Experiment 1: Proximate Analysis of Coal

This is a comprehensive experiment.

This experiment determines the percentages of moisture, ash, volatile matter, and fixed carbon
content in a coal under specified conditions, observes and evaluates the coking properties of
coke. Through this experiment, students will gain an understanding of the principle, method,
steps, instruments and equipment used in the proximate analysis of power coal.
The proximate analysis of coal employs samples air-dried ， and the percentage of each
component by weight is denoted with "ad" (air dry) as sub.

1. Experimental Principle

Fig 1-1 Ash measurement cupel Fig 1-2 Glass weighing bottle for moisture measurement

Fig 1-3 Crucible for volatile matter

Fig 1-4 Crucible tongs Fig 1-5 Crucible frame
determination
A certain mass of coal powder sample, fully dried under laboratory conditions, is taken.
By heating and decomposing the sample at different temperatures, moisture and volatile matter
in the coal are sequentially released. The moisture and volatile matter content based on the air-
dried basis are calculated by the weight loss of the sample. Subsequently, the fixed carbon is
burned out, and the remaining mass is the ash.
2. Experimental Content and Requirements

2.1 Moisture Determination

2.1.1 Key Points of the Method

A certain amount of sample is weighed and placed in an oven at 105~110ºC until it reaches
constant weight. The percentage of weight lost to the original weight of the sample is the
moisture content of the sample.

2.1.2 Experimental Equipment and Instruments

（1） One electric drying oven with an automatic temperature control device, equipped with
a blower, capable of maintaining 105~110ºC.
（2） Glass weighing bottles with ground glass stoppers, 40mm in diameter and 25mm in
height.
（3） One desiccator, containing dessicant (color-changing silicone gel).
（4） One analytical balance with a measuring range of 210g and an accuracy of 0.0002g.
（5） One small spoon.
（6） Ccoal samples with a particle size below 0.2mm.

2.1.3 Experimental Steps:

（1） Make two experimental samples. 1±0.1g of air-dried coal sample (accurate to 0.0002g)
is weighed with a particle size below 0.2mm (previously dried) into a glass bottle and
spread out evenly.
（2） Open the lid of the glass bottle and place bottle and lid into the oven preheated to
105~110ºC for drying. Under blowing conditions, dry bituminous coal for 40 minutes and
lignite or anthracite for 1 hours.
（3） After drying, remove the glass bottle from the oven, immediately cover it, let it cool
in the air for 2~3 minutes, then place it in a desiccator to cool to room temperature (about
20 minutes), and weigh it.
（4） Perform a check weighing for 30 minutes each time until the mass reduction of the
glass bottle does not exceed 0.001g or increases in mass. In the latter case, use the mass
before the increase for calculation. When the moisture content is below 2%, a check drying
is not necessary.

2.1.4 Result Calculation and Allowable Error

m1
M ad  100 (1-1)
m
M ad ——Moisture content of air-dried coal sample, %;
m1——Weight lost after drying the coal sample, g;
m——Weight of the coal sample, g.
Table 1-1 Allowable error in moisture determination:

Moisture M ad (%) Allowable Error in the Same Laboratory (%)

<5 0.20
5~10 0.30
>10 0.40

2.2 Ash Determination

Ash determination is divided into the slow ashing method and the rapid ashing method. The
slow ashing method is the arbitration method; the rapid ashing method can be used as a routine
analytical method. Here rapid ashing method is used.

2.2.1 Key Points of the Rapid Ashing Method:

Weigh 1±0.1g (accurate to 0.0002g) of coal sample and spread it evenly on the bottom of the
cupel. Heat a oven till it’s 850ºC, put the cupel into the oven slowly. When there is no more
black smoke coming out, put the cupel into the isothermal zone, close the door, and burn for 40
mins under 815 ºC ±10ºC.Remove the cupel, and expose it in air, then move it into a desiccator
to cool it till weight’s constant.

2.2.2 Experimental Equipment and Instruments

（1） Box furnace equipped with a temperature regulation device that can maintain a
temperature of 815±10 °C, with a thermocouple.
（2） Cupel (ceramic boat), with a rectangular bottom measuring 45 mm in length, 22 mm
in width, and 14 mm in height.
（3） One desiccator, containing dessicant (color-changing silicone gel).
（4） One analytical balance with a measuring range of 210g and an accuracy of 0.0002g.
（5） One small spoon.
（6） Coal samples with a particle size below 0.2mm.
（7） One crucible tong

2.2.3 Experimental Steps:

（1） Make two experimental samples. 1±0.1g (accurate to 0.0002g) of coal sample is
weighed in an ash dish and spread evenly on the bottom of the cupel.
（2） Place cupels and the coal samples in a row or two rows in sequence at the entrance of
the box electric furnace that has been heated to 850°C, open the furnace door, put the cupel
onto the edge of the furnace slowly, make sure the sample doesn’t burn with flame of
explosion, the coal sample slowly ashifies. After 5-10 minutes, when the coal sample no
longer emits smoke, push the second rows of cupel in sequence into into the isothermal
zone
（3） Close the door, and burn for 40 mins under 815 ºC ±10ºC.
（4） Remove the cupels, Expose in air for 5 minutes, move them into a desiccator to cool
for 20 minutes and weigh them.
（5） Perform a check weighing for 30 minutes each time until the mass reduction of the
cupel does not exceed 0.001g. When ash content is below 15%, the check is not necessary.
2.2.4 Result Calculation and Allowable Error
m1
Aad  100 (1-2)
m
Aad ——ash content of air-dried coal sample,%；
m1——Weight lost after burning the coal sample, g;
m——Weight of the coal sample, g.

Table 1-2 Allowable error in ash determination:

Ash Aad (%) Allowable Error in the Same Laboratory (%)

<15 0.20
15~30 0.30
>30 0.50

2.3 Volatile matter Determination

2.3.1 Key Points of the Method:

Weigh 1±0.1 g of coal sample and put it into a porcelain crucible with a cover. Heat it for 7
minutes at 900±10ºC with isolated air. Take the lost weight as a percentage of the original

weight of the coal sample and subtract the moisture( M ad ) of the coal sample as the volatiles

of the coal sample

2.3.2 Experimental Equipment and Instruments

（1） Box electric furnace, with temperature control device, can be maintained at
900ºC±10ºC, with thermocouple，
（2） Analytical balance: range: 210g, accuracy: 0.0002g.
（3） One desiccator.
（4） Crucible, the crucible is deep and covered, the outer diameter of the upper mouth is
33 mm, the height is 40 cm, the bottom diameter is 18 mm, the total weight of the crucible
is 15 to 20 grams.
（5） Crucible frame: made of nickel wire, its size can be put into the box furnace does not
exceed the constant temperature zone limit, and the crucible bottom is required to be 20~30
mm from the bottom of the furnace.

2.3.3 Experimental Steps:

（1） Make two experimental samples. 1±0.1g (accurate to 0.0002g) of coal sample is
weighed in a crucible, spread the coal sample at the bottom of the crucible and cover it.
（2） Place the crucibles on a crucible frame (see Figure 1-5 for correct installation,
otherwise the width of the support should be adjusted well at room temperature), and then
quickly place the crucible frame into the box electric furnace heated to 920ºC and close
the furnace door for accurate heating for 7min. After the crucible and shelf have just been
put in, the furnace temperature will decrease, and the furnace temperature must be restored
to 900±10 ° C within 3 minutes. The heating time includes the temperature recovery time.
（3） After 7 minutes, remove the crucible frame from the furnace, cool it in the air for 5 to
6 minutes, put crucibles in a desiccator, cool them to room temperature (about 20 minutes),
and weigh them.

2.3.4 Result Calculation and Allowable Error

m1
Vad  100  M ad (1-3)
m
Vad -- Volatile matter content, %
m1——Weight lost after burning the coal sample, g;
m——Weight of the coal sample, g.

Table 1-3Allowable error in volatile matter determination:

Volatile matter content Vad (%) Allowable Error in the Same Laboratory (%)

<20 0.30
20~40 0.50
>40 0.80

Vad
Vdaf  (1-4)
100-M ad  Aad

2.4 Experimental report

（1） Write and submit the experiment report. Please refer to the requirements of the
Academic Affairs Office for the cover sheet format of the experimental report. The content
of the experimental report can be handwritten or printed by computer. Each student writes
an experiment report.
（2） Participate in the experiment process, sign and write the experiment date;
（3） Write and submit the experimental report within one week after the end of the
experiment.
（4） Tables below you will use to record and calculate.
Table1-4 water measurement and calculation card
Weigh 2 samples of 1±0.1g (accurate to 0.0002g) and place them in 2 glass weighing bottles. Dry
at 145℃ for 40 minutes. After taking the sample from the drying oven, cool it in the laboratory
environment for about 5min, cool it to room temperature in a desiccator , and weigh it.
Experimental Parallel samples
Formula postscripts
process 1 2
Mass of the
w 0 ，g
weighing bottle
Mass of the
weighing bottle w 01 ,g
and coal sample
 Mass of the
dried weighing
w 02 ,g
bottle and coal
sample
Original mass of
m01  w 01  w 0 ,g
the sample
Mass of the
m02  w 02  w 0 ,g
dried sample

Mad M ad   m01  m02  / m01 100 ,%

Relative error %
M<5.0% <0.2%
Allowable error in the same lab
5.0%≤M≤10.0% <0.3%

Table 1-5 Ash measurement and calculation card

Weigh 2 samples of 1±0.1g (accurate to 0.0002g) and place them in 2 cupels. Put slowly into a
box furnace which temperature is 850℃. Burn at 815±10℃ for 40 minutes. After taking the
sample from the furnace, cool it in the laboratory environment for about 5 min, cool it to room
temperature in a desiccator , and weigh it.
Parallel samples
Experimental process Formula postscripts
1 2

Mass of the cupel w 0 ，g

Mass of the cupel and

w 01 ,g
coal sample
Mass of the cuple and
w 02 ,g
coal sample after burning
Original mass of the
m01  w 01  w 0 ,g
sample

Mass of the burnt sample m02  w 02  w 0 ,g

Aad Aad  m02 / m01 100 ,%

Relative error %
A<15.0% <0.2%
Allowable error in the same lab
15.0%≤A≤30.0% <0.3%

Table 1-6 Volatile matter measurement and calculation card

Weigh 2 samples of 1±0.1g (accurate to 0.0002g) and place them in 2 crucible. Put quickly into
a box furnace which temperature is 900℃. Heat at 900±10℃ for 7 minutes. After taking the
sample from the furnace, cool it in the laboratory environment for about 5 min, cool it to room
temperature in a desiccator , and weigh it.
Experimental process Formula Parallel samples postscripts
 1 2

Mass of the crucible w 0 ，g

Mass of the crucible

w 01 ,g
and coal sample
Mass of the crucible
and coal sample after w 02 ,g
heating
Original mass of the
m01  w 01  w 0 ,g
sample
Mass of heated
m02  w 02  w 0 ,g
sample

m01 -m02
Vad Vad  100-M ad ,%
m01
Relative error, %
V<5.0% <0.3%
Allowable error in the same lab
5.0%≤V≤10.0% <0.5%

Table 1-7 Fixed carbon measurement and calculation card

Proximate
Parallel samples 1 2 postscripts
analysis
Mad （from Table 1-4）
Aad （from Table 1-5）
Vad （from Table 1-6）

FCad FCad  100  (M ad  Aad  Vad )

Vad
Vdaf Vdaf  100 ，%
Vad  FCad
Relative error, %

3. Attentions

（1） Please bring a notebook and a pen；

（2） please follow the instruction and do every step safely and normatively.
（3） After experiments please restore the experimental bench to the original state, and
clean all tools and equipment used.