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Effect of pH and concentrations of
ethanol on surface change
and color stability of heat-activated
denture base resin
Youn-Hee Hong
Department of Dentistry
The Graduate School, Yonsei University
Effect of pH and concentrations of
ethanol on surface change
and color stability of heat-activated
denture base resin
Directed by Professor Kwang-Mahn Kim
The Master's Thesis
submitted to the Department of Dentistry,
the Graduate School of Yonsei University
in partial fulfillment of the requirements
for the degree of Master of Dentistry
Youn-Hee Hong
June 2016
ACKNOWLEDGEMENTS
연 학 치과 학 치과생체재 공학 실 입학 합격 식을 듣고 뛸 듯이
기뻐하 기억이 어제 일처럼 생생한 어느 졸업이 눈앞에 다가 고 저의
사학위 논문이 결실을 맺게 되었습니다.
저, 이 논문이 되기까 아낌없는 조언과 애정 어린 심으 해
주 수님께 깊은 감사를 드립니다.
또한, 자신감 잃 않 기를 아주시고 가르침을 주신 김경남
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을 주신 실 생님들과 친 들 두 감사합니다.
마 막으 제가 학위를 무사히 마칠 수 있 에 응 해주시고 믿고
켜 주신 사 하는 님과 언니에게 이 논문을 칩니다. 사 합니다.
i
TABLE OF CONTENTS
LIST OF FIGURES ····································································ⅲ
LIST OF TABLES ······································································ⅳ
ABSTRACT ·············································································ⅴ
I. INTRODUCTION ···································································· 1
1.1. Color stability ······································································ 2
1.2. Surface roughness ································································· 2
1.3. Originality of this study··························································· 2
1.4. Aims of this study ································································· 3
II. MATERIALS AND METHODS ·················································· 4
1. Material ··············································································· 4
1.1. Specimen preparation··························································· 5
1.2. Immersion solution ····························································· 5
2. Method················································································ 5
2.1. Color change measurement ···················································· 6
2.2. Surface roughness······························································· 7
2.3. Surface morphology ···························································· 7
2.4. Statistical analysis······························································· 7
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III. RESULTS ············································································ 8
1. Color change measurement ························································· 8
2. Surface roughness ··································································· 9
3. Surface morphology································································10
IV. DISCUSSION ·······································································11
V. CONCLUSION ······································································13
VI. REFERENCE·······································································14
ABSTRACT (IN KOREAN) ························································18
iii
LIST OF FIGURES
Figure 1. Denture base resin in metal flask ································4
Figure 2. Prepared specimens ······················································4
Figure 3. SEM (200x) of specimen flat surfaces following immersion
in each solution for 10 days ········································· 10
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LIST OF TABLES
Table 1. Materials used in study ·············································4
Table 2. Control and experimental group···································6
Table 3. The mean values of standard deviations of color differences
(ΔE) compared with control ·······································8
Table 4. The mean values of standard deviations SDs of Ra (㎛) ······9
v
ABSTRACT
Effect of pH and concentrations of ethanol on surface change
and color stability of heat-activated denture base resin
Youn-Hee Hong
Department of Dentistry
The Graduate School, Yonsei University
(Directed by Professor Kwang-Mahn Kim, D.D.S., Ph.D.)
Complete dentures are mostly fabricated by using acrylic resin. Consumption of
certain beverages may affect the esthetic and physical properties of acrylic resin.
Due to its low pH, ethanol can produce erosion and alter some properties of
acrylic resin, as well. This study evaluated the change in surface and color of
conventional heat-activated denture base resin by subjecting it to different pH and
concentrations of ethanol at different time intervals.
A heat-activated denture base resin (SR Triplex Hot, Ivoclar Vivadent,
Liechtenstein, Europe) was used as a material of this study. Fifty specimens (20
mm x 20 mm x 2 mm) were prepared by manufacturer’s instruction and divided
into 5 groups which were a control group (PBS, pH 7.4), group 1 (PBS + HCl, pH
4.0), group 2 (PBS + NaOH, pH 10.0), group 3 (PBS + Ethanol, ethanol
vi
concentration 20 %) and group 4 (PBS + Ethanol, ethanol concentration 40 %) for
each test solution. All groups were mixed with green pigment and prepared as the
test solutions. The specimens were immersed into the groups at 37 ℃ and stored
for 10 days. After 5 and 10 days of immersion, the surface roughness (Ra) and
color difference (ΔE) of the specimens were measured. The color change was
checked by a Spectrophotometer (CM-3500d, MINOLTA, Japan) using a CIE Lab
system. The surface roughness tester (Mitutoyo Corp, Kawasaki, Japan) was used
to measure the surface roughness of the specimens and the surface morphologies
were observed by SEM.
According to the results of color change, no significant difference was observed
among groups at T1 (p>0.05). However, group 4 at T2 showed significant
difference that compared with the other groups (p<0.05). There was significant
different between T1 and T2 in group 4 (p<0.05).
When surface roughness of groups analyzed, the highest surface roughness was
observed in group 4 followed by group 3 at T2. However, group 4 was only found
significant difference at T1 (p<0.05). There was no significant different between
the pH variations groups (group 1 and 2) and the control group (p>0.05). The
surface became rougher with time in group 3, 4 (p<0.05).
SEM evaluation at 200 x magnification showed a slightly more irregular surface
in group 3 and a distinct irregular feature in group 4.
From the obtained results, it was concluded that denture base resin is not
recommended to immerse in ethanol for cleaning and disinfection.
Key words: heat-activated denture base resin, color change, surface roughness,
surface change, pH, ethanol
- 1 -
Effect of pH and concentrations of ethanol on surface change
and color stability of heat-activated denture base resin
Youn-Hee Hong
Department of Dentistry
The Graduate School, Yonsei University
(Directed by Professor Kwang-Mahn Kim, D.D.S., Ph.D.)
I. INTRODUCTION
Complete dentures are mostly fabricated by using acrylic resin because it is a low cost
material that requires relatively easy manipulation and construction methods. However, it
is not the ideal material in every respect (Shotwell et al., 1992). A drawback of this
material is that its esthetic, physical, and mechanical properties change rapidly over time
in the oral environment. (Keyf and Etikan, 2004). Consumption of certain beverages may
affect the esthetic and physical properties (Dietschiet al., 1994) of the acrylic resin. Due
to its low pH, ethanol can produce erosion and alter some properties of acrylic resin, as
well. The chemicals in beverages can lead to wear and surface degradation of acrylic
resin, resulting in unaesthetic external pigmentation, such as, stains (Sarret et al., 2000).
- 2 -
1.1 Color stability
Staining of acrylic resin can lead to esthetic problems. denture base polymers should
have a smooth and glassy surface and be capable of matching the natural appearance of
soft tissues. The material should be translucent for the best esthetic effect. Color and
translucency should be maintained during processing, and acrylic resin should not
become stained and not change color in clinical use (Hersek et al., 1999). Color change of
prosthodontic materials may result in patient dissatisfaction and additional expense for
replacement (Sham et al., 2004).
1.2 Surface roughness
The roughened surface may accumulate plaque. A high percentage of elderly people
consume ethanol containing beverages (Kirchner et al., 2007). Ethanol is present in
several drinks and has been shown to soften the denture base PMMA (Hargreaves, 1981).
Ethanol is also thought to act as a plasticizer of the polymer matrix (Ferracane and
Marker, 1994).
1.3 Originality of this study
Although there have been some studies on the color stability of acrylic resin denture
bases (Lai, 2003), the comparison of these resins was after immersion in beverages such
as cola and red wine. However, these beverages have different composition. For example,
Cola gains its color through the addition of caramel, which exhibits colors ranging from
the palest yellow to the deepest brown and is made by heating sugar or glucose in the
presence of alkali or mineral acid (Patel, 2004). Also, cola has the low pH and it may
damage the surface of the materials. Therefore, it is difficult to determine the direct cause
of the color stability with those studies.
- 3 -
1.4 Aims of this study
The aim of the present study was to analyze the change in surface and the color stability
of conventional heat-activated denture base resin by subjecting it to different pH and
concentrations of ethanol and to find possible co-relation between the change in the
surface roughness and the color stability.
The null hypotheses were that (1) there would be no significant difference in the color
change and the surface roughness in the pH variations and concentrations of ethanol and
(2) there would be no relationship between the color change and the surface roughness.
- 4 -
II. MATERIALS AND METHODS
1. Material
Table 1. Materials used in study
Material Product Manufacturer
Heat-activated denture base
resin
SR Triplex Hot Ivoclar
Vivadent
Coloring agent Tempera Shield
Buffering solution Phosphate buffered saline (PBS) pH 7.4 Gibco
Acid Hydrochloric acid (HCl) Duksan
Alkali Sodium Hydroxide (NaOH) Duksan
Ethanol Ethyl Alcohol 99.9% (Ethanol) Duksan
Fig 1. Denture base resin in metal flask. Fig 2. Prepared specimens.
- 5 -
1.1 Specimen preparation
In this study, a heat-activated denture base resin (SR Triplex Hot, Ivoclar Vivadent,
Liechtenstein, Europe) was used to prepare the specimens. The heat-activated denture
base resin was mixed according to the powder / liquid ratio (23.4 g / 10 ml) recommended
by the manufacturer. It was then molded in a flask filled with gypsum (Fig. 1), and the
stone surfaces coated with a separator. The material was polymerized in a water bath
according to the manufacturer’s recommendations - heat up to 100 ℃ and let boil for 45
minutes. The specimens were placed cool at room temperature for 30 minutes.
Subsequently, the flask was completely cooled with cold water. After deflasking, the
specimens were abraded on both sides with no. 600 grit silicone sand paper. Slurry of
water and pumice was applied to surfaces of the specimens with a brush wheel. Fifty
specimens (Fig. 2) were made and the size of each square shape specimen was 20 mm x
20 mm x 2 mm.
1.2 Immersion solution
The 50 ml of solutions that were pH 4.0 (PBS + HCl), pH 10.0 (PBS + NaOH), ethanol
concentration 20 % (PBS + Ethanol), ethanol concentration 40 % (PBS + Ethanol) and
pH 7.4 (PBS) were prepared for immersion of the specimens and mixed with 5 ml of
green pigment which was a complementary color of the denture base resin to check the
color change (Table 1). The pHs were checked by a digital pH-meter (Orion 4 star,
Thermo Fisher scientific Inc., Singapore).
2. Method
The specimens were first divided into 5 groups for each test solution (Table 2), then for
each solution 10 specimens were coded, from 1 to 10, on the back of the specimens. They
were immersed individually in 5 ml of each solution at 37℃ and stored for 10 days.
- 6 -
Table 2. Control and experimental group
Group property Remark
Control pH 7.4 -
1 pH 4.0 experimental group
2 pH 10.0 experimental group
3 ethanol concentration 20% experimental group
4 ethanol concentration 40% experimental group
After 5 days (T1) and 10 days (T2) immersion, the specimens were rinsed with distilled
water for 3 minutes and blotted dry with tissue paper before color stability and surface
roughness measurement.
2.1 Color change measurement
The color of control group was measured before the calculation of color differences
(ΔE) of group 1 to 4. Then, the colors of specimens of group 1 to 4 were measured with a
spectrophotometer (CM-3500d, MINOLTA, Japan). Color differences (ΔE) between
control group and group 1 to 4 were calculated automatically by the appliance,
represented by the formula:
ΔE* = [(ΔL*)2+(Δa*)2+(Δb*)2] ½
Before each measurement, the spectrophotometer was calibrated according to the
manufacturer's recommendations. The measurement mode was light reflective and the
diameter was 8 mm. L∗ refers to the lightness coordinate, and its value ranges from zero
(black) to 100 (white). The a∗ and b∗ are chromaticity coordinates in the red-green axis
and the yellow-blue axis, respectively. Positive a∗ values indicate a shift to red, and
negative values indicate a shift to green. Similarly, positive b∗ values indicate the yellow
color range, and negative values indicate the blue color range (Guler et al., 2005). The
center of specimens was measured and the mean values of the ΔE data were calculated.
- 7 -
2.2 Surface roughness
The surface roughness tester SJ-400 (Mitutoyo Corp, Kawasaki, Japan) was used to
measure the specimens’ surface roughness. The profiler was set to move a diamond stylus
across the specimen surface under a constant load of 4 mN.
The surface roughness was measured with a linear variable differential transformer. The
surface roughness was derived from computing the numerical values of the surface
profile. The Ra value describes the overall roughness of a surface and is defined as the
mean value of all absolute distances of the roughness profiles from the mean line within
the measuring distance. 4.0 mm of each scanning line was carried out for each specimen
in 3 randomly selected areas. The mean Ra was calculated from three lines as the mean
roughness of the specimen.
2.3 Surface morphology
A specimen of each group (Table 2) was selected after 10 days immersion for further
study. These specimens were subsequently processed for SEM. One of the flat surfaces
was coated with gold and observed in a scanning electron microscope (AIS2300C, Seron
technologies, Inc., Gyeonggi-Do, Korea).
2.4 Statistical analysis
One-way, ANOVA was used to evaluate the effect of pH and ethanol between the groups
with the same immersion time, and the influence of different immersion time in the same
group. The relationship between color stability and surface roughness over time was
analyzed with two-way ANOVA. Mean values were compared by the Tukey HSD test
(p<0.05).
- 8 -
III. RESULTS
1. Color change measurement
The color differences (ΔE) of the specimens after T1 and T2 of immersion in the solutions are presented in Table 3, as well as the differences among groups.
Table 3. The mean values and standard deviations of color differences (ΔE) compared
with control
Group T1 T2
1 1.13 (0.54)aA 1.37 (0.87)aA
2 1.35 (0.77)aA 1.56 (0.49)aA
3 1.75 (0.64)aA 2.18 (0.61)aA
4 1.88 (0.45)aA 5.91 (2.47)bB
See Table 2 for meaning of each group
a. b: Different letters indicate dissimilarity in same groups (p<0.05)
A. B: Different letters indicate dissimilarity in same immersion time (p<0.05)
T1: 5 days. T2: 10 days
”()”: standard deviation
According to the results, no significant difference was observed among groups at T1
(p>0.05). However, group 4 at T2 showed significant difference that compared with the
other groups in color change (p<0.05). There was significant different between T1 and T2
in group 4 (p<0.05).
- 9 -
2. Surface roughness
Surface roughness tester measured the difference in the surface roughness of each group
at T1 and T2. According to the ANOVA results, mean values and SDs of surface roughness
(Ra) and group differences are listed in Table 4, respectively.
Table 4. The mean values and standard deviations of Ra (㎛)
Group T1 T2
control 0.05 (0.007)aA 0.05 (0.009)aA
1 0.04 (0.006)aA 0.05 (0.007)aA
2 0.05 (0.007)aA 0.05 (0.011)aA
3 0.06 (0.012)aA 0.15 (0.028)bB
4 0.12 (0.020)aB 0.24 (0.057)bC
See Table 2 for meaning of each group
a. b: Different letters indicate dissimilarity in same groups (p<0.05)
A. B. C: Different letters indicate dissimilarity in same immersion time (p<0.05)
T1: 5 days. T2: 10 days
”()”: standard deviation
The highest surface roughness was observed in group 4 followed by group 3 at T2
(p<0.05). However, group 4 was only found significant difference at T1 (p<0.05). There
was no significant different between the pH variations groups (group 1 and 2) and the
control group (p>0.05). The surface became rougher with time in group 3 and 4 (p<0.05).
- 10 -
3. Surface morphology
Before immersion Control
Group 1 Group 2
Group 3 Group 4
Fig 3. SEM (200x) of specimen flat surfaces following immersion in each solution for 10
days.
Fig 3 presents a micrograph illustrating surface characteristics after immersion in each
group. SEM evaluation at 200 x magnification showed a smooth aspect for the specimens
immersed in group 1 and 2. However, a slightly more irregular surface was found for
group 3 and a distinct irregular feature was evident for acrylic resin submitted to
immersion in group 4.
- 11 -
IV. DISCUSSION
Acrylic resin has been used since 1937 for making denture bases, and the most widely
used material is poly-methyl methacrylate (PMMA) (Lai et al., 2004, Machado et al.,
2007). Polymerization is an exothermic reaction by addition, consisting of the bond
between monomers, resulting in a single polymeric macromolecule characterized by its
high molecular weight. The chemical reaction of acrylic resin polymerization is
exothermic, which may be initiated by chemical substances, light and heat supplied by
heated water or microwave energy (Phillips, 1993), and these methods are routinely used
in denture laboratories (Anusavice, 1998).
This study was to evaluate the effect of pH and ethanol contents similar to the
concentration of alcoholic beverages on surface and color of conventional heat-activated
denture base resin. The denture base resins have been reported to be critical in color
stability, which is affected by different alcohol concentrations and pH solutions (Patel et
al., 2004). Several studies have reported that alcohol facilitates staining by softening the
resin matrix. Therefore, it could be possible that the alcohol component roughened the
denture base resin surfaces, thereby resulting in increased staining (Patel et al., 2004).
In this study, the roughness parameter (Ra) was analyzed, because it represents the
arithmetic mean of all the roughness values within the covered space on a certain
surface. Therefore, Ra is the most indicated value (Joniot et al., 2006, Türkün and Türkün,
2004). Also, the CIE Lab system for measuring chromaticity was chosen to record color
differences as it is well suited for the determination of small color differences (Khokhar et
al., 1991). If a material is completely color stable, no color difference will be detected
after its exposure to the testing environment (ΔE=0). Various studies have reported
different thresholds of color-difference values above which the color change is
perceptible to the human eye. These values of ΔE ranged from equal to 1 (Seghi et al.,
- 12 -
1989), between 2 and 3 (Ruyter et al., 1987), greater than or equal to 3.3 (Johnston and
Kao, 1989), and greater than or equal to 3.7 (Okubo et al., 1998). Values of ΔE between 0
and 2 were imperceptible, values of ΔE in the range of 2 to 3 were just perceptible, values
from 3 to 8 were moderately perceptible, and values above 8 were markedly perceptible
(Gross and Moser, 1977). A ΔE value of 3.7 or less was considered to be clinically
acceptable (Okubo et al., 1998, Johnston and Kao, 1989). In this study, except for group 4
at T2 (ΔE=5.91), the color changes exhibited by all specimens are at clinically acceptable
levels (ΔE≤3.7).
According to the results of this study, the specimens became significantly stained and
rougher after they were immersed in ethanol group 3 and 4. This result showed that there
was a co-relation between color stability and surface roughness. Also, as the immersion
time increased, the changes became more severe.
The denture may function as a reservoir of infection, and surface irregularities would
increase the likelihood of microorganisms remaining on the surface after the prosthesis
has been cleaned (Azevedo et al., 2006, Yannikakis et al., 2002). This roughened surface
may cause plaque accumulation as well as staining. This concept is of clinical importance
because patients need to have a smooth surface to deter the formation of a biofilm. This is
an aesthetic concern as well as an overall concern for maintaining good oral hygiene
(Berger et al., 2006). The roughness of the acrylic resin surfaces is of considerable
importance, as microorganism adhesion to a surface is a pre-requisite for the colonization
of this surface, reducing the mechanical properties of the denture base such as hardness
and flexural strength (Bafile et al., 1991). Therefore, further study should be tested to see
if any correlation exists between the microorganism adhesion to a surface and the
mechanical properties of denture base resin.
- 13 -
V. CONCLUSION
From the results obtained, and within the limitations of the study, it was concluded that:
(1) .pH did not affect both color and surface change.
(2) Specimens which were immersed in high concentrations ethanol (40%) for 10 days
showed significant change in color and surface roughness.
(3) Surface of specimens which were immersed in ethanol became rougher with time.
(4) Specimens which were immersed in high concentrations ethanol (40%) showed
significant color difference with time.
Therefore, denture base resin is not recommended to immerse in ethanol for cleaning
and disinfection.
- 14 -
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Guanabara-koogan 271.
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J Prosthodont 15:235–242.
Bafile M, Graser GN, Myers ML, Li EKH (1991). Porosity of denture resin cured
by Microwaveenergy. J Prosthet Dent 66:269–274.
Berger JC, Driscoll CF, Romberg E, Luo Q, Thompson G (2006). Surface
roughness of Denture base acrylic resins after processing and polishing.
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Dietschi D, Campanile G, Holz J, Meyer JM (1994). Comparison of the color
stability of Tennew-generation composites: An in vitro study. Dent Mater
10:353-62.
Ferracane JL, Marker VA (1994). Solvent degradation and reduced fracture toughness in
agedcomposites. J Dent Res 92:257–61.
Gross MD, Moser JB (1977). A colorimetric study of coffee and tea staining of four
composite resins. J Oral Rehabil 4:311–322.
- 15 -
Guler AU, Yilmaz F, Kulunk T, et al (2005). Effects of different drinks on
stainability of Resin composite provisional restorative materials. J Prosthet Dent
94:118-124.
Hargreaves AS (1981). The effect of the environment on the crack initiation
toughness of dentalpoly(methyl methacrylate). J Biomed Mater Res 15:757-768.
Hersek N, Canay S, Uzun G, et al (1999). Color stability of denture base acrylic
resins in three food colorants. J Prosthet Dent 81:375-379.
Johnston WM, Kao EC (1989). Assessment of appearance match by visual observation
and clinical colorimetry. J Dent Res 68:819–822.
Joniot S, Salomon JP, Dejou J, Grégoire G (2006). Use of two surface analyzers
to evaluate thesurface roughness of four esthetic restorative materials after
polishing. Operat Dent 31:39–46.
Keyf F, Etikan I (2004). Evaluation of gloss changes of two denture acrylic resin
materials In four different beverages. Dent Mater 20:244-251.
Khokhar ZA, Razzoog ME, Yaman P (1991). Color stability of restorative resins.
Quintessence Int 22:733–737.
Kirchner JE, Zubritsky C, Cody M, et al (2007). Alcohol consumption among older adults
in primary care. J Gen Intern Med 22:92-97.
Lai CP, Tsai MH, Chen M, Chang HS, Tay HH (2004). Morphology and
properties of Dentureacrylic resins cured by microwave energy and conventional
water bath. Dent Mater 20:133–141.
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ABSTRACT (IN KOREAN)
pH 에탄 도가 열중합 치상 진 변
색 안 에 미치는 향
<지도 수 만>
연 학 학원 치 학과
연
치는 아크릴릭 진 사 하여 다. 그러나 재
료 문 강 경에 따라 심미 , 물리 물 변 가
루어진다는 것 다. 특 료 비는 아크릴릭 진 심미
과 물 에 향 미칠 수 고 는 낮 pH 함 에탄
하여 아크릴릭 진 식과 물 변 에 해 초래 수
다.
따라 본 연 pH 에탄 도에 따라 열중합 치상
진 과 색 변 연 하는 것 다.
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열중합 치상 진 (SR Triplex Hot, IvoclarVivadent,
Liechtenstein, Europe) 사 하여 50개 시편 (20 mm x 20 mm x 2
mm) 사 지시에 따라 하 고 각각 5개 그룹 10개씩
나누었다. (PBS, pH 7.4), 1 (PBS + HCL, pH 4.0), 2 (PBS +
NaOH, pH 10.0), 3 (PBS + 20% Ethanol) 그리고 4 (PBS + 40%
Ethanol)에 초 색 색 어 침 할 액 준비하 고
시편 각각 액에 침 하여 37℃ 암실에 10 간 보 하 다.
5 과 10 간 침 후, 각 시편 거칠 (Ra) 색 변 (ΔE)
측 하 다. 색 변 는 도계(CM-3500d, MINOLTA, Japan)
CIE Lab system 사 하여 하 고, 과 색 차 계산하
다. 거칠 는 도측 (Mitutoyo Corp, Kawasaki, Japan)
사 하여 측 하 SEM(scanning electron microscope)
태 찰하 다.
색 변 측 결과, T1에 는 실험 간에 한 차 가 지 않았
나 (p>0.05), T2에 는 4 에 다 실험 과 한 차 보
다 (p<0.05). 또한, 4 에 는 T1과 T2 사 에도 한 차가 나타났다
(p<0.05). 거칠 결과에 따 , T2에 는 3 과 4 에 한
차 하 고 4 > 3 순 거칠 값 아 나, T1에 는 4
에 만 한 차가 나타났다 (p<0.05). pH 한 1 과 2 에 는
과 한 차 가 없었다 (p>0.05). T1과 T2 비 시에는, 3 과
4 에 거칠 값 시간에 따라 증가하는 것 하 다
(p<0.05). SEM 결과, 3 과 4 에 변 양상 보 다.
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색 변 거칠 에탄 에 침 에 많 변 보
, 상 결과 치상 진 사 시 척과 독 해 에
탄 에 담가 지 말 것 한다.
핵심 는 말: 열중합 치상 진, 색변 , 거칠 , 변 , pH, 에탄