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As advances in technology have led to increased use of bentonites, more high-quality bentonite has been sought. The volume of high-quality bentonites available is shrinking and use of bentonite reserves containing impurities is inevitable. The aim of this study was to apply Box–Behnken experimental design and response surface methodology to model a...

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... samples were collected from various stratigraphic levels of the bentonite deposits between the Mihalgazi and Sarıcakaya districts in Eski s° ehir (Western Turkey) ( Figure 2). Bentonite deposits in this region were formed by alteration of andesitic and dacitic volcanic rocks. The bentonites are classified in three groups based on their geologic features; bentonite deposits in andesitic and dacitic lavas, bentonite deposits in andesitic agglomerate, and bentonite deposits in tuff (Yıldız et al. , 2008). Characterization test results of the three samples are given in Table 1. Here, the CEC values of each bentonite group were determined by the methylene blue (MB) standard method (Rytwo et al ., 1991; O ̈ nal, 2007) and viscosity values were measured with 5, 7.5, or 10% solids at 600 rpm using a Fann viscosimeter at Turkish General Directorate of Mineral Research & Exploration. The swelling of each sample was measured as the total volume of a gel formed from a 2 g sample in 100 mL of water (ASTM D 5890-95). The CEC, viscosity, and swelling volume of the raw bentonites were relatively small (Table 1). The second group of bentonites had the best physical properties. Chemical analyses of major oxides were obtained by inductively coupled plasma- mass spectrometry (ICP-MS) at the ACME analytical laboratory, Canada (Table 2), and chemical analyses revealed that the CaO+Na 2 O totals of all three bentonites were in the range 4.28 À 7.00%. Mineralogical investigations were carried out on processed and random powder samples by means of X-ray diffraction (XRD) analysis, using a Rigaku Geiger Flex Diffractometer with Ni-filtered CuK a radiation. The scanning speed for all samples was 2 o 2 y /min. Smectite and the other mineral contents of the samples were determined by semi- quantitative interpretation of the XRD data (without standards). The reflections, peak intensity, and Reference Intensity Ratio (RIR) of minerals were analyzed by the formulae of Chung (1974), which enabled calculation of mineral abundances as weight percentages. This method was chosen because it yields reproducible results and has been used by other researchers (Biscaye, 1965; Johns et al. , 1954; G ̈ ndo ̆ du, 1982), thus giving the mineral contents of the present samples. Morphological and mineralogical studies were carried out using a LEO VP-1431 (Korea) scanning electron microscope (SEM) with EDS equip- ment. The XRD patterns indicated that smectite was the major mineral phase in the bulk samples (Table 3; Figure 3) (Grim, 1962; Brown and Brindley, 1980; Brown, 1972). Illite and chlorite were minor constitu- ents. Non-clay minerals in the samples included cristobalite/opal-CT, quartz, feldspar, calcite, and dolomite. The smectite content, which affects the performance of the bentonites in various industrial applications, was 54%, 55%, and 40% in Groups 1, 2, and 3, respectively. Feldspar was a major impurity in all groups and the amount of feldspar was 40%, 32%, and 30% in Groups 1, 2, and 3, respectively. The cristobalite/ opal-CT contents of the bentonites in Groups 1, 2, and 3 were 0 wt.%, 5 wt.%, and 7 wt.%, respectively (Table 3). Cristobalite/opal-CT minerals are somewhat similar to smectites with respect to their physical properties such as density, crystal size, etc. The XRD investigations revealed that the bentonites in Groups 1 and 2 consisted of mixed (Na-Ca) smectites; Group 3 included Na- smectites. The Na 2 O contents of bentonites were determined as 1.52 wt.% (Group 1), 3.24 wt.% (Group 2), and 2.52 wt.% (Group 3) in EDS studies (Figure 4). The XRD and EDS studies show that the Na + is the primary exchangeable cation in smectites of Groups 2 and 3. The swelling properties of the Na- smectite are commonly more developed than those of Ca-smectite (Luckham and Rossi, 1999). The Box–Behnken design (Box et al. , 1978; Box and Wilson, 1951; Box and Behnken, 1960; Montgomery, 2001; Ferreira et al. , 2004; Souza Anderson et al. , 2005; Aslan and Cebeci, 2007) is a rotatable second-order design based on three-level incomplete factorial designs. The special arrangement of the Box–Behnken design levels allows the number of design points to increase at the same rate as the number of polynomial coefficients. For three factors, for example, the design can be constructed as three blocks of four experiments consisting of a full two-factor factorial design with the level of the third factor set at zero (Souza Anderson et al. , 2005; Aslan and Cebeci, 2007). In the present study, the Box–Behnken factorial design was chosen to discover the relationship between the response functions (smectite concentration and swelling of the bentonite concentrate) and four variables of the hydrocyclone (feed solid, inlet pressure, vortex diameter, and apex diameter), while holding other operational parameters of the hydrocyclone constant (cyclone diameter of 44 mm, feed suspension of 30 L, pre-feed mixture in mixer for 5 min). Batch hydrocyclone tests were conducted at the mineral processing laboratory of Afyon Kocatepe University, Turkey. Samples were dried at 60 o C and then added to water (10% solids); the suspension was settled for 24 h and stirred for 2 À 3 h by a propeller agitator. The suspension was passed through a 500 m m sieve and then fed into the hydrocyclone. The solid:liquid ratio was regulated by addition of water. The suspension was stirred using a centrifugal pump (with by-pass valve) for 5 min to achieve homogeneity (in the system). Later, material was fed into the hydrocyclone by closing the by-pass valve, and two discrete overflow and underflow products were obtained. The samples were filtered, dried, and analyzed for smectite content and swelling (Figure 5). Response surface methodology is a collection of statistical and mathematical methods that are useful for modeling and analyzing engineering problems. The main objective is to optimize the response surface that is influenced by various process parameters. Response surface methodology also quantifies the relationship between the controllable input parameters and the response surfaces obtained (Kwak, 2005; Aslan and Cebeci, 2007; Aslan, 2007a, 2007b). The design of the response surface methodology consisted of the following (Gunaraj and Murugan, 1999; Kwak, 2005; Aslan and Cebeci, 2007; Aslan, 2007a, 2007b): (1) designing a series of experiments for adequate and reliable measurement of the response of interest; (2) developing a mathematical model of the second-order response surface with the best fittings; (3) finding the optimal set of experimental parameters to produce a maximum or minimum value of response; and (4) representing the direct and interactive effects of process parameters through two-dimensional (3D) and three-dimensional (3D) plots. If all variables are assumed to be measurable, the response surface can be expressed as follows (equation 1): where y is the response variable, and x i = x 1 , x 2 , x 3 , or x k are the controlling variables referred to as factors. The goal of this aspect of the study was to optimize the response variable y . The independent variables are assumed to be continuous and controllable by the experiments with negligible errors. A reasonable approx- imation for the true functional relationship between independent variables and the response surface is desired. A second-order model is usually used in response surface methodology (Gunaraj and Murugan, 1999; Kwak, 2005; Aslan and Cebeci, 2007; Aslan, 2007a, 2007b): where x 1 , x 2 ,..., x k are the input factors which influence the response y ; b 0 , b ii ( i = 1, 2,..., k ), b ij ( i = 1,2,..., k ; j = 1,2,. . . ,k ) are unknown parameters, and e is a random error term. The b coefficients, which should be determined in the second-order model, are obtained by the least-squares method. In general equation 2 can be written in matrix form (Kincl et al. , 2005; Kwak, 2005; Aslan and Cebeci, 2007; Aslan, 2007a, 2007b): where Y is a matrix of measured values and X is a matrix of independent variables. The matrices b and e consist of coefficients and errors, respectively. The solution of equation 3 can be obtained by the matrix approach (Gunaraj and Murugan, 1999; Kwak, 2005; Aslan and Cebeci, 2007; Aslan, 2007a, 2007b). where X is the transpose of the matrix X and ( X X ) is the inverse of the matrix X T X (Kwak, 2005; Aslan and Cebeci, 2007; Aslan, 2007a, 2007b). The coefficients, i.e. the main effect ( b i ) and the two- factor interactions ( b ij ), can be estimated from the experimental results by computer-simulation programming applying the least-squares method using Minitab 15 (Minitab Inc., 2007). Box À Behnken design requires an experiment number according to N = k 2 + k + c p , where k is the factor number and c p is the replicate number of the mid-point (Massart et al. , 1997; Neto et al. , 2001; Ferreira et al. , 2004; Souza Anderson et al. , 2005; Aslan, 2007b;). Box À Behnken is a spherical, revolving design. Viewed as a cube (Figure 6a) (Souza Anderson et al. , 2005; Massart et al. , 1997; Aslan and Cebeci, 2007), the Box– Behnken design consists of a central point and the middle points of the edges. However, it can also be viewed as consisting of three interlocking 2 2 factorial designs and a central point (Figure 6b) (Souza Anderson et al. , 2005; Massart et al. , 1997; Aslan and Cebeci, 2007). For the three-level, four-factorial Box À Behnken experimental 8 9 design, 27 experimental runs in total ( : 4 2 ; 4 þ 3 centerpoints), were needed (Table 4). Considering the effects of the main factors and also the interactions between two-factor sets, equation 2 takes the ...

Citations

... To analyse the results of the mineral concentration experiments using the hydrocyclone plant, the response variables to maximise were Sr% or Celestine%, and the continuous and controllable experimental factors were the density inside the hydrocyclone (2.7-2.9 kg/L), the hydrocyclone inclination (15)(16)(17)(18)(19)(20)(21)(22)(23)(24)(25), and the hydrocyclone inlet pressure (0.8-1.2 bar). The experimental design was adjusted to a response surface according to the BBD model with centre points [19][20][21]. ...
... To analyse the results of the mineral concentration experiments using the hydrocyclone plant, the response variables to maximise were Sr% or Celestine%, and the continuous and controllable experimental factors were the density inside the hydrocyclone (2.7-2.9 kg/L), the hydrocyclone inclination (15)(16)(17)(18)(19)(20)(21)(22)(23)(24)(25), and the hydrocyclone inlet pressure (0.8-1.2 bar). The experimental design was adjusted to a response surface according to the BBD model with centre points [19][20][21]. The DBB model is used in this study to refine the relevant experimental parameters of the mineral concentration process that need to be optimised. ...
Article
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A semi-industrial scale hydrocyclone with a 250 mm internal diameter was used to concentrate medium-grade celestine ore (75%–85% celestine) from the Montevive deposit of Granada (Spain) using a dense ferrosilicon (FeSi) medium. For this purpose, a Box–Behnken factorial design (BBD) was carried out, with the response variable being the Sr concentration measured by X-ray fluorescence (XRF), as well as the concentration of celestine measured by X-ray diffraction (XRD) of the mineral collected from the under (sunk) stream of the hydrocyclone. The experimental factors to be optimised were the density of the medium in the mixing tank (water, FeSi, and feed mineral) varying from 2.7 to 2.9 kg/L, the hydrocyclone inlet pressure from 0.8 to 1.2 bar, and the hydrocyclone inclination (from 15° to 25° from the horizontal). The range of densities of the dense medium to be tested was determined from previous sink–float experiments using medium-grade ore, in which the distribution of mineral phases with different particle size fractions was determined. To evaluate the separation behaviour, the following parameters were considered: the enrichment ratio (E), the tailings discarding ratio (R), and the mineral processing recovery (ε). From the factorial design and the response surface, the optimum parameters maximising celestine concentration in the under stream (78%), were determined. These optimised parameters were: a density of 2.75 kg/L for the dense medium, an inlet pressure of 1.05 bar, and a hydrocyclone inclination varying from 18° to 20°. Under these conditions, a 94% recovery of celestine (68% Sr) can be achieved. These results show that medium-grade celestine ore, accumulated in mine tailings dumps, can be effectively concentrated using DMS hydrocyclones and that the operating parameters can be optimised using a factorial experiment design. This study can contribute to reducing overexploitation of strategic mineral resources, avoiding blasting and environmentally damaging clearing, by applying a simple and sustainable technique.
... capacity and specific surface area . Enrichment of bentonite clays is very important step in the production of bentonite -based products for any industry [5] . ...
Article
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The aim of this work is to evaluate the efficiency of two methods of purification on Algerian bentonite clay. The first method was performed by centrifugation treatment, using sodium hexametaphosphate (NaPO3)6 as a dispersing agent. The second method involves a chemical purification with NaCl, followed by sedimentation technique. The study concerns mineralogical, chemical, structural aspects and a series of physical testing. The results have shown that the raw bentonite (RBN) contain (~ 59%) of montmorillonite, illite (~ 5) and (~26%) of quartz, and feldspar (orthoclase + albite), with 5% of calcite. In the purified state by NaCl (RBN-2), the mineralogical and physicochemical properties including cation exchange capacity and specific surface area are higher than the purified samples by physical beneficiation (by centrifugation - RBN-1). Moreover, the treatment with NaCl increased the montmorillonite content of the bentonite from 56 % to 100%. The quartz impurities were totally removed in RBN-2, whereas impurities (quartz + feldspar) were still observed by the X-ray diffraction (XRD). Finally, the results obtained from the morphological, mineralogical and chemical characterization confirm that the bentonite RBN -2 was more effective , and it has promise as an engineering material compared to the RBN and RBN-1, indicating its possible application in various industrial applications.
... The Box-Behnken design (BB) is also a quadratic model. This method is more efficient for higher number of input variables [22]. The designs are formed from combination of 2 k factorials with unfinished block designs, where k is input variables. ...
Chapter
The merits of response surface models in concrete construction need to be explored. These models have shown enormous use in the field of manufacturing and production. So in the present study, the application of response surface for concrete production is described. Their benefit in determining the results with minimum number of experiments is also discussed. The review summarizes the application of response surface models and shows that the statistical models provide additional support in analyzing the constrained targets. It reduces the test cases making the designs more economical compared to conventional methods
... Instead of the star points that are used in the CDD technique, the cube edges midpoints are used to treat the combinations between the experimental variables and the response (Fig. 8). BBD is spherical or rotatable and requires 3 levels for each experimental variable as in CDD (-1, 0, +1) expressing the variables limits (Table 4) [35,37,38]. The geometry of BBD suggests a sphere within the process space where the sphere surface protrudes through each face with the sphere surface tangential to each sphere edge midpoint. ...
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In this paper, the effect of steel fiber (SF), Metakaolin (MK) and time of curing on the concrete compressive strength (fcu) was implemented. Cylinder specimens cast from concrete with SF (0, 0.25% and 0.5%) and MK (0%, 10%, 15%, 20%, 30%, 40% and 50% as replacement of cement content) were tested in compression at different ages of curing (3, 7 and 28 days). The results assured that; the concrete strength increased as MK% increased from 0% to 15% then decreased with further increase in MK%. Also, increasing the SF% from 0 to 0.5% increased the concrete strength. The optimum values of enhancement in fcu were obtained for concrete mix with 15% MK and 0.5% SF. The enhancement percentages in fcu of this mix at 3, 7 and 28 days were 26.53%, 33.04% and 44.65% over that of the control mix at the corresponding ages respectively. Moreover, a relation between fcu, SF%, MK% and curing age were predicted using two methods (the Central Composite Design, CCD and the Box Behnken Design, BBD). The two methods were also used to construct prediction equations for the cubic strength using experimental results from previous researches. The accuracy of these equations was verified to be a base of mix design for concrete with SF and MK.
... Bunun yanında dekontasyon gibi yöntemlerle karşılaştırıldığında hidrosiklonun avantajları ön plana çıkmaktadır [17]. Türkiye'deki bentonitlerin zenginleştirilmesinde de bazı araştırmacılar da hidrosiklon kullanmışlardır [8,[18][19]. Özgen ve diğ. ...
... Koca et al., studied the evaluation of combined lignite cleaning processes, flotation and microbial treatment, and its modelling by Box Behnken methodology [17]. Ozgen et al., examined the effect of smectite content on swelling to hydrocyclone processing of bentonites with various geologic properties by Box Behnken design [18]. ...
... The XRD pattern of the rock powder (WA1) is presented in figure 3 with the characteristic dspace values and the symbols of the minerals against each respective peak. The XRD pattern revealed that the rock consists of hornblende and plagioclase with clay minerals, particularly kaolinite and smectite (Proust et al. 2006;Ozgen and Yildiz 2010;Worasith et al. 2011). The quantitative mineralogy percentage (%) of WA1 is given in figure 1 using the standard procedure of peak heights from the XRD results. ...
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Low saline water flooding (LSWF) had proved to be an efficient method for enhanced oil recovery in clay-bearing hydrocarbon reservoirs, but the interaction mechanisms among in-situ rocks – fluids and injection fluids within the reservoir – are not yet known properly. Understanding the molecular level interaction among these components is critical for designing and field scale implementation of LSWF in clay-bearing crystalline reservoir rocks, which is very limited in the existing literature. A weathered amphibolite rock and one dead crude oil from the Bakrol field (Cambay basin, India) have been used in this study. The presence of clay minerals in the weathered amphibolite rock was observed using a polarising microscope and characterised by the X-ray diffraction (XRD) and Fourier transform infrared (FTIR) techniques. The crude oil and its fractionated SARA components have been extensively studied by spectroscopic techniques for their characterisation. The interaction study among the rock powder, hydrocarbon crude oil and saline water has been performed in the present work for gaining better insight for designing the injection fluid for LSWF. The weathered amphibolite rock powder was mixed with the dead crude oil and kept for 30 days in room temperature (T) and pressure (P) for proper interaction. The XRD, FTIR and cation exchange capacity results clearly demonstrated the incorporation of crude oil components in the interlayer surfaces of clay minerals. The oil removal efficiency, from the oil-treated rock powder of three saline water samples having NaCl concentration of 3000, 5000 and 8000 ppm, was investigated using the UV–Vis and fluorescence spectroscopies. The low saline NaCl water is capable of removing the maximum amount of polar components from the oil-treated rock powder. These molecular level insights are valuable for designing effective injection fluid for enhancing the oil recovery from the clay-rich crystalline reservoir rock.
... In order to obtain the MMT fraction <2 µm, procedures such as sieving (Chipera, Guthrie, and Bish 1993;Ottner et al. 2000), magnetic separation (Chipera, Guthrie, and Bish 1993), and separation based on settling velocity (Brigatti et al. 1995;Ottner et al. 2000;Janek and Lagaly 2001;Kaufhold et al. 2002;Lee and Kim 2002;Ammann 2003;Dontsova et al. 2004;Sato 2005) were proposed (Thuc et al. 2010). Boylu et al. (2007), Özgen et al. (2009), and Özgen and Yıldız (2010) enriched bentonites with hydrocyclone; this removed non-clay (impurities) and achieved satisfactory results. However, the fact that appreciable non-clay (impurity) exists in the bentonites produced from the techniques and methods discussed above needs more research on this topic. ...
... CEC and smectite content was increased to 64% and 78%, respectively. In Author's previous studies enriching bentonites with 55% smectite content when hydrocyclone used, the smectite content increased up to a maximum of 97.74%, CEC rose up to 81.00 meq/100 g, and swelling value rose to 29.42 mls/2 g (Özgen et al. 2009;Özgen and Yıldız 2010). Enrichment using the FGC (SB-40), however, increased the smectite content to 97.74%, and removed almost all of the non-clays (impurities). ...
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As advances in technology have led to increased use of bentonites, higher quality bentonite has been sought. The volume of high-quality bentonites available is shrinking and use of bentonite reserves containing impurities is inevitable. The aim of this study was to apply Central Composite Rotatable Design (CCRD) to model and optimize some operational parameters of a Falcon Gravity Concentrator (FGC) to produce bentonite concentrate. The three significant operational parameters of FGC are gravity force, solid concentration, and water pressure and these parameters were varied and the results evaluated using the CCRD. Second-order response functions were produced for the cation exchange capacity (CEC), swelling, smectite content, and yield of smectite in the bentonite concentrates. Predicted values were calculated to be in good agreement with the experimental values (R2 values 0.897, 0.980, 0.948, and 0.904 for CEC, swelling, smectite, and yield of smectite of bentonite concentrations, respectively). Although in natural states this bentonite is not suitable for industrial use, purification enhanced its CEC, swelling properties, and smectite content to values of 92 meq/100 g CEC, 32 mls/2 g swelling, and 97% smectite, respectively.
... The statistical optimization technique using Response Surface Methodology (RSM) is a useful tool which allows one to obtain appropriate data that can be analyzed to arrive at objective conclusions and determine the optimum conditions through a relatively smaller number of systematic experiments. Several researchers attempted to use Response Surface Method (RSM) on different types of minerals, ores, materials etc. on different types of units operations ( [16], [19], [20], [21], [22], [23]). ...
... Sensitivity analysis is a general technique from the field of decision theory for studying the effects of the uncertainties in model's parameters. Neural networks can perform an approximation to a solution partially noisy and partially imprecise data, so sensitivity analysis is necessary to check if the neural network could behave erroneously [13,26,27]. In order to assess the effect of each change in the output due to the change in the input, a sensitivity analysis was performed, and according to the results, ANNs were improved to show the best results. ...
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The need of testing the quality of brickclay arises in all brick factories, with the opening of new deposits. The analyses are both time and economically consuming, so the aim of this study was to shorten the procedure using the already known data. This study was focused on determining the usability of heavy clays, when only the raw material major elements chemical composition is determined. The effects of chemical composition, firing temperature, and several shape formats of laboratory samples on the final properties were investigated. Chemical composition of major elements was determined on the basis of classical silicate analysis. Firing was conducted in an oxidizing atmosphere, while maintaining all other experimental conditions constant, except the final temperature. Principal component analysis (PCA) was used to determinate groups of samples according to similarity of chemical composition. Prediction of compressive strength (CS) and water absorption (WA) was done by developing five artificial neural networks (ANN). The average regression coefficients r2 were used to explore the confidence level of the models. Developed models were able to predict CS and WA in a wide range of chemical composition and temperature treatment data, and the highest average r2 of 0.923 for CS was obtained, while r2 for WA was 0.958. The wide range of processing variables was considered in the model formulation, and its easy implementation in a spreadsheet using a set of equations makes it very useful and practical for CS and WA prediction. As it is known from literature, all the parameters entered this analysis are dependent on each other, but their mutual relationship was not quantified yet. Most importantly—the developed neural networks can be used on a global scale.