School of Chemical and Minerals Engineering North-West University

Faculty of
Engineering

SCHOOL OF CHEMICAL AND

MINERALS ENGINEERING

PROXIMATE PROCEDURE.

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School of Chemical and Minerals Engineering North-West University

The proximate analysis gives an indication of the moisture (air-dry), volatile matter,
fixed carbon and ash in the coal sample. The guideline for this analysis is based on
ISO 17246:2005. The equipment required for the proximate analysis is:
Lab-scale balance (Figure 1).

Figure 1: Lab balance

Two furnaces (Figure 2 and Figure 3).

Figure 2: Furnace A

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School of Chemical and Minerals Engineering North-West University

Figure 3: Furnace B

Crucibles with fitting lids (Figure 4).

Figure 4: Crucible holder with crucibles.

Equipment.
Furnace A.
This furnace is required to operate at relatively low temperature compared to Furnace
B. This furnace is located in Room G09, Building G09. It is fitted with a tray which
allows for accurate temperature measurement of the sample. As shown in Figure 5 the

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School of Chemical and Minerals Engineering North-West University

furnace is on when the little red light is on, and is heating when the little orange light
is on.

Figure 5: Furnace A power buttons.

You can also see how far the furnace temperature is from the setpoint temperature by
looking at the setpoint pointer in Figure 5. If this pointer is in the middle, the furnace
is at its setpoint temperature. The furnace setpoint is changed on the knob as shown in
Figure 5. Note that all temperature readings should be taken from the thermocouple
read-out box as shown in Figure 6.

Figure 6: Thermocouple readout box.

All samples must be placed in the tray as shown in Figure 7, as the thermocouple is
located in this tray.

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School of Chemical and Minerals Engineering North-West University

Figure 7: Sample tray

Furnace B
This furnace is located in Room G09, Building G09. This furnace is capable of
reaching much higher temperatures compared to Furnace A. This furnace is on when
the little red light is on, and is heating when the little orange light is flashing also
shown in Figure 8.

Figure 8: Furnace B power buttons.

This furnace also has a temperature pointer indicating how far the furnace temperature
is from the setpoint temperature as shown in Figure 8. By rolling the little scroller
(Figure 8) downwards the setpoint is increased, and vive versa. When the two little

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School of Chemical and Minerals Engineering North-West University

pointers align, the furnace is on the setpoint temperature. As this furnace does not
have a separate thermocouple as in Furnace A; it was calibrated beforehand and the
required settings are presented in the following sections.

Sample preparation.
Firstly clean two sets of crucibles (4 per set) by washing with water and then flushing
with acetone. Carefully dry the crucibles with lab-paper. Now the crucibles must be
burnt clean. Set Furnace B to a setpoint of 925C (this corresponds to a furnace
temperature of 900C). Once the furnace has stabilized at this setpoint temperature,
put the two crucible holders (each containing 4 crucibles with lids on) into the
furnace. Leave the crucibles in the furnace for 7 minutes ( 5 seconds). Use the
extended pliers (Figure 9) to handle the crucible holders as they will be very hot.

Figure 9: Extended pliers

Place the crucible holders on a thick metal plate (Figure 10) next to the furnace and
allow to cool to room temperature ( 30 minutes). As soon as the crucibles have
cooled down to room temperature, weigh the empty crucibles with lids on (M crucible).
This is called M0. Then weigh 1g ( 0.1g) of coal with a particle diameter of less than
1mm into the crucibles. Mark the crucible with a pencil and remember in which
position you place the crucibles (cracks in the crucible holder work well as reference).

Moisture analysis (ISO 11722:1999).

Take one of the sets of crucibles (4 crucibles) to furnace A. Set this furnace to
approximately 110C, you will see there is a little scratch mark on the furnace next to

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the setting knob which corresponds to this temperature setting. Make sure the furnace
stabilizes at this temperature (110C 5C). Take out the tray part of the sample tray
(Figure 7). Then place the crucibles separately into the box part. Do not put the lids
onto the crucibles. Also remember which crucible is which. Now put the box part
back into the furnace, carefully as not to spill sample or knock over the crucibles.
Leave these samples in the furnace for 3 hours. After 3 hours take the crucibles out of
the furnace, carefully as they are hot, and allow to cool to room temperature on a
metal sheet. When the sample has reached room temperature, weigh the crucibles
again with the lids on. This mass you measure now is the dry mass (M dry). The
moisture percentage can be calculated from:
M 0 M dry
Moisture ( ) 100
M 0 M crucible

Volatile matter (ISO 562:1998)

Take the remaining set of crucibles (4 crucibles left after moisture analysis). To
furnace B. Set this furnace to 925C, as this corresponds to a temperature inside the
furnace of 900C (10C). Once the furnace has stabilized at this temperature, use the
extended pliers to out the crucible holder containing the crucibles with lids on into the
furnace. Close the furnace and leave the crucibles for 7 minutes ( 5 seconds). After 7
minutes remove the crucible holder with the crucibles from the furnace and put them
on the thick metal plate (Figure 10) to cool down, usually this takes approximately 30
minutes.

Figure 10: Thick metal plate for cooling.

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School of Chemical and Minerals Engineering North-West University

Once the crucibles have cooled down to room temperature, weigh them with lids on,
this mass is the devolatalized mass (Mdevol). Now the percentage volatile matter can be
calculated from:

M 0 M devol
Volatiles ( ) 100 % Moisture
M 0 M crucible

Ash and Fixed Carbon (ISO 1171:1997).

Take the same set of crucibles as used for the volatile matter analysis. Set furnace B to
850C, as this corresponds to a furnace temperature of 815C (5C). Once the
furnace stabilizes at this temperature, use the extended pliers to put the crucible holder
containing the crucibles without the lids into the furnace. After one hour, remove the
crucibles and allow to cool to room temperature on the thick metal plate. Then mix
the sample a bit with a spatula to remove the ash layer and mix the remaining carbon
particles. Return the crucible holder with the crucibles without the lids to the furnace,
still at a setting of 850C. Leave the samples for another hour, then remove from the
furnace and allow to cool down to room temperature on the thick metal plate. Again
check for uncombusted carbon particles and mix the sample carefully with the
spatula. Replace the crucible holder with the crucibles, without the lids to the furnace,
still at a setting of 850C and leave for one hour. Finally remove the crucible holder
with the crucibles from the furnace and cool to room temperature on the thick metal
plate. Now all of the carbon should be fully combusted (whitish ash, no black
particles). Weigh the crucibles with lids on, this is M ash. The percentage ash can be
calculated:
M ash M crucible
Ash ( ) 100
M 0 M crucible

The fixed carbon can be calculated by difference:

F / C 100 Ash Volatiles Moisture.

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School of Chemical and Minerals Engineering North-West University

Summary.
The sample for moisture determination should be put into furnace A at 110C
(5C) for 3 hours. The crucible lids must not be on.
The sample for volatile determination must be put into furnace B at 900C
(10C) for 7 minutes and cooled to room temperature on a thick metal plate.
Remember that the crucible lids must be on.
The sample for ash analysis must be put into furnace B without lids for 3
periods of 1 hour each at 815C. The sample must be continuously mixed
between the 1 hour periods after the sample has been cooled to room
temperature on a thick metal plate.

Safety considerations.
Do not handle hot crucibles with bare hands, use the extended pliers.
Make sure furnace wiring is not faulty before starting (no broken wires).
Wear a lab coat.
Wear goggles.
Wear closed shoes.

All weighing should be done on a accurate lab-scale. The preferred balance is in room
G09, building G09 as shown in Figure 1.