EFFECT OF STRESS-PATH ON THE FAILURE OF CONCRETE …
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Second LACCEI International Latin American and Caribbean Conference on Construction in the 21st Century (CITC-IIfor Engineering and Technology (LACCETI’2004))
“Sustainability and Innovation in Management and TechnologyChallenges and Opportunities for Engineering Education, Research and Development”
10-122-4 June December, 20034, Hong KongMiami, Florida, USA
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EFFECT OF STRESS-PATH ON THE FAILURE OF CONCRETE UNDER
TRI-AXIAL STRESS STATE
Model Paper Ffor EASEC-8CITC-IILACCEI ProceedingsCorrosion Behaviour of Cardiovascular Stents
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Second AuthorA. V. Datye, IngMS.
PositionReasearch Engineer , Company or UniversityFlorida International University, CitMiami,y, Stat Foridae, CountryU.S
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Third AuthorM. Jaramillo, P.E..
PositionUndergraduate rReasearch Assistant, Company orFlorida International University, CityMiami, , State, CountryFlorida, U.S
First AuthorK. H. Wu, PhD
PositionProfessor, Company or UniversityFlorida International University, Miami, City, State, Florida, CountryU.S
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Abstract :
(Times New Roman Font, Size 122pt, All CapTitle Case, Bold Face)Cyclic Potentiodynamic polarization studies were conducted to compare the corrosion resistance of Nitinol cardiovascular stents and stainless steel stents. The tests is to simulate the corrosion behavior of the stents under body condition using Phosphate Buffered Saline (PBS) solution at 37oC and following the ASTM F2129-01, Item 2, WK1749, Standard. The results of this study indicate that both NiTi and SS stents exhibit high corrosion resistance in the PBS solution. The SS stents show slightly better corrosion resistance than the Nitinol stents. The electropolished Nitinol stents appear to have slightly better corrosion resistance compared with the unpolished ones. 1 line
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Font, format, proceedings, conference, appearance, Maximum 5 keywords separated by commas (Times Roman Font, Size 101pt, justifiedjustified, Title Case).corrosion, cyclic polarization, cardiovascular stents, nitinol, pitting.
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Introduction
Cyclic Potentiodynamic polarization measurements were carried out to assess the corrosion susceptibility of Nitinol stents against stainless steel stents. The testing was performed comparing the electropolished Nitinol, non-electropolished Nitinol and stainless steel stents based on the ASTM F2129-01, Item 2 WK1749, Standard: Conducting Cyclic Potentiodynamic Polarization Measurements to Determine the Corrosion Susceptibility of Small Implant Devices. Since a stent is a Class III implantable device, the corrosion susceptibility of the material can determine the success or failure of the device.
The purpose of this study was to compare the corrosion properties of the electropolished Nitinol, non-electropolished Nitinol and stainless steel stents. Stent samples were tested for corrosion resistance “as received”. The stent samples were tested in a specially designed corrosion cell in accordance with the Practice G5 of the ASTM F2129-01 Standard.
Since this method is designed to test the device under severe conditions, corrosion and deterioration of the device is often observed. The results obtained by testing the material with several electrolytes provides with useful data for comparison of the different device materials and designs.
Experimental Procedures
1 Test Articles
Stents are small cylindrical devices that are used currently to open up closed arteries. Since the device is in constant contact with blood, which is a very corrosive environment, it is necessary to find out the effects of corrosion on the stents. Currently 316L stainless steel is the most commonly used material for cardiovascular stents. In order to evaluate the susceptibility of the coronary stents in physiological environments the corrosion testing of the stents is necessary. The following stents were tested for corrosion characteristics, five electropolished Nitinol stents, five unelectropolished Nitinol stents and five stainless steel stents.
2 2.2 Reagents
Reagent grade chemicals conforming to the specifications of the Committee on Analytical Reagents of the American Chemical Society, was used. Phosphate Buffered Saline (PBS, VRW Cat# 6505,Lot#3152 B67) was used as the standard test solution. Since PBS is deareated continuously during the experiment using high purity nitrogen, the pH of the solution maintained by the addition of NaOH or HCl as required. The ion concentration in the PBS solution is as shown in Table 2-1Table 2-1.
Table 2-1. Composition of Simuulated Physiological Solution
|PBS Components |Ion Concentration (g/L) |
|PH |7.4 |
|NaCl |8.0 |
|KCl |0.2 |
|Na2HPO4 |1.15 |
|KH2PO4 |0.2 |
4 2.3 Preparation of Samples and Conditioning
The stent wire sample is mounted by a specially designed mandrel as shown in Figure 2-1Figure 2-1. The stent wires are then carefully press-fitted over the smaller end of the cylindrical mandrel. A conductive epoxy, “Conductive Carbon Paint – Colloidal Graphite in Isopropanol – 20% Solids” is used between the stent surface and the mandrel to provide good electrical contact. This stent/mandrel interface is then sealed by a non-conductive epoxy. The mandrel is then threaded to an electrode holder. The surface area of the stent in contact with the reagent needs to be calculated carefully to avoid any errors.
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Figure 2-1. The Mounting Mandrel
The sample is then mounted in the working electrode position of the Gamry Corrosion Cell. The Cell is cleaned with deionized water and then rinsed and filled with the PBS solution prior to use. It is then immersed in a 37(C water bath. A calomel electrode is used as the reference electrode inside a Luggin Capillary. The solution is purged with ultra high purity nitrogen at a flow rate of 150 cm3/min for a minimum of 30 minutes and then the stent is inserted into the cell. The Luggin Capillary is mounted as close as possible to the stent to get readings as accurate as possible. The entire test setup shown in the figure below, is then placed in the water bath. The working, sense, reference and counter electrodes are connected to the potentiostat (model PC_400) and the cyclic potentiodynamic polarization test is conducted. The data is recorded and analyzed using the GAMRY® Instrument Framework. The solution was monitored for a change in the pH due to nitrogen purging but as reported by the CTL laboratories there is very little change in the pH of the PBS solution as compared to the Hanks and Ringers solution.
[pic]
Figure 2-2: Experimental setup.
5 2.4 Experimental Parameters
Since Nitinol and stainless steel have a similar corrosion rate, iInitially three 316L stainless steel Pplates (2 inch x 2 inch x 0.025 inch thk) were used in to perform the initial trial runs inorder to establish approximate parameters and then Nitinol and stainless steedl stents were tested for Tafel (Figure 2-3Figure 2-3) and Potentiodynamic (Figure 2-4) tests in PBS. The parameters were determined for Nitinol and later used for the cyclic potentiodynamic polarization tests carried out on the stents.
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Figure 2-3: Corrosion Potential Curve and TAFEL Curve for 316 Stainless Steel Plate in PBS.
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Figure -5: Potentiodynamic Scan for 316L Stainless Steel Plate in PBS.
The experimental parameters are then set up in the Gamry® Corrosion Cell for the Cyclic Potentiodynamic Polarization scans as below. The scan rate used for the forward and reverse scans was 1mVv/sec for the stainless steel stents and it was changed to 0.16 mV/s for the Nitinol stents due to accuracy and the fact that nitinolNitinol is an active passive metal and changes its corrosion characteristics from anode to cathode in a very small interval. The initial voltage is kept at –1.5V, the apex at +1.5 V and the final reverse scan voltage at 0 V.
Results and Discussionsand Discussions
The breakdown potential (Eb) is defined as the potential at which the pitting or crevice corrosion or both will initiate and propagate. An increase in the resistance to pitting corrosion is associated with an increase in the Eb. The protection potential (Ep) is defined as the potential at which the forward and the reverse scans intersect. This value is always less than the Eb. The zero current potential (Ezc) is the potential at which the current reaches a minimum during the forward scan. This is similar to the Ecorr values calculated.
[pic]
Figure 3-1. Cyclic Polarization Graph - Unelectropolished Nitinol Stent with Nitrogen Purging.
Figure 3-1 shows that the unelectropolished Nitinol does not exhibit a protection potential. Since there is no protection potential, this material is therefore very susceptible to crevice corrosion.
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Figure 3-2. Cyclic Polarization Graph - Electropolished Nitinol Stent with Nitrogen Purging.
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Figure 3-3. Cyclic Polarization Graph for Stainless Steel Stent with Nitrogen Purging.
The following tables (Table 3-1 to Table 3-3) summarize the results from the experiments conducted for the unelectropolished Nitinol, the electropolished Nitinol and the stainless steel stents.
Table 3-1 Summary of Results for Unelectropolished NiTi Stents
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Table 3-2 Summary of Results for Electropolished NiTi Stents
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Table 3-3 Summary of Results for Stainless Steel Stents
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Figure -3-4. Behavior of an active passive material under corrosive conditions.
When considering mixed electrodes involving an active passive metal then the peculiar S shaped curves of these metals often leads to unusual results. The figure above illustrates three possible cases that may occur when an active passive metal is exposed to an electrolyte or a corrosive environment. Reduction processes under activation polarization control are shown in the Figure 3-4. The cases shown here are general and the unpolished Nitinol, polished Nitinol and the stainless steel behavior is judged according to the data given and marked on the Figure 3-4 above.
The figure above shows a single reduction process such as hydrogen evolution with three different possible exchange current densities. In Case 1 there is only one stable intersection point, point A, which is in the active region and a high corrosion rate, is observed. Case 1 is a characteristic of nickel titanium in a dilute, air free sulphuric acid or hydrochloric acid environment. Under these conditions titanium corrodes rapidly and cannot passivate. Case 2 which represents an unpolished sample is particularly interesting due to the fact that there are three possible intersection points at which the total rate of oxidation and the total rate of reduction are equal. These points are B, C and D. Although all the three points meet the basic requirements of the mixed potential theory (rates of oxidation and reduction are equal). Point C is electrically unstable and the system cannot exist at this point. Hence both B and D are stable. B is in an active region corresponding to a higher corrosion rate and D is in a passive region therefore corresponding to a lower corrosion rate. This system may exist in either the active or the passive state.
This the reason why even though the electropolished samples even though having a higher Ecorr have a higher corrosion rate than the unelectropolished samples.
Conclusions
Among the stents that were tested the stainless steel and the electropolished Nitinol stents exhibit a protection potential (Ep) of 1.044 V and 0.9 V. In both cases, this voltage was measured against the reference voltage. The lower the protection potential the better the corrosion resistance of the device.
1 4.1 Nitinol Stents
The average breakdown potential (Eb) was 1.054 Volts for stainless steel stents. The average breakdown potential (Eb) for the electropolished stents was considerably high about 1.5V as compared to that for the unelectropolished stents about 0.4V, this is expected as shown in Figure 3.4. Usually the higher the breakdown potential the better the corrosion resistance of the device, because it means that corrosion will start at a much later voltage.
The average zero current potential (Ezc) is approximately -0.338V for stainless steel and -0.330V and -0.180V for the electropolished stents and the unelectropolished Nitinol stent. The more the number on the positive side implies that it has a better ccorrosion resistance. The Ecorr values for the electropolished Nitinol and stainless steel stents was nearly the same.
The average corrosion rates are 8.634.80E-054 and , 5.202.78E-04 and 2.11E-033 mm per year (Table 3-1 to 3-4) for the stainless steel, electropolished and the unelectropolished Nitinol stents respectively. It can be said that the corrosion rates of both the stainless steel and the electropolished Nitinol are nearly comparable groups of stents tested are negligible..
References
ASTM F2129-01, Item 2 WK1749, Standard: Conducting Cyclic Potentiodynamic Polarization Measurements to Determine the Corrosion Susceptibility of Small Implant Devices
Burke,S.R. The composition and function of Body Fluids, 3rd ed., C.V.Mosby Co., 1980.
Fotana, M.G, Corrosion Engineering, 3rd ed., McGraw Hill.
Venugopalan, R., “Corrosion Testing of Stents: An Novel Fixture to Hold the Entire Device in Deployed Form and Finish,” J Biomed Mat Res ( App Biomater) 48:829-832,1999.
4.2 Stainless Steel
The protection potential (Ep) is defined as the potential at which the forward and the reverse scans intersect. This value is always less than the Eb. Stents that were tested exhibit an average protection potential (Ep) of approximately 1.044 V. In both cases, this voltage was measured against the reference voltage. The lower the protection potential the better the corrosion resistance of the device.
The breakdown potential (Eb) is defined as the potential at which the pitting or crevice corrosion or both will initiate and propagate. An increase in the resistance to pitting corrosion is associated with an increase in the Eb. The average breakdown potential (Eb) was 1.054 Volts. The higher the breakdown potential the better the corrosion resistance of the device.
The zero current potential (Ezc) is the potential at which the current reaches a minimum during the forward scan. This is similar to the Ecorr values calculated. The average zero current potential (Ezc) is -0.338V the smaller the number implies that it has a better corrosion resistance.
Based on the above it can be concluded that the corrosion potential for the test stent was less than the control stent, which implies that the test stent has better resistance against corrosion than the control stent. The average corrosion rate is 5.53E-05 mm per. It can be said that the corrosion rates of both groups of stents (test and controls) tested are negligible.
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