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By Daniela Venter, Stephen Chryssoulis, Ken Stowe

"A sampling campaign was conducted at Kemess in order to identify and assess the chemical and physical factors, which control free gold flotation kinetics in the rougher and cleaner circuits. The rationale behind this approach was that accurate knowledge of the parameters affecting free gold flotation kinetics, can be used to determine how to accelerate free gold flotation. Collected samples were composites of 5-6 cuts over a four-hour period, at steady plant conditions.In the rougher circuit, coarser equidimensional gold particles floated ahead of the finer grained and the flaky gold. Sulphur followed by molybdenum and to a lesser extent silver enhanced gold flotation kinetics, while hydroxyl followed by carbonate ions induced depression."

Jan 1, 2003

By Matti Kongas, Kari Saloheimo, Antti Remes

"The paper studies the control performance of the flotation process as a function of the measurement accuracy and sampling frequency of an on-stream XRF analyzer, using a simple dynamic model. An additional aim is to assess how the economical result of a mineral flotation process depends on the quality of process control based on the on-line elemental assays.An on-stream XRF analyzer measures the concentrations of slurry lines in a continuous cycle from several process points. The control performance depends on the analytical accuracy and sampling frequency of the concentration measurement. With a long cycle time, the state of the process changes before a new measurement becomes available. With short measurement times the statistical variance of the counted Xray pulses increases, increasing the random error in the analysis. In addition, the measurement accuracy depends on the concentration of the component to be measured from the slurry.To quantify the effect of analysis error and frequency to process control, a simple dynamic process model is created in the Matlab environment. Data from a copper flotation circuit is used as a test case. The process model comprises a first order reaction equation and the grade-recovery -relationship estimated from process data. The control was modeled using the control strategies implemented into a rule based advanced control system. The economical performance of the control was studied by calculating the overall net smelter return at various analyzer parameter combinations."

Jan 1, 2003

By Wang Xiaotie, Yu Yongfu, Che Liping, Zhang Fuguang

The flotation process of native Rare Earth minerals such as bastnasite, monazite, mixed minerals of bastnasite and monazite, using the new effective collector Dh was studied in this paper, respectively, and the flotation properties are described. The good qualities of the new collector Dh were revealed through comparing with other collector of Rare Earth minerals. The test results of different ore samples show that at moderate pulp pH (8.5-9.5), Rare earth minerals can be effectively separated from barium, calcium and silicon bearing intergrowth minerals (barite, calcite and silicate minerals) and high quality Rare Earth concentrates can be obtained successfully by the new collector Dh, acid silica gel, turpentine and reagents fitting together rationally. In order to determine optimum technical conditions, the effect of pulp pH, pulp temperature, pulp density and the effect of dosage of reagents (Dh and acid silica gel) on the flotation were investigated in the test.

Jan 1, 2003

By G. Demi, G. Belardi, N. Shehu, S. Cico

The physico-chemical interaction between minerals such as olivine, chromite and serpentine and the ions most commonly present in solution, like Ca and Mg and flotation reagents such as EDTA and oleic acid was investigated. The study was conducted via release tests, electrophoretic measurements and microflotation of selected minerals coming from the Kukes deposit (Albania).

Jan 1, 2003

By Genrich A. Denisov

Principles of ecologically friendly geo-technologies construction are formulated on the basis of the works of the leading scientists in the field of rational processing of mineral resources of the Russian Academy of Sciences. One of these concepts is a new direction in rotational disintegration of mineral and technogenic raw material with the purpose of effective subsequent enrichment. A large amount of practical experience has been accumulated in the industry on selective destruction by application of vibrational method on initial material with consideration of its physical-mechanical properties and mineral structure. This method is successfully realised in a conic inertial pulverisation devices constructed by Mekhanobr Institute (St.-Petersburg). A new construction of conical-inertial pulverisation with a modification of disintegration force has been developed recently at Mekhanobr Institute. It allows, in some cases, to increase selectivity of subdivision and to avoid over-disintegration. Advantages of “wet” subdivision methods in conic inertial disintegration devices are proved. The efficiency of such subdivision can be increased due to rational use of the phenomenon of a dislocation-dynamic diffusion. Its advantage is proved by the effect on disintegrated material by frequency-modulated variable electrical fields of low power. It was shown in industrial conditions, that the productivity of the spherical mill can be increased by 10 %, and that it also prevents ecologically harmful surface active substances (SAS) in milling zone and it reduces the dust content in the air. The techniques of tentative estimation of efficiency of various proceedings technogenic materials and their classification are created. The scientific fundaments of rational, ecologically friendly technology of processing and regeneration of various kinds of technogenic raw material are developed. A number of effective technologies on processing of wastes is developed and inculcated in concentration factories and metallurgical factories.

Jan 1, 2003

By V. Grujic, M. Grujic, D. Salatic

"Two areas are involved in the research work of the comminution process (crushing and grinding). The first one involves the changes of the size class distribution values that are definded by the differential equations in the function of the ore property and working conditions. The second area involves the comminution of the different levels in order to optimize the working parameters and to decrease the operational costs in the grinding process.We have studied, in detail, the possibility of functioning the crusher at the maximal loading, over 4500 kN, ball mills with diameters larger than 5.0 m and semiautogenous mills with diameters larger than 10.0 m.Using the computers, we have achieved the maximal loading range of the crusher, over Fc ? 4500 kN in the crushing process. In the grinding process, using the adequate differential equations in the automation process, we have established the correlation between the pulp mass capacity in the mill, pulp dencity, ore fineness in the pulp and recirculating ore charge.With the appopriate text, equations and graphs, this paper shows the results of our several years research work in the laboratory and in the ore comminution plant of Majdanpek Copper Mine."

Jan 1, 2003

By Liping Yu Che, Xiaotie Wang, Mingli Cao, Jizu Yongfu Yuan

"It is difficult separating fluorite from Ca, Ba, Si intergrowth minerals than simple from Si, using common reagents such as combination of oleic acid or paraffin soap and water glass, but the finest quality fluorite concentrate whose grade is over 96%F must be required in chemical plant.This paper studies the flotation process of native fluorite from calcite, barite and silicate minerals whose flotation properties is similar to fluorite, using new effective collector H602 and new depressor S602 that is cheaper in cost, and describes the flotation properties. In order to determine optimum flotation separation condition, the effect of pulp pH, pulp temperature, pulp density and the effect of dosage of reagents on flotation were investigated and the flotation result was provided by oleic acid collector and the results of collector H602 were compared with those of collector oleic acid in the test. The test result of ore samples shows that at moderate pulp pH values (10.5-11.5) and other moderate technical conditions, the fluorite mineral can be obtained by new reagents and the rational reagents combination. The conclusion is 98%F of fluorite concentrate can be obtained, using the combination of H602 and S602 and only 5 steps in techniques. The paper discusses the mechanism of the flotation separation of fluorite mineral from intergrowth minerals."

Jan 1, 2003

By Scott C. Brown, Ivan U. Vakarelski

The particles commonly encountered in mineral benefication schemes have irregularites that are expressed at many different length scales. In part, this originates from preceding processes (e.g. makedown, comminution, handling and storage), which are known to chemically and physically modify the bulk particle and its surface. Interparticle tribology, dissolution and reprecipitation events along with large-scale mechanical stresses are just a handful of the interactions encountered during processing of particles prior to separation. It is feasible to imagine that each one of these events may impose a fingerprint of characteristic nanoscale, microscale, and macroscale morphological changes that can modify the overall interaction of these particles within a system. Suprisingly there are just a few works on how these resulting features can alter the performance of benefication schemes, and especially flotation.

Jan 1, 2003

By John Ralston, Stephen Grano, Yongjun Peng, Daniel Fornasiero

"A specially designed mill which allowed the control of pH throughout grinding was used to study the effect of rgrinding conditions on galena flotation and galena separation from pyrite. The various reactions occurring on the mineral surface were investigated by a range of techniques, including OH- addition to maintain the grinding pH, EDTA extraction, XPS and ToF-SIMS measurements.Galena flotation and galena separation from pyrite were strongly dependent on the metal oxidation species produced on galena and pyrite surfaces under different grinding conditions. Iron oxidation species depressed both galena and pyrite flotation, whilst lead oxidation species activated pyrite but had little effect on galena. Optimum galena flotation and galena selectivity against pyrite were achieved by selecting grinding conditions that enabled lead and iron oxidation production to be controlled."

Jan 1, 2003

By Máximo Pérez, Julio C. Videla, Rosa Dzioba

"This paper reports the hydrometallurgical treatment of gravity concentrates of gold samples and outcrops associated with graphite ores obtained from:• flotation tailings of crystalline graphite minerals• outcrop samples of graphitic rock associated with auriferous minerals and free gold located in the Villa Union district and surrounding areas - La Rioja Province - Argentina.Previous studies of the flotation potential of crystalline graphite minerals failed to consider the presence of noble metals.The samples represent a mineralized zone of crystalline graphite which is distributed in different formations with a NE - SW trend in Maz, Punta Colorada and Las Ramaditas hills, covering an area of about 300 square kilometers."

Jan 1, 2003

By Atsushi Shibayama, Toyohisa Fujita, Wan-Tai Yen, Ke-jun Liu

"A gold has been leached with ammonium thiosulfate solution and several leaching conditions have been studied. The leached solution has been recovered by solvent extraction and the optimum conditions have been investigated.SUMMARYIn this investigation, a sponge gold sample (99.92% pure) has been leached with ammonium thiosulfate solution. The effects of CuSO4, (NH4)2S2O3, (NH4)2SO4, NH4OH and retention time on the gold leaching % (extraction %) and thiosulfate oxidation % (consumption %) have been studied. The copper ion acts as a catalyst in gold dissolution. On the other hand, it also accelerates oxidation of thiosulfate (consumption). It was found in this study that the best gold extraction condition was obtained at 43.2 ks with 0.8 – 1.0x103 mol/m3 (NH4)2S2O3, 30 mol/m3 CuSO4, 2.0 – 3.0x103 mol/m3 NH4OH, 0.4 – 0.5x103 mol/m3 (NH4)2SO4, pH 10±0.2 and 150 rpm. The thiosulfate oxidation was about 15% of the initial concentration."

Jan 1, 2003

"The Merensky Reef is a platinum group minerals (PGM) bearing reef in the Bushveld Igneous Complex in South Africa. The reef has been treated by bulk PGM and sulphide flotation with the aim of maximisingthe valuable minerals recovery and gangue minerals rejection.Synthetic water with a calcium concentration of 80 ppm and 500 ppm was prepared and the flotation results obtained were compared to a simple electrolyte in order to determine the effect water quality has on pentlandite and pyroxene surface alteration and, ultimately, floatability. During the study, the possible effect of interactions between the minerals investigated and Ca2+ ions in the presence of sodium isobutyl xanthate was studied at pH 6 and pH 9 by means of zeta potential determinations, microflotation tests and ToF-SIMS analysis.The results obtained on 1:1 pentlandite-pyroxene mixtures showed that the quality of process water plays an important role in flotation. The flotation recoveries of pentlandite and pyroxene were lower in synthetic process water compared to those obtained in a simple electrolyte solution."

Jan 1, 2003

By Seoul National University, Ki-Ho Kim, Jong-Pyo Kim, Sung-Min Joo, Hee-Chan Cho, Hyung-Seok Kim

Aragonite was synthesized in addition of Mg2+ ion and SrCO3 seed by carbonation process, and the best condition and mechanism of the synthesis was studied by analysis of continuous pH change, ICP, XRD, and SEM. As MgCl2•6H2O addition increased, aragonite phase increased at condition of CO2 flow rate of 100 mL/min and stirring rate of 250 rpm. It was the dissolution of Mg(OH)2 that determined overall reaction time. As SrCO3 seed addition increased at 0.2 mole MgCl2•6H2O, the amount of aragonite increased and the aspect ratio was from 5 to 9. And it was thought that Mg2+ ion prohibited calcitetransformation of aragonite formed by SrCO3.

Jan 1, 2003

By G. Onal, E. Gock, H. Dincer

"During the conventional chromite dissolution process; chromite ore concentrates were ground to at least <90 µm using the ball mill and after adding Na2CO3 and leaning material (instead of CaCO3 also residues from the leaching process) at a ratio of e.g. 1:0.75:1.2, depending on the specific formulation, follows the digestion e.g. in a rotary kiln, heated in countercurrent. The reaction time is 3 to 8 h. The calcine is comminuted and leached with water or a thin chromate solution. Depending on the type of ore used, the yield is 75-85 %. The disadvantage of the above-described process is that it is impossible, using current technology, to achieve a complete digestion of the chromite ores and that the chromium-containing residues have to be disposed of as special waste, involving a large financial effort.The subject of this study was the investigation of the effect of vibratory milling on chromite dissolution. The impact stress in the vibratory mill causes the mechanical activation of chromite, which is characterised by lattice defects. The degree of mechanical activation can be quantified by measuring the relative X-ray diffraction intensities at the parent lattice planes of chromite. Each relative X-ray diffraction ratio correlates with a certain degree of digestion. As opposed to vibratory milling, a complete digestion of chromite using a ball mill is impossible, even at extremely long grinding times.In this investigation a chromite concentrate from Pulpinar/Kayseri with content of 44 % Cr2O3 and the Eccentric Vibratory Mill was used. In order to verify the effect of the vibrating grinding on chromite dissolution, reaction kinetic investigations on digestion and leaching were carried out."

Jan 1, 2003

By Elena L. Chanturiya, Vladimir A. Bocharov, Roman A. Amosov

"In many volcanogenic base metal deposits of Russia the gold is closely associated with copper sulphides and pyrite. The recovery of gold associated with pyrite is especially difficult problem.Investigations of gold chemical state and mineral forms in copper-zinc sulphide ores of Gay and Barsuchiy Log deposits in the Urals have been made using EPMA, optic image-analysis, XRA, SEM, thermo-electrical force measurements and selective gold leaching experiments.Two gold varieties are determined: 1) free native gold particles (from 5 µm up to 0,25-1,0 mm), which can be liberated after grinding of ore up to 0,074 µm and named “free gold”; 2)”invisible” gold, including finely disseminated native gold and chemically bound gold. The second variety can’t be disclosed during grinding. Free gold can be recovered by gravitation and flotation while the processing behaviour of “invisible” gold is determined by properties of gold-bearing sulphides: pyrite and chalcopyrite. According to results of diagnostic leaching experiments in ores of deposits mentioned above the part by weight of free gold reaches 70%, the part by weight of the ”invisible” gold is up to 20%. About 10% of gold is enclosed in quartz and acid-soluble minerals.Theoretically (taking into account gold distribution data) it’s may anticipate gold recovery by gravitation up to 60%. However after grinding up to 50-60% of class –0,074 mm only about 40% of gold passes into oversize product including 30% of free gold and 8% of ”invisible” one. It can be recovered by gravitation. Remaining free gold and ”invisible” gold can be extracted by flotation – 25% in total. Inevitable gold losses in tailings may reach 8-10%."

Jan 1, 2003

By Natalie J. Shackleton, Deryck de Vaux, Cyril T. O’Connor, Vratislav Malysiak

"The major losses of PGM and base metals in the beneficiation of platinum group deposits occur during the separation of gangue from the value minerals by selective flotation. A number of studies have shown that this negative impact on flotation is due to surface passivation, caused by various ions that may originate from the external water supply or, as is likely in the majority of cases, from the oxidation of the mineral surfaces and the grinding media. The objective of the study was to investigate the effect surface passivation and inadvertent activation have on flotation and how this can be managed so as to increase the separation of pentlandite and pyroxene. The aim was to minimise the percentage pyroxene reporting to the concentrate and simultaneously maximise the pentlandite recovery. The testwork incorporates the addition of an activator (copper sulphate), a complexing agent, such as DETA (diethylenetriamine) and a dispersant (polyphosphate) at pH 6 and pH 9 in an attempt to alleviate the surface passivation of pentlandite and inadvertent activation of pyroxene. Both synthetic minerals and plant ores were studied in order to determine the effect surface passivation and inadvertent activation have on mineral surface alteration and floatability. Zeta potential determinations, microflotation, ToF-SIMS (Time of Flight Secondary Ion Mass Spectrometry) analyses, laboratory batch flotation tests and continuous flotation testwork were used as tools to study the surface alteration and/or floatability.Zeta potential determinations and ToF-SIMS analyses showed that copper adsorption is non-selective. Both pentlandite and pyroxene become copper (II)-activated in the presence of copper sulphate and subsequently, in the presence of xanthate, adsorption of the collector will occur onto copper activated mineral surfaces. Zeta potential determinations also showed an alteration of the surface charge in the presence of polyphosphate, thereby inhibiting surface passivation of sulphides by slime coatings due to surface repulsion."

Jan 1, 2003

By Buks Kruger

"After the milling and flotation of the platinum bearing ore, the flotation concentrate is electrically smelted in 6-in-line electric arc furnaces and the resulting furnace matte treated in Peirce Smith converters to remove the iron sulphide. The iron free (less than 1% Fe) converter matte is then granulated and sent to the Base Metals- and Precious Metals Refineries for further processing.During the smelting and converting processes two distinct gas streams are produced.The Peirce Smith converter off gas contains 4% - 9% SO2 which is treated in a conventional Sulphuric Acid Plant to produce sulphuric acid (H2SO4).The electric furnace off gas contains 0.9% SO2 and was (until September 2002) vented through a 91 meter high stack to atmosphere.Off gasses which contain less than 3% SO2 is difficult to handle and quite a few processes had been developed over the years to cope with this gas. A broad spectrum of process suppliers and technology approaches is available and the different technologies can be divided into a few main approaches i.e.Scrubbing of the off gas with an alkaline solution to produce an environmentally friendly and stable waste product which can be discharged onto a tailings dam or permanent landfill site.Physical absorption of the SO2 into a chemical solution to produce high quality chemically pure process chemicals.Catalytic reaction of SO2 with O2 to produce SO3 which is absorbed in water to produce sulphuric acid of less than 90% strength.In October 2002 Impala Platinum commissioned a Sulfacid Plant at its Smelter in Rustenburg which recovers the SO2 from the electric furnace off gasses into a weak sulphuric acid solution.The Sulfacid Plant technology is widely used in the paint pigment industry. This is, however, the first application of the technology on electric furnace off gas.The furnace off gasses contains flue dust which is removed in electrostatic precipitators. The gas exiting the precipitators normally still contains between 40 mg/Nm3 and 60 mg/Nm3 dust and passes through a quench-scrubber before entering the reactors. The quench-scrubber cools the electric furnace offgas down from ± 200 °C to 60 °C and act as a final dust removal stage."

Jan 1, 2003

By André Mans, Frans B. Waanders

"Ferrosilicon (Fe-Si) is an important commercial material and it forms the basis of the powder used in dense medium separation (DMS) of various minerals in a minerals beneficiation process. Current losses of Ferrosilicon (Fe-Si), which is used in the dense medium separation (DMS) of iron ore at Kumba Resources, Sishen, South Africa occur due to adhesion to the separation products and also by being present in the effluent stream, due to abrasion. The losses contribute greatly to the running cost of the plant and the purpose of this project was to determine the characteristics of the unused Fe-Si and then to characterise the changes that occur during storage and the use thereof.A Scanning Electron Microscope (SEM) and Mössbauer Spectroscopy (MS) were used to investigate the characteristics of the fresh and used Fe-Si. The SEM analyses of the Fe-Si yielded a composition of 15 wt.% Si and 85 wt.% Fe with minor impurities of Mn and Cr (<1 wt. %), resulting in an ordered phase with a calculated composition of Fe2Si. The average density of the Fe-Si was found to be 7.177 g.cm-3 whilst the size distribution was determined with the d50 of the particles being approximately 30 µm. A slurry, containing 10% solids was prepared, which had a density of about 1.1 g.cm-3 and this slurry was used to conduct the various experiments under laboratory conditions at the university. Samples were taken at regular intervals from a storage container containing a lime solution as well as from a closed circulation circuit system, kept at a constant temperature of about 60°C. Mössbauer Spectroscopy yielded, for the new fresh Fe-Si-samples, a two-sextet spectrum with hyperfine magnetic field strengths of 19.9T and 30.7T respectively, and the yellow-brown froth was found to be akaganeite or ß-FeOOH.It was found that the biggest loss of Fe-Si was due to the abrasion of the particles during the DMS process. A possible change in magnetic properties was also observed, leading to further losses that could occur during prolonged use of the medium. No clear changes to the Fe-Si occurred during correct storage methods, as was initially thought."

Jan 1, 2003

By Barda K. Mishra, Surya P. Mehrotra

"INTRODUCTIONIn a jig, which is primarily a coarse mineral concentration device, the bed of mineral particles is pulsated with a stream of water resulting in the particles of different specific gravities. It operates in a cyclic manner – the jig cycle consists of four stages, namely, inlet, expansion, exhaust and compression. In the inlet stage the bed lifts up en masse. Near the end of the lift stroke the particles at the bottom of the bed start falling resulting in the loosing of the bed which, in turn, causes its expansion or dilation. During the third and fourth stages the particle resettle through the fluid, and the bed collapses back to its original volume. The pulsation and suction are repeated to bring about stratification with respect to specific gravity across the bed height. Various parameters affecting the stratification process include amplitude and frequency of pulsation, bed thickness, rate of hutch water flow, and feed characteristics. This paper first presents a review of various jigging theories and then describes a new approach to mathematical modeling of jigging employing the discrete element method.JIG MODEL BASED ON DISCRETE ELEMENT METHOD (DEM) APPROACHThe jig models based on DEM essentially involve tracking the position of each particle incrementally, applying Newton’s law of motion and a force displacement law at the contact. The model presented here is based on a three dimensional mathematical description of solid-solid and fluid-solid interactions. In this model, the force balance on a particle is extended to account for the effect of continuously varying fluid on the particle. The total force on each particle is made up of a known external body force, fluid particle interaction force and particle-particle and/or particle-wall interaction force. The fluid-particle interactive force is primarily made of drag and buoyancy. Di Felice’s correlation is used to evaluate the drag force. Solid-solid interaction is described by treating particles as discrete elements that are indestructible but interact with each other and any other elements present, such as walls, when they make physical contacts. A pair of spring and dashpot represents a contact The contact forces are computed from the amount and the rate of overlap of the particles at the contact. The motion of the particle is due to movement of the fluid, which transmits its energy through the particle-particle contacts. A computer program incorporating both the contact and the fluid model has been developed. It takes the operating parameters such as amplitude and frequency of the pulsating fluid, pertinent data concerning particle properties and the geometry of the jig bed as inputs."

Jan 1, 2003

By A. Güney, G. Önal

"Karagedik Chromite Concentrator of the ETI Holding Co., which is located in Fethiye (south Turkey), has been producing chromite concentrate assaying 47-48 % Cr2O3 from the chromite ores containing 30-35 % Cr2O3 by using gravity separation methods since 1920. The tailings having 13-14 % Cr2O3, which had been removed from this plant, were accumulated at the stockpiles amounting about 1.2 million tons. In order to recover the ultra fine chromite particles from the Karagedik Concentrator tailings, the new process including Wet High Intensity Magnetic Separation and column flotation, was developed and the Karagedik Research Pilot Plant based on this process was commissioned in 2000. At this plant, the final concentrates assaying 46-48% Cr2O3 were produced and overall plant recoveries are about 60-65%.At the chromite concentrators using gravity separation methods, if their material size is about minus 1.0 mm, chromite particles especially pass to fine fractions according to their mineralogical structures and the ore-genesis (Önal and Güney, 1990). Generally, after crushing and grinding, the shaking tables and spirals are used at the chromite concentrators; therefore fine size chromite particles (-0.038 mm) are removed as tailings. Cr2O3 content of the -0.1 mm size fraction with 52.3% of the total amount is 19.58 % with Cr2O3 distribution of 82.6%.In order to upgrade the minus 0.1 mm size fraction of the tailings, assaying about 20% Cr2O3, Karagedik Research Pilot Plant (KRPP), which includes Wet High Intensity Magnetic Separator (WHIMS) and Column Flotation units, was installed by Istanbul Technical University (ITU), Mineral Processing Section in 2000.Feeding material of the KRPP having 5 tons per hour capacity is obtained from stockpiles amounting 1.2 million tons. After attrition scrubbing, the feed is sent to a screen with aperture of 1.0 mm. The screen overflow, assaying 5-6 % Cr2O3 is removed as tailings. Screen underflow is classified to –1.0+0.1 mm and minus 0.1 mm size fractions by using cyclone and sieve bend. –1.0+0.1 mm size fraction assaying 6-7 % Cr2O3, is sent to existing gravity separation plant. Minus 0.1 mm size fraction is firstly fed to WHIMS for pre-concentration and non-magnetic product assaying 10-11 % Cr2O3 consisting of serpentine, talc and olivine minerals are separated as tailings. Also magnetic product (25-30 % Cr2O3) obtained from WHIMS is fed to the two stages conditioners after dewatered to 30 % solid ratio."

Jan 1, 2003