7A SOP - Coal Samplin, Preparation & Analysis

VEDANTA LIMITED
ALUMINIUM & POWER, JHARSUGUDA

INTEGRATED MANAGEMENT SYSTEM
DEPARTMENT: QAQC-COAL
WORK INSTRUCTION TITLE: Sampling, Preparation & Analysis of Coal
QA &
PAG
TECH/QA
VER.NO: 02 REV.NO : 00 DATE: 01.01.2020 E 1 OF 35
COAL
LAB/CPP/007A
Management Standard ISO 9001 ISO 14001 ISO 45001
Element Number 8.1 4.4 8.1.3
Element Name Operational Control Operational Control Operational Control
1. PURPOSE : This work instruction is to define the step-by-step activity involved in the
sampling of coal.
2. SCOPE: This instruction covers the manual sampling of coal to get representative gross
sample during wagon unloading in steady motion, truck sampling, preparation of final sample and
proximate analysis at plant and GCV.
3. REFERENCES : IS 436(Part 1 & Part 2) Method for manual sampling of coal

IS 1350(Part 1 & Part 2) Method for proximate analysis of coal
ASTM D 2234-00 Standard Practice for collection of gross sample of coal
ASTM 2013-00 Standard Practice for preparing coal samples for analysis .
4. DEFINITION : NIL
5. ANNEXURE : NIL
Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
6. DISTRIBUTION: Head (QA), DCIC, MR (VAJ)
7. AMENDMENT HISTORY
Sl no. Amendment Description Current Ver. No. Current Rev.No Issue Date
1 Truck sample preparation procedure
00 01 10.02.2016
changed
2 DROP BOX for BOBRN rake sampling 00 01 15.09.2016
3 Company Name & Logo changed 00 01 01.06.2017
4 BOXN Sampling procedure changed 00 01 13.02.2018
5 Updating from OHSAS 18001:2007 to
00 01 01.01.2020
ISO 45001:2018

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
8. WORK INSTRUCTIONS:
COAL:
1.1 Principle:
Sampling without reduction of grain size manually according to the circumstances. Storage in close
packed bags. The sample shall remain in the same physical and chemical state in which it is found at
the time sampling until the time of its laboratory examination.
1.2 Apparatus:
3.1 Pointed shovels
3.2 Flat shovels
1.2.3 Clean and sound bags
1.2.4 Polythene bags of 2 kg capacity
1.2.5 Labels
1.2.6 Threads
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
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TECH/QA
COAL
LAB/CPP/007A
1.2.7 Seals
TYPE OF COAL NORMAL SIZE
Run of Mine(ROM) 0 to 230 mm
Coal Large 50mm to 150 mm
Coal Small 0 to 50mm
Consignment size: Over 3000 MT for Rakes and 10MT for Trucks.
1.3 Sample collection from RAKE:-
1.3.1 Sampling Point: Track Hopper (Rake)
Increments shall be collected from bottom discharge point in case of BOBRN boxes & for N type
wagons during the course of progressive unloading or from the top of Wagons in case of Wagon
Tippler.
1.4 Procedure: 25% of the wagons shall be selected as per random table (enclosed herewith) as per
Table 2 (given in IS: 436(PART 1/SEC 1)). Therefore, minimum 18 wagons out of total 58 or 59
wagons have to be selected for each time.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
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TECH/QA
COAL
LAB/CPP/007A
After collection sample should be sealed in plastic bags.
RANDOM NUMBER TABLE

(Reference: IS: 436 (Part I/See 1) Clause A-2.1)
81 74 67 95 70 56 51 54 50 53
61 37 42 62 93 96 34 18 22 89
52 7 16 29 39 4 71 14 76 78
43 8 77 25 72 49 86 3 83 45
65 32 27 40 63 57 97 84 82 87
21 58 11 23 80 10 30 1 100 44
31 90 55 88 13 36 24 91 19 64
73 98 20 5 68 46 69 85 94 59
33 15 35 26 79 92 38 12 41 17
75 66 99 9 6 47 48 60 28 2
1.4.1 The coal getting discharged from bottom opening wagons, a Drop Box is to be used for
collecting the sample during unloading process.
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
DROP BOX DESIGN:- As shown in Figure 1, Drop box is to be made of mild steel with dimensions
90cm x 60 cm x 30 cm and of at least 5mm thickness. It shall be supported by handles on 4 sides.
30cm
60cm
Direction to use the DROP BOX
- In the case of a BOBRN wagon, the operator is to first place a mat on the grates beside the
wagon. He should then step on the mat and place the drop box directly below the wagon. The
doors of the wagon are then to be opened, and once the box is filled with coal, the operator is to
remove the box using the handles provided.
- In the case of a BOXN wagon, while sampling from the top of the wagon, shovel is to be used for
sample collection and sampling should be carried out in a single location sampling point which is
placed at wagon tippler.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
1 . Samples shall be drawn from three locations from each selected wagon to a depth of minimum
50 cm from the surface towards the bottom of the rake. One increment shall be drawn from each
point by making a diameter of not less than 30 cm.
Weight of Gross Sample and Number of Increments for Wagons:
Sl No. Sample ROM Coal Coal, Large Coal, Small
1 Weight of Gross Sample, Min 350 Kg 175 Kg 75 Kg
2 Weight of Increment (Approx.) 7 Kg 7 Kg 5 Kg
3 Number of Increments, Min per lot 50 25 15
2. Quantity collected for each wagon should be minimum 20-25 Kg.
3. In the case of bigger lumps it should be collected and crushed separately and increments shall be
drawn correspondingly from the crushed material.
4. The bags are tied airtight and a tag to be fixed after entering the relevant details. The bags are
sealed immediately with a unique digit code after the sampling and before handing over to the
person responsible for the transportation of the samples to the preparation site.
1.5 SAMPLE COLLECTION FROM TRUCK (MANUAL)
1.5.1. In order to get the representative gross sample, coal samples should be collected as far as
possible from Sampling Points/Augur Sampling Machine during standstill condition of truck before
unloading or progressively during unloading at coal yard or truck tippler.
1.5.2. Sample is to be collected from each and every truck.
1.5.3. Sampling is to be carried out separately for mine wise transporter wise basis.
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
1.5.4. Before sampling, Challan paper of each truck has to be scanned through bar code scanner.
1.5.4. Increment should be collected with the help of scoop/ shovel depending upon the size and
type of coal at regular intervals at the time of Sampling of each truck by digging 30 cm and collecting
samples from three different location of a truck forming a triangle.
1.5.5. An approximate quantity of approx. 9 KG (3 Scoop) gross sample per truck will be drawn for
both TM (2 KG) and Quality (7 KG) analysis.
1.5.6. If contamination or stone mixed coal is observed details should be maintained in the provided
format (Annexure: 1).The same needs to be communicated on daily basis to commercial for their
record and further action.
1.5.7. The bag is to be airtight and a tag to be fixed after entering the relevant details. The bags are
sealed immediately after the sampling.
1.5.8. Samples from 3 trucks in case of dala body trucks are to be kept in a bag in case of Vedanta,
Jharsuguda as the receipt is more.
1.5.9. For a particular mines and transporter, whatever quantity is received within a day will
represent a lot (For a particular lot, maximum quantity is 1100).
1.5.10. Serial number is to be given during the preparation of representative samples for a lot. All the
quantity details must be recorded.
1.5.11. In case of Multiaxle truck , increment shall be drawn with the help of scoop/ shovel
depending upon the size and type of coal at regular intervals at the time of Sampling of each truck
by digging 30 cm and collecting samples from five different location of a truck. Samples from 2
trucks are to be kept in a bag.
1.6 SAMPLE COLLECTION FROM TRUCK (AUGER)( Ref: WI-LAB/003)
1.6.1. The truck is to be placed at auger sampling point before unloading at coal yard.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
1.6.2. The auger operator needs to collect the Challan paper from the truck driver and note down the
relevant details.
1.6.3. The boom of the auger is inserted in the truck to pick the coal.
1.6.4. The sampling should be carried out in a random manner collecting sample from any one point
of the truck. But the same point should not be repeated for each and every truck.
1.6.5. The Auger operator has to ensure that he is not inserting the boom of the Auger at the same
location every time.
1.6.6. Sample should be collected in the container separately mines wise.
1.6.7. For a particular mines and transporter, whatever quantity is received within a day will
represent a lot (For a particular lot, maximum quantity is 1100).
1.6.8. Once the sample is collected from the auger and crushed to 12.5 mm by the crusher installed
in the Auger, the samples are sealed and shifted to sample preparation room.
1.6.9. Sample obtained from Augers and manual samplings are to be tested separately.
1.7 Sample Preparation:
INDIAN COAL
1.7.1. Plant QAQC shift in charge in collaboration with the third party has to ensure that the entire
sample preparation process is to be carried out as per IS 436 for Indian coal and ASTM
D2013/D2013M for Import coal.
1.7.2. Sample preparation shall be carried out as per procedures by using primary and secondary
crusher and hammer mill pulverizer.
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
1.7.3. In case the sample is collected through an auto sampler or an auger with a crusher installed,
the sample size shall be 12.5 mm already so there is no further crushing required.
1.7.4. However, in case the sample was obtained through a drop box or manually from rake and
truck, the gross sample shall be crushed to 5 cm, preferably by mechanical means. Sample is to be
crushed at once to 30 mm in case of Indian coal and 4.75 mm in case of Import coal.
1.7.5. In case of rake, all the 18 bags need to be mixed together and then divide it into two sub lots.
In case of truck sample, the bags collected for a particular mines and transporter represent one lot.
1.7.6. Preferably pass the entire gross sample through 30 mm crusher. 2 kg of moisture sample
should be obtained after coning and quartering through rotary divider. However, if encounter with
boulders and higher size coal, the gross sample shall be crushed to 5 cm, mixed thoroughly and
quartered. The retained material shall be further mixed and quartered. The material so obtained
shall be crushed to 12.5mm by jaw crusher. The moisture sample should be packed in covers and
sealed with LIMS generated alphanumeric code (Ref: WI-LAB-013) and should be sent for
determination of moisture to the lab.
1.7.7. Reduce the quantity by riffle divider/rotary divider and then passed through the secondary
crusher to obtain NTS 3.35 mm fraction.
1.7.8. The 3.35 mm fraction is reduced by riffle divider air dried if necessary before pulverization.
Pulverize the entire NTS 3.35 mm fraction (around 400g) and pass through 212-micron sieve.
1.7.9. The pulverized samples are then carried to lab in a locked box. The box should be opened by
QAQC representative in the lab and shall be air dried in air drying cabinets. The cabinets should be
capable of maintaining a temperature of 10 to 15ºC above ambient temperature with a maximum
oven temperature of 40ºC..

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
Reduction of Gross Samples
ORIGINAL >5cm
(-) 5cm
(Preferably Mechanical)
Reduce to half quantity by riffle divider / incremental reduction and
use the half portion for analysis sample preparation
2kg Sample for Crush entire

Moisture Sample to <NTS12.5mm Size
Crush entire
Sample to
<NTS12.5mm Size Divide and reduce to half quantity by riffle
divider / incremental reduction
Pass entire through secondary crusher to get NTS3.35

10kg Sample
mm size fraction to min 3kg, divide the sample
for Reference
Air-dry if necessary Then Pulverize to get 212m size fraction, divide the
2Kg Sample
sample to min 400g
for reference
Sample-1 Sample-2 Sample-3 Sample-4

@100 Grams @100Grams @100 Grams @100Grams
Analysis Part Referee Part Referee CL Referee Shipper

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
IMPORT COAL
1. Sample preparation shall be carried out as per procedures by using primary and secondary
crusher and hammer mill pulverizer.
2. Pass the entire gross sample through primary crusher and reduce to 4.75 mm size. Thoroughly
mix the crushed sample and divide by rotary divider and prepare 2 kg moisture sample. The
moisture sample should be packed in covers and sealed and should be sent for determination
of moisture.
3. The entire quality sample is passed through primary crusher to get NTS of 4.75 mm.
4. Reduce the quantity by riffle divider/rotary divider and then passed through the secondary
crusher to obtain NTS 2.36 mm fraction.
5. The 2.36 mm size sample is further reduced by riffle divider and air dry if necessary before
pulverizing. Pulverize the entire NTS 2.36 mm fraction (around 400g) and pass through 250
micron sieve.
6. The pulverized samples shall be air dried in air drying cabinets. The cabinets should be
capable of maintaining a temperature of 10 to 15ºC above ambient temperature with a
maximum oven temperature of 40ºC. In case of highly oxidize coal the temperature should
not be more than 10ºC above ambient temperature.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
Reduction of Gross Samples
ORIGINAL >5cm
(-) 5cm
(Preferably Mechanical)
Reduce to half quantity by riffle divider /

incremental reduction and use the half portion for
analysis sample preparation
Crush entire
2kg Sample for Sample to <NTS 4.75mm Size
Moisture
Crush entire
Sample to <NTS Divide and reduce to half quantity by riffle
4.75mm Size divider / incremental reduction
10kg Sample Pass entire through secondary crusher to get NTS

for Reference 2.36 mm size fraction to min 3kg, divide the sample
2Kg Sample Air-dry if necessary Then Pulverize to get 250m size fraction, divide
for reference the sample to min 400g
Sample-1 Sample-2 Sample-3 Sample-4

@100 Grams @100Grams @100 Grams @100Grams
Analysis Part Cross check Cross check at Referee
FORM:MRJ/DOC/01-01 other lab
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
Annexure-1:
Daily contaminated trucks format:
Declaration
The following Vehicles with their respective identities have been observed to bring foreign materials
along with coal , the visible severity has been marked in the respective column. The vehicles were
being detained and the identity of the vehicles was communicated to the Coal Commercial Team,
upon whose consent the vehicles were allowed further movement for unloading. On certain cases,
Special Sample has been taken on mutual agreement with Coal Commercial Team.
Sl. PO. Sign for Informed Severity (%)

Vehicle No. Transporter
No. No. Transporter to CMT 0-30 30-60 60-100

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
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TECH/QA
COAL
LAB/CPP/007A
1.9 Sample preparation procedure:
Refer point 1.7
1.9.1 Samples distribution:
- At 3.35mm stage, 2 kg sample shall be retained by third party for reference purpose.
- At 12.5 mm stage, 10 kg sample shall be retained for central lab for rechecking purpose.
- At 212 µ stage, PO wise / Party wise for single Lot – 4 analysis samples to be prepared @
100Grams each
- Out of four packets
o One for Third party – Jharsuguda for Analysis.

o One for ILC
o One for CPP/IPP/Balco for cross check (if required).
o One sample for reference of 3 months.
2.0 SAMPLE STORAGE AND DISPOSAL
Record to be maintained by third party sampling agent for all incoming coal consignments. All
samples should be preserved properly in a secure place. The other lab in plant may randomly cross
check the preserved samples.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
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TECH/QA
COAL
LAB/CPP/007A
The retention period of 30 mm sample is till report declaration, 3.35 mm & 12.5 mm is for one month
and 212 µ is for 3 months and record need to be maintained with signature for disposal. Any sample
can be rechecked anytime in Lab or by any Standardized lab by approval of HOD.
3.0 SAFETY - MAJOR FACTOR:

a. Proper illumination near the sampling area should be there.
b. Safe and secure path is to be given so that movement of the trucks and people won’t get affected.
c. Ensure handrails at the stair case so as to prevent slip of a person climbing into the sampling point.
d. Dust control activities like sprinkling of water should be done.
e. Proper PPE’s by the people in the working area is to be maintained.
f. Care must be taken that HDPE bags containing coal are properly labelled and need to be shifted to
the preparation site safely.
g. Proper care must be taken while stepping out of the truck after sampling. [ ROU: 2.1,2.2; Refer WI-
LAB/013]
h. Boulders at rake unloading area should be removed regularly to avoid accident or hitting of a
person. [ ROU: 3.1; Refer WI-LAB/013 ]
i. Care should be taken and proper training should be given to person for hammering and crushing of
coal samples.
Procedure for performing laboratory tests

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
a) On receipt of the sample at laboratory, the chemist should verify the seal and tag of the sample
received.
b) While performing the tests, the crucibles and other apparatus being used should be identified with
the sample being tested.
c) The analysis should be performed by the chemist who was not involved in sample collection and
preparation.
d) The register used for test results recording should also contain details of the person who has
performed the tests and who all have witnessed the tests.
e) Based on the results entered in the register, a test report should be prepared.
f) The report reference number should be maintained in the register. All plants to graduate to LIMS.
g) Report should be declared within 72 hours from the time of sampling.
4. SAMPLE ANALYSIS
4.1 For Indian coal
DETERMINATION OF TOTAL MOISTURE IN COAL SAMPLE

Ref: IS 1350 (Part -1)
Definition: The coal, which has been exposed to contact with water in seam or in a washery, or coal
or coke wetted by rain may carry free or visible moisture. This water plus the moisture within the
material is referred as Total Moisture.
Apparatus:

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
1) Air oven- Ventilated drying oven in which a constant and uniform temperature of 108± 2 degree
Celsius can be maintained.
2) Non corrodible or S.S Tray of approx. 1,000 sq.cm in area and 5 cm in depth.
3) Weighing vessel.
Procedure
Determination of TM is carried out in two stages i.e. Air drying followed by Oven drying.
A) Air drying
1. Let the weight of the moisture free empty dry tray be W1 g.
2. Take about 1 kg of 12.5 mm coal samples and spread it uniformly in the tray. Let the weight of
tray + sample is W2 g.
3. Allow the samples in the tray to air dry at atmospheric temperature in a well-ventilated place
free from dust.
4. Leave the samples for air drying for 24 hours. Let the weight of the tray + sample be W3 g
after air drying.
5. Calculation:
The percentage loss in mass of the original sample in air-drying
(Air Dry Loss, ADL), x =100*(W2-W3)/ (W2-W1)
B) Oven drying
1. Heat the empty capsule at 108 +/- 2 0C and weigh after cooling. Let the weight of the empty
capsule be M1 gm. Crush the air-dried sample to pass through 2.90 mm sieve.
2. Spread about 10 gm of 2.90 mm samples uniformly in the capsule. Let the weight of the
(capsule + sample) be M2 gm before heating.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
3. Note the time and place the uncover capsule in the hot air oven at 108 +/- 2 0still constant
weight is obtained (it will take approx. 2 hours)
4. Remove the capsule from the air oven, replace the cover, cool in desiccators for 20 minutes
and weigh. Let the weight of (capsule + sample) be M3 gm after heating.
5. The percentage loss in mass of the air-dried sample on oven drying

(Residual Moisture) % Y=
100 x (M2 – M3)
(M2– M1)
6. Calculation:
Total Moisture % = X + Y [1 – (X/100)]
DETERMINATION OF TOTAL ASH CONTENT IN COAL SAMPLE

Ref: IS 1350 (Part -1)-1984
Description:
Ash content of coal is the non-combustible residue left after coal is burnt. It represents the
bulk mineral matter after carbon, oxygen, sulphur, water has been driven off during combustion.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
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TECH/QA
COAL
LAB/CPP/007A
Apparatus:
1) Muffle Furnace
2) Silica Dish
Procedure:
Step 1: The final prepared sample is air dried in air drying cabinets till constant wt (time)
Step 2: Weigh a clean and dry empty dish. Let its weight be W1 gm.
Step 3: Approximately weigh about 1gm of the sample and let the weight of the
(Dish+ash) be W3 gm
Step 4: Then insert the dish into the muffle furnace at 500 °C for 30 min from cold
raised to 815±10°C in a further 30 to 60 minutes and maintain the temperature for
60 minutes.
Step 5: Then remove the dish from the furnace and then allow it to cool. Let the weight of
the (dish + ash) be W3 gm.
CALCULATION:
The ash content of the sample on air dried basis is to be calculated as per following
formula:
Ash % = W3 – W1 × 100
Sample Weight

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
DETERMINATION OF VOLATILE MATTER IN COAL SAMPLE

Ref: IS 1350 (Part -1)-1984
Definition:
The volatile matter refers to components of coal which are liberated at high temp. in the
absence of air. Usually a mixture of short & long chain hydrocarbon, aromatics hydrocarbons and
some sulphur.
Apparatus:
1) Crucible and lid.
2) VM Stand.
3) Muffle furnace.
Procedure:
Step –1: The final prepared sample is air dried in air drying cabinets
Step- 2: Let the weight of (empty crucible + lid) be W1 gm.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
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TECH/QA
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LAB/CPP/007A
Step- 3: Take about 1 gm and spread it uniformly in the crucible.

Let the weight of the (sample + crucible+ lid) be W2 gm
Step- 4: Place the sample with crucible and lid in the muffle furnace.
Heat it for exactly 7 minutes at a temperature of 900 ± 10 °C
Step- 5: Remove the crucible. Then cool it for 20 minutes and then weigh it.
Let the weight of the (sample+crucible+lid) be W3 gm.
CALCULATION:
The Volatile matter of the sample on air dried basis is to be calculated as per the following formula:-
VM % = [ W2 - W3 × 100] - % of Inherent Moisture

Sample weight
DETERMINATION OF INHERENT MOISTURE IN COAL SAMPLE

Ref: IS 1350 (Part -1)-1984
Description:
Inherent Moisture means moisture that exists as an integral part of the coal seam in its
natural states, including water in pores, but excluding that present in macroscopically visible
fractures, as determined. It is the moisture in coal which has been air-dried under air drying cabinets
condition prior to analysis and is determined as a part of proximate analysis.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
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TECH/QA
COAL
LAB/CPP/007A
Apparatus:
1) Air Oven
2) Weighing Vessel
3) Crucible
Procedure:
Step 1: The prepared sample is first air dried in air drying cabinets.
Step 2: Let the weight of empty crucible be W1 gm.
Step 3: Take about 1 gm sample and spread it uniformly. Let the weight of (crucible +
sample) be W2 gm before heating.
Step 4: Note the time and place the uncover crucible in the hot air-oven at 110 degree Celsius.
Step 5: Remove the crucible from the air-oven, replace the cover, cool in a desiccator for 20
minutes and weigh. Repeat the process till constant weight is obtained. Let the weight of ( crucible +
sample ) be W3 gm after heating.
CALCULATION:
The inherent moisture of the sample on air dried basis is to be calculated as per following formula:
Inherent moisture, IM % = W2 - W3 × 100

Weight of sample

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
DETERMINATION of GCV (Gross Calorific Value)
1.1. Apparatus:
1.1.1. Analytical Balance
1.1.2. Hand gloves
1.1.3. Distill water
1.1.4. Soft Tissue Paper
1.2. Procedure:
Sample Weighing:
1.2.1. Place the crucible in the centre of weigh pan inside of the balance.
1.2.2. A thin disc of mica or a layer of fine ignited sand, silica or powdered quartz should be placed
on the bottom of the crucible of a known weight say 0.01 to 0.03 gm. Mica, sand, silica or
powdered quartz acts as an accelerator which increase the combustion rate as coal contain high
percentage of inorganic matter give a fused residue which may enclose a considerable
proportion of unburnt carbon.
1.2.3. Add the sample to the crucible.
1.2.4. Record the weight from the balance.
Analysis Procedure:
1.2.5. Prepare the combustion vessel.
(Fill the bucket with water and then put the bomb in the combustion vessel bucket and cover
it with combustion vessel bucket lid.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
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TECH/QA
COAL
LAB/CPP/007A
1.2.6. Login sample weight and id.

1.2.7. Click the sample menu and select Analyse to start analysis.
1.2.8. During the Pre-Fire, the current bucket temperature will be displayed in the lower right
corner of the status bar. The timer left before ignition is displayed in the lower left corner of the
status bar. Six seconds before ignition a beeper will sound and a message will flash (lower left
corner) warning the operator to stay away from the calorimeter.
1.2.9. During post fire, the bucket water temperature will be displayed in the lower right corner of
the status bar. In the lower left corner of the status bar will be displayed the time remaining for
analysis.
1.2.10. If it’s necessary to abort an analysis, an “Abort” will appear under analysis date. From the
sample menu, click Abort. The analysis in progress will be aborted.
1.2.11. After an analysis is complete, lift the combustion vessel bucket lid to the 60° vertical position
so that droplets from the stirrer and thermistor will not fall onto the jacket insulation. Hold a
cloth under the stirrer and dry the blade and thermistor probe. Do not allow any water to drip
onto the insulation.
1.2.12. Open the combustion vessel bucket lid completely.
1.2.13. Disconnect the combustion vessel fuse leads and dry them with a cloth. Drape the leads
outside the jacket. The insulation must be kept dry or the instrument precision will degrade.
Calculation:
GCV in DB: GCV (ADB)*100/ (100-IM)

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
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COAL
LAB/CPP/007A
GCV in ARB: (100-TM)/ (100-IM)*GCV
4.1 For Import coal
DETERMINATION OF TOTAL MOISTURE IN COAL SAMPLE

Ref: D 3302
Definition: The coal, which has been exposed to contact with water in seam or in a washery, or coal
or coke wetted by rain may carry free or visible moisture. This water plus the moisture within the
material is referred as Total Moisture.
Apparatus:
1) Air oven
2) Air drying cabinet
3) Non corrodible or S.S Tray of approx. 1,000 sq.cm in area and not more than 25 mm in depth.
4) Weighing vessel.
Procedure:

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
Step-1: a) Floor drying:- This procedure is applicable if the gross moisture sample is too wet to
handle. Weigh and record the weight of the gross moisture sample. Let the weight of the tray be W1
and the weight of the tray and sample be W2
b) Keep the trays with the sample on the drying floor. Continue the air-drying till the surface of
the sample appears dry. Repeat the entire process weighing sat 1 to 2 hr intervals until the weight
loss of the total sample becomes not more than 0.1%. Weigh the entire sample and record the
weight as W3.
Step-2: a) Air drying cabinet- Distribute the 4.75mm crushed sample into the tray (refer to-7.1)
Let the weight of the tray be W4. Let the weight of the tray and sample be W5.
b) Place the trays in air drying cabinet and maintain temperature not more than 40° C. Continue
drying with intermittent stirring until the coal appears to be dry. Remove from cabinet, weigh and
record the weight. Return the pan with the sample to the cabinet and continue the operation.
Calculate the % weight loss. Repeat the drying and weighing process at 1 to 2hrs intervals until the
weight loss is less than 0.1%.Allow the sample to reach equilibrium with ambient temperature and
humidity before the final air dry weight is recorded. Take out the tray and cool in desiccators for 20
minutes and weigh.
Let the final weight of (tray + sample) be W6 gm.
Step-3:- Oven Drying:- Distribute the 2.36 mm size sample over the trays. Let the weight of the
tray be W7gm and weight of the tray and sample be W8gm. Place the tray in a preheated oven at
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
107±3 °C. Heat it for one hour and cool it and record the weight. Repeat the process till the constant
weight is achieved. Let the final weight be W9gm.
CALCULATION:
Calculate the total moisture, M when two stage of air drying has been used.
At 12.5mm stage:-
ADL % = W2 - W3 × 100
Sample weight
Where ADL = air dry loss of uncrushed gross sample.
At 4.75mm stage :-
ADL’ % = W5 - W6 × 100
Sample weight
Where ADL’ = air dry loss in the air drying cabinet.
At 2.36mm stage:-
R% = W8 - W9 × 100
Sample weight
M’ = ADL’+ R (100-ADL’)/ 100
Where M’ = moisture in crushed and divided laboratory sample.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
M= ADL+M’ (100-ADL)/100
Where M= TOTAL MOISTURE
DETERMINATION OF TOTAL ASH CONTENT IN COAL SAMPLE

Ref: ASTM D 3174
Description:
Ash content of coal is the non-combustible residue left after coal is burnt. It represents the
bulk mineral matter after carbon, oxygen, sulphur, water has been driven off during combustion.
Apparatus
1) Muffle Furnace
2) Porcelain Capsules
3) Balance
Procedure:
Step 1: Weigh a clean and dry empty dish. Let its weight be W1 gm.
Step 2: Approximately weigh about 1gm of the prepared sample of 60 meshes and let the
weight of the (Dish+sample) be W2 gm
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
Step 3: Then insert the dish into the muffle furnace and heat gradually at such a rate that the
temperature reaches 450-500°C in 1 hour and then further heat coal sample so that
the final temperature of 700-750°C is reached by the end of second hour.
Step 4: Then remove the dish from the furnace and allow it to cool. Let the weight of
the (dish + ash) be W3 gm.
CALCULATION:
The ash content of the sample on air dried basis is to be calculated as per following
formula:
Ash % = W3 – W1 × 100
Sample Weight
DETERMINATION OF VOLATILE MATTER IN COAL SAMPLE

Ref: ASTM D 3175-07
Definition: The volatile matter refers to components of coal which are liberated at high temp. in the
absence of air usually a mixture of short & long chain hydrocarbon, aromatics hydrocarbons and
some sulphur.

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
Apparatus:
1) Crucible
2) VM Stand.
3) Vertical tube furnace.
Procedure:
Step- 1: Let the weight of (empty crucible + lid) be W1 gm.
Step- 2: Take about 1 gm of the 250µm pulverized sample and spread it uniformly in the
crucible. Let the weight of the (sample + crucible+ lid) be W2 gm
Step- 3: Place the sample with crucible and lid in the vertical furnace.
Heat it for exactly 7 minutes at a temperature of 950 ± 20 °C
Step- 4: Remove the crucible. Cool it and then weigh it.
Let the weight of the (sample+crucible+lid) be W3 gm.
CALCULATION:
The Volatile matter of the sample on air dried basis is to be calculated as per the following formula:-
VM % = [ W2 - W3 × 100] - % of Inherent Moisture

Sample weight
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
DETERMINATION OF INHERENT MOISTURE IN COAL SAMPLE
Ref: D 3173-03
Description: Inherent Moisture means moisture that exists as an integral part of the coal seam in its
natural states, including water in pores, but excluding that present in macroscopically visible
fractures, as determined. It is the moisture in coal which has been air-dried under air dry cabinets
condition prior to analysis and is determined as a part of proximate analysis.
Apparatus:
1) Air Oven
2) Weighing Vessel
3) Silica Crucible
Procedure:
Step 1: Let the weight of empty crucible be W1 gm.
Step 2: Take about 1 gm of the prepared 60 mesh sample and spread it uniformly. Let the
weight of (crucible +sample) be W2 gm before heating.
Step 4: Note the time and place the uncover crucible in the hot air-oven which is capable of
temperature regulation between the limits of 104 - 110 degree Celsius for 1 hour.
Step 5: Remove the crucible from the air-oven, and cover it with the lid. Cool it for sometimes
in the desiccator and weigh. Repeat the process till constant weight is obtained. Let
the weight of (crucible + sample) be W3 gm after heating.
CALCULATION:
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
The inherent moisture of the sample on air dried basis is to be calculated as per following
formula:
Inherent moisture, IM % = W2 - W3 × 100
Weight of sample
Reporting of Results
Purpose & Scope: Reporting of analysis results
Reference: IS: 1350 (Part 1/SEC 9.2) – 1984 (Reaffirmed 2007).
Procedure: The results of proximate analysis and calorific value of coal are reported in as received
basis / Equilibrated basis.
The results of parameters may be reported in the following manner.
Parameters Air Dried Basis As Received Basis

T. M. -- M1
I. M. M --
Eq.M. Eq M --
A x (100 – M1)
A1 = -------------------
ASH A (100 – M)

FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A
V x (100 – M1)
V1 = -------------------
V. M. V
(100 – M)
F x (100 – M1)
F1 = -------------------
F. C. F
(100 – M)
Q x (100 – M1)
Q 1 = -------------------
GCV Q
(100 – M)
Q x (100 –Eq M)
GCV Qe 1 = -------------------
Qe
Equilibrated (100 – M)
Sample Storage and Disposal

Sample Size 212 micron should be store for 90 days or as per requirement. Any sample can be
rechecked anytime in Lab or by any Standardized lab with the approval of HOD.
Sample should be disposed with approval of HOD and should be recorded.
Safety:
The work Coal sampling, preparation and testing should be strictly complied with relative rules and
should be supervised.
Flushing water and first aid medicine should be available at site.
Always wear proper hand gloves, Heating Gloves, nose mask, safety googles and safety shoes during
handling of coal sampling and preparation.
Reporting of near miss, unsafe act and unsafe condition.
FORM:MRJ/DOC/01-01
VEDANTA LIMITED
QA &
PAG
TECH/QA
COAL
LAB/CPP/007A

FORM:MRJ/DOC/01-01

7A SOP - Coal Samplin, Preparation & Analysis

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VEDANTA LIMITED

ALUMINIUM & POWER, JHARSUGUDA

Management Standard ISO 9001 ISO 14001 ISO 45001

Element Number 8.1 4.4 8.1.3

Element Name Operational Control Operational Control Operational Control

proximate analysis at plant and GCV.

3. REFERENCES : IS 436(Part 1 & Part 2) Method for manual sampling of coal

ASTM D 2234-00 Standard Practice for collection of gross sample of coal

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

6. DISTRIBUTION: Head (QA), DCIC, MR (VAJ)

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

1.2.4 Polythene bags of 2 kg capacity

TYPE OF COAL NORMAL SIZE

Run of Mine(ROM) 0 to 230 mm

Coal Large 50mm to 150 mm

Coal Small 0 to 50mm

1.3 Sample collection from RAKE:-

1.3.1 Sampling Point: Track Hopper (Rake)

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

After collection sample should be sealed in plastic bags.

RANDOM NUMBER TABLE

Direction to use the DROP BOX

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

Weight of Gross Sample and Number of Increments for Wagons:

Sl No. Sample ROM Coal Coal, Large Coal, Small

1 Weight of Gross Sample, Min 350 Kg 175 Kg 75 Kg

2 Weight of Increment (Approx.) 7 Kg 7 Kg 5 Kg

3 Number of Increments, Min per lot 50 25 15

2. Quantity collected for each wagon should be minimum 20-25 Kg.

1.5 SAMPLE COLLECTION FROM TRUCK (MANUAL)

1.5.2. Sample is to be collected from each and every truck.

1.6 SAMPLE COLLECTION FROM TRUCK (AUGER)( Ref: WI-LAB/003)

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

1.6.6. Sample should be collected in the container separately mines wise.

1.7 Sample Preparation:

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

Reduction of Gross Samples

2kg Sample for Crush entire

Pass entire through secondary crusher to get NTS3.35

Sample-1 Sample-2 Sample-3 Sample-4

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

Reduction of Gross Samples

Reduce to half quantity by riffle divider /

10kg Sample Pass entire through secondary crusher to get NTS

Sample-1 Sample-2 Sample-3 Sample-4

Daily contaminated trucks format:

Sl. PO. Sign for Informed Severity (%)

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

1.9 Sample preparation procedure:

Refer point 1.7

1.9.1 Samples distribution:

- Out of four packets

o One for Third party – Jharsuguda for Analysis.

2.0 SAMPLE STORAGE AND DISPOSAL

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

3.0 SAFETY - MAJOR FACTOR:

d. Dust control activities like sprinkling of water should be done.

e. Proper PPE’s by the people in the working area is to be maintained.

Procedure for performing laboratory tests

Prepared by: IMS Co-ordinator Reviewed by: HOD Approved by: MR

g) Report should be declared within 72 hours from the time of sampling.

4.1 For Indian coal