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DOE Application by Compilation of Taguchi and RSM in Optimization…


DOE Application by Compilation of Taguchi and RSM in Optimization-Case Study: Interaction Parameters Flotation of Zinc Oxide Minerals
A. Hajati
Department of Mining Engineering, Iran University of Science and Technology, Arak Branch, Iran E-mail:,

ABSTRACT: One of the aims important to increase of quality is design of methods for improved of quantity and quality production of system. Statistical program tests are the base for this part effectiveness. Today, Designs of Experiment (DOE) tests are used engineering tools for control and optimization varies system. In this research, by compilation of design of experiment methods by taguchi and RSM (Response Surface Method) used for optimization of Zinc oxide minerals flotation system. Almost, most parts of benefit minerals as ore in extraction mining are oxidized. Then, flotation of these minerals will be difficult. The aim minerals of this dam tailing (Irankuh Company in Iran) are Smithsonite, Sphalerite, Galena, cerussite and Ferro oxide minerals. The grade of Zn, Pb and Fe are 7.5%, 3.4% and 13% respectively. In this flotation tests, oxine and dithizone are chelating agent collectors and the surface of particle is not sulfide. By study of interaction parameters and optimization of them and analysis of results and use of DOE methods, oxine is better than dithizone. In the optimum condition of flotation test; the grade of Zn, Pb and Fe are 15.55%, 2.77% and 3.51% and recovery are 40.12%, 7.75% and 10.11% respectively.

1. INTRODUCTION Almost in the all systems, optimization and knowledge of action parameters is very important. One of the aim basic to increase of quality, is design of methods for improve of quantity and quality production of systems. Statistical program tests are the base for this part effectiveness. Today, Designs of Experiment (DOE) tests are used engineering tools for control and optimization of varies factors effective systems. Design experiment by taguchi method is one of the family fractional factorials. It can used in varies condition of systems. By using of this method, the stability of process and decrease of variable around of results are aim. But some results have a few uncertain. It has tried that decrease of distance between of Xi (much of parameter test) and X (average of results). Then, it possible that optimum condition focused on the other point. It seems that, knowledge of interaction parameters effect system by three dimensional is help to conceive of complex process. Compilation of the Response Surface Methodology (RSM) and taguchi method is very benefit method for solving of this problem. RSM

or surface knowledge is combination technique of mathematics and statistics for modeling and simulation of problems. By using of two methods, end results of tests will be uphold and correct. Application of this method is very suitable for analysis of any systems of industry laboratory, pilot plant and other tests. Different technologies such as pyrometallurgy, hydrometallurgy, bioleaching and flotation have been employed to extract metal from ore; however, with the new crisis in environmental issues, flotation methods seem more amenable [1]. Today, selecting collector for flotation of zinc oxide is very important, and among the collectors, chelating agents are promising ones. One of the most significant applications of chelating agents in flotation is in enrichment of low-grade ore recovery. In this research, by sampling of oxide dam tailing at Goshfill Mine (Bama Co.) and use of DOE for analysis of results, optimization of parameters act by chelating agent (oxine) and non sulfidation of surface zinc minerals [2].

136  2. MATERIAL AND METHODS The material is provided by Bama Company from Goshfil Mine Tailing. The Tailing include the 7.65% zinc (Smithsonite and Sphalerite) 3.5% lead (galena and cerusite) and 13% of iron (hematite and goethite). One Kg of the sample were crushed with jaw crusher. The crushed samples were ground with ball mill to fine sizes in different time scales (0, 5, 10, 20, 30, 40, 50, 60 min).The fine particles then sieved with screen size of (18, 50, 100, 200, 270, 325, 400 mesh) and the accumulated weight of passing particles were measured. After obtaining the selection of appropriate time (10 minute were selected for this study) for the grinding, and then samples were taken from each size on the screen. The selection samples were fixed through the resin and polished the surface of the minerals. The prepared sample was used for the microscopic analysis by the counting the number of minerals and the percentage of liberated ones. The degree of liberation can magnificently optimize flotation processes. For these specific minerals it can be concluded that all samples should grind under 90 micron size in which 80100% of smithsonite and 50-100% of iron oxides (hematite + goethite) are liberated. The details study of degree of liberation can be found [2]. In order to reduce the iron contents of the samples, the prepared samples were also passed through 2 Tesla Magnetic field. For the flotation test, an experimental cell similar to the Halimound cell was used. The dimension of the considering the liberation of smithsonite, were selected in the range of 38-90 micron. Oxine is a chelating agent and it was used as a collector. Oxine (C9H7NO) is a white

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crystal with molecular weight of 145.16 g/mole. Oxine is insoluble in water and mostly organic chemicals likely, ethers, alcohols, aromatic hydrocarbons acetone, acetic acid and chloroform are used as solvent. In this test acetone was employed as solvent (Figure 1). The oxine concentration was kept below 2%. This is because of solubility of acetone in water may remove oxine from the system Pine oil with a range of 120 g/ton was selected as frother. The conditioning time was 12 min. In this study the main parameters which were used for flotation include pH, oxine concentration, corn starch, sodium thiosulfate, sodium citrate, sodium silicate and conditioning time. Preliminary tests were carried out in order to evaluate the effectiveness of oxine with various concentrations of oxine, corn starch, sodium tiosulfate, sodium citrate and sodium silicate. during the experiment.

Fig. 1: Chelating of Zinc by Oxine

To optimize the experimental parameters, the Taguchi experimental design was employed. According to the method, an array of L32 was suggested and the data were analyzed by Qualitek-4 software. Table1 demonstrates the main parameters and their levels investigated in this research.

Table 1: Demonstrate the main parameters and their ranges investigated
Parameters 1- pH 2- Oxine (g/ton) 3- Corn Starch (g/ton) 4- Sodium Thiosulfate (g/ton) 5- Sodium citrate(g/ton) 6- Sodium Silicate (g/ton) 6- Time Condition (min) Level 1 3 20 500 20 20 20 5 Levels of parameter Level 2 Level 3 6 9 60 180 1000 1500 60 180 60 180 60 180 10 15 Level 4 12 540 2000 540 540 540 30

DOE Application by Compilation of Taguchi and RSM in Optimization…


3. RESULTS AND DISCUSSIONS The results of mineralogical analysis through XRF are tested. Nearly 80% of zinc minerals are smithsonite. The most gangue minerals for the flotation process are including of iron and lead metals. For iron removal, it prepared samples were passed through the wet-high magnetic intensity field. The results of magnetic separation test caused that grade of Pb, Zn and Fe viruses to 3.01%, 7.85% and 5% and recovery in non magnetite part are 91.81%, 90.55 and 65.68% respectively. The results of parameter optimization technique using taguchi method indicated that the parameters which effect on the experimental results in 1st stage, are include corn starch with concentration of 1400 g/ton, sodium silicate 100 g/ton and time conditioning 12 min. The other parameters which are variable include pH, oxine, sodium thiosulfate and sodium citrate.
Table 2: Results of L9 array taguchi method
Series 1 2 3 4 5 6 7 8 9 Gread (%) Zn 11.45 Fe Pb 7 4 4 4 4 4 4 4 4 4 Recovery (%) Zn Fe Pb
Recovery (%)

45 40 35 30 25 20 15 10 5 0 500 1000 1500 2000 Concentration of Oxine (gr/ton)

Zn Pb Fe


Fig. 2: Recovery of zinc, Iron and Lead by Oxine

The results of the Taguchi for the interaction of sodium citrate and sodium tio sulfate through the RSM (Response Surface Method) for grade of zinc is shown in Figure 3.

29.06 17.92 10.24 20.40 21.76 24.89 14.60 45.81 22.04 5.44 6.80 9.44

11.25 12 10.98 6 11.48 10.6 11.6 12.12 12.30 12.76 7 6 5 4 5 4

Fig. 3: Interaction of Citrate-Thiosulfate on the Recovery of zinc by RSM

70.95 40.16 26.77 49.18 21.20 16.96 14.57 14.45 24.82 4.46 5.47 7.47 4.48 4.28 5.60

Thus, the above mentioned variable parameters were optimized. The results of L9 taguchi method is shown in Table 2{Limit factors are: pH = (10, 12, 14), Oxine = (800, 1500, 2000 gr/t), sodium thiosulfate = (0, 1000, 2000 gr/t) and sodium citrate = (0, 1000, 2000 gr/t) by L9 array}. As shown in Table 2, pH is one of the most contribution factor which affect the recovery of zinc. This is also demonstrated in Fig. 2.

As shown in Figure 3 for study interaction of sodium citrate with sodium thiosulfate indicats, show that sodium citrate did not affect on the increasing recovery of zinc. Whereas, with elimination of sodium citrate the optimized condition for the sodium tiosulfate for the recovery of zinc was obtained at a few gather than 2000 gr/ton. Finally, optimum condition was obtained when fuel oil mixed ¼ with oxine. In this condition the grade of zinc was obtained 15.89 % and the recovery was 52.56%. 4. CONCLUSIONS AND RECOMMENDATION The feasibility of zinc recovery from mine residue was shown by this study. Oxine as a chelating agent collector in the floatation process

138  exhibits potential for selective recovery of smithzonite minerals ore. Through the Taguchi experimental design the optimum condition was obtained. The optimum condition for the above mentioned parameter is as follows: Size range 38-90 micron, pH = 12.5, Sodium Citrate: Removed, Sodium Tiosulfate: 1000-1500 g/ton, Sodium Silicate: 100 g/ton, Corn Starch: 1400 g/ton, Time Condition: 12 min, High Tention of Magnetite separation: 2 Tesla, Fuel Oil: ¼ Concentration Of Oxine, Frother (Pine Oil): 120 g/ton, Solid Percent: 10%. The results also indicate that pH was one of the most important parameter which affects the recover of zinc oxide. As the results of the study demonstrated, the disturbing parameters which affected the results of smithsonite recovery in the tailing were high surface oxidation all minerals including iron lead and zinc.

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[1] Barbaro, M, “Comparison of Pb-Zn Selective Collectors Using Statistical Methods”, Mineral Processing Institute, Roma, Italy, 1998. [2] A. Hajati, et. al., determination of degree of liberation zinc and iron oxide minerals in Goshfill mine, mining Eng. conference, Iran, 2004. [3] Rinelli, G., Marabini, “Selective separation of zinc and lead from oxide ores through formation of organo-metallic compounds”. XIIth IMPC, Sao Paulo, Brazil, 1977. [4] Quast, K.B.,"A review of Hematite Flotation Using 12-Carbon Chain Collectors", School of Geonce, University of South Australia, Mawson Lakes, Australia, 2000. [5] Song, S. (2002) “Magnetic Separation of Hematite and Hematite limonite Fine as Hydrophobic flocs From Iron Ores”, [6] King, R.P. (1982) “Flotation of Fine Particle”, In Principles of Flotation Ed. King, R.P., Afr., Institute Mining Metallurgy Johannesburg Chap. 11.