Thermal deterioration of marbles: Gloss, color changes

Construction and Building Materials 102 (2016) 416–421

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Construction and Building Materials journal homepage: www.elsevier.com/locate/conbuildmat

Thermal deterioration of marbles: Gloss, color changes Didem Eren Sarıcı Department of Mining Engineering, Inonu University, 44280 Malatya, Turkey

h i g h l i g h t s
This article define marble behavior to slow and fast temperature changes.
Changes in surface gloss and color parameters (L, a, b) due to thermal shock and thermal ageing cycles.
Effects of L, a, b changes on surface gloss changes highlighted.

a r t i c l e

i n f o

Article history: Received 26 May 2015 Received in revised form 14 October 2015 Accepted 28 October 2015 Available online 13 November 2015 Keywords: Thermal shock Thermal ageing Gloss Color parameters

a b s t r a c t Marbles are widely used as construction materials because of their high resistivity to common conditions, and to their aesthetic appeal. Aesthetic qualities such as color, gloss and polishability are important for rock used as constructions materials. But marbles as building stones show complex weathering phenomena. Thermal effects are important weathering factors affecting the aesthetical and physico-mechanical properties of marbles. This study assesses changes to surface aesthetic properties of some marble samples due to heat. For this purpose thermal ageing and thermal shock cycles were inflicted on six types of marble samples of differing colors. Marble samples of shiny surfaces were prepared. In thermal shock cycles, samples were heated up to 105 °C for 18 h then placed for 6 h in distilled water. In thermal ageing cycles, the samples were placed in an oven for 18 h then allowed to cool for 6 h at room temperature. At the end of cycles 4, 8, 12, 16 and 20, gloss measurements were recorded; at the end of the last cycles color changes were evaluated. The relationships between gloss and color parameters were also investigated. Thermal shock has more important effects on marble surface properties than the thermal ageing cycle. L⁄ and b⁄ parameters constituted an important effect on glossiness and these parameters were strong indicators for predicting gloss loss. Ó 2015 Elsevier Ltd. All rights reserved.

1. Introduction Natural stones and marbles have special characteristics such as color, texture and grain size. Accordingly, they have been commonly used as a decorative material for cladding the outside of walls and buildings either with structural (columns, floors, etc.) or decorative purposes (reliefs, statues, etc.) [1,2]. The aesthetic properties depend on several factors, such as texture, shape and size of grains, color, and surface gloss [3,4]. With a fine surface finish, the aesthetic properties of marbles are maximized. According to their function, natural stone products can be grouped to the following categories: – Slab products. – Rough products. – Special products. E-mail address: [email protected] http://dx.doi.org/10.1016/j.conbuildmat.2015.10.200 0950-0618/Ó 2015 Elsevier Ltd. All rights reserved.

Sawed marbles have surface irregularities. Accordingly, marble slabs or other products are usually polished. At the end of the polishing, the surface becomes shiny reflective (glossy) and mirroring [4]. The gloss and color are key parameters for evaluating the efficiency and value of the polishing process [5–11]. Gloss is defined by ASTM as the capability of a surface to reflect incident light. It is related to polishing and has an effect on the aesthetic attributes of rock [12,13]. Gloss is related to roughness, because reflectance capacity of surface are related surface smoothness [2,14]. Color is the other main physical property that influences the marketability of marble. Chemical content and physical properties of marble leads to varying colors. The final color of marbles varies depending on the impurities. For example iron-oxides gives rise to yellow, yellowish or reddish colors, and manganese oxides and carbonic impurities give rise to dark bluish, violet or black colors. In the marble industry, color identification is described by wellknown colors (brown, red, white, honey, lilac, cherry, sky blue,

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etc.) and textures are described as leopard, tiger, etc. In Turkey there are specific marbles named Aksßehir beige, Elazıg cherry, Marmara gray, etc. [15]. When compared to such building materials as wood or mud, stone is generally assumed to be the most durable material. But despite this common belief, stone can deteriorate and many factors will affect it [16]. Marble marketability is affected by many factors such as thermal changes, chemical contaminants, salt crystallization, solar radiation, pollution (notably acid rain) and bio deterioration [4,17]. In marble decay, thermal effects play an important role. Thermal effects, especially when coupled with other environmental factors such as water content, and chemical exposure, change petrographic, mechanic and surface properties of marble. These changes lead to deterioration from increased porosity and loosening of rock cohesion [18,19]. Increasing temperature and related thermal expansion cause tensions that lead to cracks and increased pore volume. Such deformations lead to oxidation, decomposition and polymorphic transformation, and these effects decrease marble surface quality [20,21]. Stone durability is usually more affected in urban environments. Usually changes in color, stains, efflorescence, and material loss are common aspects of stone materials decay. In order to avoid such decay, accelerated durability tests were carried out and decay processes observed [3,22]. This study investigates thermal shock and thermal ageing effects on the color and gloss values of the polished surfaces of some Turkish marble. The samples were subjected to a thermal shock and thermal ageing chamber, and the influence of these stresses on color and gloss and the relationship between gloss and color changes were determined. 2. Experimental setup Two thermal cycles of thermal ageing and thermal shock were inflicted on differently colored marbles, and two main measuring instruments were used: a gloss-meter and color meter. 2.1. Materials Six marbles were investigated. The sample code, commercial names, and stone types of the samples are given in Table 2.1. The samples were examined in two groups. Sample of the first group have light color, samples of the second group dark color. The polished surface and 200 mm  200 mm  20 mm sized samples were collected from marble processing plants in Turkey. The physical properties were determined suggested by TSE procedures [23–25]. The physico-mechanical properties of marbles are shown in Table 2.2, results of XRF analysis in Table 2.3 and results of XRD in Table 2.4. 2.2. Thermal cycles Two sets of samples from each rock type were prepared and thermal treatments were inflicted on samples prior to starting the cycles; every four cycles gloss measurements were performed on the surface of the samples. Six samples were prepared from each marble. A total of 20 thermal ageing and thermal shock cycles were performed. Prior to starting the cycles and at the end of the cycles, color analyses were performed at nine different points marked on the sample surfaces. Two different thermal treatments were used. 2.2.1. Thermal ageing chamber The first thermal treatments were performed with procedures suggested by Lam dos Santos et al. 2011, with minor modification [26]. To provide uniformity, thermal condition at the thermal shock and thermal ageing cycles 200 °C indicated in Santos 2011 was applied at 105 °C. The specimens were subjected to cycles of heating (105 °C) and cooling in air (room temperature 20 °C). The samples spent 18 h in an oven, then 6 h at room temperature (20 °C). This type of test is called thermal ageing. At the end of the every four cycles gloss measurements were recorded. 2.2.2. Thermal shock chamber The second thermal treatments were performed with procedures suggested by TS 14066 [27]. The specimens were heated in the same way as explained in (a) and then were rapidly immersed in distilled water at 20 °C. The water was kept constant

Table 2.1 Sample code, commercial names, stone types of samples. Sample code

Commercial name

Stone type

Color type

MB

Best Cream

Limestone

Beige

E

Crystal Emperador

Dolomite

Light brown

KT

Red Travertine

Travertine

Light red

EV

Rosso Levanto

Limestone

Dark red

HY

Verde Antico

Limestone

Dark green

SI_

Black Pearl

Limestone

Black

at 20 ± 1 °C. Test samples spent 18 h in an oven then stayed in distilled water for 6 h. In this study, a Nuve KD400 oven was used. This type of test is called thermal shock. At the end of every four cycles, the gloss measurements were recorded. In this study the gloss measurement was done using a Q TQC GL0010 60° solo gloss meter at 60° angles for each stone sample. A gloss-meter sends light at a certain angle to the surface and determines the surface gloss numerically based on the reflection angle of the light. It can be done on rough surfaces. Gloss-meters are less sensitive to vibrations and seem to be partially appropriate for quality-control measurements conducted in commercial facilities [1]. Gloss values are expressed in GU (gloss units). The color was assessed using a Hunter CIELAB colorimeter. In the CIELAB system, the color is quantified according to three chromatic coordinates: L parameter represents lightness or luminosity (L = 0 dark; L = 100 white); ‘‘a” parameter is the red–green axis (a > 0 red; a < 0 green); and ‘‘b” parameter is the yellow–blue axis (b > 0 yellow; b < 0 blue1) [28]. The CIELAB coordinate system is shown that in Fig. 2.1.

3. Result and discussion 3.1. Gloss changes owing to the thermal chamber Figs. 3.1 and 3.2 indicate the gloss values of the marble samples during thermal ageing and the thermal shock chamber. As can be seen in Figs. 3.1 and 3.2, cycle progressions led to a decrease of the surface gloss value. In addition, the glossiness of the marbles was not uniformly affected by the thermal shock and thermal ageing. The graphics show that depending on the increase in the number of cycles, surface gloss values decreased very slowly and at on a changeable scale. As the thermal shock cycle was increased, glossiness decreased in all of the marbles. The most important decrease was realized in Light red travertine. Especially in the first four cycles, Red travertine showed a different loss of gloss values. It was fast in the early stages and slower later on. This may owe to the fact that Red travertine has many open porous. 1 For interpretation of color in Fig. 2.1, the reader is referred to the web version of this article.

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Table 2.2 Physical properties of marble samples. Sample

Natural unit weight (g/cm3)

Saturated unit weight (g/cm3)

Dry unit weight (g/cm3)

Water absorption by weight (%)

Water absorption by volume (%)

Mohs hardness

Best Cream Crystal Emperador Red Travertine Verde Antico Black Pearl Rosso Levanto

2.69 ± 0.010 2.62 ± 0.043 2.40 ± 0.04 2.62 ± 0.03 2.64 ± 0.04 2.71 ± 0.03

2.69 ± 0.011 2.65 ± 0.040 2.44 ± 0.04 2.63 ± 0.03 2.64 ± 0.04 2.71 ± 0.03

2.69 ± 0.012 2.62 ± 0.043 2.38 ± 0.04 2.61 ± 0.03 2.63 ± 0.04 2.70 ± 0.03

0.15 ± 0.043 1.36 ± 0.297 2.36 ± 0.04 0.69 ± 0.08 0.215 ± 0.03 0.336 ± 0.14

0.41 ± 0.114 3.56 ± 0.744 3.55 ± 0.04 2.52 ± 0.23 0.568 ± 0.09 0.90 ± 0.036

4 3–4 3 4 4 4

Table 2.3 Result of XRF analysis of marble samples. Crystal Emperador

0.47 0.08 0.089 0.73 54.77 33.21 1.48 19.2 0.014 2.72 0.0012 0.001 0.24 2.168 0.014 0.00846 0.0024 0.33610 0.019 0.02266 – – 41.91 40.95

SiO2 Fe2O3 CaO MgO Na2O K2O Al2O3 P2O5 ZnO SrO Co2O3 LOI

Red Verde Travertine Antico

Black Pearl

Rosso Levanto

0.001 1.050 54.56 0.023 1.304 <0.0012 0.0814 0.01 0.0036 0.0074 0.0048 42.90

1.33 0.34 52.40 1 0.04 0.07 0.53 0.35 0.01 0.18 0.04 43.30

23.18 7.335 20.71 26.25 <0.014 <0.0012 1.328 0.3611 0.00476 0.012 0.022 20.30

25.60 8.62 18.70 25.40 0.05 – 0.26 0.07 0.01 0.06 0.01 20.30

The percentage in the loss of gloss value of the rock samples between the starting points and at the end of the 20th cycle in the thermostatic chamber experiments are shown in Table 3.1. Greater reduction was realized among dark color marbles than light color marbles. Thermal shock cycles were more effective on reducing glossiness than thermal ageing was. This is because thermal heating and cooling may also cause deterioration of the marble due to the anisotropic thermal expansion and contraction of calcite [21].

Fig. 2.1. CIELAB coordinate system.

Best Cream

3

Crystal Emperadore Red Traverne Gloss value (gu)

Sample Best Cream

Rosso Levanto Verde Anco 2

Black Pearl

1 0

5

10

15

20

25

Cycles

3.2. Color changes

Fig. 3.1. Gloss values of marble samples during thermal shock chamber.

For the six studied marble samples, color modification occurred as a result of thermal ageing and thermal shock cycles. Differences in color between reference and thermal shocked and thermal aged specimens were expressed as a single numerical value (in CIELAB units), DE. Total color differences, DE, show the total color change magnitude but they do not specify in what way colors varied [29]. At the end of the thermal chambers color and lightness values of samples are given in Table 3.2. Changes of the L⁄, a⁄, b⁄, E⁄ and gloss values measured at the end of the thermal ageing and thermal shocks are given in Tables 3.3 and 3.4. DE⁄ is defining total color changes. It was determined by Eq. (3.1). [22]. Results of the gloss measurements are given Table 3.5.

DEab ¼

qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 2 ðDL2 Þ þ ðDb Þ

ð3:1Þ

The color changes due to thermal ageing and thermal shock cycles in case of lightness (L) are different in all rock. In the light-colored marble group, the biggest differences occurred in

red travertine samples. In the dark-colored marble group at the Verde Antico sample darkening in color at the other sample lightening was occurred. Except for the black-colored sample, the color changes due to thermal ageing and thermal shock cycles as measured by parameters (redness–greenness) were similar. The biggest differences occurred in red travertine samples. The redness of Red Travertine, Empradore, and Rosso Levantino samples decreased, but increased at the end of the thermal shock cycles and thermal ageing cycles in beige, Verde Antico, and Black Pearl. All reference samples had large yellowness. Thermal shock cycles have negative effects on yellowness in the light-colored group. In the dark-colored group only Black Pearl samples showed a negative effect. Dark red and dark green samples had a positive effect. Thermal ageing has a negative effect on yellowness in Beige and Black Pearl but a positive effect on other samples. Trends in color differences of samples are given in Fig. 3.3.

Table 2.4 Result of XRD analysis of marble samples. Sample

Best Cream

Crystal Emperador

Red Travertine

Verde Antico

Black Pearl

Rosso Levanto

Calsite

Dolomite

Calsite. Hematite

Dolomite. calcite. illite

Calcite

Casite, dolomite, bentonite clay, silica

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D. Eren Sarıcı / Construction and Building Materials 102 (2016) 416–421 Table 3.4 After thermal ageing treatment changes of L, a, b, E and gloss value.

Gloss value (gu)

3

2

Best Cream

Samples

DL

Da

Db

DE

Dgloss

Crystal Emperadore

Best Cream Crystal Emperador Red Travertine Rosso Levanto Verde Antico Black Pearl

1.66 0.26 19.63 2.39 1.96 3.37

0.26 0.23 12.39 0.74 0.13 0.12

3.92 0.76 11.15 0.76 0.94 0.11

4.25 0.80 22.57 2.50 2.17 3.37

0.1904 0.45 0.3474 0.37 0.05 0.211

Red Traverne Rosso Levanto Verde Anco 1 0

5

10

15

20

Black Pearl

25

Cycles

Fig. 3.2. Gloss values of marble samples during thermal ageing chamber.

Table 3.5 Initial, intermediate and final data of gloss values.

Table 3.1 Gloss changes % at thermal chambers. Gloss value loss (%) in thermal shock test

7.91 20.66 16.07 22.88 4.22 15.37

16.66 13.09 26.90 4.69 15.25 24.91

Thermal shock

Thermal ageing

Table 3.2 Color and lightness values of samples. Sample

L

a

b

Best Cream (References) Best Cream (Thermal ageing) Best Cream (Thermal shock) Crystal Emperedor (References) Crystal Emperedor (Thermal ageing) Crystal Emperedor (Thermal shock) Red Travertine (References) Red Travertine (Thermal ageing) Red Travertine (Thermal shock) Rosso Levanto (References) Rosso Levanto (Thermal ageing) Rosso Levanto (Thermal shock) Verde Antico (References) Verde Antico (Thermal ageing) Verde Antico (Thermal shock) Black Pearl (References) Black Pearl (Thermal ageing) Black Pearl (Thermal shock)

92.75 94.41 93.81 81.38 81.64 84.95 78.42 58.79 59.54 56.79 59.18 58.58 67.52 65.56 65.83 50.03 53.40 47.83

0.42 0.16 0.10 1.55 1.78 1.59 13.97 26.36 26.31 3.51 4.25 4.35 1.11 1.24 0.85 1.80 1.68 1.34

7.65 3.73 4.87 9.43 10.19 8.92 21.31 32.46 18.68 5.41 4.65 5.53 6.88 7.82 8.24 5.06 4.95 3.79

Table 3.3 After thermal shock treatment changes of L, a, b, E and gloss value.

Initial End of End of End of End of End of gloss the 4. the 8. the 12. the 16. the 20. cycle cycle cycle cycle cycle

Best Cream Crystal Emperador Red Travertine Rosso Levanto Verde Antico Black Pearl

2.61

2.56

2.39

2.31

2.22

2.18

2.12

1.92

1.88

1.9

1.88

1.84

2.36

1.94

1.95

1.80

1.75

1.72

1.37

1.32

1.31

1.31

1.30

1.30

1.56

1.35

1.34

1.33

1.32

1.32

1.50

1.27

1.23

1.22

1.18

1.13

Best Cream Crystal Emperador Red Travertine Rosso Levanto Verde Antico Black Pearl

2.40

2.08

2.2

2.37

2.32

2.11

2.17

2.10

2.08

2.04

2.06

1.72

2.16

2.03

1.98

1.92

1.90

1.81

1.61

1.54

1.54

1.4

1.38

1.24

1.37

1.33

1.32

1.35

1.35

1.32

1.37

1.22

1.16

1.25

1.23

1.16

30 20 E

Best Cream Crystal Emperador Red Travertine Rosso Levanto Verde Antico Black Pearl

Gloss value loss (%) in thermal ageing test

Sample

10 Thermal ageing 0

thermal shock

Samples

Samples

DL

Da

Db

DE

Dgloss

Best Cream Crystal Emperador Red Travertine Rosso Levanto Verde Antico Black Pearl

1.06 3.57 18.88 1.79 1.69 2.2

0.32 0.04 12.37 0.84 0.26 0.46

2.78 0.51 2.63 0.12 1.36 1.27

2.97 3.606 19.06 1.79 2.169 2.54

0.436 0.278 0.635 0.0645 0.238 0.375

Thermal effects show different weathering values in terms of light- and dark-colored marble samples. At the end of the thermal cycles the travertine sample shows large color changes and gloss decreases. The reason is that the travertine sample has many micro and macro pores and a high water absorption capacity. The same trend can be seen on the Emperador samples, which also a have high water absorption capacity. In the light-colored sample group, there were more changes of color than in the dark-colored group. Light-colored samples contain more calcite minerals.

Fig. 3.3. Trends in color difference of samples. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

3.3. Effects of color changes on glossiness The relationship between Dgloss and DL, Da, Db, and DE of samples are given in Figs. 34–37 respectively. Figs. 3.4–3.7 show that in thermal shock cycles, DL, Db, and DE have an effect on gloss change. The effects of these factors have different significance on gloss loss. There are positive relationships between DL and Db gloss loss, and negative relationships between Da, DE and gloss loss. In the thermal ageing cycles, there aren’t important relationships between color parameters and gloss changes. Total color changes have led to gloss loss in marble samples. Moisture effect cause to gloss loss. L, a, b and DE has important role to determination of marble surface quality characteristics.

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D. Eren Sarıcı / Construction and Building Materials 102 (2016) 416–421 10

y = 32,645x + 8,301 R² = 0,5938

5 0

-0.6

-0.4

L changes

-0.8

-0.2

0 -5

y = 10,439x + 0,548 R² = 0,0317

Thermal shock cycle Thermal ageing cycle

-10 -15 -20 -25

Gloss change

Fig. 3.4. The relationship between Dgloss and DL.

In the next phase of the study, using different geological origin rocks and investigating the effects of rock parameters such as structural and petrographical properties would be useful.

14 12

y = -17,968x - 3,9471 R2 =0,47

and contraction more rapidly occurred in thermal shock. Additionally, in the thermal shock cycles there was not only the effect of heat but also the presence of water in the pores, and this is thought to have a disrupting effect on surface quality. – The travertine sample (Red travertine) showed a higher percentage gloss loss and color change than did the other samples. For outdoor use, among the rock samples used in this study, it is better to use travertine that has a lower resistance to thermal effect. – The relationship between color parameters and gloss as evaluated by L and b parameters is a strong indicator for predicting gloss loss. L represents whiteness, b represents yellowness and blueness. B parameters have negative effects and L parameters have positive effects on gloss loss.

10

a changes

8 6

Thermal shock cycle

4

y = -10,631x - 0,7265 R2 = 0,0,9

2

The author gratefully acknowledge the financial support of the BAP Project ( Inönü University, Project No: 2012/181).

0 -0.8

-0.6

-0.4

-0.2

Acknowledgement

Thermal ageing cycle

0

-2 -4

Gloss changes

References

Fig. 3.5. The relationship between Dgloss and Da.

12 10 8 b changes

y = -11,157x - 1,4136 6 R2 = 0,10 4

-0.8

-0.6

-0.4

-0.2

2

Thermal shock cycle

0 -2 0

Thermal ageing cycle

-4

y = 6,6114x + 1,2813 R2 = 0,62 Gloss changes

-6

Fig. 3.6. The relationship between Dgloss and Db.

30 25

E changes

y = -32,887x - 5,0974 R2 = 0,59

20 15 Thermal Shock cycle 10

y = -13,184x + 2,9623 R2 = 0,04

Thermal ageing cycle

5 0

-0.8

-0.6

-0.4 Gloss change

-0.2

-5

0

Fig. 3.7. The relationship between Dgloss and DE.

4. Conclusions This study aims to determine the effects of thermal changes (abruptly and slowly) on gloss and color of differently colored marbles. Laboratory studies were performed on six different marble samples using thermal ageing and thermal shocks. The main conclusions drawn from this study are: – As thermal shock and thermal ageing cycles increase, surface gloss values slowly decrease. Thermal shock cycles were more effective on gloss than thermal ageing due to thermal expansion

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