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A STUDY ON IN VIVO AND IN VITRO AMALGAM CORROSION (아말감의 구강내 부식 및 인공 부식에 관한 연구)

  • Lim, Byong-Mok;Kwon, Hyuk-Choon;Um, Chung-Moon
    • Restorative Dentistry and Endodontics
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    • v.22 no.1
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    • pp.1-33
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    • 1997
  • The objective of this study was to analyze the in vitro and in vivo corrosion products of low and high copper amalgams. The four different types of amalgam alloy used in this study were Fine cut, Caulk spherical, Dispersalloy, and Tytin. After each amalgam alloy and Hg were triturated according to the directions of the manufacturer by means of the mechanical amalgamator(Amalgam mixer. Shinhung Co. Korea), the triturated mass was inserted into a cylindrical metal mold which was 12mm in diameter and 10mm in height. The mass was condensed by 150Kg/cm compressive force. The specimen was removed from the mold and aged at room temperature for about seven days. The standard surface preparation was routinely carried out by emery paper polishing under running water. In vitro amalgam specimens were potentiostatically polarized ten times in a normal saline solution at $37^{\circ}C$(potentiostat : HA-301. Hukuto Denko Corp. Japan). Each specimen was subjected to anodic polarization scan within the potential range -1700mV to+400mV(SCE). After corrosion tests, anodic polarization curves and corrosion potentials were obtained. The amount of component elements dissolved from amalgams into solution was measured three times by ICP AES(Inductive Coupled Plasma Atomic Emission Spectrometry: Plasma 40. Perkim Elmer Co. U.S.A.). The four different types of amalgam were filled in occlusal and buccal class I cavities of four human 3rd molars. After about five years the restorations were carefully removed after tooth extraction to preserve the structural details including the deteriorated margins. The occlusal surface, amalgam-tooth interface and the fractured surface of in vivo amalgam corrosion products were analyzed. In vivo and in vitro amalgam specimens were examined and analyzed metallographically by SEM(Scanning Electron Microscope: JSM 840. Jeol Co. Japan) and EDAX(Energy Dispersive Micro X-ray Analyser: JSM 840. Jeol Co. Japan). 1. The following results are obtained from in vitro corrosion tests. 1) Corrosion potentials of all amalgams became more noble after ten times passing through the in vitro corrosion test compared to first time. 2) After times through the test, released Cu concentration in saline solution was almost equal but highest in Fine cut. Ag and Hg ion concentration was highest in Caulk spherical and Sn was highest in Dispersalloy. 3) Analyses of surface corrosion products in vitro reveal the following results. a)The corroded surface of Caulk spherical has Na-Sn-Cl containing clusters of $5{\mu}m$ needle-like crystals and oval shapes of Sn-Cl phase, polyhedral Sn oxide phase. b)In Fine cut, there appeared to be a large Sn containing phase, surrounded by many Cu-Sn phases of $1{\mu}m$ granular shapes. c)Dispersalloy was covered by a thick reticular layer which contained Zn-Cl phase. d)In Tytin, a very thin, corroded layer had formed with irregularly growing Sn-Cl phases that looked like a stack of plates. 2. The following results are obtained by an analysis of in vivo amalgam corrosion products. 1) Occlusal surfaces of all amalgams were covered by thick amorphous layers containing Ca-P elements which were abraded by occlusal force. 2) In tooth-amalgam interface, Ca-P containing products were examined in all amalgams but were most clearly seen in low copper amalgams. 3) Sn oxide appeared as a polyhedral shape in internal space in Caulk spherical and Fine cut. 4) Apical pyramidal shaped Sn oxide and curved plate-like Sn-Cl phases resulted in Dispersalloy. 5) In Tytin, Sn oxide and Sn hydroxide were not seen but polyhedral Ag-Hg phase crystal appeared in internal space which assumed a ${\beta}_l$ phase.

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Development of a Simultaneous Analysis Method for DDT (DDD & DDE) in Ginseng (인삼 중 DDT(DDD 및 DDE) 분석법의 개발)

  • Kim, Sung-Dan;Cho, Tae-Hee;Han, Eun-Jung;Park, Seoung-Gyu;Han, Chang-Ho;Jo, Han-Bin;Choi, Byung-Hyun
    • Korean Journal of Food Science and Technology
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    • v.40 no.2
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    • pp.123-128
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    • 2008
  • The MRLs (maximum residue limits) of DDT (DDD and DDE) in fresh ginseng, dried ginseng, and steamed red ginseng are set as low as 0.01 mg/kg, 0.05 mg/kg, and 0.05 mg/kg, respectively. Therefore, this study was undertaken to develop a simple and highly sensitive analysis method, as well as to reduce interfering ginseng matrix peaks, for the determination of DDT isomers (o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in fresh ginseng, dried ginseng, and steamed red ginseng at the 0.01 mg/kg level. The method used acetonitrile extraction according to simultaneous analysis, followed by normal-phase Florisil solid-phase extraction column clean-up. The purification method entailed the following steps: (1) dissolve the concentrated sample extract in 7 mL hexane; (2) add 3 mL of $H_2SO_4$; (3) vigorously shake on avortex mixer; (4) cetrifuge at 2000 rpm for 5 min; (5) transfer 3.5 mL of the supernatant to the Florisil-SPE (500 mg/6 mL);and (6) elute the SPE column with 1.5 mL of hexane and 10 mL of ether/hexane (6:94). The determination of DDT isomers was carried out by a gas chromatography-electron capture detector (GC-${\mu}$ECD). The hexane and ether/hexane (6:94) eluate significantly removed chromatographic interferences, and the addition of 30% $H_2SO_4$ to the acetonitrile extract effectively reduced many interfering ginseng matrix peaks, to allow for the determination of the DDT isomers at the 0.01 mg/kg level. The recoveries of the 6 fortified (most at 0.01 mg/kg) DDT isomers from fresh ginseng, dried ginseng, and steamed red ginseng ranged from 87.9 to 99.6%. The MDLs (method detection limits) ranged from 0.003 to 0.009 mg/kg. Finally, the application of this method for the determination of DDT isomers is sensitive, rapid, simple, and inexpensive.

Studies on the Durability of Mortars (모르타르의 내구성에 관한 연구)

  • 고재군
    • Magazine of the Korean Society of Agricultural Engineers
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    • v.11 no.1
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    • pp.1604-1615
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    • 1969
  • This experiment was carried out as one of the basic studies to improve the acid resistance of concrete and it was conducted to investigate some relations among physical properties such as basorption, ratio of water to cement, compressive strength, density and ratio of mix to weight losses of mortar when exposed to 0.1 N solution of hydrochrolic acid. The results obtained from the limited data secured so far in this experiment are summarized as follows: 1. The specimens used in the experiment were made of 5 cubic centimeters of mortar having such various ratios of mix by weight as 1 : 1, 1 : 3, 1 : 5, 1 : 7, 1 : 10. 2. Physical tests included compressive strengths at 7 days, 28 days, 3 months, and 6 month, and 5 hour boiling absorption test. 3. In acid test, every specimen was immersed into 0.1 N solution of hydrochrolic acid. The specimens exposed to the acid solution were weighed to determine the weight losses of the acid-corroded at one week interval for 7 weeks exposure, and the old acid solutions were also changed to fresh one when weighed the weight losses by acid attack at one week interval. 4. The correlative relations were found among physical properties and they are expressed by certain formulas as follows; i) Relation between ratio of mix and absorption Y = 1.036x + 13.53 where Y: absorption(%) X: ratio of mix ii) Relation between ratio of mix and ratio of water-cement Y = 0.204x + 0.214 where Y: ratio of water-cement. X: ratio of mix iii) Relation between ratio of water-cement and absorption Y = 5.01x + 12.53 where Y: absorption(%). X: ratio of water-cement iv) Relation between density and absorption Y = 50.6 - 0.0176X where Y: absorption(%). X: density($kg/m^3$) v) Relation between density and ratio of water cement Y = 7.2183 - 0.0033X where Y: ratio of water-cement . X: density($kg/m^3$) 5. After completing the acid exposure test the specimens were corroded and , the per cent ranges of weight losses varies from a minimum of 20.4 per cent at a 1 : 1 mix to a maximum of 92.0 per cent at a 1:10 mix 6. The correlative relations of physical properties of mortar to weight losses by acid attak were found and they are also expressed by certain formulas as follows: i) Relation between weight losses and ratio of mix Y = 8.59X + 8.63 where Y: weight losses(%), X: ratio of mix ii) Relation between wieght losses and absorption Y = 0.121x + 12.43 where Y: absorption(%). X: weight losses(%) iii) Relation between weight losses and ratio of w/c Y = 0.0226X + 0.07 where Y: ratio of w/c X: weight losses(%) iv) Relation between weight losses and compressive strength LogY = 3.6097 - 0.05058X + 0.00022$X^2$ where Y: compressive strength ($kg/cm^3$) X: weight losses(%) v) Relation between weight losses and density Y = 2153.1 - 6.62X where Y: density($kg/m^3$) X: weigh losses(%) 7. In order to make better acid resistant mortar, it could be concluded that a 1 : 3 mix or richer mixes, adequate mixing water to minnimize the ratio of water-cement considering the workability, 16 per cent or less absorption by 5 hour boiling water, 1,800 kilogram per cubic meter or denser density by absolute weight base and 200 kilogram per square meter or compressive strength at 20 day, etc are required so as to obtain acid-resistant mortar. In addition to the above, it might be recommonded to select the fine aggregate and to use better equipments such as a mechanical vibrator, a mechanical mixer etc. in concrete manufacturing works.

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