SAMPLING OF SPONGE IRON
Every hour (alternative klin1 &klin2) a sponge iron sample 10-12 kg is taken from I/BINCD Belt in a bag
Mag and Dolochar separation
-05 mm fines separation from Mag
+05mm sponge iron
Coarse Crushing (- 12 mm)
Conning and quartering
Homogenization
Disc Pulverization
Screen 150 micron sieves
Homogenization
Coning and Quartering
50 – 100 g
Chemical Analysis
SAMPLING OF COAL (RAKE)
Total 15 sample collect from a Rake.
Collect a sample from 10 to 15 vehicles from a RAKE
Collect 12-15 kg coal
Coarse Crushing (- 25 mm)
Conning and quartering
2.5Kg
Fine Crushing (- 5 mm)
Homogenization
Riffle Sampling
0.6 kg
0.3 kg
Screen 212 micron sieves
Homogenization
Coning and Quartering
30 – 40 g
Proximate Analysis
SAMPLING OF COAL (TRUCKS)
Collect a Coal sample from every trucks
Collect 12-15 kg coal
Coarse Crushing (- 25 mm)
Conning and quartering
2.5Kg
Fine Crushing (- 5 mm)
Homogenization
Riffle Sampling
0.6 kg
0.3 kg
Screen 212 micron sieves
Homogenization
Coning and Quartering
30 – 40 g
Proximate Analysis
SAMPLING OF DOLOMITE
Collect a Dolomite sample from every trucks
Collect 12-15 kg Dolomite
Conning and quartering
2.5Kg
Fine Crushing (- 3 mm)
Homogenization
Riffle Sampling
0.6 kg
0.3 kg
Screen 150 micron sieves
Homogenization
Coning and Quartering
30 – 40 g
Proximate Analysis
SAMPLING OF IRON (ORE/PELLETS RAKE)
Total 15 sample collect from a Rake.
Collect a sample from 10 to 15 vehicles from a RAKE
Collect 12-15 kg Iron
Coarse Crushing (- 10 mm)
Conning and quartering
2.5Kg
Fine Crushing (- 5 mm)
Homogenization
Riffle Sampling
0.6 kg
0.3 kg
Homogenization
Coning and Quartering
Screen 74 micron sieves
50 – 100 g
Chemical Analysis
SAMPLING OF IRON (ORE/PELLETS TRUCK)
Collect a sample from every vehicles
Collect 12-15 kg Iron
Coarse Crushing (- 10 mm)
Conning and quartering
2.5Kg
Fine Crushing (- 5 mm)
Homogenization
Riffle Sampling
0.6 kg
0.3 kg
Homogenization
Coning and Quartering
Screen 74 micron sieves
50 – 100 g
Chemical Analysis
SAMPLING OF SPONGE IRON
A sponge iron sample 10-12 kg is taken from bunker despatch in a bag
Coarse Crushing (- 12 mm)
Conning and quartering
Homogenization
Disc Pulverization
Screen 150 micron sieves
Homogenization
Coning and Quartering
50 – 100 g
Chemical Analysis
SAMPLING OF COAL (EVERY SHIFT)
Collect Coal sample from stock houseconveyer belt
Collect 12-15 kg coal
Coarse Crushing (- 25 mm)
Conning and quartering
2.5Kg
Fine Crushing (- 5 mm)
Homogenization
Riffle Sampling
0.6 kg
0.3 kg
Screen 212 micron sieves
Homogenization
Coning and Quartering
30 – 40 g
Proximate Analysis
SAMPLING OF IRON (ORE/PELLETS)
Collect a sample from stock house conveyer belt every day
Collect 12-15 kg Iron
Coarse Crushing (- 10 mm)
Conning and quartering
2.5Kg
Fine Crushing (- 5 mm)
Homogenization
Riffle Sampling
0.6 kg
0.3 kg
Homogenization
Coning and Quartering
Screen 74 micron sieves
50 – 100 g
Chemical Analysis
SAMPLING OF COAL
DETARMINATION OF METALLIC IRON IN SPONGE IRON
METHOD: Mercuric Chloride (HgCl2)
Reagents: Mercuric chloride
Mixed acid (Oxygen free water 700ml+ Concentrated H2SO4 150ml+ H3PO4 150ml
Barium Di-phenylamine Sulphate (BDS) solution
K2Cr2O7 solution (1 litre distilled water+ 4.9035 gmK2Cr2O7)
PROCEDURE: Take 0.20gm of sample to a 250ml beaker and add distilled water 100ml heat at 200 degree
celcious up to the solution became 50ml. Filter the solution into a 500ml conical flux by 41
no filter paper and cool the solution up to room temperature. Add 20-30ml acid mixture and
4-5 drops of BDS as indicator. Tritate with K2Cr2O7. At the end point the solution colour will
be violet.
Calculation: Volume of K2Cr2O7×0.5585/sample weight in gm=%Fe(M)
DETARMINATION OF METALLIC IRON IN SPONGE IRON
METHOD: Ferric Chloride (FeCl2)
Reagents: Ferric chloride [10%(m/v)]- Dessolve 100gm of ferric chloric (FeCl3 ), 6H2O) in water and
dilute to one litre.
Barium Di-phenylamine Sulphate (BDS) solution (0.32gm of BDS to 100ml hot water)
K2Cr2O7 solution (1 litre distilled water+ 4.9035 gmK2Cr2O7
Hydrochloric Acid
Phosphoric Acid
PROCEDURE: Transfer g of sample ina 500ml conical flask and add 200 ml of ferric chloride solution.
Create an inert atmosphere in the flask obtainedthrough displacement of air by nitrogen,
stopper the flask and agitate the solutionwith polypropylene coated magnetic stirrer for 1
hr. Filter the solution through medium texture filter paper. Wash the residue with ferric
chloric solution. Transfer the filtrate to one litre beaker containing 400ml water, 25ml
sulphuric acid., 25ml phosphoric acid, 3-4 drops of BDS and titrate with (N/10) K 2Cr2O7.
Calculation: Volume of [(N/10) K2Cr2O7×0.5585)/3]/sample weight in gm=%Fe(M)
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WORK INSTRUCTION
DETARMINATION OF SULPHUR IN PLAIN CARBON STEEL
1. METHOD : EVOLUTION METHOD
2. REAGENTS : a) Dilute Hydrochloric Acid(HCL) 1:1(v:v)
b) Cadmium chloride (CdCl2 ) solution – 22gm CdCl2 + 1 lit. H2o + NH4OH
c) Starch solution – 1gm starch + 100 ml H2o
d) Sodium Thiosulphate solution – N/32(0.03N)
Sodium Thiosulphate( Na2S2O3,H2O ) : 8.1 g Na2S2O3 + 0.5 g NaHCO3 + 1 lit H2O
e) Potassium Iodate (KIO3) – N/32(0.03N)
Potassium Iodate (KIO3) : 1.07 g KIO3 + 10 g KI + 2 g KOH + 1 lit H2O
3. PROCEDURE : 2.5 g sample + 1.1 hot HCL in a 500 ml flask fitted with thistle funnel and
Delivery tube dipped in another measuring cylinder with CdCl2 solution. After receiving all
H2S gas from big 500 ml flask to small 250 ml flask, the cadmium sulphate(yellow colour) will
be titrated after addition of HCl and locate solution using the Starch as an indicator/ end
point: Blue - White
4. CALCULATION : A) Blank test : with solution ((d)) and ((e))
B) (vol of KIO3 – vol of Na2S2O3) × 0.02 % = % S
5. REPRODUCIBILLITY: ±0.005 %
6. REFERANCE : IS 228 (PART 9) – 1989
WORK INSTRUCTION
DETARMINATION OF CARBON IN PLAIN CARBON STEEL
1. METHOD : VOLUMETRIC
2. APPARATUS : STROHLEIN
3. PROCEDURE :
A) Before use the apparatus should be tested for satisfactory working against standard steel of appropriate
value of carbon.
B) Take 1gm accurately weighed sample in a porcelain boat and introduce in the combustion tube in the
furnace kept at 11000C to 11500C.
C) Close the furnace inlet with rubber stopper. Allow the sample to heat for 1 to 1.5 minute regulate flow
of Oxygen to 300 to 400 ml per minute into the furnace and establish connection with the burette which
has been filled with acidulated water coloured with methyl orange, so that the liquid level in the gas
burette does not rapidly. After about a minutes the level of water in the burette begins to fall more
rapidly through the same rate of Oxygen is maintained, indication completion of combustion.
D) Equalizing the levels of burette and connected aspiration bottle take the reading. Then the pass the
collected gas into the absorbing jacket filled with KOH solution. After absorption of carbon-di-oxide (CO 2)
by KOH take the second reading after equalizing the level.
4. CALCULATION : a) First reading = pressure of CO2 + other oxide + Oxygen
b) Second reading = Pressure of oxides except CO2
c) Difference in readings = Pressure of CO2 difference × Pressure / Temperature Correction
factor = % Carbon
5. REPRODUCIBILITY : 0.01 % up to 1.5 % Carbon
0.02 % above 1.5 % Carbon
6. REFERENCE : IS 228 (part 1) – 1987
WORK INSTRUCTION
DETARMINATION OF SILICON BY THE GRAVIMETRIC METHOD
(FOR SILION 0.05 TO 5.00 PERCENT)
METHOD : GRAVIMETRIC METHOD
REAGENTS :a) Mixed Acid: Add 450 ml of concentrated nitric acid to 500 ml water and cool. To another
500 ml of water add 250 ml of concentrated sulphuric acid and cool. Mix both the dilute
acid
b) Dilute Hydrochloric acid, 1:1, 3:1 and 1:20 (v:v)
c) Dilute sulphuric acid, 1:1 (v:v)
d) Hydrofluoric acid 40%.
e) Concentrated Nitric acid, Relative density= 1.42 (Conforming to IS 264:1976).
f) Per chloric Acid, 70%.
g) Concentrated Sulphuric acid, Relative Density= 1.84 (Conforming to IS 266:1977).
h) Dilute Nitric Acid, 1:1 (v:v)
Procedure: For Plain carbon Steels: Take 5.0gm of sample containing up to 0.1% silicon content, 2.5gm
of sample for silicon content up to 1% and 1gm of sample for silicon content up to 5%, in a 300ml porcelain
casserole, add 30ml of mixed acid to dissolve the sample, heat until nitrous fumes is expelled and continue
heating till SO3 fumes are evolved. Cool and add 50ml of dilute hydrochloric acid (1:1) and heat again. Cool,
dilute to 100 ml with warm water and add filter paper pulp. Stir well and filter immediately through medium
texture filter paper. Wash the residue with hot dilute hydrochloric acid(1:20) and then with hot water till
residue is free from chloride (check the solution in presence of chloride by 0.5% AgNO 3 Solution). Transfer
the residueand filter paper to a platinum crucible and dry at 1100C and ignite at 1050 degree celceus for 30
minutes. Cool in a desiccator and weight. Add 1-2 drops of dilute Sulphuric acid to moisten the residue and
then add 3-5ml of Hydrofluric acid. Evaporate to dryness and ignite at 1050 degree celcius to constant mass.
Calculation:
Silicon percentage by mass= [(A-B)×46.75]/C
Where: A= Mass in gram of silica obtained sample
B=Mass in gram of silica obtained 1 blank and
C= Mass in gm sample taken
Reproducibility:
±0.02 at 0.5 % level
±0.05 at 2.0 % level
±0.07 at 4.0 % level
WORK INSTRUCTION
DETARMINATION OF PHOSPHOROUS IN PLAIN CARBON STEEL
Method: Alkali metric Method by Ammonium Molybdate.
Reagents: 1. Dilute HNO3(1:1)
2. potassium Permanganate (KMNO4)-2%(M/V)
3. Sodium Nitrate (NaNO2)
4. Ammonium Hydroxide (NH4OH)
5. Potassium Nitrate (KNO3)
6. Ammonium Molybdate Solution
Flask-A: Ammonium Molybdate=59gm
NH4OH =73gm
H2O= 135ml
Flask-B: H2O = 575ml
HNO3=245ml
After cooling the both flasks add ‘A’-‘B’
7. (N/10) NaOH (4gm NaOH/1000ml H2O)
8. (N/10) HNO3 (7ml Concentrate HNO3/1000ml H2O, N/10HCl)
9. Phenolphthalein Indicator (1% in M. Alcohol)
Procedure: 1 g of sample+ 1:1 HNO3- Dissolve+ 2% KMNO4-Boil till MnO2- Cool-NH4OH + Dilute HNO3+ 40ml
Ammonium Molybdate)+ Filter- Wash with 1%KNO3. Take the residue+ H2O+10ml (N/10) NaOH+ 4-5 drops of
Phenolphthalein Indicator- Titrate with (N/10) HClor HNO3 (End point: Pink- colourless)
Calculation: (Volume of (N/10)NaOH- Volume of (N/10) HCl)×0.01347=% Phosphorous
Reproducibility: ±0.015%
Reference: IS 228 (Part 3)- 1987
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WORK INSTRUCTION
DETARMINATION OF MOISTURE OF IRON ORE/PELLETS SAMPLE
Surface Moisture: Take approximate 2kg of well mixed sample in a iron sample tray and weight it (weigh 2) and
put into the hot dry oven (100-120 Degree Celsius) for 2 hours. After removing the tray cool
and weight (weight 3) again.
Calculation: [(Weight 2 – Weight 3)/(Weight 2-Weight 1)]/100= % Surface Moisture, Weight 1= Tray
weight
Inner Moisture: Take 10-15gm of sample powder in a lean paper and weight (weight 2) it and put into the
hot dry oven (100-120 Degree Celsius) for 1 hours. After removing the tray cool and weight
(weight 3) again.
Calculation: [(Weight 2 – Weight 3)/(Weight 2-Weight 1)]×100= % Inner Moisture, Weight 1= paper
weight
WORK INSTRUCTION
DETARMINATION OF MOISTURE OF DOLOMITE SAMPLE
Surface Moisture: Take approximate 2kg of well mixed sample in a iron sample tray and weight it (weigh 2) and
put into the hot dry oven (100-120 Degree Celsius) for 2 hours. After removing the tray cool
and weight (weight 3) again.
Calculation: [(Weight 2 – Weight 3)/(Weight 2-Weight 1)]×100= % Surface Moisture, Weight 1= Tray
weight
Inner Moisture: Take 10-15gm of sample powder in a lean paper and weight (weight 2) it and put into the
hot dry oven (100-120 Degree Celsius) for 1 hours. After removing the tray cool and weight
(weight 3) again.
Calculation: [(Weight 2 – Weight 3)/(Weight 2-Weight 1)]×100= % Inner Moisture, Weight 1= paper
weight
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WORK INSTRUCTION
DETARMINATION OF RROXIMATE ANALYSIS (Coal Analysis)
Surface Moisture: Take approximate 2kg of well mixed sample in a iron sample tray and weight it (weigh 2) and
put into the hot dry oven (100-120 Degree Celsius) for 2 hours. After removing the tray cool
and weight (weight 3) again.
Calculation: [(Weight 2 – Weight 3)/(Weight 2-Weight 1)]×100= % Surface Moisture, Weight 1= Tray
weight
Inner Moisture: Take 10-15gm of sample powder in a lean paper and weight (weight 2) it and put into the
hot dry oven (100-120 Degree Celsius) for 1 hours. After removing the tray cool and weight
(weight 3) again.
Calculation: [(Weight 2 – Weight 3)/(Weight 2-Weight 1)]×100= % Inner Moisture, Weight 1= paper
weight
Volatile Matter (VM): Weight (Weight 1) a VM crucible and pour approx. 1gm of sample and weight (weight 2) it.
Cover the crucible suitable lid. Now the crucible put into a muffle furnace (Temperature
900±10 degree Celsius) for 7 minutes. After removing the crucible cool it ant weight (Weight
3) again.
Calculation: [(Weight 2 – Weight 3)/(Weight 2-Weight 1)]×100= % VM
ASH: Weight (Weight 1) a ash crucible and fill approx. 1gm of sample and weight (weight 2) it.
Now the crucible put into a muffle furnace (Temperature 900±10 degree Celsius) for 1hour.
After removing the crucible cool it ant weight (Weight 3) again.
Calculation: [(Weight 3– Weight 1)/(Weight 2-Weight 1)]×100= % Ash
Fixed Carbon (F.C): 100-(%Ash+%VM)=%F.C
WORK INSTRUCTION
DETARMINATION OfLoss On Ignition(LOI)
ISO 11536:2015(en)
Iron ores — Determination of loss on ignition — Gravimetric method
Introduction:The measurement of loss on ignition (LOI) is a technique widely used in the iron ore industry.
Ignition loss is the sum of contributions from the mass loss of volatile compounds water vapour, carbon
dioxide and sulfides (due to the decomposition of goethite and carbonaceous materials), and the mass gain
due to oxidation [Fe(II) to Fe2O3]. Its use is complementary to the determination of elemental or oxide
concentrations. It serves to allow for an addition of the oxides, generated at the ignition temperature, and the
LOI, to arrive at total (oxide + LOI). The determination of LOI is essential in sinter plant and blast furnace
balance calculations, as it is used to calculate calcinated elemental concentrations.
LOI determination procedure:Take weight (Weight-1) of an empty ash crucible and fill approximate
1gm of dry sample and weight (weight-2) again. Put this
crucible inside the muffle furnace for 1 hour. After removing the
crucible cool in at room temperature and weight (Weight-3)
again.
Calculation: [(Weight2-Weight3)/(Weight2-Weight1)]×100=%LOI
WORK INSTRUCTION
DETARMINATION Of loss on ignition(LOI) of Dolomite
Dolomite is an anhydrous carbonate mineral composed of calcium magnesium carbonate, ideally
CaMg(CO₃)₂. The term is also used for a sedimentary carbonate rock composed mostly of the
mineral dolomite. An alternative name sometimes used for the dolomitic rock type is dolostone.
Density: 2.84 g/cm³ (Average)
Crystal system: Hexagonal crystal family
LOI determination procedure: Take weight (Weight-1) of an empty ash crucible and fill approximate
1gm of dry sample and weight (weight-2) again. Put this
crucible inside the muffle furnace for 1 hour. After removing the
crucible cool in at room temperature and weight (Weight-3)
again.
Calculation: [(Weight2-Weight3)/(Weight2-Weight1)]×100=%LOI
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SAMPLING OF SPONGE IRON(IS 15774:2007)
1) SAMPLING FROM CONVEYORS :
The sponge iron 25 kg is taken from a moving conveyor, by mechanically
assisted device from the falling stream. Sampling shall be carried out while a
lot is being transferred.
2. SAMPLING FROM BUNKER DISCHARGE :
The sponge iron 25 kg is taken from bunker discharge in a bag.
3. STRUCTURE :
SPONGE IRON (25 KG)
15 Kg(Screen analysis) 10 KG
↓
Coarse Crushing (- 10 mm)
Conning and quartering
2.5Kg
↓
Fine Crushing (- 5 mm)
↓
Homogenization
↓
Riffle Sampling
↓
0.6 kg
↓
0.3 kg
↓
Disc Pulverization
↓
Screen 150/212 micron sieves
↓
Homogenization
↓
Coning and Quartering
30 – 40 g
Chemical Analysis
SAMPLING OF COAL (IS 15774:2007)
The sample of the coal shall be done at the following points :
A) ON PILES :For every 300 tonnes of coal sample, a minimum of one gross sample be collected. This 25 kg coal
sample shall be used for both proximate and screen analysis report.
B) On Truck: From each truck one increment for suitable weight shall be drawn. The gross 25kg sample shall be
used for both proximate and screen analysis report.
C) On Conveyor: From Conveyor, increments of suitable weight shall be drawn at regular intervals. All
increments thus drawn shall constitute a gross sample. The total mass of the gross sample shall be 25 kg
which shall be used for both chemical and screen analysis as shown in figure.
D) STRUCTURE :
Coal Sample (25 KG)
15 KG(Screen analysis and Physical Analysis)
10 KG (Chemical Analysis)
Coarse Crushing (- 10 mm)
Conning and quartering
2.5Kg
↓
Fine Crushing (- 5 mm)
↓
Homogenization
↓
Riffle Sampling
↓
0.6 kg
↓
0.3 kg
↓
Disc Pulverization
↓
Screen 150/212 micron sieves
↓
Homogenization
↓
Coning and Quartering
30 – 40 gm
For Chemical Analysis
SAMPLING OF IRON ORE/PELLETS (IS 15774:2007)
The sample of the Iron Ore / Pellets shall be done at the following points :
A) ON PILES :For every 300 tonnes of coal sample, a minimum of one gross sample be collected. This 25 kg coal
sample shall be used for chemical,Physical and screen analysis report.
B) On Truck: From each truck one increment for suitable weight shall be drawn. The gross 25kg sample shall be
used for chemical,Physical and screen analysis report.
C) On Conveyor: From Conveyor, increments of suitable weight shall be drawn at regular intervals. All
increments thus drawn shall constitute a gross sample. The total mass of the gross sample shall be 25 kg
which shall be used for chemical,Physical and screen analysis as shown in figure.
D) STRUCTURE :
Coal Sample (25 KG)
15 KG(Screen analysis and Physical Analysis)
10 KG (Chemical Analysis)
Coarse Crushing (- 10 mm)
Conning and quartering
2.5Kg
↓
Fine Crushing (- 5 mm)
↓
Homogenization
↓
Riffle Sampling
↓
0.6 kg
↓
0.3 kg
↓
Disc Pulverization
↓
Screen 150/212 micron sieves
↓
Homogenization
↓
Coning and Quartering
30 – 40 gm
For Chemical Analysis
SAMPLING OF DOLOMITE (IS 15774:2007)
The sample of the Iron Dolomite will be done at the following points:
A) ON PILES: For every 300 tonnes of coal sample, a minimum of one gross sample be collected. This 25 kg coal
sample shall be used for chemical,Physical and screen analysis report.
B) On Truck: From each truck one increment for suitable weight shall be drawn. The gross 25kg sample shall be
used for chemical,Physical and screen analysis report.
C) STRUCTURE :
Coal Sample (25 KG)
15 Kg (Screen analysis) 10 KG (Chemical
and LOI Analysis)
Coarse Crushing (- 10 mm)
Conning and quartering
2.5Kg
↓
Fine Crushing (- 5 mm)
↓
Homogenization
↓
Riffle Sampling
↓
0.6 kg
↓
0.3 kg
↓
Disc Pulverization
↓
Screen 150/212 micron sieves
↓
Homogenization
↓
Coning and Quartering
30 – 40g
For Chemical and LOI Analysis
