CN205683702U - A kind of sample centrifugal filter without shifting solution - Google Patents

A kind of sample centrifugal filter without shifting solution Download PDF

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Publication number
CN205683702U
CN205683702U CN201620509847.7U CN201620509847U CN205683702U CN 205683702 U CN205683702 U CN 205683702U CN 201620509847 U CN201620509847 U CN 201620509847U CN 205683702 U CN205683702 U CN 205683702U
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China
Prior art keywords
filter
pipe
adapter
filter tube
tube
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Withdrawn - After Issue
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CN201620509847.7U
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Chinese (zh)
Inventor
朱鹏飞
刘文卫
凌霞
孔令灿
姚誉阳
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Wuxi Center for Disease Control and Prevention
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Wuxi Center for Disease Control and Prevention
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Abstract

This utility model relates to a kind of sample centrifugal filter without shifting solution, belongs to laboratory sample pretreatment technology field.It is formed by receiving pipe, filter tube, adapter and screw lid, all threaded by match each other;Described reception pipe upper end open, lower end closed, filter tube upper end open, lower end is latticed, the equal opening in the upper and lower two ends of adapter, for a connecting pipe, screw lid upper end closed, lower ending opening;During filter centrifugation, filter tube is arranged at above reception pipe, and filter tube top is by screw cap closures;When sample introduction is analyzed, adapter is arranged at above reception pipe, and adapter top is by screw cap closures.This utility model centrifugal filter overcomes existing filter to use loaded down with trivial details drawback, it is possible to simplifies the filtration step before sample Instrumental Analysis, is effectively improved work efficiency.

Description

A kind of sample centrifugal filter without shifting solution
Technical field
This utility model relates to a kind of sample centrifugal filter without shifting solution, belongs to laboratory sample pre-treatment skill Art field.
Background technology
High performance liquid chromatograph (HPLC) is large-sized analytic instrument conventional in physicochemical analysis work, chromatographic column conduct Playing the main consumptive material of liquid phase separation effect, expensive, the height of its performance determines the effect of liquid phase separation, and chromatographic column Post pressure is one of major parameter weighing column performance, and along with chromatographic column uses the increase of time, it is by sample solution The blocking of particulate matter also can be day by day serious, and the post pressure of chromatographic column also can increase accordingly, the performance of chromatographic column is also the most corresponding reduces.With The upgrading of HPLC, Ultra Performance Liquid Chromatography instrument (UPLC) becomes increasingly popular, provisioned chromatographic column aperture and the grain of filler Footpath is less, it is easier to the phenomenon of chromatographic column blocking occurs, and its price is the most more expensive, and sample pre-treatments final step is filtered step Rapid requirement is higher.Therefore, when sample pre-treatments, remove the particulate matter in sample solution, be beneficial to reduce chromatographic column blocking Risk, keep the performance of chromatographic column, extend the service life of chromatographic column, thus reduce experimental cost.At present, typically used The particulate matter in sample solution, float etc. are removed in filter, centrifugal method may block the material of chromatographic column.
But prior art there is problems in that
1, the most conventional using method for proceeding to injection needles, after connecting filter, by sample solution by liquid By filter membrane, and collect filtrate in sample introduction bottle.The defect of the method is inefficient when batch samples pre-treatment, needs The most manually to pipette operation, there is also injection needles head in use and stab the possibility of experimenter's hands, and physics and chemistry divides There is the standard solution of a large amount of high toxicity, high concentration in analysis laboratory, has potential health hazard;
2, there is product to use the mode of centrifugal filter, but remain a need for after being centrifuged filtrate is manually transferred to sample introduction bottle In, add manual labor and error experimentally may be brought.
Summary of the invention
The purpose of this utility model is to provide a kind of sample centrifugal filter without shifting solution, this sample centrifugal filtration Device overcomes the shortcoming that existing filter uses operation, it is possible to simplifies the filtration step before sample Instrumental Analysis, is effectively improved Work efficiency.
The technical solution of the utility model, a kind of sample centrifugal filter without shifting solution, it is by receiving pipe, filtering Pipe, adapter and screw lid composition, all threaded by match each other;
Described reception pipe upper end open, lower end closed, filter tube upper end open, lower end is latticed, adapter upper and lower two Hold equal opening, for a connecting pipe, screw lid upper end closed, lower ending opening;
During filter centrifugation, filter tube is arranged at above reception pipe, and filter tube top is by screw cap closures;When sample introduction is analyzed, Adapter is arranged at above reception pipe, and adapter top is by screw cap closures.
Described reception pipe upper end inwall is provided with the first female thread;Filter tube upper end is provided with the first pin thread, and lower end is provided with Two pin threads;Adapter upper end is provided with the 3rd pin thread, and lower end is provided with the 4th pin thread;Screw lid inwall is provided with the second cloudy spiral shell Stricture of vagina;
During filter centrifugation, the second pin thread of filter tube lower end is connected with the first female thread coupling receiving pipe upper end, mistake First pin thread of chimney filter upper end is connected with the second female thread coupling of screw lid inwall;
When sample introduction is analyzed, the 3rd pin thread of adapter upper end is connected with the second female thread coupling of screw lid inwall, suitable 4th pin thread of orchestration lower end is provided with the first female thread coupling with reception pipe upper end inwall and is connected.
Described reception pipe is made up of the reception pipe pipe shoulder receiving pipe body be arranged at reception pipe body top;Filter tube by Filter tube body and filter tube pipe shoulder composition, filter tube pipe shoulder is arranged in the middle part of filter tube body;Adapter is by adapter body With adapter tube shoulder composition, adapter tube shoulder is arranged in the middle part of adapter body;
During filter centrifugation, receive pipe with the relative position between filter tube by connecing that reception pipe pipe shoulder and filter tube pipe are takeed on Touch and be defined;
During sample introduction analysis, receive pipe with the relative position between adapter by connecing that reception pipe pipe shoulder and adapter tube are takeed on Touch and be defined.
Described reception pipe is provided with the first graduation mark and the second graduation mark.First graduation mark corresponding solution volume is 0.5mL, Second graduation mark corresponding solution volume is 1.0mL.
One layer of filter membrane it is provided with bottom described filter tube.
Described screw lid hollow, has a through hole at upper end closed, fix one layer of sample introduction pad in through hole.
Receive pipe size a be 11mm, b be 9mm, c be 4mm, d be 2mm, e be 19mm, f≤10mm, purpose is centrifugal for coupling The aperture requirement of machine.
Described filter tube size g be 7mm, h be 4mm, i be 17mm, j be 4mm, k be 2mm, l be 10mm, m be 8mm.
Described adapter size n be 10mm, o be 7mm, p be 4mm, q be 4mm.
Described screw lid size r be 11mm, s be 6mm, t be 5mm, u be 9mm.
Described reception pipe, filter tube, adapter, screw lid are polypropylene material, according to the character of filter solvents not With, the filter membrane material in filter tube includes nylon, cellulose, politef etc.;According to filter after particulate matter size want Asking, filter membrane aperture can be divided into 0.22 μm or 0.45 μm.
This utility model compared with prior art, has the following advantages and effect:
1, this product centrifugal filter material is simple, cheap, is suitable to promote the use of in physico-chemical analysis field;
2, the screw lid used is consistent with the specification of the sample injection bottle screw lid of the instruments such as chromatograph of liquid, enhances this sample The versatility of product centrifugal filter;
3, this product centrifugal filter is when carrying out sample solution filter operation, is designed as this centrifugal filter overall length (c+d + e+i+h) it is less than 10mm less than 46mm, the bottom external diameter f of receptor, with the size of adaptive centrifuge;
4, this product centrifugal filter is after centrifugal, have employed adapter, by ingenious to receptor and screw lid connection, and will The design of its overall length is less than 34mm, with adaptive high performance liquid chromatograph specimen disc and the dimensional requirement of sampling system;
5, this product centrifugal filter uses centrifugation to filter sample, it is to avoid what disposable syringe stabbed staff can Can, and reduce the tedious steps of conventional process filtration;
6, this product each several part is provided with pipe shoulder, receives pipe pipe shoulder and enable to receive pipe clamp centrifugal in centrifugation step On machine rotor, filter tube pipe shoulder, adapter tube shoulder make filter tube receive on pipe with adapter card the most respectively, add screw thread The coupling of end uses so that this product centrifugal filter is more firm when operation;
7, the filter membrane in filter tube is divided into various material, mainly includes nylon, cellulose, politef etc., favorably Filtration in heterogeneity solution;
8, this product centrifugal filter is applicable to the pre-treatment of batch sample, without shifting solution after filtration, eliminates mesh Before have method to use centrifugal segregation impurity or centrifugal filtration after, still need to shift the step of sample solution, greatly reduce artificial In labor time, improve work efficiency.
Accompanying drawing explanation
Fig. 1 is this utility model structural representation.
Fig. 1-1 assembles schematic diagram for filter centrifugation;Fig. 1-2 is that sample introduction analysis assembles schematic diagram.
Fig. 2 is this utility model decomposition texture schematic diagram.
Fig. 2-a is for receiving tubular construction schematic diagram, and Fig. 2-b is filter tube structural representation, and Fig. 2-c is adapter structure signal Figure, Fig. 2-d is screw lid structural representation.
Description of reference numerals: 1, receive pipe;1-1, reception pipe body;1-2, reception pipe pipe shoulder;1-3, the first graduation mark;1- 4, the second graduation mark;2, filter tube;2-1, filter tube body;2-2, filter tube pipe are takeed on;2-3, filter membrane;3, adapter;3-1、 Adapter body;3-2, adapter tube are takeed on;4, screw lid;4-1, sample introduction pad;5-1, the first female thread;5-2, the second female thread; 6-1, the first pin thread;6-2, the second pin thread;6-3, the 3rd pin thread;6-4, the 4th pin thread.
Detailed description of the invention
Embodiment 1 one kinds is without shifting the sample centrifugal filter of solution
As shown in Figure 1-2, it is formed by receiving pipe 1, filter tube 2, adapter 3 and screw lid 4, all by matching each other Threaded;
Described reception pipe 1 upper end open, lower end closed, filter tube 2 upper end open, lower end is latticed, adapter about 3 The equal opening in two ends, for a connecting pipe, screw lid 4 upper end closed, lower ending opening;
During filter centrifugation, filter tube 2 is arranged at above reception pipe 1, and filter tube 2 top is closed by screw lid 4;Sample introduction is analyzed Time, adapter 3 is arranged at above reception pipe 1, and adapter 3 top is closed by screw lid 4.
Described reception pipe 1 upper end inwall is provided with the first female thread 5-1;Filter tube 2 upper end is provided with the first pin thread 6-1, under End is provided with the second pin thread 6-2;Adapter 3 upper end is provided with the 3rd pin thread 6-3, and lower end is provided with the 4th pin thread 6-4;Screw lid 4 inwalls are provided with the second female thread 5-2.
Described reception pipe 1 is by receiving pipe body 1-1 and being arranged at the reception pipe pipe shoulder 1-2 group on reception pipe body 1-1 top Become;Filter tube 2 is takeed on 2-2 by filter tube body 2-1 and filter tube pipe and is formed, and filter tube pipe shoulder 2-2 is arranged at filter tube body 2-1 Middle part;Adapter 3 is takeed on 3-2 by adapter body 3-1 and adapter tube and is formed, and adapter tube shoulder 3-2 is arranged at adapter body In the middle part of 3-1;
During filter centrifugation, receive the relative position between pipe 1 and filter tube 2 by receiving pipe pipe shoulder 1-2 and filter tube pipe The contact of shoulder 2-2 is defined;
When sample introduction is analyzed, receive the relative position between pipe 1 and adapter 3 by receiving pipe pipe shoulder 1-2 and adapter tube The contact of shoulder 3-2 is defined.
Described reception pipe 1 is provided with the first graduation mark 1-3 and the second graduation mark 1-4.First graduation mark 1-3 corresponding solution body Amassing as 0.5mL, the second graduation mark 1-4 corresponding solution volume is 1.0mL.
One layer of filter membrane 2-3 it is provided with bottom described filter tube 2.
Described screw lid 4 hollow, has a through hole at upper end closed, fix one layer of sample introduction pad 4-1 in through hole.
Receive pipe 1 size a be 11mm, b be 9mm, c be 4mm, d be 2mm, e be 19mm, f≤10mm, purpose for coupling from The aperture requirement of scheming.
Filter tube 2 size g be 7mm, h be 4mm, i be 17mm, j be 4mm, k be 2mm, l be 10mm, m be 8mm.
Adapter 3 size n be 10mm, o be 7mm, p be 4mm, q be 4mm.
Screw lid 4 size r be 11mm, s be 6mm, t be 5mm, u be 9mm.
Described reception pipe, filter tube, adapter, screw lid are polypropylene material, according to the character of filter solvents not With, the filter membrane material in filter tube includes nylon, cellulose, politef etc.;According to filter after particulate matter size want Asking, filter membrane aperture can be divided into 0.22 μm or 0.45 μm.
When this utility model carries out sample solution filter operation, first by the second pin thread 6-2 of filter tube 2 lower end with connect First female thread 5-1 coupling of closed tube 1 upper end connects, the of the first pin thread 6-1 of filter tube 2 upper end and screw lid 4 inwall Two female thread 5-2 couplings connect;Then reception pipe 1 is put in centrifuge, now, make this reality by receiving pipe pipe shoulder 1-2 Carry out spacing with novel with centrifuge;After centrifugal filtration, remove the end of thread at two;
3rd pin thread 6-3 of adapter 3 upper end is connected with the second female thread 5-2 coupling of screw lid 4 inwall, adaptive The first female thread 5-1 coupling that 4th pin thread 6-4 of device 3 lower end is provided with reception pipe 1 upper end inwall is connected, and can be directly used for The Instrumental Analysis such as chromatograph of liquid.
Application Example 1
Hereinafter the sample centrifugal filter without shifting solution provided by the utility model is applied to liquid chromatograph string Clenobuterol hydrochloride, Ractopamine, the residual quantity of albuterol in connection mass spectrometric determination Carnis Sus domestica:
Weigh 2g(and be accurate to 0.01g) sample through smashing to pieces in 50mL politef centrifuge tube, add 8mL sodium acetate Buffer, fully mixes, and adds 50 μ L β-glucal glycosides enzyme/aryl sulfatase, mixes rear 37 DEG C of water-baths hydrolysis 12h. Add the internal standard of 10 μ L 1ng/mL, fully mix and be centrifuged (4000r/min), take 4mL supernatant and add 0.1mol/L perchloric acid Solution 5mL, mix homogeneously, with perchloric acid regulation pH value to 1 ± 0.3.After 4000r/min is centrifuged 5min, whole supernatant are turned Move on in 50mL centrifuge tube, with the sodium hydroxide regulation pH value of 10mol/L to 11, add 10mL saturated nacl aqueous solution and 10mL Isopropanol-ethyl acetate (6+4) mixed solution, fully extracts, centrifugal 5min under 4000r/min.
Shift whole organic facies, dried up with nitrogen under 40 DEG C of water-baths.Add 5mL sodium acetate buffer, ultrasonic mixed Even, standby after making residue fully dissolve.
60mg, 3mL cation exchange solid-phase extraction column MCX is placed in solid-phase extraction device, successively with 3mL methanol, 3mL water Activation, crosses post by above-mentioned residue solution, and successively with 2mL water, 2mL 2% formic acid water and 2mL methanol washing pillar, and employing is taken out true Empty mode pumps the solvent in solid-phase extraction column.Then with 2mL 5% ammonia methanol solution eluting, eluent is 40 DEG C of water-baths Lower nitrogen dries up.Accurately add 1mL 0.1% formic acid/water-methanol solution (95+5), after vortex oscillator fully mixes, Pipetting in complete soln extremely filter tube 2 of the present utility model, now the filter membrane 2-3 in filter tube 2 is nylon material.
Second pin thread 6-2 of filter tube 2 lower end is connected with the first female thread 5-1 coupling receiving pipe 1 upper end, filters After first pin thread 6-1 of pipe 2 upper end connects with the second female thread 5-2 coupling of screw lid 4 inwall, it is placed in a centrifuge, Centrifugal 5min under 4000r/min.
After being centrifuged, filtrate is automatically transferred to receive in pipe 1, removes the end of thread at above-mentioned two, by adapter 3 lower end 4th pin thread 6-4 connects with the first female thread 5-1 coupling receiving pipe 1 upper end, the 3rd pin thread 6-3 of adapter 3 upper end Connect with the second female thread 5-2 coupling of screw lid 4 inwall, can be directly used for the Instrumental Analysis such as chromatograph of liquid.
Chromatographic condition: performance liquid chromatographic column: Agilent C18 post (granularity 1.7 μm, 2.1 mm × 50 mm);Column temperature: 30℃;Sampling volume 20 μ L.Flowing phase: A is 1mmol/L ammonium acetate, 0.1% formic acid water, and B is 1mmol/L ammonium acetate, 0.1% first Acid acetonitrile water (acetonitrile+water=90+10).Flow velocity is 0.2 mL/min.
Mass Spectrometry Conditions: electron spray (ESI), positive ion mode, multiple-reaction monitoring (MRM) scan mode;Ion injection electric (IS): 5500V;Atomization gas temperature: 500 DEG C;GS1:55psi;GS2:35psi;Collision gas CAD:Medium;Gas curtain gas CUR: 30psi.Use MRM monitoring pattern, go a bunch voltage, collision energy should be optimized to optimum sensitivity, monitoring ion pair: hydrochloric acid gram human relations Special sieve 277.1/203.1(quota ion), 77.1/259.1;Ractopamine 302.2/164.2(quota ion), 302.2/ 284.2;Albuterol 240.2/148.1(quota ion), 240.2/222.3.Deuterated salt Clenbuterol 286.1/204.1 (quota ion);Deuterated Ractopamine 308.3/168.3(quota ion);Deuterated albuterol 243.2/151.1(quantitatively from Son).
Sample filter without shifting solution provided by the utility model is compared with conventional filter, it is to avoid Disposable syringe stabs the possibility of staff, simplifies the tedious steps of conventional process filtration, when reducing sample solution transfer There is error and human cost, it is adaptable to the quick process of batch sample, it is ensured that sample pretreatment process high efficiency operates.
Polypropylene material used in centrifugal filter without shifting solution provided by the utility model, filter membrane material Material is commercially available thing, and simple to operate, easy, can apply to various sample Pesticides, veterinary drug, mycotoxin pre-treatment work In filtration step.

Claims (10)

1. one kind without shifting the sample centrifugal filter of solution, it is characterised in that: it is by receiving pipe (1), filter tube (2), suitable Orchestration (3) and screw lid (4) composition, all threaded by match each other;
Described reception manages (1) upper end open, and lower end closed, filter tube (2) upper end open, lower end is latticed, on adapter (3) The equal opening in lower two ends, for a connecting pipe, screw lid (4) upper end closed, lower ending opening;
During filter centrifugation, filter tube (2) is arranged at reception pipe (1) top, and filter tube (2) top is closed by screw lid (4);Sample introduction During analysis, adapter (3) is arranged at reception pipe (1) top, and adapter (3) top is closed by screw lid (4).
The most according to claim 1 without shifting the sample centrifugal filter of solution, it is characterised in that: described reception manages (1) Upper end inwall is provided with the first female thread (5-1);Filter tube (2) upper end is provided with the first pin thread (6-1), and lower end is provided with the second sun spiral shell Stricture of vagina (6-2);Adapter (3) upper end is provided with the 3rd pin thread (6-3), and lower end is provided with the 4th pin thread (6-4);In screw lid (4) Wall is provided with the second female thread (5-2);
During filter centrifugation, second pin thread (6-2) of filter tube (2) lower end and the first female thread (5-1) receiving pipe (1) upper end Coupling connects, and first pin thread (6-1) of filter tube (2) upper end mates with second female thread (5-2) of screw lid (4) inwall even Connect;
When sample introduction is analyzed, the 3rd pin thread (6-3) of adapter (3) upper end and second female thread (5-2) of screw lid (4) inwall Coupling connects, and the 4th pin thread (6-4) of adapter (3) lower end manages, with receiving, the first female thread (5-that (1) upper end inwall is provided with 1) coupling connects.
The most according to claim 1 without shifting the sample centrifugal filter of solution, it is characterised in that: described reception manages (1) By receive pipe body (1-1) and be arranged at receive pipe body (1-1) top reception pipe pipe take on (1-2) form;Filter tube (2) by Filter tube body (2-1) and filter tube pipe shoulder (2-2) composition, filter tube pipe shoulder (2-2) is arranged in filter tube body (2-1) Portion;Adapter (3) is takeed on (3-2) by adapter body (3-1) and adapter tube and is formed, and adapter tube shoulder (3-2) is arranged at adaptation Device body (3-1) middle part;
During filter centrifugation, receive the relative position between pipe (1) and filter tube (2) by receiving pipe pipe shoulder (1-2) and filter tube The contact of pipe shoulder (2-2) is defined;
When sample introduction is analyzed, receive the relative position between pipe (1) and adapter (3) by receiving pipe pipe shoulder (1-2) and adapter The contact of pipe shoulder (3-2) is defined.
The most according to claim 1 without shifting the sample centrifugal filter of solution, it is characterised in that: described reception manages (1) It is provided with the first graduation mark (1-3) and the second graduation mark (1-4).
The most according to claim 1 without shifting the sample centrifugal filter of solution, it is characterised in that: described filter tube (2) Bottom is provided with one layer of filter membrane (2-3).
The most according to claim 1 without shifting the sample centrifugal filter of solution, it is characterised in that: described screw lid (4) Hollow, has a through hole at upper end closed, fix one layer of sample introduction pad (4-1) in through hole.
The most according to claim 5 without shifting the sample centrifugal filter of solution, it is characterised in that: described filter membrane (2- 3) aperture is 0.22 μm or 0.45 μm.
The most according to claim 5 without shifting the sample centrifugal filter of solution, it is characterised in that: described filter membrane (2- 3) material is nylon, cellulose or politef.
The most according to claim 1 without shifting the sample centrifugal filter of solution, it is characterised in that: described reception pipe (1), Filter tube (2), adapter (3) and screw lid (4) are polypropylene material.
10. according to one of claim 1-9 Suo Shu without shifting the sample centrifugal filter of solution, it is characterised in that:
The described pipe (1) that receives: receiving pipe pipe shoulder (1-2) diameter a is 11mm, and receiving pipe body (1-1) internal diameter b is 9mm, external diameter f ≤ 10mm, the first female thread (5-1) width c are 4mm;
Described filter tube (2): filter tube pipe shoulder (2-2) diameter l is 10mm, and filter tube body (2-1) internal diameter g is 7mm, external diameter m Being 4mm for 8mm, the first pin thread (6-1) width h, the second pin thread (6-2) width j is 4mm;
Described adapter (3): adapter tube shoulder (3-2) diameter n is 10mm, and adapter body (3-1) external diameter o is 7mm, the 3rd sun Screw thread (6-3) width p is 4mm, and the 4th pin thread (6-4) width q is 4mm;
Described screw lid (4): external diameter r is 11mm, internal diameter u be 9mm, highly t be 5mm, through-hole diameter s is 6mm.
CN201620509847.7U 2016-05-31 2016-05-31 A kind of sample centrifugal filter without shifting solution Withdrawn - After Issue CN205683702U (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105935514A (en) * 2016-05-31 2016-09-14 无锡市疾病预防控制中心 Solution transfer-free sample centrifuge filter

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105935514A (en) * 2016-05-31 2016-09-14 无锡市疾病预防控制中心 Solution transfer-free sample centrifuge filter
CN105935514B (en) * 2016-05-31 2017-11-28 无锡市疾病预防控制中心 A kind of sample centrifugal filter that need not shift solution

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Granted publication date: 20161116

Effective date of abandoning: 20171128