Bomb Calorimeter used for Coal Testing Process

Start Up:
 Open the O2-Cylinder valve, and let the gas stabilizer for one-two minutes.
 Check for 30 Bar on the output gauge.
 Turn on the chiller and check the water level.it should be near maximum
level.
 Turn on Bomb Calorimeter.
 Turn on the balance and let it stabilizer for 15 minutes.

Configuration Setup:
 Turn on Computer.
 Open SE Calorimeter Software from desktop.
 Click on Analyzer icon.

Procedure:
 Weighted the empty crucible =0.0005
 Now, Take the “Coal sample “in crucible nearest to 1g in the crucible.
 Make Sure that the sample is “free from atmosphere moisture”.
 Enter the weight value in the sample menu, enter the user name etc.
 Prepare the bomb and introduce inside the calorimeter carefully.
 Press start button and let the sample run.
 After completion the results will be automatically displayed on the display.
GCV=7000°C (For perfect Coal)
GCV=3000-6000°C (For Normal Coal)
Shutdown:
Take the bomb calorimeter out from the calorimeter.
Select Exit and press OK.
Turn off the on/off switch.
Turn off the chiller.
Turn off the gas cylinder valve.
 Analysis of Coal

Coal is analysis in two ways:

 Proximate Analysis
 Ultimate Analysis
Ultimate Analysis:
The ultimate analysis of coal involves determination of the
weight percent Carbon as well as Sulfur, Nitrogen and Oxygen. Trace element that
occur in coal are typically included as apart of the ultimate analysis. Nitrogen occurs
almost exclusively in the organic matter of coal.
Proximate Analysis:
The system consists of the analytical determination of;
 Moisture Content
 Volatile Matter
 Ash Content
 Fixed Carbon

 Moisture Content:
Moisture Content is simply telling us, how much water in a product. It influences
the physical properties of a substance, including weight, density, viscosity,
conductivity, and other. It generally determined by weight loss upon drying. There
are many methods for determination of moisture content.
 If a coal is heated in electric hot air oven at a temperature of 105-110 °C. And
take it out after of the oven after one hour. And put in a Desiccator to cool.
Then we determined how much moisture content in a product.

Percentage of Moisture = Loss in weight / Weight of coal × 100

  Volatile Matter:
Volatile matter is one of the most common is one of the
most common parameters measured in coal. It is measured as the weight percent
of gas (emissions) from the coal sample that is released during heating to 950°C in
an oxygen-free environment, excepts for moisture (which will evaporate as water
vapor), at a standardized temperature.
Percentage of volatile matter =loss of weight /weight of sample × 100

 Ash Content:
The ash content is a measure of inorganic impurities in the
fuel (typically sand, nickel, Aluminium, silicon, sodium, and vanadium), which can
cause different kinds of problems. Typically, the ash value is in the range 0.03%-
0.07% by mass. In a process temperature is required as 700-800°C. The high
percentage of ash is undesirable. It reduces calorific value of coal.
Ash comes from two primary sources:
 Intrinsic ash
 Extrinsic ash
Intrinsic ash:
Inorganic content found inside the plant cells and tissues as a result of normal
physiological processes.

Extrinsic ash:
And extrinsic ash, typically soil or dust contamination either adhered
to the surface of the biomass or collected with the biomass during the harvest
process.
  Fixed Carbon:
Fixed Carbon is the solid combustible residue that remains after a coal particle is
heated and the volatile matter is expelled. The fixed carbon content of a coal is
determined by subtracting the percentages of moisture, volatile, matter and ash
from a sample.
If carbon content in a coal is higher than the calorific value will be higher.
Percentage of fixed carbon=100- (% of moisture + volatile matter +Ash)

Water Analysis

 Hardness:
To a 50ml of sample add to 2ml of ammonia buffer & 2-3 drops
of “Erichrome Black-T as indicator” & titrate the mixture against 0.01M ETDA until
the color changes from red to blue. The volume of the EDTA used is noted and the
total hardness is calculated as follow:
TH as CaCO3=1000 × ml of EDTA used/ml of sample
 Calcium Hardness:
Take a 50 ml of water sample and add 2ml of 10%
potassium hydroxide and 0.2 of CaH indicator and titrate it against 0.01 EDTA
until the color changes from red to blue. The volume of EDTA used is noted and
the calcium hardness is calculated as follows:
CaH as CaCO3=1000× ml of EDTA used/ml of sample

 TDS (Total Dissolved Solids):

Filter the sample with the help of
Whatman filter paper. Weight out approximately 100ml of the sample and allow it
to evaporate in a water bath. The resides is then dried at 105°C. Calculate the total
dissolved solids in the sample as follows:
Total Dissolved Solids in PPM= Wt. of the of the resides ×1000/Wt. of the
Sample

 Chlorides:
Take 50ml of the sample and adjust with 0.2N sulphuric acid to
the methyl end point. Add ten drops of potassium chromate indicator and
titrate it with N/3.5 silver nitrate until the first tinge of reddish-brown color
appears. Note the burette reading and calculate the chloride as follows:
Chlorides PPM as Cl= 1000× ml of silver nitrate /ml of sample

Alkalinity

Phenol Alkalinity:
Take 50ml of sample 2-4drops of phenolphthalein indicator are added and titration
done with 0.02N sulphuric acid until the pink color just disappears. The volume of
acid is noted. This titration gives the total alkalinity due to hydroxide and half of
that due to carbonates. The phenol alkalinity can be calculated as follows:
Phenol Alkalinity= 1000× ml of H2SO4 /ml of the sample

Caustic Alkalinity:
Take 50 ml of water sample 5ml of 10% barium chloride and phenolphthalein
indicator are added and the titration is done with N/25 Sulphuric acid until pink
color just disappear. The caustic alkalinity is calculated as follows:

Caustic Alkalinity =1000×ml of H2SO4/ml of the sample

Methyl Orange Alkalinity:

Take 50 ml of sample eater add 3-4 drops of methyl orange indicator and the
titration is done against 0.02 sulphuric acids. The color changes from yellow to red.
Methyl orange alkalinity is then calculated as follows:

Methyl Orange Alkalinity=1000×ml of H2SO4/ml of sample

  Sulphur analysis of coal:

The sulfur concentration in a coal sample was found between 3.5 mg/g and 33.7
mg/g with typically repeatability around 10%. The limit of detection for the direct
analysis of solid coal samples was better than 0.1ug S.

 Take a coal sample & weighted 0.05 gram.

 Take a weighted coal in a crucible.
 And add tungsten in a weighted coal sample.
 Place a sample boat in a sample holder and shift near instrument.
 Then we click on add sample & Analyzed.
 The sample entered and burn 1150°C and a current is produced.
 Now, Sulphur reading is formed.