Manual of Procedure for Chemical and Instrumental Analysis of

1 Government of India Ministry of Mines Indian Bureau of Mines Ore Dressing Division Manual of Procedure for Chemical and Instrumental Analysis of Ores, Minerals, Ore Dressing Products and Environmental Samples Issued by Controller General Indian Bureau of Mines NAGPUR Revised Edition February, 2012 Price : (Inland) A 750; ( foreign ) $ or Printed at IBM Press, 48/500/February, 2012 INDIAN BUREAU OF MINES PROJECT CREDIT OVERALL GUIDANCE Controller General FORMULATION & GENERAL GUIDANCE MOHAN RAM Suptdg. Officer (Ore Dressing) COLLECTION AND COMPILATION OF TECHNICAL DATA SHENDE BHAISARE Suptdg. Officer (Ore Dressing) (Retired) Suptdg. Chemist (Retired) JAIN MORONEY Senior Chemist (Retired) Suptdg.

2 Chemist SHYAMJI SINGH Dr. SOLANKI Chemist (Retired) Chemist REVISION MORONEY Suptdg. Chemist Mrs. JYOTI SHRIVASTAVA Chemist DTP COMPOSING AND PAGE MAKING GULKOTWAR Stenographer (Retired) PUBLICATION SECTION Chief Editor Asstt. Editor Junior Technical Assistants PREFACE The chemistry of rock/ore is the key to understand the concentration of elements and presence of other associated elements. There is no doubt that Chemical Analysis reveals economic value of any mineral/rock. The Chemical Analysis of samples shall guide and aid the future course of exploration with reference to the quantum, quality and the time frame. Chemical assay is also very important and helps the beneficiation engineers to plan their test work and do the required improvement during the beneficiation process.

3 The Chemical Analysis of ore/processed products speaks of their suitability for various mineral based industries. Ores and minerals have variety of elements and radicals, which offer interference with one another during Analysis . The chemist has to choose the exact Procedure of Chemical Analysis depending upon the nature of ore samples and radicals/elements to be analyzed. The choice of any analytical Procedure or Instrumental analytical techniques also depends on the concentration of elements in parts per million (PPM) or otherwise. Thus each Procedure of Chemical Analysis has its own merits and demerits and selection of method is based on desired accuracy. Instrumental Analysis using instruments like XRF, AAS, ICPA, Ion-chromatograph, FTIR brought a modernization and sophistication to the analytical data.

4 The analyst needs to develop techniques very carefully for the standardization and calibration of the instrument for obtaining the reproducibility and accuracy in the results. The Analysis of environmental samples for the various parameters in waste, water, drinking water, soil and ambient air help in preparing a baseline data and environmental management plans for the mines. The methods based on ISI procedures and using modern sophisticated instruments have been selected and mentioned in the Manual . Rapid and accurate Analysis of samples holds the key to success in exploration, mineral based mining, marketing and assess quality of mineral based products. This revised edition is brought for the industry. ( ) Nagpur Controller General Dated.

5 21st February, 2012 Indian Bureau of Mines CONTENTS SUBJECT PAGE NO 1 METHODS OF Analysis USING WET CLASSICAL AND COLOURIMETRIC procedures 1 OPENING OF ORE/MINERAL SAMPLE 1 DETERMINATION OF MAJOR AND MINOR CONSTITUENTS FROM STOCK SOLUTION 5 ALUMINIUM ORES 22 ALUMINO SILICATE & OTHER SILICATES 24 ANTIMONY ORES 26 ARSENIC ORES 28 BARIUM ORES 28 BISMUTH ORES 34 CHROME ORES 36 COBALT ORES 39 FLUORSPAR ORES 41 GYPSUM 44 IRON ORES 46 LIMESTONE, DOLOMITE, MAGNESITE AND ALLIED MATERIALS 47 MANGANESE ORES 48 MOLYBDENUM ORES 51 NICKEL ORES 55 COPPER, LEAD, ZINC (POLYMETALLIC ORES) 58 PYRITES 59 ROCK PHOSPHATE AND APATITE 60 SELENIUM AND TELLURIUM 62 SILICA 64 TIN ORE 65 TITANIUM BEARING ORES 67 TUNGSTEN ORES 70 VANADIUM ORES 73 ZIRCONIUM ORES 75 COAL AND GRAPHITE 77 CEMENT 80 DETERMINATION OF CaF2 IN FLUORSPAR BY Chemical PHASE TECHNIQUE 80 Chemical QUALITY EVALUATION AND STANDARDISATION OF SODIUM OLEATE FOR APPLICATION AS FROTH FLOTATION REAGENT 83 SPECTROMETRIC (COLOURIMETRIC) METHODS OF Analysis 87 STANDARD SOLUTION AND STANDARDIZATION 111 GENERAL SAFETY PRECAUTIONS 118 TITRE EQUIVALENT PER ML OF STANDARD SOLUTION 121 2.

6 METHODS OF Analysis USING X-RAY FLUOROSCENCE (XRF) ANALYSER 123 X-RAY FLUOROSCENCE SPECTROMETRY 123 CHOICE OF Instrumental PARAMETERS 132 SAMPLE PREPARATION TECHNIQUE 144 3. METHODS OF Analysis USING ATOMIC ABSORPTION SPECTROPHOTOMETRY 150 ATOMIC ABSORPTION SPECTROPHOTOMETRY 150 ATOMIC ABSORPTION 150 RELATION BETWEEN ATOMIC ABSORPTION & CONCENTRATION 151 ATOMIZATION OF SAMPLE 152 SAMPLE PREPARATION FOR AAS 160 DETERMINATION OF LITHIUM IN LITHIUM, RUBIDIUM, CESIUM IN TUNGSTEN ORES, MINERALS & BENEFICIATION PRODUCTS AND MICA 162 DETERMINATION OF RUBIDIUM IN LITHIUM RUBIDIUM, CESIUM IN TUNGSTEN ORES, MINERALS BENEFICIATION PRODUCTS AND MICA 164 DETERMINATION OF CESIUM IN LITHIUM RUBIDIUM, CESIUM IN TUNGSTEN ORES, MINERALS & BENEFICIATION PRODUCTS AND MICA, 165 DECOMPOSITION AND Analysis OF CHROMIUM IN ORE, MINERALS AND BENEFICATED PRODUCTS FOR CHROMIUM, IRON.

7 NICKLE & COBALT 168 DETERMINATION OF SILVER BY ATOMIC ABSORPTION SPECTROSCOPY IN POLYMETALLIC ORES & BENEFICIATED PRODUCTS 171 DETERMINATION OF MOLYBDENUM IN TUNGSTEN & POLYMETALLIC ORES, MINERALS AND BENEFICIATION PRODUCTS 173 DETERMINATION OF BISMUTH IN TUNGSTEN & POLYMETALLIC ORE, MINERALS AND BENEFICIATION PRODUCTS BY ATOMIC ABSORPTION TECHNIQUES 174 DETERMINATION OF OXIDISED ZINC IN ZINC ORE, ZINC CONCENTRATE & OTHER BENEFICIATED FRACTION 176 DETERMINATION OF OXIDISED LEAD IN LEAD ORE, LEAD CONCENTRATE & OTHER BENEFICIATED FRACTIONS 177 DETERMINATION OF OXIDISED COPPER IN COPPER ORE CONCENTRATE 178 DETERMINATION OF NIOBIUM & TANTALUM IN ORES AND ORE DRESSING PRODUCTS OF TUNGSTEN AND TIN 179 DETERMINATION OF GALIUM, INDIUM, THALLIUM IN ZINC AND LEAD ORE AND BENEFICIATION PRODUCTS BY ATOMIC EMISSION ON ATOMIC ABSORPTION SPECTROPHOTOMETER 181 4.

8 PRINCIPLE AND Procedure OF CARBON & SULPHUR ANALYSER 184 5. METHODS OF Analysis USING INDUCTIVELY COUPLED PLASMA (ICP) INSTRUMENT 186 ICP(AES)- TECHNIQUES AND APPLICATIONS 186 Analysis OF PLATINUM GROUP ELEMENTS 192 APPLICATION OF ICP-OES TO WATER Analysis 195 THE ICP OES IN ENVIRONMENTAL APPLICATIONS 198 6. METHODS OF Analysis OF ENVIRONMENTAL SAMPLES 199 DETERMINATION OF DISSOLVED FLUORIDE, CHLORIDE, NITRATE, ORTHOPHOSPHATE, SULPHATE IONS USING ION CHROMATOGRAPHIC METHOD 199 Analysis OF SODIUM & POTASSIUM IN WATER, WASTE WATER, EFFLUENTS, SOLIDS, SOILS ETC. USING FLAME PHOTOMETER 201 DETERMINATION OF TURBIDITY IN WATER, WASTE WATER USING TURBIDITY METER/NEPHELOMETER 203 DETERMINATION OF COLOUR IN WATER AND WASTEWATER (UV-SPECTROPHOTOMETRIC METHOD) 204 DETERMINATION OF SUSPENDED SOLIDS, TOTAL SOLIDS, DISSOLVED SOLIDS, INORGANIC MATTER AND VOLATILE MATTER IN WATER, WASTE WATER, EFFLUENT ETC.

9 205 DETERMINATION OF Chemical OXYGEN DEMAND IN WASTE WATER/EFFLUENT 208 DETERMINATION OF BIOCHEMICAL OXYGEN DEMAND (BOD) IN WASTE WATER AND EFFLUENTS 210 DETERMINATION OF DISSOLVED OXYGEN IN WATER AND WASTEWATER 212 DETERMINATION OF PHENOLIC COMPOUNDS AS C6H5OH(DIRECT COLORIMETRIC METHOD) 214 DETERMINATION OF OIL AND GREASE IN WATER AND WASTE WATER 216 Analysis OF SULPHATE IN WATER AND WASTE WATER/EFFLUENT 217 DETERMINATION OF SULPHIDE IN WATER & WASTE WATER 219 Analysis OF SILICA IN WATER AND WASTE WATER 221 Analysis OF PHOSPHOROUS IN WATER AND WASTE WATER 224 DETERMINATION OF PHOSPHORUS BY STANNOUS CHLORIDE METHOD (SOLUABLE PHOSPHATE) 224 DETERMINATION OF PHOSPHORUS BY ASCORBIC ACID METHOD (SOLUABLE PHOSPHATE) 225 Analysis OF NITRITE NITROGEN (NO2-N) IN WATER AND WASTE WATER 226 DETERMINATION OF NITRATE NITROGEN (NO3-N) IN WATER AND WASTE WATER 228 DETERMINATION OF NITRATE NITROGEN (NO3-N) IN VISIBLE RANGE at 410 nm 228 DETERMINATION OF NITRATE NITROGEN (NO3-N) IN ULTRA VIOLET REGION OF SPECTROPHOTOMETER AT 220 nm & 275 nm 229 Analysis OF AMMONICAL NITROGEN (NH3-N)

10 IN WATER AND WASTE WATER 231 Analysis OF RESIDUAL CHLORINE IN WATER AND WASTEWATER SAMPLES 232 Analysis OF CHLORIDE IN WATER, WASTE WATER AND SOIL SAMPLES 234 DETERMINATION OF ACIDITY IN WATER, WASTE WATER 236 DETERMINATION OF ALKALINITY IN WATER & WASTE WATER 238 Procedure FOR THE DETERMINATION OF PHENOLPHTHALEIN ALKALINITY 239 Procedure FOR THE DETERMINATION OF TOTAL ALAKINITY 240 DETERMINATION OF HARDNESS IN WATER SAMPLES 240 Analysis OF HEXAVALENT CHROMIUM IN DRINKING WATER, WASTE WATER BY COLOURIMETRIC METHOD USING 1-5 PHENYLCARBAZIDE 243 Analysis OF CYANIDE IN WATER, WASTE WATER AND SOLID WASTES USING ION SELECTIVE ELECTRODE AND COLORIMETRIC METHODS 247 Analysis OF FLUORIDES IN WATER, WASTE WATER, MINERALS, ORES AND SOIL SAMPLES USING ION-SELECTIVE ELECTRODE AND COLORIMETRIC METHODS 250 Analysis OF MERCURY IN WATER/WASTE WATER, MINERALS, ORES AND SOIL SAMPLES USING MERCURY ANALYSER 255 SOIL Analysis 259 AMBIENT AIR QUALITY MONITORING 283 Addenda 1 BORON ORES 290 Addenda 2 LOSS ON IGNITION 292 Addenda 3 DETERMINATION OF TOTAL SILICA IN SILICATE MINERAL (A COMBINATION OF GRAVIMETRIC AND PHOTOMETRIC METHOD) 295 1.