J Bagh College Dentistry Vol. 28(4), December 2016 The Effect of Restorative Dentistry 22 The Effect of Silver-Zinc Zeolite Incorporation on Some Properties of Condensation Silicone Impression Material Rehab A. Al-Azawi, B.D.S., H.D.D. (a) Widad A. Al-Naqash, B.D.S., H.D.D., M.Sc. (b) ABSTRACT Background: elastomeric impression materials are indicated when a high degree of accuracy is required, due to their excellent properties like details reproduction, dimensional stability and tear strength but with main two disadvantages those are their hydrophilicity as well as the absence of antibacterial activity. This study aimed to evaluate the effect of incorporation of 0.5% wt Ag-Zn zeolite into condensation silicone through the following tests; setting time, dimensional stability, reproduction of details, wettability, and hardness . Materials and methods: one hundred specimens were constructed of condensation silicone, divided into two groups for the first 50 specimens one0.5% by wt Ag -Zn zeolite was added, keeping the other fifty specimens without addition. Then each group further subdivided into five subgroups according to the conducted test. The tests performed were; setting time, dimensional stability, reproduction of details, hardness and wettability. Results: A statistically non-significant effect on the setting time and reproduction of details tests was observed, combined with a highly significant increase of wettability of condensation silicone after incorporation of 0.5% wt Ag- Zn zeolite with non-significant increase of dimensional change of condensation silicone following incorporation of 0.5% wt Ag-Zn zeolite. Hardness test results shoed statistically significant increase following the addition of Ag-Zn zeolite. Conclusion: Ag-Zn zeolite incorporated into condensation silicone, improved wettability which determine the extent to which an impression material replicates the structures of the oral cavity and production of bubble-free gypsum die. It also showed a statistically significant increase in the hardness of condensation silicone impression material, and had no effect on setting time, reproduction of details and dimensional stability. Key words: Condensation silicone impression materials, Antimicrobial agent, Ag- Zn Zeolite, wettability. (J Bagh Coll Dentistry 2016; 28(4):22-27) INTRODUCTION Elastomeric impression materials include a group of synthetically polymerized impression materials that are chemically cross-linked when set and could be stretched and recover to their original dimensions. There are three types based on the chemical backbone of polymer chains: polysulfide, polyether, and silicone; the condensation and addition (1). Condensation silicone impression materials are widely used nowadays is supplied in a two consistencies light and putty-like. The curing of this material involves a reaction of tri- and tetra- functional alkyl silicates in the presence of stannous octoate as a catalyst. The material sets by cross-linking between terminal groups of the silicone polymers and the alkyl silicate to form a three-dimensional network, the ethyl alcohol as a byproduct. Its subsequent evaporation accounts for much of the contraction that takes place in the setting impression (1,2). Nowadays infection control takes interest in order to prevent cross infection between the patients and dental staff. The threat of infections could be transferred by blood, saliva, and/or plaque is a potential occupational risk as they include pathogenic microorganisms (3). (a)M.Sc. student. Department of Prosthodontics. College of Dentistry, University of Baghdad. (b)Professor. Department of Prosthodontics. College of Dentistry, University of Baghdad. The incorporation of zeolite as filler in polymers was reported in literatures and proved that it enhanced the antibacterial activity of these polymers. Silver ion exchanged zeolites have excellent antibacterial activity and therefore have a potential in the medical field to enhance antimicrobial properties.(4) The present study was conducted to assess the incorporation of Ag-Zn zeolite into condensation impression material and evaluate its effects on their properties MATERIALS AND METHODS One hundred specimens of condensation silicone were prepared, divided into two groups; fifty specimens control (without addition) and fifty experimental specimens (with addition of 0.5% Ag-Zn zeolite) with fifty specimens, then each group was subdivided according to the test conducted; each subgroup containing ten specimens for each test. The percentage 0.5 % is chosen in this study as this percentage representing the minimum percentage as an effective bactericidal agent as proved by many authors (5,6). Physical and mechanical tests: 1- Dimensional change test: The test block and ring mold were fabricated for this study (ADA/ANSI) specification no.19. Consisted of two parts; a circular stainless steel J Bagh College Dentistry Vol. 28(4), December 2016 The Effect of Restorative Dentistry 23 block, and a hollow stainless steel ring was used to retain and confine the impression material. Three vertical lines a 25 mm length and of 25 μm, 50 μm and 75 μm width were engraved on the metal surface of the stainless steel block (line a 50μm, line b 25 μm, and line c 75 μm).Two additional horizontal lines 25 mm apart from each other were engraved perpendicular to the previously marked lines, each have 50 μm width, (line d1 and d2) as in (fig. 1) Figure 1: The lines of the test mold: 1 line a (50 um thick.), 2 line b(25 um thick.), 3 line c (75 um thick.), 4 line d1(50 um thick), 5 line d2 (50 um thick).(7) 2-Reproduction of details test The same mold used for dimensional change test (fig. 1) was again used for this test. Following the separation and washing of the specimen an enter-estimation by three independent examiners was carried on to assess the reproduction of details by examining the continuity of the line b (25 µm) on the impression surface. Where line b is the smallest in diameter among the die lines, so if it is clearly reproduced the other larger lines would be already reproduced (8-10). 3-Setting time test Vicat penetrometer has been used, with a needle of 3-mm diameter and a total weight of 300g. A metal ring of8 mm high and diameter of 16 mm was filled with newly mixed material and positioned on the penetrometer base. Then needle was applied to the surface of the impression material for 10 sec. and a reading was recorded. This step was repeated every 30 sec. The initial set is that time when the needle no longer penetrates the specimen completely to the bottom of the specimen. While the final set is the first of three non-maximum identical penetration readings (2). 4-Wettability test: Wettability assessed by measuring the advancing contacting of liquid on the surface of the set impression material. Specimens were poured in cylindrical metal mould A drop of distilled water falling down above a set specimen and after one minute measure the angle between the surface of the drop and the surface of specimen by dino-litemicroscope (11). 5- Hardness test: The specimens made for this test by using a cylindrical mold. Then the hardness of condensation silicone impression material was tested by shore A hardness durometer instrument. This device was firmly grasped and insert it's indenter in the set specimen as shown in the (fig.2) the specimen was placed on a stable bench where the readings were recorded on the device screen. Two readings were obtained, the first represented the hardness 1.5 minutes after setting, where the second reading was for the hardness after 2 hours.(12) Four specific indentations were measured each time distributed it in a 90 ° manner at a location12 mm from any edge and at least 6 mm from any previous indent (the same selected area of each specimen), measurements followed ASTM D2240–05specification for Shore A hardness measurements. The average of the four readings in order to measure the whole surface of the specimen (13). Figure 2: Hardness sample with the sites of penetration RESULTS 1- Dimensional change test: Mean values, number of specimens, standard deviation, t-test, and p-values of dimensional change test for control and experimental groups of 1 2 3 25mm 4 5 J Bagh College Dentistry Vol. 28(4), December 2016 The Effect of Restorative Dentistry 24 condensation silicone are presented in table 1, table 2 and fig. 3. The results of dimensional test indicated non- significant difference between experimental and control groups which exhibited a mean values - 0.877 and -0.917 respectively. Table 1: descriptive data of dimensional change test for control and experimental groups Group N Mean% SD Control 10 -0.917 0.47 Experimental 10 -0.877 0.4 Table 2: t-test and p-value for dimensional change test t-test p-value Sig. -0.2 0.84 NS Figure 3: Bar chart of dimensional change for condensation silicone 2-reproduction of details The results of reproduction of details test are listed in table 3, showed the similarity in descriptive data for both groups; control and experimental. Table 3: reproduction of details results for the control and experimental groups. Group N Satisfactory Unsatisfactory Control 10 100% 0% Experimental 10 100% 0% 3- Wettability Mean values, number of specimens, standard deviation, t-test, and p-values of wettability test, are presented in tables 4, 5 and fig4. The results indicated very clear and highly significant difference between means of the experimental (62.27) and control (72.84) groups. Table 4: Descriptive data of wettability test for control and experimental groups. Group N Mean° SD Control 10 72.84 1.28 Experimental 10 62.27 2.38 Table 5: t-test and p-value for wettability test t-test p-value Sig. 12.346 0.00 HS Figure 4: Bar chart for wettability test. 4-Setting time test: Mean values, number of specimens, standard deviation, t-test, and p-values of setting time test, are presented in table 6, table 7 and fig. 5. These results indicated a similar mean values for both groups; experimental and control, which is (216 seconds). Table 6: Descriptive data of setting time test for control and experimental groups Group N Mean(sec) SD Control 10 216 12.64 Experimental 10 216 12.64 Table 7: t-test and p-value for setting time test t-test p-value Sig. 0.00 1 NS Figure 5: Bar chart for setting time test. 0.85 0.86 0.87 0.88 0.89 0.9 0.91 0.92 cond_contr cond_exp dimensional_change 56 58 60 62 64 66 68 70 72 74 cond_contr cond_exp wettability 0 50 100 150 200 250 cond_contr cond_exp setting_time_seconds J Bagh College Dentistry Vol. 28(4), December 2016 The Effect of Restorative Dentistry 25 5-Hardness test: A– After 1.5 minute: Mean values, number of specimens, standard deviation, t-test, and p-values of hardness test at 1.5 minute, are presented in table 8,table 9 and fig. 6. Figure 6: Bar chart for hardness at 90 second Their results indicated a non-significant difference between experimental and control means which are 16.62 and 16.14 respectively Table 8: Descriptive data of hardness test at 90 sec. for control and experimental groups. Group N Mean(°) SD Control 10 16.14 1.58 Experimental 10 16.62 0.94 Table 9: t-test and p-value for hardness test at 90 sec. t-test p-value Sig. -0.595 0.42 NS B-Hardness test at 2 hour Mean values, number of specimens, standard deviation, t-test, and p-values of hardness test at 1.5 minute, are presented in table 10, table 11 and fig. 7. The results indicated very clear and highly significant difference between means of the experimental and control groups, which are; 35.04 and 31.39 respectively. Table 10: Descriptive data of hardness test at 2hr. for control and experimental groups. Group N Mean(°) SD Control 10 31.39 1.77 Experimental 10 35.04 0.78 Table 11: t-test and p-value for hardness test at 2hr. t-test p-value Sig. -0.82 0.00 HS Figure 7: Bar chart for hardness at 2 hour DISSCUSION Zeolite was selected as a vehicle for antimicrobial cations because of its characteristics, including prolonged antimicrobial activity, non-toxicity and lack of odor or flavor (14- 16). Zeolite type X was used in this study due to the fact that zeolite X has got an excellent ionic conductivity as well as superior hydrophilicity. As zeolite X has low Si/Al ratio where the cation concentration, ion exchange capacity and hydrophilicity are inversely proportional to that ratio (15-17) Hydrophilicity is a beneficial attribute to prevent air bubbles formation within gypsum replica (18). Sliver and zinc ion as the cations of choice to be used in this study because they proved to possess strong antibacterial and antifungal activity (19,20). The concentration of 0.5 % selected in this study was optimized as this percentage representing the minimum percentage as an effective bactericidal agent (5,6). The results of dimensional change test in this study shows that the incorporation of Ag-Zn zeolite into condensation silicone because a non- significant change in the dimensional change of condensation silicone, this could be due to that the zeolite slightly decreases the evaporation of ethanol as by product. Another explanation is that it could be due to that the condensation silicone already contain silica in its basic ingredients in a percentage between (35-70%) so the added 0.5% by wt well probably has no sensible effects on condensation properties (12,21). Concerned with reproduction of details test it was noticed that the experimental group of condensation silicone showed almost identical results with those of control group, as an explanation it could be due to the small particles of incorporated zeolite in a range of (0.5–1µm) which was in accordance with the requirements of ADA/ANSI specification no. 19 for elastomeric impression material (7,8,21). Also it could be due to 15.8 16 16.2 16.4 16.6 16.8 cond_contr cond_exp hardness_90seconds 28 30 32 34 36 cond_contr cond_exp hardness_2hours J Bagh College Dentistry Vol. 28(4), December 2016 The Effect of Restorative Dentistry 26 the small percentage of Ag-Zn zeolite incorporated (22). Another explanation is that may be due to an increase in the hydrophilicity of the impression material as a result of incorporation of zeolite. As the hydrophilicity increased the reproduction of details enhanced (1). The wettability test results showed a highly significant increase in wettability of the experimental groups for condensation silicone in comparison to its control group. This increase of wettability could be explained by hygroscopic property of zeolite (23-25). The setting time results experimental and control groups for condensation silicone had nearly the same mean values of setting time test which was statistically non-significant. This may be contributed to the fact that only small percentage as well as small particle size (in range of 0.5-1µm) of the Ag-Zn zeolite incorporated into experimental material (21,22,24). The results of hardness test showed that the hardness after 1.5 min. of setting exhibit a statistically non-significant increase but with highly significant increase after 2 hours of setting time. Generally, zeolite incorporation may increase the hardness values of the material, and this increase in hardness was directly proportional to the increases in concentration of incorporated Ag-Zn zeolite (25). As an explanation that it could be attributed to the randomly distributed particles of a hard material into impression material matrix. Other explanation; it could be due to that zeolite is mainly composed of silica with small particle size and high surface area leading to better interfacial adhesion of the test material (25). REFERENCES 1. Anusavice KJ, Shen C, Rawls HR. Phillips’ science of dental materials.12th ed. St. Louis: Saunders, Elsevier Inc.; 2013. pp.153. 2. Craig RG, Powers JM. Restorative dental materials.12th ed. St. Louis: Elsevier; 2006. pp.291. 3. Samra RK, Bhide SV. Efficacy of different disinfectant systems on alginate and addition siliconee impression materials of indian and international origin: A comparative evaluation. J Indian Prosthodont Soc 2010; 10(3):182–9. 4. Kamişoğlu K, Aksoy EA, Akata B, Hasirci N, Baç N. Preparation and characterization of antibacterial zeolite–polyurethane composites. J Appl Polymer Sci 2008; 110: 2854–61. 5. Mutneja P, Raghavendraswamy KN, Gujjari AK. Flexural strength of heat cure acrylic resin after incorporation of different percentage of Sliver-zinc zeolite an in-vitro study. IJCI 2012; 4(4): 25-31. 6. Kawahara K, Tsuruda K, Morishita M, Uchida M. Antibacterial effect of silver-zeolite on oral bacteria under anaerobic condition. Dent Mater 2000; 16: 452- 5. 7. American National Standardization Institute / American Dental Association, Specification No.19 for elastomeric impression material. 2004. Chicago IL: ANSI/ADA. 8. Johnson GH, Lepe X, Aw TC. The effect of surface moisture on detail reproduction of elastomeric impressions. J Prosthet Dent 2003; 90: 354-64. 9. Petrie CS, Walker MP, O’Mahony AM, Spencer P. Dimensional accuracy and surface detail reproduction of two hydrophilicvinyl polysiloxane impression materials tested under dry, moist, and wet conditions. J Prosthet Dent 2003; 90: 365-72. 10. Katyayan PA, Kalavathy N, Katyayan M. Dimensional accuracy and detail reproduction of two hydrophilic vinyl polysiloxane impression materials tested under different conditions. Indian J Dent Res 2011; 22: 881- 2. 11. Zgura L, Beica T, Mitrofan IL, Mateias CG, Pirvu D, Patrascu I. Assessment of the impression materials by investigation of the hydrophilicity. Dig J Nanomater Bios 2010; 3: 749-55. 12. Powers JM, Sakaguchi RL. Craig’s Restorative dental materials.13th ed. Philadelphia: Mosby Co.; 2012. 13. ASTM International D2240–05. Standard test method for durometer hardness. 2010. West Conshohocken, PA. 14. Zhang Y, Zhong S, Zhang M, Lin Y. Antibacterial activity of silver-loaded zeolite A prepared by a fast microwave-loading method. J Mater Sci 2009; 44: 457–62. 15. Matsuura T, Sato AY, Okamoto K, Ueshige M, Akagawa Y. Prolonged antimicrobial effect of tissue conditioners containing silver-zeolite. J Dent Mater 1997; 25: 373–7. 16. Bekkum HV, Flanigen EM, Jansen JC. Introduction to zeolite science and practice. Amsterdam: Elsevier; 1991. pp.58. 17. Čejka J, Bekkum H, Corrma A, Schűth F. Introduction to zeolite science and practice. 3rd Revised ed. St. Louis: Elsevier; 2007. 18. Forch R, Schonherr H, Tobias A. Surface design: applications in bioscience and nanotechnology. Wiley- VCH; 2009. 19. Nikawa H, Yamamoto T, Hamada T, Rahardjo MB, Murata H, Nakanoda S. Antifungal effect of zeolite- incorporated tissue conditioner against Candida albicans growth and/or acid production. J Oral Rehabil 1997; 24: 350–7. 20. Abe Y, Ueshige M, Akagawa TM. Cytotoxicity of antimicrobial tissue conditioners containing silver- zeolite. Int J Prosthodont 2003; 16:141-4. 21. Azeez ZA, Hattor NA. The effect of incorporation of prepared Ag-Zn zeolite on some properties of heat polymerized acrylic denture base materials. J Bagh Coll Dentistry 2015: 27(1): 63-9. 22. Nakanoda S, Nikawa H, Hamada T, Yamamoto T, Nakamoto T. The material and antifungal properties of antibiotic zeolite incorporated acrylic resin.J Jpn Prosthodont Soc1995; 39: 926. 23. Kaali P, Pérez-Madrigal MM, Strömberg E, Aune R E, Czél G, Karlsson S. The influence of Ag+, Zn2+ and Cu2+ exchanged zeolite on antimicrobial and long term in vitro stability of medical grade polyether polyurethane. EXPRESS Polymer Lett 2011; 5(12):1028–40. J Bagh College Dentistry Vol. 28(4), December 2016 The Effect of Restorative Dentistry 27 24. Park YJ, Kim HO, Kim MK, Han HS, Song HJ, Vang MS. Effects of zeolite filler in surfactant-containing silicone rubber impression materials. 86th IADR, 2008. 25. Bussaya R. The development of rubber compound based on natural rubber and ethylene propylene die ne monomer for playground rubber material. A master thesis, Kasetsart University, 2007. mailto:yjpark@chonnam.ac.kr