CN101975740A - Medical magnesium alloy biodegradability in-vitro dynamic simulation test equipment - Google Patents
Medical magnesium alloy biodegradability in-vitro dynamic simulation test equipment Download PDFInfo
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Abstract
The invention discloses medical magnesium alloy biodegradability in-vitro dynamic simulation test equipment, which comprises a power tank, a test bin, a lower sample loading device, an air metering device, a liquid suction pipe, a first return pipe, a second return pipe and the like, wherein the liquid suction pipe, the first return pipe and the second return pipe are arranged in a liquid tank respectively; the liquid tank is placed in a constant-temperature tank; a flowmeter is fixed vertically; the lower sample loading device is positioned in the test bin; the air metering device is vertically fixed over the lower sample loading device; the power tank and the test bin are horizontally fixed an adjustable-height base respectively; and the suction pipe and the inlet of a circulating pump as well as the outlet of the circulating pump and the inlet of the flowmeter, the outlet of the flowmeter and the inlet pipe of the power tank, the outlet pipe of the power tank and the inlet pipe of the test bin, the outlet pipe of the test bin and the first return pipe and the overflow pipe of the power tank and the second return pipe are connected by water pipes to form a liquid medium circulating path. The equipment can realize the controlled flowing of liquid in a circulating system and the real-time collection and synchronous accurate metering of an insoluble gas product.
Description
Technical field
The invention belongs to material properties test technology and equipment field, relate to a kind of equipment that in fluid media (medium), the material corrosion degradation property is carried out the dynamic simulant test evaluation, be specially adapted to the external dynamic simulant test of bio-medical material/apparatus such as medical magnesium alloy and medical device product biodegradability thereof.
Background technology
Be on active service material in liquid environment, as the medicine equipment in the implant into body, naval vessels boats and ships etc. in the seawater, and the relative motion between medium has crucial influence to its corrosion degradation behavior.Studies show that this relative motion not only can change the corrosion degradation speed of material/apparatus, and can change its corrosion degraded type and mechanism thereof.Therefore, simulate the especially relative motion between surrounding medium and material/apparatus of actual duty status, medium degraded aggressivity and material/true rule of apparatus corrosion degradation behavior, exploitation new material/new apparatus and degraded control technology thereof etc. are significant for disclosing.
With the bio-medical metal material is example, magnesium alloy is with its resource, price and performance especially biodegradation-absorbability, biocompatibility and mechanical compatibility advantage, being expected to becomes desirable bio-medical metal new material, is used for design, the manufacturing of the high medical device product of added values such as coronary artery bracket, tissue engineering bracket, nail, hone lamella, skeletal framework and artificial bone.But the too fast problem of biodegradation is but restricting the bio-medical of magnesium alloy always.Therefore, research magnesium alloy biodegradation behavior rule, exploitation magnesium alloy biodegradation control technology (comprising new alloy exploitation, surface modification etc.) are significant.In the research and development process of biologic medical magnesium technology, the test and appraisal of magnesium alloy biodegradability are one of core missions.Existing dynamic simulation tester or be principle of design with the performance test of material such as iron to satisfy general industry is not considered the singularity that the biomaterial test condition requires, as seal, aseptic, constant temperature etc.; Or be starting point with the performance test of conventional bio-medical metal material such as stainless steel, titanium alloy etc., do not consider the singularity of magnesium alloy---biodegradability and the slightly solubility of cathode drop hydrolysis products in aqueous medium.Therefore, existing dynamic simulation test device is applied to the magnesium alloy Study on Biodegradability and has many shortcoming.Be so limited, the existing test and appraisal of magnesium alloy biodegradability are still soaked etching test entirely based on classics.Though this method is simple, there is following main drawback: 1) ignored the material impact of the relative motion of material/medium except that convection current to the material corrosion degradation behavior.And magnesium alloy bio-medical within sight, when especially using as coronary artery bracket etc., the inevitable shear action of the human body fluid that can be flowed such as blood, tissue fluid etc.; 2) as 1) direct result, correlated results and body are implanted into test findings and greatly differ from each other, and are difficult to accurately to predict biodegradability in the body of material/apparatus, cause its clinical reference value to be had a greatly reduced quality, thereby have lost the due meaning of in vitro study.Therefore, design, exploitation adapt to the dynamic simulation test device of magnesium alloy biodegradation character, have become the task of top priority of biologic medical magnesium technical research work.
Summary of the invention
Purpose of the present invention is exactly the deficiency at prior art and equipment, provides a kind of medical magnesium alloy biodegradability external dynamic simulant test equipment.The present invention can the Simulated Service state under relative motion state between media/material, can estimate medium degraded aggressivity and material corrosion degradability convenient, fast, exactly.
Above-mentioned purpose of the present invention is achieved through the following technical solutions: the external dynamic simulant test equipment of a kind of medical magnesium alloy biodegradability comprises calibration cell, fluid reservoir, ebullator, flowmeter, power jar, test chamber, the next load sampler, amount gas device, pipette, first recirculatory pipe and second recirculatory pipe; Pipette, first recirculatory pipe and second recirculatory pipe place fluid reservoir respectively, fluid reservoir places calibration cell, flowmeter is vertically fixing, the next load sampler places in the test chamber, amount gas device vertically is fixed in directly over the next load sampler, and power jar and test chamber difference horizontal fixed are on the adjustable base of difference in height; Pipette is positioned between the inlet of the outer mouth of pipe of fluid reservoir jar and ebullator, between the inlet of the outlet of ebullator and flowmeter, between the tube for entering can of the outlet of flowmeter and power jar, the power jar go out jar pipe and test chamber advance between the pipe of cabin, the deliver from vault pipe and first recirculatory pipe of test chamber be positioned between the outer mouth of pipe of fluid reservoir jar, outside the power jar run-down pipe and be positioned between the outer mouth of pipe of fluid reservoir jar with second recirculatory pipe and link to each other formation liquid medium circulation path respectively by water pipe.
Described power jar comprises tube for entering can, goes out a jar pipe, outer run-down pipe and main tank body; Main tank body is a closed cylinder, and its inner chamber is divided into three separate chamber in left, center, right by first dividing plate and second partition; Tube for entering can is positioned at the nearly upper end of main tank body left surface, and its tube chamber directly communicates with the left chamber of main tank body; Go out a jar pipe and be positioned at the nearly jar bottom of main tank body right flank, its tube chamber directly communicates with the right chamber of main tank body; Outer run-down pipe is positioned at the nearly upper end of main tank body leading flank, and the chamber directly communicates among its tube chamber and the main tank body; First dividing plate is being provided with intercommunicating pore near a jar bottom, and second partition is being provided with spout hole in rectangular first near upper end, and the first interior spout hole geometric center and outer run-down pipe axis are parallel to the plane of main tank body tank deck altogether; Go out jar pipe and outer run-down pipe and be respectively equipped with variable valve; Top of chamber is provided with first air hole of band filter among the main tank body; Power tank outer wall with jar at the bottom of on the plane be that measuring point indicates deep calibration, and the scale area tank body is transparent.
Described test chamber comprises into cabin pipe, main cabin and deliver from vault pipe, and the tube chamber that wherein advances cabin pipe and deliver from vault pipe directly communicates with cabin, main cabin respectively; Main cabin is the sealing cuboid container, and its bilge is provided with the register pin that is used for fixing the next load sampler, and register pin is positioned on the main cabin bilge center line that is parallel to the long limit of the main cabin bilge; The gas collection hole that the air scoop that is provided with the amount of being convenient to gas device covers the next load sampler is pushed up in cabin, main cabin, gas collection hole is positioned at directly over the register pin, its hole heart is positioned on top, cabin, the main cabin center line that is parallel to long limit, top, cabin, main cabin, and its diameter is greater than the external diameter of the air scoop big open end end of amount gas device; Be respectively equipped with second air hole of circular instrument connection and band filter around the gas collection hole; Main cabin is transparent, and the external wall in cabin indicates deep calibration and cabin body length and width, and deep calibration is a measuring point with plane on the bilge; Advance the cabin pipe and be positioned at the nearly bilge of left surface center, main cabin, the deliver from vault pipe is positioned at center, top, the nearly cabin of main cabin right flank; Each 21-35mm place, left and right side, main cabin is provided with the porous stabilier respectively in distance.
Described fluid reservoir is sealing side's body container, is divided into left and right two independent tank bodies by the 3rd dividing plate, and wherein right tank volume is more than 2.1 times of left tank volume; The fluid reservoir tank deck is provided with the 3rd air hole, liquid sucting port, first refluxing opening and second refluxing opening of supply mouth, band filter; Liquid sucting port is positioned at a left side jar tank deck of fluid reservoir and the left surface and the leading flank of close fluid reservoir, first refluxing opening and second refluxing opening all are positioned at the right side jar tank deck of fluid reservoir and the right flank and the leading flank of close fluid reservoir, liquid sucting port, first refluxing opening and second refluxing opening are respectively pipette, first recirculatory pipe and second recirculatory pipe passages by tank deck, are tightly connected between pipe and the mouth; Differing heights at the 3rd dividing plate is interval with spout hole in second, and the second interior spout hole is near side after the fluid reservoir; The left surface and the right flank of fluid reservoir are respectively equipped with leakage fluid dram, and leakage fluid dram is near at the bottom of the jar of fluid reservoir and trailing flank; All seamless nested rifled tube in spout hole and the leakage fluid dram in second, the screw thread pipe close of internal thread pipe racks coupling.
Described the next load sampler comprises base and support, and the base upper end is provided with the internal thread hole that is used for mounting bracket, and the base lower end is provided with the pilot hole that is used for fixing base, and the size of pilot hole and the size of register pin are complementary; Support comprises fastening end, pillar and load terminal, and wherein the fastening end is positioned at the lower end of pillar, for the screw rod of base upper end internal thread hole coupling, be used for being fastenedly connected between support and the base; Load terminal is positioned at the upper end of pillar, for round platform, positive terrace with edge or right cylinder, is used to load sample; Base is cylinder, round platform or terrace with edge, and its lower end is provided with the following exhaust/outage that communicates with internal thread hole, and its upper end is provided with the last exhaust/outage that communicates with pilot hole; Base and support are individual member, make greater than 1 material by proportion.
Described amount gas device is made up of eudiometer tube, air scoop, stopcock and drainage tube, and wherein the eudiometer tube tube wall is with containing mark and altitude scale respectively, and the scale area tube wall is transparent; Air scoop is the cone of hollow and open at both ends, and its cover body wall thickness everywhere is identical; One end of eudiometer tube links to each other with drainage tube by stopcock, and the other end links to each other with the little opening end of air scoop.
The described pipette and first recirculatory pipe, second recirculatory pipe are the hard water pipe, and the nose end that the three is positioned at fluid reservoir jar height of medial surface at the bottom of the jar is 3.5-14mm.
Described tube for entering can, go out jar pipe, outer run-down pipe and advance cabin pipe, deliver from vault pipe and drainage tube to be the uniform hollow ring of internal diameter pipe, wherein the deliver from vault bore is more than 2.1 times of cabin bore into; First air hole, gas collection hole, instrument connection, second air hole, supply mouth and the 3rd air hole are through hole, the sealing-plug of band coupling.
Compare with prior art and equipment, the present invention has advantages such as compact conformation, easy to use, highly versatile.Utilize the present invention to carry out the dynamic simulant test of material/apparatus corrosion degradation property, have following outstanding effect:
1) utilization of calibration cell, the said structure design of fluid reservoir can guarantee that tested media has the abundant residence time in cycle period in fluid reservoir, helps the regulation and control of calibration cell to its temperature, is convenient to accurately study temperature variation to medium and effect of material performance.
2) said structure of power jar and test chamber design, and provide the thinking of power for liquid flow in the test chamber by the liquid level difference between power jar and test chamber can be guaranteed tested media mobile steady, controlled in test chamber.
3) invention and the supporting use of the next load sampler and amount gas device can realize function---the next loading of a. sample in fluid media (medium) that existing dynamic simulant test equipment can't be realized; B. the cathode drop hydrolysis products---insoluble gas is H
2Real-time collecting and accurate measurement synchronously thereof; C. the collection of material corrosion degradation kinetics data.
4) utilize this equipment to be easy to realize the controlled flowing of liquid medium in test chamber, important parameter such as speed of related movement and surface to volume ratio, medium temperature, pH value and component can test and assess between material/medium convenient, fast, exactly to the influence of erosion medium resistance and material corrosion degradability, have important value to disclosing application technologies such as material corrosion degradation behavior rule, exploitation new material/new apparatus and degraded control thereof, to improve efficiency of research and development and research and development quality, the reduction R﹠D costs are significant.
5) this equipment is not only applicable in the analogue body physiological environment such as dynamic blood/tissue liquid etc. to the degradation of bio-medical metal material such as magnesium alloy, titanium alloy etc. and degradable biological medical macromolecular material such as PLLA, SR-PLLA etc. and medical device product thereof, and is applicable to conventional engineering material and military project material etc. and the dynamic similation of corrosive medium interphase interaction such as seawater and the accelerated test of correlated performance.
Description of drawings
Fig. 1 is an one-piece construction synoptic diagram of the present invention.
Fig. 2 is the present invention's power jar structure synoptic diagram.
Fig. 3 is second partition side-looking structural representation in the present invention's the power jar.
Fig. 4 is the present invention's test chamber structural representation.
Fig. 5 is the present invention's fluid reservoir master TV structure synoptic diagram.
Fig. 6 is the present invention's fluid reservoir plan structure synoptic diagram.
Fig. 7 is the 3rd bulkhead sides TV structure synoptic diagram in the present invention's the fluid reservoir.
Fig. 8 is position load sampler structural representation under the present invention.
Fig. 9 is the present invention's amount gas device structural representation.
Among the figure: 1-calibration cell, 2-fluid reservoir, 3-ebullator, 4-flowmeter, 5-power jar, 6-test chamber, the next load sampler of 7-, 8-amount gas device, the 9-pipette, 10-first recirculatory pipe, 11-second recirculatory pipe, 12-tube for entering can, 13-goes out a jar pipe, and 14-advances the cabin pipe, 15-deliver from vault pipe, the outer run-down pipe of 16-, 17-master's tank body, 18-first dividing plate, 19-second partition, 20-intercommunicating pore, spout hole in the 21-first, 22-variable valve, 23-first air hole, 24-master cabin, 25-register pin, 26-air scoop, the 27-gas collection hole, 28-instrument connection, 29-second air hole, the 30-stabilier, 31-the 3rd dividing plate, 32-supply mouth, 33-the 3rd air hole, 34-liquid sucting port, 35-first refluxing opening, 36-second refluxing opening, spout hole in the 37-second, 38-leakage fluid dram, the 39-base, 40-internal thread hole, 41-pilot hole, the 42-fastening end, the 43-pillar, 44-load terminal, exhaust/outage under the 45-, last exhaust/the outage of 46-, the 47-eudiometer tube, the 48-stopcock, the 49-drainage tube.
Embodiment
Below in conjunction with accompanying drawing concrete enforcement of the present invention is described further, but protection scope of the present invention and enforcement are not limited thereto.
As shown in Figure 1, the present invention is connected in sequence through supporting piping by calibration cell 1, fluid reservoir 2, ebullator 3, flowmeter 4, power jar 5, test chamber 6, pipette 9, first recirculatory pipe 10 and second recirculatory pipe 11, and be the sample loading attachment with the next load sampler 7, amount gas device 8 is gas collection and proportioning device.Wherein pipette 9, first recirculatory pipe 10 and second recirculatory pipe 11 place fluid reservoir 2 respectively, and liquid medium circulates when being convenient to test.Fluid reservoir 2 places calibration cell 1, helps the regulation and control of 1 pair of fluid reservoir 2 medium temperature of calibration cell, thereby guarantees in the test chamber 6 to be in preset range with the temperature of the fluid of sample effect.Flowmeter 4 is vertically fixing, is convenient to fluid flow rate and regulates and control as required.The next load sampler 7 places in the test chamber 6, for the loading of sample and load the stability of sample under the fluid effect guarantee is provided.Amount gas device 8 vertically is fixed in directly over the next load sampler 7, when being convenient to collect the insoluble gas that reaction produces between sample/medium it is carried out accurate measurement.Power jar 5 and test chamber 6 respectively horizontal fixed on the adjustable base of difference in height, be convenient to adjust between the two liquid level difference so that control test chamber 6 in the flow velocity of media.Pipette 9 is positioned between the inlet of 2 jars of outer mouths of pipe of fluid reservoir and ebullator 3, between the inlet of the outlet of ebullator 3 and flowmeter 4,12 of the tube for entering can of the outlet of flowmeter 4 and power jar 5, the cabin of advancing that goes out jar pipe 13 and test chamber 6 of power jar 5 is managed 14, the deliver from vault pipe 15 of test chamber 6 and first recirculatory pipe 10 are positioned between 2 jars of outer mouths of pipe of fluid reservoir, run-down pipe 16 is positioned between 2 jars of outer mouths of pipe of fluid reservoir with second recirculatory pipe 11 and links to each other by water pipe respectively outside the power jar 5, constitute the liquid medium circulation path, be convenient to be stored in tested media in the fluid reservoir 2 and under the power that ebullator 3 provides, enter test chamber 6 and in pipe system, circulate, guarantee the controllability of power jar 5 liquid levels simultaneously through power jar 5.Pipette 9 and first recirculatory pipe 10, second recirculatory pipe 11 are the hard water pipe, can guarantee that its exit position is stable; The nose end that the three is positioned at 2 jars of fluid reservoirs height of medial surface at the bottom of the jar is 3.5-14mm, the disturbance effect that produces when reducing tested media into and out of fluid reservoir 2.
As Fig. 2, shown in Figure 3, power jar 5 comprises tube for entering can 12, goes out a jar pipe 13, outer run-down pipe 16 and main tank body 17, and it mainly acts on and is power to be provided and to guarantee the steady, controlled of test chamber 6 interior velocity of medium for the media flow in the test chamber 6.Main tank body 17 is a closed cylinder, and its inner chamber is divided into three separate chamber in left, center, right by first dividing plate 18 and second partition 19, so that tested media enters test chamber 6 before abundant degasification and current stabilizations.Tube for entering can 12 is positioned at the nearly upper end of main tank body 17 left surfaces, and its tube chamber directly communicates with the left chamber of main tank body 17.Go out a jar pipe 13 and be positioned at the nearly jar bottom of main tank body 17 right flanks, its tube chamber directly communicates with the right chamber of main tank body 17.Outer run-down pipe 16 is positioned at the nearly upper end of main tank body 17 leading flanks, and the chamber directly communicates among its tube chamber and the main tank body 17.First dividing plate 18 is being provided with intercommunicating pore 20 near a jar bottom, and the tested media in the formation left chamber enters the passage of middle chamber.Second partition 19 is being provided with spout hole 21 in rectangular first near upper end, constitutes the passage that the interior tested media of middle chamber enters right chamber.Spout hole 21 geometric centers and outer run-down pipe 16 axis are parallel to the plane of main tank body 17 tank decks altogether in first, be convenient to surpass when going out the liquid measure of jar pipe 13 outflows when the liquid measure that enters main tank body 17 through tube for entering can 12, for unnecessary liquid measure provides outlet, thereby the liquid measure of guaranteeing to enter right chamber is steady, controlled.Go out jar pipe 13 and outer run-down pipe 16 and be respectively equipped with variable valve 22, be convenient to the rate-of flow that enters test chamber 6 is regulated.Top of chamber is provided with first air hole 23 of band filter among the main tank body 17, is convenient to the 5 outside exhausts of power jar and keeps stablizing of air pressure in the power jar 5.Power jar 5 tank walls with jar at the bottom of on the plane be that measuring point indicates deep calibration, and the scale area tank body is transparent, a level condition in being convenient to observe jar.Tube for entering can 12, go out jar pipe 13, outer run-down pipe 16 is the uniform hollow ring of internal diameter pipe, is convenient to the impermeability that is fastenedly connected and guarantees the junction of 5 in extension tube attached and power jar.
As shown in Figure 4, test chamber 6 comprises into cabin pipe 14, main cabin 24 and deliver from vault pipe 15, is the core cell of equipment set.The tube chamber that wherein advances cabin pipe 14 and deliver from vault pipe 15 directly communicates with 24 cabins, main cabin respectively.Main cabin 24 is the sealing cuboid container, its bilge is provided with the register pin 25 that is used for fixing the next load sampler 7, register pin 25 is positioned on main cabin 24 bilge center lines that are parallel to the long limit of main cabin 24 bilge, thus the next load sampler 7 and the stability of loading sample in fluid media (medium) thereof when guaranteeing actual use.Top, 24 cabins, main cabin is provided with the gas collection hole 27 of the next load sampler 7 of air scoop 26 coverings of the amount of being convenient to gas device 8, gas collection hole 27 is positioned at directly over the register pin 25, its hole heart is positioned on top, 24 cabin, the main cabin center line that is parallel to long limit, top, 24 cabins, main cabin, and the amount of being convenient to gas device 8 covers the sample that loads on the next load sampler 7 and collects the insoluble gas that its degraded produces.Gas collection hole 27 diameters are greater than the external diameter of the air scoop 26 big open end ends of amount gas device 8, and air scoop 26 that can the amount of guaranteeing gas device 8 immerses tested media and follow-up medium is filled.Be respectively equipped with second air hole 29 of circular instrument connection 28 and band filter around the gas collection hole 27.The real-time monitoring that is designed to physical and chemical parameters such as tested media pH value, conductivity, temperature of instrument connection 28 provides convenience, and the existence of second air hole 29 is convenient to test chamber 6 outside exhausts and is kept the stable of air pressure in the test chamber 6.Main cabin 24 is transparent, is convenient to sample corrosion degradation process in the astrodome.The external wall in cabin indicates deep calibration and cabin body length and width, and deep calibration is measuring point with plane on the bilge, helps adjusting specimen height and measuring and calculating velocity of medium.Advance cabin pipe 14, deliver from vault pipe 15 is the uniform hollow ring of internal diameter pipe, is convenient to the impermeability that is fastenedly connected and guarantees the junction of 6 of extension tube attached and test chambers.Advance cabin pipe 14 and be positioned at the nearly bilge of main cabin 24 left surfaces center, deliver from vault pipe 15 is positioned at center, top, the nearly cabin of main cabin 24 right flanks; Deliver from vault pipe 15 internal diameters are that into more than 2.1 times of 14 internal diameters are managed in the cabin; Each 21-35mm place, 24 left and right sides, main cabin is provided with porous stabilier 30 respectively in distance.Advance the position of cabin pipe 14 and deliver from vault pipe 15 and the existence of size relationship design and stabilier 30, help the steady, controlled of main cabin 24 interior media and flow velocity thereof.
As Fig. 5, Fig. 6 and shown in Figure 7, fluid reservoir 2 is sealing side's body container, is divided into left and right two independent tank bodies by the 3rd dividing plate 31, and wherein right tank volume is more than 2.1 times of left tank volume.Fluid reservoir 2 tank decks are provided with the 3rd air hole 33, liquid sucting port 34, first refluxing opening 35 and second refluxing opening 36 of supply mouth 32, band filter.Supply mouth 32 provides convenience for add tested media in fluid reservoir 2, and the offering of the 3rd air hole 33 is convenient to fluid reservoir 2 outside exhausts and kept stablizing of air pressure in the fluid reservoir 2.Liquid sucting port 34 is positioned at a left side jar tank deck of fluid reservoir 2 and the left surface and the leading flank of close fluid reservoir 2, first refluxing opening 35 and second refluxing opening 36 all are positioned at the right side jar tank deck of fluid reservoir 2 and the right flank and the leading flank of close fluid reservoir 2, liquid sucting port 34, first refluxing opening 35 and second refluxing opening 36 are respectively pipette 9, first recirculatory pipe 10 and second recirculatory pipe 11 passages by tank deck, are tightly connected between pipe and the mouth.The above-mentioned design of liquid sucting port 34, first refluxing opening 35 and the 3rd dividing plate 31 can guarantee that tested media has the abundant residence time in cycle period in fluid reservoir 2, help the regulation and control of calibration cell 1, be convenient to accurately study temperature variation medium and effect of material performance to its temperature.The differing heights of the 3rd dividing plate 31 be interval with in second in the spout hole 37, the second spout holes 37 near fluid reservoirs 2 after the side.The left surface of fluid reservoir 2 and right flank are respectively equipped with leakage fluid dram 38, and leakage fluid dram 38 is near at the bottom of jars of fluid reservoir 2 and trailing flank, are convenient to after the end of test (EOT) discharging of raffinates in the fluid reservoir 2 and reach follow-up cleaning to fluid reservoir 2.All seamless nested rifled tube in spout hole 37 and the leakage fluid dram 38 in second, the screw thread pipe close of internal thread pipe racks coupling is convenient to according to the opening and closing of spout hole 37 and leakage fluid dram 38 in the control second flexibly of actual operating position.
As shown in Figure 8, the next load sampler 7 comprises base 39 and support, and base 39 upper ends are provided with the internal thread hole 40 that is used for mounting bracket, and base 39 lower ends are provided with the pilot hole 41 that is used for fixing base 39, and the size of the size of pilot hole 41 and register pin 25 is complementary.The design of pilot hole 41 can be guaranteed the next load sampler 7 and go up the stability of sample in fluid media (medium) of loading.Support comprises fastening end 42, pillar 43 and load terminal 44, and wherein fastening end 42 is positioned at the lower end of pillar 43, for the screw rod of base 39 upper end internal thread holes 40 coupling, be used for being fastenedly connected between support and the base 39.Load terminal 44 is used to load sample, be positioned at the upper end of pillar 43, be round platform, positive terrace with edge or right cylinder, this geometry design of load terminal 44, the loading needs of test specimen both can have been satisfied with load sample hole, different aperture, improve the versatility of device, can guarantee secure fixation and the support of support again test specimen.Base 39 is cylinder, round platform or terrace with edge, and can be support and loading sample provides stable support.Base 39 lower ends are provided with the following exhaust/outage 45 that communicates with internal thread hole 40, base 39 upper ends are provided with the last exhaust/outage 46 that communicates with pilot hole 41, this design both can effectively avoid sample to load or the base position fixing process in gas or liquid in pilot hole or internal thread hole, accumulating assembling resistances such as producing pneumatic/hydraulic, influence support installation or base location, can eliminate the buoyancy that trapped gas produces again, bring convenience also for simultaneously the cleaning and the sterilization of the next load sampler 7 in dismounting back.Base 39 and support are individual member, are convenient to select for use different individual members to carry out free assembly according to the concrete needs of reality, and the back of finishing using is detachable, carry and use all very convenient.In addition, by selection, can realize control to the test specimen loading height to stent strut length.Base 39 and support are made greater than 1 material by proportion, as stainless steel, PTFE, titanium alloy etc., can guarantee the loading test sample after, the next load sampler 7 and load the stability of sample under liquid medium and adsorbed gas buoyancy.This equipment is because the invention and the utilization of the next load sampler 7, realized test specimen fix from the lower end and is supported, and solved the difficult problem that traditional " suspension type " load sample method runs into.
As shown in Figure 9, amount gas device 8 is made up of eudiometer tube 47, air scoop 26, stopcock 48 and drainage tube 49, and wherein eudiometer tube 47 tube walls are with containing mark and altitude scale respectively, and the scale area tube wall is transparent.Therefore gas volume can directly obtain by liquid level change in the pipe in the eudiometer tube 47, and range, precision and sensitivity etc. all can be selected to control flexibly by caliber, is convenient to satisfy needing of trace or a large amount of gas reaction of formation application; But the altitude scale in eudiometer tube 47 pipes, on outer liquid level difference throughput tracheae 47 tube walls of pipe directly obtains, and is convenient to gas actual pressure in the pipe is accurately calculated.Air scoop 26 is the cone of hollow and open at both ends, and its cover body wall thickness everywhere is identical.The above-mentioned geometrical construction of air scoop 26 can guarantee that the insoluble gas product of separating out finally can be pooled in the eudiometer tube 47 smoothly, has avoided the delay at other position; In addition, effective overlay area of air scoop 26 can be by controlling the selection of its big opening end internal diameter flexibly, be convenient to adjust according to the physical size of test specimen effective collecting zone of insoluble gas product, the generation of the phenomenon of can avoiding becoming flat.One end of eudiometer tube 47 links to each other with drainage tube 49 by stopcock 48, and the other end links to each other with the little opening end of air scoop 26.The smooth filling of fluid media (medium) in preceding eudiometer tube 47 of gas collection test beginning and the air scoop 26 is convenient in the supporting design of drainage tube 49 and stopcock 48.Drainage tube 49 is the uniform hollow ring of an internal diameter pipe, is convenient to being fastenedly connected to use air-breathing instrument such as ear washing bulb etc. of 8 of extension tube attached and amount gas devices and forms negative pressure in amount gas device 8, thereby guarantee the smooth filling of tested media to air scoop 26 and eudiometer tube 47.
Embodiment
Be example with the dynamic simulant test that utilizes the present invention to carry out the medical magnesium alloy biodegradability below, introduce usage of the present invention in detail: with the supply mouth 32 injection fluid reservoirs 2 by fluid reservoir 2 tank decks such as pre-configured tested media such as Hank ' s simulated body fluid; Open the power switch of calibration cell 1, preset temperature heats tested media and it is carried out constant temperature; The sample that is processed with the dress sample hole of mating with load terminal 44 is carried out pre-treatments such as metallographic polishing, cleaning, drying, the differential of the arc/anodic oxidation, bionical passivation, afterwards it is screwed in/be pressed into the load terminal 44 of the next load sampler 7; The next load sampler 7 is fixed in test chamber 6 bilge through pilot hole 41 and register pin 25; Open ebullator 3, tested media is sent into power jar 5 and test chamber 6; To measure gas device 8 and vertically be fixed in directly over the sample, adjustment amount gas device 8 highly makes its air scoop 26 pass the gas collection hole 27 on top, test chamber 6 cabins and immerses tested media; The stopcock 48 of opening gas device 8; At the external silicone tube of drainage tube 49 free ends, use formation negative pressure in amount gas device 8 such as air-breathing instrument such as ear washing bulb, tested media is entered and be full of air scoop 26 and eudiometer tube 47; Liquid level in the adjustment amount tracheae 47; Cut-out tap valve 48; Adjust rate-of flow/flow velocitys by flowmeter 4, the liquid inlet and the discharge of regulating power jars 5 simultaneously by variable valve 22, to medium with preset flow rate steady flow in test chamber 6.
With the carrying out of interface reaction between simulated body fluid/test specimen, cathode drop hydrolysis products H
2Compile to eudiometer tube 47 through air scoop 26, discharge solution wherein, cause the liquid level in the eudiometer tube 47 to descend.During time t, obtain H in the eudiometer tube 47 by the containing mark of amount gas device 8
2Growing amount Δ V (t) obtains interior, the pipe outer liquid level difference h (t) of eudiometer tube 47 pipes by the altitude scale of measuring gas device 8.H in the binding capacity tracheae 47 initial liquid level recorder calculated amount tracheaes 47
2Dividing potential drop P (t) again by Δ V (t), P (t) and gas actual temperature T, calculates H according to the equation of gas state
2Amount of substance, and then calculate H
2Generating rate, and finally obtain the information of magnesium alloy biodegradability aspect.
Close ebullator 3 after the specific period, unload the next load sampler 7, take out the sample on the load terminal 44, afterwards according to known method carry out subsequent operation as clean, dry, weigh and surface/cross-section analysis test etc., can obtain the material corrosion degraded and enrich and comprehensive information, as mass change, catabolite phase composition, element composition and microscopic appearance etc.
Claims (8)
1. the external dynamic simulant test equipment of medical magnesium alloy biodegradability is characterized in that comprising calibration cell (1), fluid reservoir (2), ebullator (3), flowmeter (4), power jar (5), test chamber (6), the next load sampler (7), amount gas device (8), pipette (9), first recirculatory pipe (10) and second recirculatory pipe (11); Pipette (9), first recirculatory pipe (10) and second recirculatory pipe (11) place fluid reservoir (2) respectively, fluid reservoir (2) places calibration cell (1), flowmeter (4) is vertically fixing, the next load sampler (7) places in the test chamber (6), amount gas device (8) vertically is fixed in directly over the next load sampler (7), and power jar (5) and test chamber (6) difference horizontal fixed are on the adjustable base of difference in height; Pipette (9) is positioned between the inlet of fluid reservoir (2) jar outer mouth of pipe and ebullator (3), between the inlet of the outlet of ebullator (3) and flowmeter (4), between the tube for entering can (12) of the outlet of flowmeter (4) and power jar (5), manage between (14) in the cabin of advancing that goes out jar pipe (13) and test chamber (6) of power jar (5), the deliver from vault pipe (15) of test chamber (6) and first recirculatory pipe (10) are positioned between fluid reservoir (2) jar outer mouth of pipe, run-down pipe (16) is positioned between fluid reservoir (2) jar outer mouth of pipe with second recirculatory pipe (11) and links to each other by water pipe respectively outside the power jar (5), constitutes the liquid medium circulation path.
2. the external dynamic simulant test equipment of a kind of medical magnesium alloy biodegradability according to claim 1 is characterized in that: described power jar (5) comprises tube for entering can (12), goes out jar pipe (13), outer run-down pipe (16) and a main tank body (17); Main tank body (17) is a closed cylinder, and its inner chamber is divided into three separate chamber in left, center, right by first dividing plate (18) and second partition (19); Tube for entering can (12) is positioned at the nearly upper end of main tank body (17) left surface, and its tube chamber directly communicates with the left chamber of main tank body (17); Go out a jar pipe (13) and be positioned at the nearly jar bottom of main tank body (17) right flank, its tube chamber directly communicates with the right chamber of main tank body (17); Outer run-down pipe (16) is positioned at the nearly upper end of main tank body (17) leading flank, and the chamber directly communicates among its tube chamber and the main tank body (17); First dividing plate (18) is being provided with intercommunicating pore (20) near a jar bottom, second partition (19) is being provided with spout hole in rectangular first (21) near upper end, and first interior spout hole (21) geometric center and outer run-down pipe (16) axis are parallel to the plane of main tank body (17) tank deck altogether; Go out jar pipe (13) and outer run-down pipe (16) and be respectively equipped with variable valve (22); Top of chamber is provided with first air hole (23) of band filter among the main tank body (17); Power jar (5) tank wall with jar at the bottom of on the plane be that measuring point indicates deep calibration, and the scale area tank body is transparent.
3. the external dynamic simulant test equipment of a kind of medical magnesium alloy biodegradability according to claim 1, it is characterized in that: described test chamber (6) comprises into cabin pipe (14), main cabin (24) and deliver from vault pipe (15), and the tube chamber that wherein advances cabin pipe (14) and deliver from vault pipe (15) directly communicates with cabin, main cabin (24) respectively; Main cabin (24) is the sealing cuboid container, and its bilge is provided with the register pin (25) that is used for fixing the next load sampler (7), and register pin (25) is positioned on main cabin (24) bilge center line that is parallel to the long limit of main cabin (24) bilge; The gas collection hole (27) that the air scoop (26) that is provided with the amount of being convenient to gas device (8) covers the next load sampler (7) is pushed up in cabin, main cabin (24), gas collection hole (27) is positioned at directly over the register pin (25), its hole heart is positioned on top, cabin, main cabin (24) center line that is parallel to long limit, top, cabin, main cabin (24), and its diameter is greater than the external diameter of air scoop (26) the big open end end of amount gas device (8); Gas collection hole (27) is respectively equipped with second air hole (29) of circular instrument connection (28) and band filter on every side; Main cabin (24) is transparent, and the external wall in cabin indicates deep calibration and cabin body length and width, and deep calibration is a measuring point with plane on the bilge; Advance cabin pipe (14) and be positioned at the nearly bilge of main cabin (24) left surface center, deliver from vault pipe (15) is positioned at center, top, the nearly cabin of main cabin (24) right flank; Each 21-35mm place, left and right side, main cabin (24) is provided with porous stabilier (30) respectively in distance.
4. the external dynamic simulant test equipment of medical magnesium alloy biodegradability according to claim 1, it is characterized in that: described fluid reservoir (2) is sealing side's body container, be divided into left and right two independent tank bodies by the 3rd dividing plate (31), wherein right tank volume is more than 2.1 times of left tank volume; Fluid reservoir (2) tank deck is provided with the 3rd air hole (33), liquid sucting port (34), first refluxing opening (35) and second refluxing opening (36) of supply mouth (32), band filter; Liquid sucting port (34) is positioned at a left side jar tank deck of fluid reservoir (2) and the left surface and the leading flank of close fluid reservoir (2), first refluxing opening (35) and second refluxing opening (36) all are positioned at the right side jar tank deck of fluid reservoir (2) and the right flank and the leading flank of close fluid reservoir (2), liquid sucting port (34), first refluxing opening (35) and second refluxing opening (36) are respectively pipette (9), first recirculatory pipe (10) and second recirculatory pipe (11) passages by tank deck, are tightly connected between pipe and the mouth; Differing heights at the 3rd dividing plate (31) is interval with spout hole in second (37), and the close fluid reservoir (2) of the second interior spout hole (37) is the side afterwards; The left surface of fluid reservoir (2) and right flank are respectively equipped with leakage fluid dram (38), and leakage fluid dram (38) is near at the bottom of the jar of fluid reservoir (2) and trailing flank; All seamless nested rifled tube in spout hole (37) and the leakage fluid dram (38) in second, the screw thread pipe close that the internal thread pipe racks mates.
5. the external dynamic simulant test equipment of a kind of medical magnesium alloy biodegradability according to claim 1, it is characterized in that: described the next load sampler (7) comprises base (39) and support, base (39) upper end is provided with the internal thread hole (40) that is used for mounting bracket, base (39) lower end is provided with the pilot hole (41) that is used for fixing base (39), and the size of the size of pilot hole (41) and register pin (25) is complementary; Support comprises fastening end (42), pillar (43) and load terminal (44), and wherein fastening end (42) are positioned at the lower end of pillar (43), for the screw rod of base (39) upper end internal thread hole (40) coupling, be used for being fastenedly connected between support and the base (39); Load terminal (44) is positioned at the upper end of pillar (43), for round platform, positive terrace with edge or right cylinder, is used to load sample; Base (39) is cylinder, round platform or terrace with edge, and its lower end is provided with the following exhaust/outage (45) that communicates with internal thread hole (40), and its upper end is provided with the last exhaust/outage (46) that communicates with pilot hole (41); Base (39) and support are individual member, make greater than 1 material by proportion.
6. the external dynamic simulant test equipment of a kind of medical magnesium alloy biodegradability according to claim 1, it is characterized in that: described amount gas device (8) is made up of eudiometer tube (47), air scoop (26), stopcock (48) and drainage tube (49), wherein eudiometer tube (47) tube wall is with containing mark and altitude scale respectively, and the scale area tube wall is transparent; Air scoop (26) is the cone of hollow and open at both ends, and its cover body wall thickness everywhere is identical; One end of eudiometer tube (47) links to each other with drainage tube (49) by stopcock (48), and the other end links to each other with the little opening end of air scoop (26).
7. the external dynamic simulant test equipment of a kind of medical magnesium alloy biodegradability according to claim 1, it is characterized in that: described pipette (9) and first recirculatory pipe (10), second recirculatory pipe (11) are the hard water pipe, and the nose end that the three is positioned at fluid reservoir (2) jar height of medial surface at the bottom of the jar is 3.5-14mm.
8. the external dynamic simulant test equipment of a kind of medical magnesium alloy biodegradability according to claim 1, it is characterized in that: described tube for entering can (12), go out jar pipe (13), outer run-down pipe (16) and advance cabin pipe (14), deliver from vault pipe (15) and drainage tube (49) to be the uniform hollow ring of internal diameter pipe, wherein deliver from vault pipe (15) internal diameter is that into more than 2.1 times of (14) internal diameter are managed in the cabin; First air hole (23), gas collection hole (27), instrument connection (28), second air hole (29), supply mouth (32) and the 3rd air hole (33) are through hole, the sealing-plug of band coupling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102652092A CN101975740B (en) | 2010-08-27 | 2010-08-27 | Medical magnesium alloy biodegradability in-vitro dynamic simulation test equipment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102652092A CN101975740B (en) | 2010-08-27 | 2010-08-27 | Medical magnesium alloy biodegradability in-vitro dynamic simulation test equipment |
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| CN101975740A true CN101975740A (en) | 2011-02-16 |
| CN101975740B CN101975740B (en) | 2012-08-08 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103837465A (en) * | 2014-03-07 | 2014-06-04 | 大连交通大学 | Drip-feed type corrosion environment simulation device for flexural fatigue test |
| CN108593489A (en) * | 2018-07-12 | 2018-09-28 | 中北大学 | 3D printing magnesium alloy materials degradation system safety testing device and application |
| CN109557021A (en) * | 2018-12-30 | 2019-04-02 | 浙江工业大学 | Double acting state degradation property analytical equipment outside a kind of medical magnesium alloy implantation material bodies |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57190250A (en) * | 1981-05-20 | 1982-11-22 | Mitsubishi Heavy Ind Ltd | Testing method for long life, corrosion, and fatigue |
| CN101788452A (en) * | 2009-12-18 | 2010-07-28 | 山东省特种设备检验研究院临沂分院 | Dynamic corrosion test method and equipment thereof |
| CN201811911U (en) * | 2010-08-27 | 2011-04-27 | 华南理工大学 | Medical magnesium alloy biodegradability in-vitro dynamic analogue test equipment |
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2010
- 2010-08-27 CN CN2010102652092A patent/CN101975740B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57190250A (en) * | 1981-05-20 | 1982-11-22 | Mitsubishi Heavy Ind Ltd | Testing method for long life, corrosion, and fatigue |
| CN101788452A (en) * | 2009-12-18 | 2010-07-28 | 山东省特种设备检验研究院临沂分院 | Dynamic corrosion test method and equipment thereof |
| CN201811911U (en) * | 2010-08-27 | 2011-04-27 | 华南理工大学 | Medical magnesium alloy biodegradability in-vitro dynamic analogue test equipment |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103837465A (en) * | 2014-03-07 | 2014-06-04 | 大连交通大学 | Drip-feed type corrosion environment simulation device for flexural fatigue test |
| CN108593489A (en) * | 2018-07-12 | 2018-09-28 | 中北大学 | 3D printing magnesium alloy materials degradation system safety testing device and application |
| CN108593489B (en) * | 2018-07-12 | 2020-11-06 | 中北大学 | 3D printing magnesium alloy material degradability testing device and application |
| CN109557021A (en) * | 2018-12-30 | 2019-04-02 | 浙江工业大学 | Double acting state degradation property analytical equipment outside a kind of medical magnesium alloy implantation material bodies |
| CN109557021B (en) * | 2018-12-30 | 2024-06-11 | 浙江工业大学 | External double dynamic degradation performance analysis device for medical magnesium alloy implant material |
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| CN101975740B (en) | 2012-08-08 |
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