Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 1 of 8

Author Reviewed & Approved By

Name Mohamed Saleh Mohamed Abd Elrazek

Position Technical team leader TOTL Manager

Signature
Date 05/08/2020 05/08/2020

Control of Amendments

Issue Amendments Echoed

Date Reason for amendments
No. Summary Pages
0.0 05.08.2020 First issue - -
1.0
2.0
3.0
4.0
5.0

Review Frequency : Annually.

 Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 2 of 8

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 ....................................................................................................... 4
7.0 Apparatus ........................................................................................................................... 4
8.0 Reagents and Materials ...................................................................................................... 4
9.0 Sampling and Test Specimens ........................................................................................... 5
10.0 Instrument preparation ....................................................................................................... 5
11.0 Procedure ........................................................................................................................... 6
13.0 Quality Control .................................................................................................................. 7
14.0 Report................................................................................................................................. 7
15.0 Precision and Bias .............................................................................................................. 7
15.1 Repeatability ...................................................................................................................... 8
16.0 Equipment Maintenance .................................................................................................... 8
17.0 Records .............................................................................................................................. 8
 Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 3 of 8

1.0 Scope
1.1 This Test Method covers the determination of carbon in the range of 54.9 % to 84.7
%, hydrogen in the range of 3.25 % to5.10 %, and nitrogen in the range of 0.57 % to
1.80 % in the analysis samples (8.1) of coal and of carbon in analysis samples of coke
in the range of 86.6 % to 97.9 %.
1.2 All percentages are percent mass fractions unless otherwise noted.

2.0 Definitions of Terms

For definitions of terms used in this standard, refer Terminology D121..

3.0 References
ASTM D 5373 -2016

4.0 Responsibility
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 In this Method carbon, hydrogen, and nitrogen in coal or carbon in coke are
determined in a single instrumental procedure using a furnace operating at
temperatures in the range of 900 °C to 1050 °C for carbon, hydrogen and nitrogen in
coal or 950 °C to 1150 °C for carbon in coke. The quantitative conversion of the
carbon, hydrogen, and nitrogen into their corresponding gases (CO2, H2O, and NOx)
occurs during combustion of the sample at an elevated temperature in an atmosphere
of oxygen. Combustion products which can interfere with the subsequent gas analysis
are removed. Oxides of nitrogen (NOx) are reduced to N2 before detection. The
carbon dioxide, water vapor and elemental nitrogen in the gas stream are determined
by appropriate instrumental detection procedures.
5.2 In Method B, carbon in coal and coke is determined by combusting the sample in a
1350 °C furnace. The H2O in the combustion gases is removed and CO2 is
determined by infrared absorption.
 Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 4 of 8

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-F15 CHNS Verification by CRM
TOTL-SP04-F03 Internal Calibration Report Form

7.0 Apparatus
7.1 An instrument capable of analyzing a test portion of 6 mg or greater. For coal, it
includes a furnace capable of maintaining a temperature in the range of 900 °C to
1050 °C to ensure quantitative recovery of carbon, hydrogen, and nitrogen. (Thermo
scientific Flash smart 2000)
7.2 combustion promoters, including tin foil or capsule, shall be utilized as required by the
apparatus manufacturer.
7.3 Analytical balance stand-alone balance or a balance integrated with the instrument,
with a resolution of at least 0.1 % relative of the test portion mass.

8.0 Reagents and Materials

8.1 Carrier Gas, as specified for the instrument by the manufacturer.

8.2 Oxygen, as specified for the instrument by the manufacturer

8.3 Additional Reagents, of types and qualities as specified for the instrument by the
manufacturer.

8.4 Calibration Materials—Calibration materials shall be accompanied by a

certificate of analysis stating the purity of the material. If the certificate of analysis
does not provide assigned values for carbon, hydrogen or nitrogen use the purity as
stated on the certificate to establish carbon, hydrogen and nitrogen from the
 Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 5 of 8

theoretical values. Store these pure substances in a desiccator under conditions that
maintain the compounds in a dry state.

8.6 Reference Materials—Certified reference material (CRM) coal(s) prepared by a

recognized authority to monitor changes in instrument response that can be affected
by constituents not present in the calibration materials and to verify the acceptability
of nitrogen results. Coal(s) and coke(s)traceable to a certified reference material
(CRM) coal(s) and coke(s) can also be used.
Follow instructions on the reference material certificate with respect to storage of the
reference material and use of assigned values. Use only those carbon,
hydrogen and nitrogen values that have an assigned uncertainty or are traceable to
a value with an assigned uncertainty

9.0 Sampling and Test Specimens

The sample shall be the analysis sample prepared to atop size of less than 250 μm (No.
60). Coal samples shall be prepared in accordance with Practice D2013.

10.0 Instrument preparation

10.1 Instrument Set-Up—Verify all instrument operating parameters meet the specifications
in the instrument operating manual. Verify the condition and quantities of all
chemicals currently in use are satisfactory for the number of samples to be analyzed.
Prior to any analysis, check for and, if necessary correct any leaks in the combustion
system, and the carrier gas system.

10.2 Blank Analyses—Perform blank analyses to establish carbon, hydrogen and nitrogen
levels in the combustion and carrier gases as required by the specific method. The
level of carbon, hydrogen or nitrogen in these gases shall not exceed 1 % relative of
the instrument response for the lowest mass of calibration material for each analyte.
Re-determine blank analyses whenever the carrier gas or oxygen supplies are changed
or any chemicals are renewed.

10.3 Conditioning—Select a conditioning sample in the range of 75 % (or more) carbon dry
basis. It is recommended that the moisture content be less than 3 %. Carry out four
determinations on the conditioning sample. Discard the first determination. If the
range of the three retained determinations for either carbon, hydrogen or nitrogen
values exceed 1.2r where r is the repeatability of this standard, instrument stability is
suspect. In this case take corrective action before proceeding with calibration.

10.4 Calibration—If the instrument has been previously calibrated in accordance with Annex
A1, determinations can proceed provided the calibration is verified in accordance
with Annex A2. Otherwise calibrate the instrument as described in Annex A19.4.
 Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 6 of 8

11.0 Procedure
11.1 Determination:
11.1.1 Carry out a determination of the moisture content of each analysis sample or each
reference material, or both, inaccordance with Test Method D3173 or Test Methods
D7582within 48 h of the determination of carbon, hydrogen and
nitrogen on each analysis sample.

11.1.2 Carry out the determination by weighing out a test portion of each analysis sample
within a mass range recommended by the manufacturer. Conduct determinations on
consecutive test portions of an analysis sample as needed to meet quality control
requirements.

11.1.3 Verify the calibration upon completion of all test determinations and as needed to
meet quality control requirements according to Annex A2. 0.1.4

11.1.4 Prior to conducting any test determinations, up oncompletion of all test

determinations and as needed to meet quality control requirements conduct
determinations on consecutive test portions of a reference material (RM) (7.6).
Verifythe acceptability of results for the RM in accordance with Annex A3.

12.0 Calculation and expression of results

12.1.1 Record the total carbon, hydrogen and nitrogen as analyzed as a percentage by
mass. Report the results on dry basis to the nearest 0.1 % for carbon, 0.01 % for
hydrogen and to the nearest 0.01 % for nitrogen.
12.1.2 Use the following equations for the calculation to dry basis:

where:
 Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 7 of 8

d = dry basis,
ad = as determined (as analyzed) basis,
C = content of carbon, %,
N = content of nitrogen, %,
H = content of hydrogen, %, and
Mad = moisture content of the sample as analyzed, %.

13.0 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.

14.0 Report
- The result of the determination shall be reported to one decimal place.

15.0 Precision and Bias

The precision data for Test Method A for the determination of carbon, hydrogen, and nitrogen
in coal and carbon in
 Reference TOTL-WI-18

Office Egypt

ISO/IEC 17025 Working Instructions Issue n° / Date 00 / 05 August 20

Determination of Carbon, Hydrogen and Nitrogen Author / Approver M.Saleh / M. Abd Elrazek

in Coal Page n° Page 8 of 8

15.1 Repeatability
The value below which the absolute difference between two test results calculated to a dry
basis (Practices D3180 and D3176) of separate and consecutive test determinations, carried
out on the same sample, in the same laboratory, by the same operator, using the same
apparatus on samples taken at random from a single quantity of homogeneous material,
may be expected to occur with a probability of approximately 95 %.

15.2 Reproducibility
The value below which the absolute difference between two test results calculated to a
dry basis (Practices D3180 and D3176), carried out in different laboratories, using samples
taken at random from a single quantity of material that is as homogeneous as possible, may
be expected to occur with a probability of approximately 95 %.

16.0 Equipment Maintenance

Balance: clean weighing pan and sub pan with alcohol, verify level bubble position.
(monthly or when necessary.
17.0 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-F15 CHNS Verification by CRM Technical team TOTL
3 years
leader, Chemist Facility
TOTL-SP04-F03 Internal Calibration Report Form Technical team TOTL
3 years
leader, Chemist Facility