UNIVERSITY OF MINNESOTA, DEPARTMENT OF BIOMEDICAL ENGINEERING

BMEn3301: Lab Report 1

Surface Characterization

David Gilleland

Timothy Solberg

Fluvio Lobo

2/14/2012

1 ABSTRACT The following report contains the results of a surface characterization procedure completed to determine the surface tension of an unknown material. Using a Goniometer and four (4) different solutions (water, formamide, ethylyne glycol, and tween-80), the objective of the experiment was to measure contact angles, and to generate a Zisman plot in order to calculate the surface tension of the given unknown material. This type of procedure is a great important towards the design of invasive medical devices and biomaterials that will be in contact with bodily fluids, chemicals, and molecules which could adhere and cause inflammation, clotting, etc. Due to incorrect pre-conditioning and storing of some of the testing solutions (water and formamide) our analysis turned out to be inaccurate and unreliable. Despite this error, we were capable of narrowing our search to either polytetrafluoroethylene or polyvinylidine fluoride. Both of these were compared based on their chemical characteristics and applications

2 INTRODUCTION The purpose of this lab was to calculate the critical surface tension of Teflon tape using a Zisman plot. This was accomplished using contact angle analysis, a common method of finding a surfaces hydrophobicity. When a drop of liquid is placed on a surface, three components control how the drop spreads. These are the liquid-vapor surface ( lv), the solid-liquid surface ( sl), and the solid-vapor surface ( sv). These three components interact to cause the droplet to take on a shape. The angle the edge of the droplet creates with the surface, called the contact angle, can then be measured. The surface tension can be calculated using the following equation: =0 sv - sl - lv cos Measuring contact angles of various liquids with known liquid-vapor surfaces ( lv) on a surface can be plotted on a graph. This graph, called a Zisman plot, follows a linear line. The point where this line intersects with cos = 1 is the critical surface tension of the surface. Critical surface tension is important in materials designed to be placed within the body. Atoms on the surface of a material experience excess energy due to unfilled valence shells, attracting other molecules to adhere. Higher surface tensions can lead to protein adsorption and inflammation. Calculating the surface tension of a material, such as Teflon tape, can give us an idea of how it may react within the body. METHODS AND MATERIALS Contact angle goniometer Teflon Tape Scissors Scotch tape Syringes Water Formamide Ethylene Glycol Concentrated Solution of TWEEN-80 EXPERIMENTAL PROCEDURE Goggles were donned and a sample of Teflon tape long enough to cover the goniometer stage was cut from a roll with scissors. This sample was stretched tight over the goniometer stage and its sides were taped down with Scotch tape. The goniometer lamp was turned on and the image was focused using the lens assembly. The goniometer stage was adjusted so the horizontal shadow of the sample was aligned with the horizontal axis. One of the samples of liquid in the appropriate syringe was obtained and a drop of the liquid was placed on the Teflon tape. Two additional drops of the same liquid were placed on the Teflon tape close to, but not touching, the original drop. The goniometer stage was adjusted to place the contact angle of the reflected image of the first drop in line with the angle point. The rotating angle red-line was moved to intersect the drop at its apex and its corresponding angle was recorded. The same was repeated for the other two drops.

3 Afterwards, the Teflon tape was disposed of and a new piece was obtained. The process is then repeated for each sample liquid until measurements for the four liquids were taken.

RESULTS The measured angles for the three trials of the four liquids and their means and standard deviations are included in table one. Table 1: Measured Angles and Statistics Trial 1 124 108 105 75 Trial 2 115 100 105 70 Trial 3 115 105 107 75 Average 118.00 104.33 105.67 73.33 Standard Deviation 5.20 4.04 1.15 2.89

Water Formamide Ethylene Glycol TWEEN-80

A Zisman plot of the average angles is provided in figure one. The standard deviation and a trendline are included for reference. Figure 1: Zisman Plot of Teflon Tape

Zisman Plot of Teflon Tape

0.4 0.3 0.2 0.1 0 -0.1 20 -0.2 -0.3 -0.4 -0.5 -0.6 -0.7 y = -0.0189x + 0.853 R = 0.7588

Cos( )

30

40

50

60

70

80

Surface Tension (dynes/cm)

Using the equation provided by the trendline (line of best fit), it is made clear that the critical surface tension is -7.78 dynes/cm. If we ignore the values of the water and formamide, the new trendline reveals that the critical surface tension is 25.87 dynes/cm. Using the table of materials properties (surface tension specifically), given in the original lab procedure [Figure 2] [Appendix-A], we can determine the material we implemented in the experiment. Based on the table [Figure 2] [Appendix-A], Teflon or polytetrafluoroethylene (PTFE) has a critical surface tension of 19 dynes/cm and Poly(vinylindine flouride) has a critical surface tension of 25 dynes/cm. Compared to our experimental result, these

4 accepted value could represent a 36.16% error or 3.48%, but because of the different sources of error during the experiment choosing either one could be a mistake. Instead, as you will see in our discussion, we will compare between the two options. DISCUSSION The results we obtained were inconclusive at best. The problems started with the testing materials. The water was ionized and the formamide was incorrectly stored, making all values obtained by them unusable. This left us with two samples and the resulting trendline [Figure 1] directing us to a critical surface tension higher than the known surface tensions of the two liquids used. This would be understandable if the liquids were presenting a cosine of one, but they were not. Therefore the trendline is not linear and would be best fit by a wet noodle. A R2 value of .7588 is far from accurate [ Figure 1]. The problem grew out of random error. No one can plan for material degradation. The only thing affected by systemic error was the further accuracy of the angle measured. The goniometer was not accurate any further than the ones digit. Like we mentioned in the data analysis portion of our report, our critical surface tension values lead to either polytetrafluoroethylene or polyvinylidine fluoride. Polytetrafluoroethylene would result in a non-adhesive implant, while polyvinylidine fluoride would result in a slightly more adhesive material. The polytetrafluoroethylene is most likely incorrect due to the errors caused by the water and formamide and therefore polyvinylidine fluoride is the most likely material of the tape. By comparing only our error results, these would lead us to select polyvinylidine as our material, but because we had to throw out two data points in our graph (water and formamide) this conclusion would be inaccurate. The less adhesive a material is, the better it is at reducing clotting and inflammation. This leads to the material being less useful as an implant, but more useful as a clotting agent. It would result in blood clots or inflammation, and would retain all but the tensest of fluids. With all of the errors raised during this investigation, one cannot walk away from this experiment without feeling unfulfilled. We dont have a clear answer on what material the tape truly was. This experiment would perhaps be much more successful with materials that had not degraded. Hopefully the next foray is more lustrous. CONCLUSIONS The Goniometer can be implemented efficiently to determine the contact angle between a liquid and the surface of a material. Using the Young-Dupree equation, and the measured contact angle, we can relate the tension coefficients between the different phases (liquid-vapor, soli-liquid, and soli-vapor). A key element towards determining the surface tension of a material is the implementation of a Zisman plot. The plot relates critical surface tension with surface energy. The greater the surface tension, the more adhesive the material is. In terms of biomaterials, a less adhesive surface allows for minimal inflammation, clotting, or any rejection by the body. Therefore, a non-adhesive material is better for implants.

5 APPENDIX-A Figure 2: Critical Surface Tension of Different Materials