Reference TOTL-WI-02

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 01 April 19

Author / Approver M.Saleh / M. Abd Elrazek
Determination of Ash in Coal
Page n° Page 1 of 6

Author Reviewed & Approved By

Name Mohamed Saleh Mohamed Abd Elrazek

Position Technical team leader TOTL Manager

Signature
Date 01/04/2019 01/04/2019

Control of Amendments

Issue Amendments Echoed

Date Reason for amendments
No. Summary Pages
0.0 01.04.2019 First issue - -
1.0
2.0
3.0
4.0
5.0

Review Frequency : Annually.

 Reference TOTL-WI-02

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 01 April 19

Author / Approver M.Saleh / M. Abd Elrazek
Determination of Ash in Coal
Page n° Page 2 of 6

Contents
1.0 Scope .................................................................................................................................. 3
2.0 Definitions of Terms .......................................................................................................... 3
3.0 References .......................................................................................................................... 3
4.0 Responsibility .................................................................................................................... 3
5.0 Summary of Test Method .................................................................................................. 3
6.0 Associated Documents ....................................................................................................... 3
7.0 Apparatus ........................................................................................................................... 4
8.0 Reagents and Materials ...................................................................................................... 4
9.0 Sampling and Test Specimens ........................................................................................... 4
10.0 Procedure ........................................................................................................................... 4
11.0 Quality Control .................................................................................................................. 5
12.0 Report................................................................................................................................. 5
13.0 Precision and Bias .............................................................................................................. 5
13.1 Repeatability ...................................................................................................................... 5
13.2 Reproducibility .................................................................................................................. 6
14.0 Equipment Maintenance .................................................................................................... 6
15.0 Records .............................................................................................................................. 6
 Reference TOTL-WI-02

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 01 April 19

Author / Approver M.Saleh / M. Abd Elrazek
Determination of Ash in Coal
Page n° Page 3 of 6

1.0 Scope
1.1 Test method covers the determination of Ash in Coal.

2.0 Definitions of Terms

2.1 Ash: The remaining after coal has been incinerated in air is derived from
inorganic complexes present.

3.0 References
3.1 Instruction Manual AAF 1100.
3.2 ISO 1171:2010

4.0 Responsibility
4.1 It is the responsibility of the Technical team leader and Chemist to have this
Work Instruction implemented as needed.

5.0 Summary of Test Method

5.1 The test portion is heated in air at a specified rate up to a temperature of 815
°C ± 10 °C and maintained at this temperature until constant in mass. The ash is
calculated from the mass of the residue after incineration.

6.0 Associated Documents

Reference Title
TOTL-SP03-F04 Equipment Maintenance Register and History Card
TOTL-SP03-F05 Equipment Maintenance Requisition through a Third Party
TOTL-SP03-F06 Out of Service Label
TOTL-SP03-F07 Troubleshooting Record
TOTL-SP05-F01 Purchased Products, Reagents and Consumable Materials Check Form
TOTL-SP05-F10 Purchase Requisition
TOTL-SP08-F02 Raw Data Sheet
TOTL-WI-F01 Balance Verification Log Form
TOTL-WI-F02 Oven Verification Log Form
TOTL-WI-F03 Muffle Verification Log Form
 Reference TOTL-WI-02

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 01 April 19

Author / Approver M.Saleh / M. Abd Elrazek
Determination of Ash in Coal
Page n° Page 4 of 6

TOTL-WI-F09 Experimental Investigation of regeneration for Silica-gel

7.0 Apparatus

7.1 Balance, capable of weighing to the nearest 0,1 mg.

7.2 Furnace, capable of giving a zone of substantially uniform temperature at the
levels required by the procedure and reaching these levels in the specified
times. The ventilation through the furnace shall be such as to give five to ten
air changes per minute.
7.3 Dish, of silica, porcelain or platinum, 8 mm to 15 mm deep, of such a size that
the sample loading does not exceed 0,15 g/cm2 for coal.
7.4 Desiccator or other closed container.

8.0 Reagents and Materials

N/A

9.0 Sampling and Test Specimens

9.1 The coal used for the determination of ash is the general analysis test sample
(ground to pass a sieve of 212 μm aperture).
9.2 The sample shall be well mixed and in moisture equilibrium with the laboratory
atmosphere.

10.0 Procedure
10.1 Weigh to the nearest 0,1 mg, the clean, dry dish, spread approximately 1 g of
the sample evenly in the dish and reweigh.
10.2 If a silica or porcelain dish is used, before its initial mass is determined, it
should be heated to 815 °C ± 10 °C, maintained at this temperature for 15 min
and then cooled under conditions specified for the actual determination.
10.3 Insert the dish in the furnace (3.2) at room temperature. Raise the furnace
temperature evenly to 500 °C over a period of 60 min and hold at this
temperature for 30 min.
10.4 Continue heating to 815 °C ± 10 °C in the same furnace. Maintain this
temperature for at least 60 min.
10.5 When the incineration period is complete, remove the dish from the furnace
and allow to cool on a thick metal plate for 10 min. At the end of the 10 min
cooling period, transfer the dish to a desiccator or other closed container
without desiccant and allow to cool to room temperature. When cool, weigh to
the nearest 0,1 mg.
 Reference TOTL-WI-02

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 01 April 19

Author / Approver M.Saleh / M. Abd Elrazek
Determination of Ash in Coal
Page n° Page 5 of 6

10.6 If there is any doubt that incineration is incomplete (e.g. unburned carbon
particles are visible), reheat at 815 °C ± 10 °C for further 15 min periods until
the change in mass does not exceed 1 mg.
10.7 Calculation:

Where,
m1 is the mass, expressed in grams, of the empty dish;
m2 is the mass, expressed in grams, of dish plus test portion;
m3 is the mass, expressed in grams, of dish plus ash.

11.0 Quality Control

- Quality control sample will be checked monthly.
- Quality control sample will be checked monthly for the working ranges covering
work load.
- Quality control result will be recorded on QC chart.

12.0 Report
- Report the result, as a mean of duplicate determinations, to the nearest 0,1 %
mass fraction.

13.0 Precision and Bias

13.1 Repeatability
The results of duplicate determinations (carried out over a short period of time, but
not simultaneously) in the same laboratory by the same operator with the same
apparatus on two representative portions taken from the same analysis sample, shall
not differ by more than the values given in Table 1.
Table 1 — Repeatability and reproducibility limits for ash
 Reference TOTL-WI-02

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 01 April 19

Author / Approver M.Saleh / M. Abd Elrazek
Determination of Ash in Coal
Page n° Page 6 of 6

13.2 Reproducibility
- The means of the results of duplicate determinations performed in each of two
laboratories, on representative portions taken from the same analysis sample,
shall not differ by more than the values given in Table 1.

14.0 Equipment Maintenance

14.1 Balance: clean weighing pan and sub pan with alcohol, verify level bubble
position. (monthly or when necessary).
14.2 Furnace: cleaning furnace internally and externally (monthly or when
necessary).
14.3 Desiccator: check silica gel color and dry it if necessary.

15.0 Records

Min.
Records
Records Custodian Retention
Location
Time
TOTL-SP03-F04 Equipment Maintenance Register Technical team TOTL
and History Card 3 years
leader, Chemist Facility
TOTL-SP03-F05 Equipment Maintenance Technical team TOTL
Requisition through a Third Party 3 years
leader, Chemist Facility
TOTL-SP03-F06 Out of Service Label Technical team TOTL
3 years
leader, Chemist Facility
TOTL-SP03-F07 Troubleshooting Record Technical team TOTL
3 years
leader, Chemist Facility
TOTL-SP05-F01 Purchased Products, Reagents and Technical team TOTL
Consumable Materials Check Form 3 years
leader, Chemist Facility
TOTL-WI-F01 Balance Verification Log Form Technical team TOTL
3 years
leader, Chemist Facility
TOTL-WI-F02 Oven Verification Log Form Technical team TOTL
3 years
leader, Chemist Facility
TOTL-WI-F03 Muffle Verification Log Form Technical team TOTL
3 years
leader, Chemist Facility
TOTL-WI-F09 Experimental Investigation of Technical team TOTL
regeneration for Silica-gel 3 years
leader, Chemist Facility