region of the charging barrel of the injection molding machine is independently preferably 160-185 ℃, more preferably 163-178 ℃, and even more preferably 172 ℃; the feeding temperature is independently preferably 220 to 245 ℃, more preferably 224 to 241 ℃, and even more preferably 237 ℃.
In the present invention, the pressure of the blow molding in the process for producing a body is preferably 0.5 to 1.2MPa, more preferably 0.7 to 1.1MPa, still more preferably 0.9MPa; the time for blow molding is preferably 1 to 60 seconds, more preferably 5 to 50 seconds, and still more preferably 24 seconds.
In the present invention, the temperature of extrusion granulation in the method for producing the bottle cap is preferably 180 to 240 ℃, more preferably 187 to 232 ℃, and still more preferably 206 ℃.
The invention also provides an application of the high-tightness isotope sampling bottle in a device for collecting underground water-dissolved inorganic carbon radioactive analysis samples, a device for acidolysis and sample preparation of liquid-flash carbon fourteen samples or an organic carbon high-temperature airtight combustion system.
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a high airtight isotope sampling bottle, and this sampling bottle includes body, bottle lid and gasket, and the gasket is arranged in the bottle lid.
The preparation method of the body of the sampling bottle comprises the following steps:
(1) 70 parts of high-density polyethylene, 623 parts of nylon, 11 parts of POE, 5 parts of intercalated montmorillonite, 3 parts of attapulgite, 7 parts of HDPE-g-MAH, 4 parts of tributyl citrate, 10105 parts of antioxidant, 6 parts of nano titanium dioxide with the particle size of 100nm and 6 parts of nano silicon dioxide with the particle size of 100nm are mixed to obtain a mixture;
(2) Injecting the mixture into an injection molding machine, wherein the temperature of the front area of a charging barrel is 175 ℃, and the feeding temperature is 225 ℃ to obtain a bottle blank;
(3) Placing the bottle blank into a blow molding die, wherein the blow molding pressure is 1MPa, and the time is 20s, so as to obtain a molded bottle body; and demolding the formed bottle body in a mold to obtain the bottle body with the volume of 1L and the thickness of 3.8 mm.
The preparation method of the bottle cap of the sampling bottle comprises the following steps:
70 parts of polypropylene, 625 parts of nylon, 4 parts of intercalated montmorillonite, 7 parts of PP-g-MAH, 6 parts of acetyl tributyl citrate and 10105 parts of antioxidant are mixed, extruded and granulated at 220 ℃ by an extruder; and then injection molding is carried out in an injection molding machine, the temperature of the front area of the charging barrel is 165 ℃, and the feeding temperature is 235 ℃, so as to obtain the bottle cap.
The gasket is a polytetrafluoroethylene-silica gel composite gasket.
The preparation method of the intercalated montmorillonite in the bottle body and the bottle cap comprises the following steps: 5g of sodium montmorillonite and 100mL of water are mixed to obtain montmorillonite solution; mixing 4g of cetyl ammonium bromide with 150mL of water to obtain an intercalating agent solution; mixing the intercalation agent solution and the montmorillonite solution, stirring at 70 ℃ for 3 hours, and standing for layering; washing the precipitate obtained by standing and layering with water until 0.1mol/L silver nitrate solution is added dropwise into the supernatant without precipitation, thus obtaining the intercalated montmorillonite.
Example 2
The embodiment provides a high airtight isotope sampling bottle, see in particular embodiment 1, and the difference is that the raw materials of the bottle body are: 62 parts of high-density polyethylene, 630 parts of nylon, 6 parts of POE, 8 parts of intercalated montmorillonite, 6 parts of attapulgite, 3 parts of HDPE-g-MAH, 3 parts of tributyl citrate, 7 parts of antioxidant BHT, 5 parts of nano titanium dioxide with the particle size of 200nm and 10 parts of nano zinc oxide with the particle size of 200 nm; the thickness of the bottle body is 2.8mm.
Example 3
The embodiment provides a high airtight isotope sampling bottle, see in particular embodiment 1, and the difference is that the raw materials of the bottle body are: 80 parts of high-density polyethylene, 616 parts of nylon, 15 parts of POE, 10 parts of intercalated montmorillonite, 5 parts of attapulgite, 1 part of HDPE-g-MAH, 2 parts of acetyl tributyl citrate, 8 parts of antioxidant MB, 5 parts of nano silicon dioxide with the particle size of 50nm and 5 parts of nano zinc oxide with the particle size of 100 nm; the thickness of the bottle body is 2.2mm.
Comparative example 1
This comparative example provides a sampling bottle, see in particular example 1, with the difference that the body thickness is 1mm.
Comparative example 2
This comparative example provides a sampling bottle, see in particular example 1, except that the raw materials of the body do not contain nylon 6, POE.
The body obtained in examples 1 to 3 and comparative examples 1 to 2 was subjected to performance test, and the results are shown in Table 1.
Table 1 results of body Performance test
Sample of Tensile strength MPa Oxygen transmission rate g/(m) 2 ·d) Water transmittance g/(m) 2 ·d)
Example 1 106.4 0.054 0.043
Example 2 103.7 0.063 0.056
Example 3 104.9 0.057 0.067
Comparative example 1 87.2 1.369 1.794
Comparative example 2 75.3 1.428 1.921
As shown in Table 1, the sampling bottle of the invention has excellent mechanical properties, has higher barrier property for oxygen and water, and can meet the requirements of storage and test of samples with higher requirements on tightness. From comparative examples 1 to 2, it is evident that the thickness of the body and the addition of the barrier material have significant effects on mechanical properties, air permeability and water permeability.
The sample bottle of the embodiment 1 is used for storing a certain water sample, and after the water sample is stored for 3 years, the apparent age of carbon fourteen can reach 43.75 kiloyears, and the detection result is ideal, so that the sample bottle can store the sample for a long time, and has excellent tightness and gas barrier property.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (6)

1. The high-tightness isotope sampling bottle is characterized by comprising a bottle body, a bottle cap and a gasket, wherein the gasket is arranged in the bottle cap;
the body of the sampling bottle is prepared from the following raw materials in parts by mass:
60-80 parts of high-density polyethylene, 10-30 parts of polyamide, 1-15 parts of polyolefin elastomer, 5-15 parts of filler, 1-10 parts of compatilizer, 1-5 parts of plasticizer, 3-8 parts of antioxidant and 10-15 parts of nano particles;
the filler is a mixture of intercalated montmorillonite and attapulgite; the mass ratio of the intercalated montmorillonite to the attapulgite is 3-5: 1 to 3; the intercalation montmorillonite is one of cetyl ammonium bromide, cetyl ammonium chloride or dodecyl trimethyl ammonium bromide;
the thickness of the bottle body is 2-4 mm.
2. The high closure isotope sampling bottle of claim 1 wherein the polyamide is nylon 6; the polyolefin elastomer is POE.
3. A highly airtight isotope sampling bottle according to claim 1 or 2, wherein said compatibilizer is HDPE-g-MAH; the plasticizer is tributyl citrate or acetyl tributyl citrate; the antioxidant is one or more of antioxidant 1010, antioxidant 168, antioxidant MB and antioxidant BHT; the nano particles are any two of nano titanium dioxide, nano silicon dioxide and nano zinc oxide.
4. The high-tightness isotope sampling bottle as claimed in claim 1, wherein the bottle cap is prepared from the following raw materials in parts by weight: 60-80 parts of polypropylene, 620-30 parts of nylon, 1-10 parts of intercalated montmorillonite, 1-10 parts of compatilizer, 1-10 parts of plasticizer and 1-5 parts of antioxidant;
the gasket is made of polytetrafluoroethylene-silica gel composite gasket.
5. The method for preparing a high-tightness isotope sampling bottle according to any one of claims 1 to 4, wherein the method for preparing the bottle body comprises the following steps: mixing raw materials of the bottle body, and sequentially performing injection molding, blow molding and demolding to obtain the bottle body of the high-tightness isotope sampling bottle;
the preparation method of the bottle cap comprises the following steps: extruding, granulating and injection molding the raw materials of the bottle cap to obtain the bottle cap of the high-tightness isotope sampling bottle.
6. The use of a highly airtight isotope sampling bottle as claimed in any one of claims 1 to 4 in a groundwater dissolved inorganic carbon radioactivity analysis sample collection device, a liquid flash carbon fourteen sample acidolysis sample preparation device or an organic carbon high temperature airtight combustion system.
CN202211307664.3A 2022-10-25 2022-10-25 High-tightness isotope sampling bottle and preparation method and application thereof Active CN115651297B (en)

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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101768302A (en) * 2008-12-29 2010-07-07 上海杰事杰新材料股份有限公司 Preparation method of high barrier property polyethylene/nylon 6 in-situ nanocomposite material
CN113121903A (en) * 2021-04-12 2021-07-16 金富科技股份有限公司 High-barrier plastic bottle cap and preparation method thereof

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Publication number Priority date Publication date Assignee Title
KR100508907B1 (en) * 2001-12-27 2005-08-17 주식회사 엘지화학 Nanocomposite blend composition having super barrier property
US7368496B2 (en) * 2001-12-27 2008-05-06 Lg Chem, Ltd. Nanocomposite composition having super barrier property and article using the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101768302A (en) * 2008-12-29 2010-07-07 上海杰事杰新材料股份有限公司 Preparation method of high barrier property polyethylene/nylon 6 in-situ nanocomposite material
CN113121903A (en) * 2021-04-12 2021-07-16 金富科技股份有限公司 High-barrier plastic bottle cap and preparation method thereof

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