(DOE) System Procedures, Work Instructions, and Forms For Coal Analysis

Issue Date:
Department of Energy 01 – 2018

ERTLS – Geoscientific Research & Fuel Testing MANAGEMENT SYSTEM Rev No.: Page 1 of 6
Laboratory 11
Code: DMRRS-SP
Document Masterlist, Review and Revision Status
Manual on Systems Procedures
Document Document Issue Review Status Revision Status

Code Title Date
Review No. Date Reviewed Revision No. Date Revised
SP Systems Procedures on Quality 11-2015 2 03-2017 3 11-2015
Flow of Samples and Documents
SP1.1 11-2015 2 03-2017 4 11-2015
(One Loop)
Receipt of Additional Test Parameters
SP1.1a 11-2015 2 03-2017 2 11-2015
for External Customer
Receipt of Additional Test Parameters
SP1.1b 11-2015 2 03-2017 2 11-2015
for Internal Customer
Monthly Maintenance Program of
SP2.1 11-2015 2 03-2017 1 11-2015
Analytical Balances
SP2.2 11-2015 2 03-2017 3 11-2015
Ovens and Furnaces
SP2.3 Calorimeters, CHN and Sulfur 11-2015 2 03-2017 3 11-2015
Analyzers
Recording of Ambient Temperature
SP2.4 05-2017 2 03-2017 4 05-2017
and Humidity
External Calibration of Laboratory
SP2.5.1 11-2015 2 03-2017 2 11-2015
Equipment and Apparatus
Monitoring of External Calibration of
SP2.5.1.1 01-2016 1 03-2017
Equipment
Calibration of Laboratory Equipment/
SP2.5.2 01-2016 2 03-2017 1 01-2016
Furnaces and TGA-1000
Issue Date:
Laboratory 11
Code: DMRRS-SP

Code Title Date
SP2.5.3 01-2016 2 03-2017 1 01-2016
Parr 6200 Isoperibol Calorimeter
SP2.5.4 01-2016 2 03-2017 1 01-2016
SC 432 DR Sulfur Analyzer
SP2.5.5 01-2016 2 03-2017 1 01-2016
Leco Truspec CHN Analyzer
SP3.1 Preparation of Final Test Results 01-2016 2 03-2017 2 01-2016
Release of Test Report to Internal
SP4.1 01-2016 2 03-2017 3 01-2016
Customer
Release of Test Report to External
SP4.2 01-2016 2 03-2017 3 01-2016
Customer
Release of Test Report to External
SP4.3 01-2016 2 03-2017 1 01-2016
Customer Through Electronic Mail
SP5.1 Wastes Treatment and Storage 01-2016 2 03-2017 1 01-2016
Storage and Disposal of Heavy
SP5.2 01-2016 2 03-2017 1 01-2016
Metals
Handling of Coal Wastes from
SP5.3 01-2016 2 03-2017 2 01-2016
Sample Preparation
Retention and Disposal of Coal File
SP5.4 05-2017 2 03-2017 2 05-2017
and Analysis Samples
Issue Date:
Laboratory 11
Code: DMRRS-SP

Code Title Date
Management Review of Laboratory
SP6.1 01-2016 2 03-2017 2 01-2016
Quality Systems
Maintaining Records of Management
SP6.2 01-2016 2 03-2017 2 01-2016
Review
Submission and Approval of
SP6.3 Documents on Quality 01-2016 2 03-2017 2 01-2016
(Internal Laboratory)
Submission and Approval of
SP6.4 Documents on Quality 01-2016 2 03-2017 2 01-2016
(External Communication)
Conduct of Preventive Maintenance
SP6.5 01-2016 2 03-2017 2 01-2016
for Laboratory Equipment
SP6.6 Internal Quality Audit 01-2016 2 03-2017 1 01-2016
SP7.1 Document Issuance and Distribution 01-2016 2 03-2017 2 01-2016
Reflecting Changes in Existing
SP7.2 01-2016 2 03-2017 2 01-2016
Document in Hard and Soft Copy
SP7.3 Handling of obsolete Documents 01-2016 2 03-2017 1 01-2016
SP7.4 Review of Documents 01-2016 2 03-2017 1 01-2016
Entering Into and Review of
SP8.1 01-2016 2 03-2017 2 01-2016
MOA/MOU
Issue Date:
Laboratory 11
Code: DMRRS-SP

Code Title Date
SP9.1 Inventory of Chemicals and Supplies 01-2016 2 03-2017 1 01-2016
Request for Purchase of Chemicals
SP9.2 01-2016 2 03-2017 1 01-2016
and Other Supplies
Procurement of Equipment that
SP9.3 Provides New Capability for the 01-2016 2 03-2017 1 01-2016
Laboratory
Purchase of Replacement of
SP9.4 01-2016 2 03-2017 1 01-2016
Equipment/Other Apparatus
Bidding Procedure on Procurement
SP9.5 01-2016 2 03-2017 1 01-2016
and Repair
Reception and Storage of Purchased
SP9.6 Reagents and Other Laboratory 10-2015 2 03-2017 1 10-2015
Consumable Materials
Obtaining Test Results Outside
SP10.1 10-2017 2 03-2017 3 10-2017
Repeatability Range
Addressing Nonconformance in the
SP10.2 10-2015 2 03-2017 3 10-2015
Laboratory Quality System/Others
Control/Prevention of Non-conforming
SP10.3 01-2016 2 03-2017 3 01-2016
Work on Coal Analysis
SP10.4 Resolution of Complaint 01-2016 2 03-2017 3 01-2016
Issue Date:
Laboratory 11
Code: DMRRS-SP

Code Title Date
Preventive/Corrective Action on
SP10.5 05-2017 2 03-2017 4 05-2017
Quality Control Failure
SP10.6 Analysis of Customer’s Feedback 01-2016 2 03-2017 4 01-2016
SP10.7 Root Cause Analysis 01-2016 2 03-2017 1 01-2016
Quantifying Uncertainty for Proximate
SP11.1 05-2017 2 03-2017 2 05-2017
Analysis (Using ISO Method)
Quantifying Uncertainty for Calorific
SP11.2 Value, Sulfur, Carbon, Hydrogen and 01-2016 2 03-2017 1 01-2016
Nitrogen
SP12.1 Cleaning of Glassware 01-2016 2 03-2017 1 01-2016
Monitoring Accuracy of Test Results
SP13.1 01-2016 2 03-2017 3 01-2016
on Coal Analysis
SP14.1 Identifying Training Needs 10-2015 2 03-2017 1 10-2015
Providing Training To Personnel/
SP14.2 01-2016 2 03-2017 3 01-2016
Nomination and Selection
Evaluation of Effectiveness of
SP14.3 Training Provided to Newly- 01-2016 2 03-2017 1 01-2016
Hired/Newly-Assigned Personnel
Issue Date:
Laboratory 11
Code: DMRRS-SP

Code Title Date
Evaluation of Effectiveness of
SP14.4 Training Received by Laboratory 01-2016 2 03-2017 2 01-2016
Personnel
Request for Leave of Absence/Sick
SP14.5 01-2016 2 03-2017 3 01-2016
Leave
Department of Energy Issue Date:
MANAGEMENT 01- 2018
ERTLS – Geoscientific Page 1 of 1
SYSTEM Rev No.:
Research & Fuel 7
Testing Laboratory
Code: DMRRS-CP
Procedures on Sample Preparation and Coal Analysis
Review Status Revision Status

Document Document Issue
Review Date Revision Date
Code Title Date
No. Reviewed No. Revised
Collection of Channel Samples of
CP1a Coal From Coal Seam/ Adopted 11-2015 2 03-2017 1 11-2015
from ASTM D 4596-99
Preparation of Coal Secondary
CP1b 11-2015 2 03-2017 1 11-2015
Standard
Preparation of Coal Samples for
CP1 01-2016 2 03-2017 1 01-2016
Analysis/ Adopted from ISO 5069
Performing Sieve Analysis of Coal
CP2 and Designating Coal Size/ 01-2016 2 03-2017 1 01-2016
Adopted from ASTM D 4749
Determination of Moisture
CP3 Content/ Adopted from ISO 5068/ 01-2018 2 03-2017 2 01-2018
Indirect Gravimetric Method
Determination of Volatile
CP4 Combustible Matter/ Adopted from 11-2015 2 03-2017 1 11-2015
ISO 562
Determination of Ash/ Adopted
CP5 11-2015 2 03-2017 1 11-2015
from ISO 1171
Determination of Fixed Carbon/
CP6 11-2015 2 03-2017 1 11-2015
Using ISO 17246:2010
Determination of Calorific Value/
CP7 11-2015 2 03-2017 1 11-2015
Adopted from ASTM D 5865 - 04
Determination of Forms of Sulfur
CP8 in Coal/ Adopted from ASTM 01-2016 2 03-2017 1 01-2016
D 2492
Determination of Total Sulfur by IR
CP9a Method/ Adopted from ASTM D 01-2016 2 03-2017 1 01-2016
4239 – 05 using SC 432 DR
Determination of Total Sulfur by IR
CP9b Method/ Adopted from ASTM D 01-2016 1 03-2017
4239 – 05 using TruSpec S
Sulfur Determination by Eschka
CP10 and Bomb Washing Methods/ 01-2016 2 03-2017 1 01-2016
Carbon, Hydrogen and Nitrogen
CP11 (CHN) Analysis/ Adopted from 11-2015 2 03-2017 1 11-2015
ASTM D 5373 - 02
Issue Date:
Department of Energy 01– 2018
ERTLS – Geoscientific Research & Fuel Testing MANAGEMENT SYSTEM Rev No.:
Page 1 of 5
Laboratory 11
Code: DMRRS-F
Forms

Form #
Code Title Date
CF1 Request for Laboratory Services
RLS1 05-2015 2 03-2017 3 05-2015
(External Customer)
CF2 Request for Laboratory Services
RLS2 11-2015 2 03-2017 2 11-2015
(Internal Customer)
CF3 LWO Laboratory work Order 04-2017 2 03-2017 4 03-2017
CF4 Coal Analysis/Laboratory Work
LWO1 10-2017 2 03-2017 3 10-2017
Order -1 (Sample Preparation)
CF5 Coal Analysis/Laboratory Work
LWO2 11-2015 2 03-2017 2 11-2015
Order - 2 (Required Analysis)
CF6 ADL Air Drying Loss 11-2015 2 03-2017 2 11-2015
CF7 PTR Preliminary Test Results 11-2015 2 03-2017 2 11-2015
CF8a Laboratory Analysis Test Report -
LATR ODC
RLS No- From Coal Unit to ODC 01-2016 2 03-2017 6 01-2016
to OD (a)
to OD with PAB Endorsement
CF8b Laboratory Analysis Test Report -
LATR ODC
RLS No- From Coal Unit to ODC 11-2015 1 03-2017
to OD (b)
to OD without PAB Endorsement
CF9a Laboratory Analysis/Test Report -
LATR LWO - From Coal Unit to ODC to
01-2016 2 03-2017 5 01-2016
Internal (a) OD to Internal Customer with PAB
Endorsement
CF9b Laboratory Analysis/Test Report -
LATR LWO - From Coal Unit to ODC to
11-2015 1 03-2017
Internal (b) OD to Internal Customer without
PAB Endorsement
Issue Date:
Laboratory 11
Code: DMRRS-F
Forms

Form #
Code Title Date
CF10a LATR Laboratory Analysis/Test Report -
OD to From OD to External Customer 01-2016 2 03-2017 6 01-2016
External (a) with PAB Endorsement
CF10b LATR Laboratory Analysis/Test Report -
OD to From OD to External Customer 10-2015 1 03-2017
External (b) without PAB Endorsement
CF11 COR Complaint Report 11-2015 2 03-2017 2 11-2015
Customer Rating (Submission of
CF12a CRa 05-2017 2 03-2017 3 05-2017
Sample)
Customer Rating (Submission of
CF12b CRb 05-2017 1 03-2017 1 05-2017
Sample)
CF13 Non Conformance and Action
NCAR 05-2017 2 03-2017 3 05-2017
Report
CF14 PR Proficiency Rating 11-2015 2 03-2017 3 11-2015
CF15 Document Issuance/Change
DICN 10-2015 2 03-2017 2 10-2015
Notice
CF16 AMR Ambient Monitoring Report 01-2016 2 03-2017 2 01-2016
CF19a Monthly Equipment Maintenance
EMPCoal-
& Program/ Acculab Analytical 01-2017 2 03-2017 3 01-2017
Bal Acculab
CF19b Balance
CF20a EMPCoal- Monthly Equipment Maintenance
& Bal Leco Program/ Leco 250 Analytical 01-2017 2 03-2017 3 01-2017
CF20b 250 Balance
Issue Date:
Laboratory 11
Code: DMRRS-F
Forms

Form #
Code Title Date
CF22a & EMPCoal- Monthly Equipment Maintenance
CF22b Bal Program/ Sartorius Analytical 01-2017 2 03-2017 3 01-2017
Sartorius Balance
CF23b Calo Leco Program/ Leco AC 350 Isoperibol 01-2017 2 03-2017 3 01-2017
AC 350 Calorimeter
CF24b Calo Parr Program/ Parr 6200 Isoperibol 01-2017 2 03-2017 3 01-2017
6200 Calorimeter
CF25b CHNS Leco Program/ Leco Truspec CHNS 01-2017 2 03-2017 3 01-2017
Tru Analyzer
CF26b Furnace Program/ Prufer Furnace I 01-2017 2 03-2017 3 01-2017
Prufer 1
01-2017
CF27b Furnace Program/ Prufer Furnace II 01-2017 2 03-2017 3
Prufer 2
CF28a & Monthly Equipment Maintenance
EMPCoal –
CF28b Program/ MA-2000 Mercury 01-2017 2 03-2017 3 01-2017
MA2000
Analyzer
Issue Date:
Laboratory 11
Code: DMRRS-F
Forms

Form #
Code Title Date
CF29a & EMPCoal - Monthly Equipment Maintenance
CF29b Oven Air Program/ Coal Air Drying Oven 01-2017 2 03-2017 3 01-2017
Drying
CF30 EMPCoal – Monthly Equipment Maintenance
01-2016 2 03-2017 2 01-2016
Oven Jouan Program/ Jouan Oven
EMPCoal –
CF31b Program/ Carbolite Minimum Free 01-2017 2 03-2017 3 01-2017
Oven MFS
Space Oven
CF32a & EMPCoal - Monthly Equipment Maintenance
CF32b Sulfur SC Program/ Leco SC 432 DR Sulfur 01-2017 2 03-2017 3 01-2017
432 DR Analyzer
EMPCoal –
CF33b Program/ Las Navas TGA-1000 01-2017 2 03-2017 3 01-2017
TGA1000
Thermogravimetric Analyzer
CF35a & Monthly Housekeeping Program
MHP 01-2017 2 03-2017 3 01-2017
CF35b
CF36 DR Document Review 01-2016 2 03-2017 1 01-2016
CF37a & EMPCoal – Monthly Equipment Maintenance
01-2017 2 03-2017 2 01-2017
CF37b Bal Kern Program/ Kern Analytical Balance
Issue Date:
Laboratory 11
Code: DMRRS-F
Forms

Form #
Code Title Date
CF38b Furnace Program/ Carbolite Ashing
01-2017 2 03-2017 2 01-2017
Carbolite Furnace AAF 1100
AAF
CF39b Furnace Program/ Carbolite Vol. Matter
01-2017 2 03-2017 2 01-2017
Carbolite Furnace VMF 1000
VMF
CF40 TE Training Evaluation 11-2015 2 03-2017 1 11-2015
CF41 IQA Internal Quality Audit Checklist 08-2016
1 03-2017
Checklist
Issue Date:
Department of Energy SYSTEMS 11 - 2015
ERTLS – Geoscientific PROCEDURE Page 1 of 1
Research & Fuel Rev No.:
MANUAL
3
Testing Laboratory
Code: SP
SYSTEMS PROCEDURES ON QUALITY
The Geo-Coal implements standard operating procedures in receiving coal samples,

conducting required analysis, releasing test results and performing other activities
associated with these major functions.
The procedures are detailed in the succeeding flowcharts.

Issue Date:
Department of Energy SYSTEMS
PROCEDURE 11 - 2015
Research & Fuel MANUAL Rev No.:
4
Testing Laboratory
Code: SP 1.1
RECEIPT, RECORDING AND ANALYSIS OF SAMPLE/S AND RELEASE OF TEST REPORT
Flow of Samples and Documents (One-loop)
Receipt of Sample/s from Customer

-------------------------------------------
Procedure Responsible Personnel Details/Emphasis
Start
romExternal Customer
From
 Customer proceeds to OD Personnel
OD.
Test requirements of
 Customer discusses customer.
his test requirements.
From Internal Customer

 Customer proceeds to ODC Personnel
the ODC to get RLS.
 Customer proceeds to
Senior SRS
Geo-Coal & discusses
his test requirements.
OD Personnel/ If sample/s are not

 Examine the sample/s.
Senior SRS coal (but belong to
“other related
samples”) & may
have problem/s on
sample
preparation/other
equipment, OD
Personnel will ask
Determine No advice from Geo-
the nature & Recommends that Coal’s Lab
approximate customer submit Tech/Analysts/
mass of the another sample. Supervisor
sample/s.
Yes
A
Issue Date:
PROCEDURE 11 - 2015
4
Testing Laboratory
Code: SP 1.1
 Accept the sample OD Personnel

 External customer fills in
the RLS Form 1.
 Internal customer fills in
the RLS Form 2.
External Customer
 Check information OD Personnel Correct information
in RLS Form 1. written in RLS Form.
 Sign RLS Form 1. ERTLS Director
 Transmit RLS Form 1 to
ODC. OD Personnel
Internal Customer
 Check information in
RLS Form 2 & sign. Senior SRS
 Check & sign RLS Geo-Coal Supervisor
Form 2.
 Transmit RLS Form 2 to Laboratory Technician
ODC.
External Customer RLS Form 1 (photocopy

 Receive RLS Form 1. ODC Personnel copy) is retained at ODC
while a copy of RLS Form
Internal Customer 2 is transmitted to Geo-
 Check information in RLS Coal together with the
Form 2 & sign. Division Chief LWO for internal
customers.
ODC Personnel
 Prepare LWO.
Division Chief
 Sign LWO.
ODC Personnel
 Issue LWO to Geo-Coal.
B
Issue Date:
PROCEDURE 11 - 2015
4
Testing Laboratory
Code: SP 1.1
Recording of Sample/s
---------------------------------
A designated table
 Receive RLS/LWO & Geo-Coal Supervisor near sample tracer is
coal sample/s. provided for the
purpose of receiving
sample/s.
 Assign laboratory Senior SRS Laboratory number as

number to coal
laboratory code for
sample/s.
each sample.
 Record the date Geo-

Laboratory Technician
Coal receives the
sample, RLS number,
laboratory number,
sample description &
analysis required in
coal Sample Tracer.
Determine if
sample No
preparation C Senior SRS
is
necessary.
Yes
 Issue LWO-1 to Senior SRS

Laboratory Technician.
D
C
Issue Date:
PROCEDURE 11 - 2015
4
Testing Laboratory
Code: SP 1.1
 Receive the sample/s. Laboratory Technician

 Record in the logbook
the date Geo-Coal
receives the sample,
RLS number,
laboratory number,
sample description,
analysis required &
special instructions, if
any.
 Put sample/s in vial/s

and label. Laboratory Technician
 Submit vial/s to Senior
SRS.
E
Issue Date:
PROCEDURE 11 - 2015
4
Testing Laboratory
Code: SP 1.1
Recording & Analysis of Sample/s (Sample Preparation Included)

----------------------------------------------------------------------------------------
 Receive the sample/s Laboratory Technician

and LWO-1.
 Record in the logbook
the date Geo-Coal
receive the sample,
RLS number,
laboratory number,
sample description,
analysis required &
special instructions, if
any.
 Prepare sample
according to CP1.
 Submit prepared Laboratory Technician

sample/s to Senior
SRS.
E
Issue Date:
PROCEDURE 11 - 2015
4
Testing Laboratory
Code: SP 1.1
 Issue prepared Senior SRS

sample/s and LWO-2
to analyst/s.
Analysts Certified Reference

 Perform analysis of
required parameters Material/ secondary
using coal standard/s standard is used.
as reference; while
recording results of
analysis in the
analysis logbook or
print test results (for
other equipment).
 Check repeatability of
test results.
 Check results for the
reference coal
standard/s.
Compute dry
Senior SRS Values in the
basis & No
Certificate of
determine if
Analysis or values
values are
within range. obtained for
secondary standards
after homogeneity &
stability tests.
Yes
F
Issue Date:
PROCEDURE 11 - 2015
4
Testing Laboratory
Code: SP 1.1
Preparation & Release of Test Report

---------------------------------------------------
 Issue PTR form to Senior SRS

analyst/s.
 Write test results in Analyst/s

the PTR form.
 Check test results in Senior SRS

the PTR form if
correctly transferred
from analysis
logbook &/or print-
out.
 Prepare test report
(by Geo-Coal) using
CF8 for external
customers and CF9
for internal
customers.
Analyzed
 Check CF8/CF9 & Analysts/Senior By/Checked
sign. SRS/Supervising SRS By/Noted By
G
Issue Date:
PROCEDURE 11 - 2015
4
Testing Laboratory
Code: SP 1.1
 Transmit test report to Laboratory Technician

ODC.
 Check test report & Division Chief
sign.
 Transmit test report to ODC Personnel

OD.
For internal customers Director is the
 Signs test report. final signatory.
For external customers

 Transfer test results OD Personnel
using CF10.
 Transmit to ODC. OD Personnel
 Transmit test report to ODC Personnel
Geo-Coal.
 Check & sign test Supervising SRS
report.
 Transmit to ODC. Laboratory Technician

 Check & sign test Division Chief
report.
 Transmit to OD. ODC Personnel

 Sign test report. Director
 Release test report. OD Personnel
End
Issue Date:
PROCEDURE 11 - 2015
ERTLS – Geoscientific Page 1of 1
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.1
ANALYSIS OF SAMPLE/S
Monthly Maintenance Program of Analytical Balances
Start
 Perform monthly SRS II / Senior SRS Monthly maintenance is

maintenance of analytical conducted every end of the
balances. month on top of the internal
calibration being done during
sample analysis.
 Clean the weighing
chamber and pan with
brush and soft SRS II / Senior SRS
cloth/paper towel.
 Check dessicant and
replace if necessary.
 Level the balance such

that the bubble is in the SRS II / Senior SRS Refer to the User’s Manual for
middle of the circle. the procedure of internal
 Go through internal calibration.
calibration.
 Calibrate against a Check for off center errors by

calibrated 1-g standard SRS II / Senior SRS
weighing the 1-g standard
mass. mass at the center of the pan
 Record the reading. and at the back, front, left and
 Fill out the equipment right portions.
maintenance program
form provided for each
balance.

 Check accomplished
Geo-Coal Supervisor
form.
End
Issue Date:
PROCEDURE 11 - 2015
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 2.2
Monthly Maintenance Program of Ovens and Furnaces

(Coal Air-Drying Oven, Jouan Oven, MFS Oven, Prufer Furnace I and II)
Start
 Perform monthly SRS II / Senior SRS Monthly maintenance is

maintenance of ovens conducted every end of the
and furnaces. month.
Ovens
 Check if the unit is SRS II / Senior SRS
working.
 Check gas supply, lines
and accessories if
applicable.
 Make sure that all air inlet
and outlet are free from
clog.
 As a routine check, verify
the temperature reading
against set point.
 Ensure tight closing of the
door. Lubricate
mechanical parts of the
door hinges and movable
parts of the door lock if
necessary.
 Clean the unit using soft
cloth.
 Make sure that the
equipment area is clean.
 Fill out equipment
maintenance program
form.
A
Issue Date:
PROCEDURE 11 – 2015
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 2.2
Monthly Maintenance Program of Ovens and Furnaces

(Coal Air-Drying Oven, Jouan Oven, MFS Oven, Prufer Furnace I and II)
Furnaces
 Check if the unit is SRS II / Senior SRS
working.
 Make sure that air
inlet/outlet located at the
top of the furnace is free
from clog.
 As a routine check, verify
the temperature reading
against set point.
 Ensure tight closing of the
door. Lubricate
mechanical parts of the
door hinges and movable
parts of the door lock if
necessary.
 Clean the unit using soft
cloth.
 Make sure that the
equipment area is clean.
 Fill out equipment
maintenance program
form.
 Check accomplished
equipment maintenance Geo-Coal Supervisor
program form.
End
Issue Date:
PROCEDURE 05 - 2017
4
Testing Laboratory
Code: SP 2.4
Recording of Ambient temperature and Humidity
Procedure Responsible Personnel Details/emphasis
Start
 Turn on the SRS II / Senior SRS Reading and recording is

hygrometer before made every hour for the
the start of analysis first year to third year to
on moisture, volatile establish trends/
matter, ash, calorific seasonality/pattern.
value, sulfur, carbon,
hydrogen and
nitrogen
 Record the temperature SRS II

and relative humidity in
the logbook at 9:00 am
to 2:00 pm.
End
Issue Date:
PROCEDURE 11 - 2015
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 2.5.1
External Calibration of Laboratory Equipment and Apparatus
External calibration by ISO accredited service provider

(Furnaces, Analytical Balances, Ovens, TGA-1000, Thermohygrometers, Calorimeter,
Sulfur Analyzer, CHN Analyzer and timer)
Start
 Solicit quotations SRS II, Lab. Tech. Periodic calibration of

from ISO accredited equipment at least once
calibration facilities. a year.
 Prepare RFS and
submit to the office of
the Division Chief and
office of the Director
for signature.
 Receive/log request
for calibration. GSD
 Inform ODC of the
status of request,
including the winning
bidder.
 Set schedule for the Senior SRS, SRS II

calibration.
 Attend/check quality
of work rendered by
the service provider.
 File calibration
certificate and apply
necessary adjustment.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
Testing Laboratory
Code: SP 2.5.1.1
Monitoring of Calibrated Laboratory Equipment and Apparatus
Start
 Prepare RFS and Sr. SRS, SRS II, Lab. RFS to LATL-
submit to the office of Tech. Calibration Section to
the Division Chief and conduct intermediate
office of the Director checks to maintain
for signature. confidence once a year
in between date
calibrated and due date
 Receive/log request
for calibration.
status of request, and
follow up status. Sr. SRS
 Set schedule for the

calibration.
of work rendered by Senior SRS
the service provider.
 File calibration
certificate and apply
necessary adjustment.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.2
Calibration of Laboratory Equipment
Calibration of furnaces and TGA-1000 using certified reference materials
Procedure Responsible Personnel

Details/Emphasis
Start
 Perform at least two Senior SRS, SRS II Periodic calibration of

trials using proximate furnaces and TGA once
coal standard. a year using proximate
coal standard.
 Read/observe test Senior SRS, SRS II

results on volatile
matter and ash.
Determine if
values are within
repeatability and
reproducibility No
B
range indicated
in the Certificate
of Analysis.
Yes
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.2

Details/Emphasis
 Consider the results SRS II, Senior SRS

and record/update
calibration logbook.
 For TGA-1000 use
the results in the
analysis of samples.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.2

Details/Emphasis
No
B
 Perform another trial. SRS II, Senior SRS
Check the
new value if
No
within the  Repeat
repeatability/ B
reproducibility
limits.
Yes
 Consider the results SRS II, Senior SRS

and record/update
calibration logbook.
 For TGA-1000 use
the results in the
analysis of samples.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.3
Calibration of Parr 6200 Isoperibol Calorimeter
Start
 Perform initial
standardization for SRS I / SRS II / Senior SRS Initial standardization is done
each set of bomb after the equipment is installed
and bucket. prior to sample analysis to
 Make at least 10 establish the energy equivalent
runs of benzoic acid for each bomb.
pellets for each set.
SRS I / SRS II / Senior SRS For 10 new runs, the range of

Check the results is +/- 12.0 cal/°C and
 Perform additional the standard deviation must not
repeatability No
runs until 10 exceed 6.5 cal/°C.
of results.
repeatable results
are obtained.
Yes
 Compute for the SRS I / SRS II / Senior SRS

mean energy
equivalent, standard
deviation and
percent relative
standard deviation
(%rsd) for each set
of bomb and bucket
using the 10 runs.
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.3
SRS I / SRS II / Senior SRS The relative standard

Check if the deviation of ten
%rsd does No  Perform additional acceptable runs shall
not exceed runs until the be 0.15% or less of
0.15%. condition is met. the mean energy
equivalent.
Yes
 Input the mean

energy equivalent for SRS I / SRS II / Senior SRS
each set of bomb
and bucket in the
calorimeter.
 The inputted value
will be used by the
calorimeter during
test runs/sample
analysis.
 Set the EE value
“Protect ON” in order
to disable the
calorimeter from
automatically
updating.
B
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.3
B
For monthly
standardizations, the single
new run shall not differ from
the existing EE value by
 After the initial 10 more than +/- 4 cal/°C. If this
runs, monthly SRS I / SRS II / Senior SRS
condition is not met, an
standardization is additional run shall be made.
carried out to update The difference between the
the EE value, two runs shall not exceed +/-
standard deviation 5.0 cal/°C and their average
and %rsd. shall not differ from the
 Perform one run for existing EE value by more
each set. than +/-3.0 cal/°C. If such
 Remove the conditions are not met, 2
first/oldest data then more runs shall be made.
include the new one The difference between the
(completing 10 runs). four runs shall not exceed +/-
 Compute for the new 8.0 cal/°C and their average
mean EE value, shall not differ from the
standard deviation existing EE value by more
and %rsd. than +/-2.0 cal/°C. If still, the
conditions are not met, 2
additional runs shall be
made. The range of results
of the 6 runs shall not
End
exceed +/-10.0 cal/°C and
the average shall not differ
from the existing EE value by
more than +/-2.0 cal/°C. In
the event that the foregoing
conditions are not met, four
more runs shall be made.
The range of the 10 new
runs shall not exceed +/-12.0
cal/°C and the relative
standard deviation shall not
be more than 0.15% of the
mean value. (Refer to
Calorimeter Calibration
Logbook and ASTM D 5865
– 04.)
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.4
Calibration of SC 432 DR Sulfur Analyzer
Start
 Select and define the SRS II / Senior SRS The standard to be used should
standard to be used have a sulfur value slightly higher
for calibration by than the range of samples to be
inputting the ID code analyzed.
(Part #) and the %S
value.
 Select the Low sulfur method is to be used
appropriate method for samples with below 4% sulfur
from the method content. For 4% and higher sulfur
menu. (low or high values, High sulfur method is
sulfur). most appropriate.
 Analyze 6 standard SRS II / Senior SRS Weights of standard to be used

samples at different should be 0.09 g, 0.10 g, 0.11 g,
weights (single point 0.12 g, 0.13 g and 0.14 g.
calibration).
 Perform the In including/excluding results,
calibration in the there must be a minimum of at
standard calibration least 3 runs in the linear curve. It
menu by should be based on the true
including/excluding value of the standard with the
results to obtain allowable tolerance.
linear calibration
curve.
SRS II / Senior SRS
Determine For a calibration to be

whether No  Add more standard acceptable, the fit of the curve
calibration is runs until calibration should be approaching zero.
acceptable is acceptable
or not.
Yes
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.4
Calibration of SC 432 DR Sulfur Analyzer
 Print the new

calibration and
recalculate the initial
results of the
standard.
 Run check standard
before the analysis
of coal samples, in
between samples
(for more than 4
samples) and after
the analysis of
samples to verify if
calibration done is
okay all through out
the analysis period.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.5
Calibration of Leco Truspec CHN Analyzer
Start
Blank Calibration
Senior SRS Blank calibration is done
 Analyze at least before every analysis.
three acceptable
runs of blank.
 Perform blank
calibration to
compute for the
system blank.
Standard Calibration
Senior SRS Standard calibration is on a
semi-annual basis.
 Analyze standard
samples according
Analyze one standard for
to the method
single-point calibration. At
selected.
least three standard
 Perform calibration
samples for multi-point.
by accessing the
configuration menu.
 Select element to
calibrate (C, H or N)
and the curve type.
 Evaluate the curve fit
by means of root
mean square error.
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.5
Senior SRS The curve fit by means of

root mean square must be
Determine approaching zero.
whether No  Add more standard
calibration is runs until calibration
acceptable is acceptable
or not.
Yes
 Accept and save Senior SRS

calibration.
 Analyze standard
as check sample to
verify calibration.
 Value obtained
must be within the
acceptable range. If
not, perform minor
troubleshooting.
Drift Correction
 Perform drift Senior SRS The drift standard is
correction before automatically selected by
every analysis to the software as indicated
adjust the original by X mark.
calibration response
to match the current
instrument
response.
 Analyze 2-3
standard samples.
B
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 2.5.5
Senior SRS The software will

automatically calculate the
Determine drift correction of the
No  Select last 2 results system.
whether and perform drift
results are correction in the
acceptable configuration menu.
or not.
Yes
 Analyze standard Senior SRS

as check sample.
 Value obtained
must be within the
acceptable range. If
not, perform minor
troubleshooting.
End
Issue Date:
PROCEDURE 01 - 2016
2
Testing Laboratory
Code: SP 3.1
PREPARATION OF TEST REPORTS
Preparation of Final Test Results
This document is already incorporated in SP1.1 Flow of Samples and Documents (One
Loop); subtitle Preparation and Release of Test Report, Page 7 of 8.
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 4.1
RELEASE OF TEST REPORTS TO CUSTOMER
Release of Test Report to Internal Customer
Issue Date:
PROCEDURE 01 - 2016
3
Testing Laboratory
Code: SP 4.2
Release of Test Report to External Customer
Issue Date:
PROCEDURE 01 - 2016
1
Testing Laboratory
Code: SP 4.3
Release of Test Report to External Customer Through Electronic Mail
Start
 Check/confirm the Director of ERTLS Request should be

identity, authority, made via fax or
and rationale of the electronic mail to the
requesting party. OD.
 Approve request.
 Transmit test report EA

electronically
 Keep documents of
transaction on file
End
Issue Date:
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 5.1
MANAGEMENT OF LABORATORY WASTES
Wastes Treatment and Storage
Start
 Conduct analysis.
 Bring the chemical Senior SRS/ SRS II
wastes to the
lavatory.
Sorting is segregating
 Sort the wastes/ Laboratory
the wastes to acid,
select the acidic and Technician
base or heavy metals.
basic wastes and
Acid & base wastes go
heavy metals.
No to neutralization
 Transfer the wastes container, while heavy
to respective B metals go to the 5-gal
containers. B amber bottle.
 Check the volume of
the neutralization
container, i.e., if it
needs emptying.
Yes
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 5.1
Wastes Treatment and Storage
Determine the pH Senior SRS The pH of the

of the accumulated Yes accumulated wastes
wastes in the
should be within 6.5 to
neutralization
container. 6.9 (DENR
recommended limits).
No
B Senior SRS/Laboratory pH should fall within 6.5

 Add lime. Technician to 6.9.
 Dispose the wastes Laboratory Technician

through the sink.
End
Issue Date:
Department of Energy SYSTEMS 01 – 2016
PROCEDURE
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 5.2
STORAGE AND DISPOSAL OF HEAVY METALS
Start
 After transferring the Laboratory Technician

heavy metals to the
appropriate
container/check if
container is full.
 When full, inform/
consult senior SRS
in-charge/ transfer the
container to the
CWSB.
 If total volume allows,

the wastes will be
picked up by a
recognized
transporter/recycler/
treater.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 5.3
Handling of Coal Wastes From Sample Preparation

Details/Emphasis
Start
Waste After Passing

the Riffle
These coal wastes go
 Crush coal into small directly to drum/container
sizes Laboratory Technician for disposal (Note: Coal is
 Pass into a riffle. not hazardous as per
 Set aside the mass on DENR-EMB R.A. 6969 and
the front of the riffle for can be disposed like any
further crushing and municipal waste).
proceed to pulverizing
and quartering.
 Put aside the mass at
the back of the riffle
and transfer more or
less 800 grams in a
plastic bottle (File Coal wastes are disposed
Sample). in designated container,
e.g. drum.
 Gather the remaining
mass and dispose.
Waste After Quartering
 Create a round shape

of the pulverized coal Laboratory Technician
mass.
 Divide into 4.
 Scoop some and put
inside a 50-gram Coal wastes are disposed
plastic vial from two in designated container,
opposite quarters. e.g. drum.
 Gather the remaining
coal and dispose.
End
Issue Date:
PROCEDURE 05 - 2017
2
Testing Laboratory
Code: SP 5.4
Retention and Disposal of Coal File and Analysis Samples
Start
Obtaining Analysis
Sample
 Conduct sample
preparation.
 During quartering,
obtain portions from
two opposite quarters
and place in a 50-
gram plastic vial
(Analysis Sample). Coal wastes are disposed in
 Hand in to analyst. designated container, e.g.
 Dispose of the drum.
remaining coal from
the four quarters.
Monitoring & Disposal Laboratory Technician Six (6) months retention time
of Analysis and File after the release of test
Samples results is implemented.
 Dispose of file sample As coal disposal takes place

with the remaining every end-month, a checking
sample from analysis by the Geo-Coal Supervisor
after the specified will be performed during the
retention time. first week of succeeding
 Update coal waste month.
logbook and record
the sample disposed Coal wastes are disposed in
(lab #, mass and date designated container, e.g.
of disposal should be drum.
reflected).
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 6.1
IMPLEMENTATION OF LABORATORY MANAGEMENT SYSTEM
Management Review of Laboratory Management System
Start
 Prepare areas for Geo-Coal Personnel The Top Management,

review. Quality Manager and
 Propose appropriate Assistant Quality
improvement/s. Manager conduct
meeting every second
semester of the year.
 Review areas and the Top Management

proposed
improvement/s.
 Discuss with the
Quality Manager/
others the possible
courses of actions.
 Select a course of
action.
 Plan and implement

Quality Manager
necessary activities.
 Monitor effectiveness.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 6.2
Maintaining Records of Management Review
Start
 Jot down discussion on Assistant Quality Manager

the review of the
laboratory management
system.
 Affix initials/signature on DC/Quality Manager

the review’s final output.
 Transmit the document to Laboratory Technician
the ODC and OD for
review and approval.
DC/Quality Manager
 Affix signature on the Director/Top Management
review’s final output.
 Transmit the document
back to the Quality
Manager.
 Implement/disseminate DC/Quality Manager

information.
 Keep record of review. Document Control Officer
End
Issue Date:
ERTLS – Geoscientific PROCEDURE Page 1of 1
2
Testing Laboratory
Code: SP 6.3
Submission and Approval of Documents on Quality

(Internal of Laboratory)
Start
 Prepare/submit draft Assistant Quality Manager All management

management system system documents
documents to the should bear the
Quality Manager. initial/signature of the
Quality Manager and
DC of GRFTL.
DC/Quality Manager
 Review draft and
make necessary
corrections. Clerk IV
 Transmit back the
document to the
Quality Manager.
DC/Quality Manager
 Finalize the
document.
 Affix initial/signature. Laboratory Technician
 Transmit revised
document to the ODC
 Approve/affix DC/Quality Manager

signature on the
revised document.
 Transmit the Clerk IV

document back to the
Geo-Coal Section.
End
Issue Date:
2
Testing Laboratory
Code: SP 6.4
Submission and Approval of Documents on Quality

(External Communication)
Start
All management
 Prepare/submit draft Assistant Quality Manager
system documents
management system
should bear the
documents to the ODC.
initial/signature of the
Quality Manager and/or
Head of Geo-Coal, DC
 Review draft and make of GRFTL and Director.
DC/Quality Manager
necessary corrections.
 Transmit document to Copies of outgoing
Clerk IV
the Quality Manager. documents shall be
provided to the
Document Control
Officer.
Quality Manager
 Finalize the document.
 Affix initial/signature.
 Transmit revised Laboratory Technician
document to the ODC.
 Approve/affix signature
DC/Quality Manager
on the revised
document.
Clerk IV
 Transmit the document
to the OD.
 Approve/affix Director
signature.
 Transmit the EA
document back to the
ODC/external party.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 6.5
MAINTENANCE OF EQUIPMENT
Conduct of Preventive Maintenance for Laboratory Equipment

(Furnaces, Ovens, TGA-1000, Parr Calorimeter, SC 432 DR and CHNS TruSpec)
Start
 Receive/log request for GSD

PM.
status of request,
including the winning
bidder.
 Set schedule for the Senior SRS

preventive SRS II
maintenance.
of work rendered by
the service provider,
including the scope
as stipulated in the
contract.
End
Issue Date:
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 6.6
Internal Quality Audit
Start
 Prepare memorandum
for Quality Manager to Internal quality audit is
request for approval of Senior Science conducted once every
schedule and selection Research Specialist third quarter of the
of auditors for the year.
conduct of IQA.
 Select auditors and

approve schedule of Quality Manager
IQA.
 Prepare IQA plan.

 Provide checklist and
reference documents Senior Science
(manuals, reports, Research Specialist
etc.) to auditors.
 Provide program of
audit, including
timetable and Auditors
auditors’ assigned
areas to be assessed.
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 6.6
IMPLEMENTATION OF LABORATORY MANAGEMENT SYSTEMS
Internal Quality Audit
 Conduct IQA:
- Document review
- Pre-audit meeting Auditors Internal quality audit is
- Audit interviews conducted once every
- Post-audit meeting third quarter of the
year.
 Prepare report and

obtain acceptance of Auditors
findings.
Are the findings No  Incorporate agreed

accepted? comments in report.
Yes
 Distribute report.
 Implement and
submit corrective
action report, at an Auditee
agreed timeframe
with the auditors.
 Confirm the clearance

of non-conformities. Quality Manager
 Prepare a final report

of the internal quality Senior SRS
audit.
End
SYSTEMS
01 - 2016
ERTLS – Geoscientific PROCEDURES Page 1 of 2
Testing Laboratory 2
Code: SP7.1
CONTROL OF DOCUMENTS
Document Issuance and Distribution
Start
 Identify the need for Document Requester/Originator All documents must be

a new document prepared with a Document
 Formalize request Issuance / Change Notice
by filling out a DICN Form
form
Document Requester/Originator
 Route the
Affected Personnel
accomplished DICN
form to the affected
personnel for
review/signature
 Submit the request Document Requester/Originator
to the Quality
Manager for
approval
Determine Quality Manager

if request
is  Transmit back to
approved the requester
Yes
A
SYSTEMS
01 - 2016
Code: SP7.1
Document Issuance and Distribution
 Approve/affix
Quality Manager
signature on the
DICN form
 Proceed to create Document Requester/Originator Indicate issue date while
the new document the revision number is
 Submit the new left blank (for new and
document with the not yet revised documents)
DICN to the Quality
Manager for
signature
 Approve/affix Quality Manager

signature on the new
document
 Transmit document
to the Document
Control Officer
Document Control Officer Refer to the Document

 Mark the document Distribution List for the
“CONTROLLED” recipients
 Update soft and
hard copies of the Recipients must affix their
document masterlist signatures on the DICN form.
and revision status
 File the soft copy of
the new document in
the controlled soft
copy files
 Distribute the new
document to
relevant manual
holder
End
Issue Date:
PROCEDURE
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 7.3
Handling of Obsolete Documents
Procedure Responsible Personnel Details
Start
Include in labeling
● Sort documents. Document Control Officer
the section, division,
● Label the
title of the documents
folder/envelope of
and date coverage
the documents.
Refer to the Retention

Determine the and Disposition Schedule
need to channel Of Quality Documents
No
obsolete
documents to The policy of the DOE is
the GSID to channel the obsolete
documents to the GSID
● Store the
documents in the
opposite end of the
Yes staff room.
 Formalize requisition Assistant Quality

to transfer obsolete Manager
document.
 Transmit requisition
to the Office of the
Division Chief.
A
Issue Date:
PROCEDURE
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 7.3
Handling of Obsolete Documents
Office of the
Division Chief
Division Chief
 Approve the request.
 Transmit the request Clerk
to the Document
Control Officer.
 Coordinate with Documentation

GISD. Control Officer
 Make necessary
actions.
 Transfer obsolete
documents.
End
SYSTEMS
01 - 2016
Code: SP7.4
Review of Documents
Start
 Assign document for Assistant Quality Manager All document reviews

review must be done with a
 Acknowledge receipt Sr. SRS / SRS II Document Review Form
of assigned
document for review
 Fill out the

Document Review
Sr. SRS / SRS II
Form
 Review document
 Discuss with
concerned Sr. SRS / SRS II
personnel if the
policies and
procedures stated in
the document are
still suitable or need
revision. Reflect Relevant Personnel
signature
Sr. SRS / SRS II

Does the No
document
need B
revision?
Yes
A
SYSTEMS
01 - 2016
Code: SP7.4
Review of Documents
 Specify in the
“Remarks” portion of Sr. SRS / SRS II
the Document
Review Form that
revision is
necessary.
 Sign in the
“Reviewed By:” Sr. SRS / SRS II
 Sign in the “Noted
Assistant Quality Manager
By:”
 File the Document Control Officer After document review,
accomplished the Document
Document Review Masterlist, Review and
Form and update Revision Status is
review status in the updated.
Document Masterlist
 Proceed with the
revision of the
document.
 Follow the
procedure in SP7.2
End
SYSTEMS
01 - 2016
Code: SP7.4
Review of Documents
 Specify in the
“Remarks” portion of Sr. SRS / SRS II
the Document
Review Form that
the document has
been reviewed and
found suitable
 Sign in the Sr. SRS / SRS II
“Reviewed By:”
 Sign in the “Noted Assistant Quality Manager
By:”
 File the Document Control Officer After document review,
accomplished the Document
Document Review Masterlist, Review and
Form and update Revision Status is
review status in the updated.
Document Masterlist
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 8.1
CONTRACTING COAL LABORATORY SERVICES
Entering Into and Review of MOA/MOU
Start
Make known his/her

 Customer
intention to
coordinates with
collaborate with the
the Office of the
Geo-Coal on specific
Director.
project.
 He writes/makes
letter of intent.
Director The project should

Determine if contribute to national
the proposal No research and growth
is a as well as serve the
worthwhile interest of customer.
endeavor/
consult DC
 Disregard the proposal
 Inform the customer
Yes
 Inform the
customer to make Director
a draft of
MOA/MOU.
 Upon receipt,
review the draft.
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 8.1
 Forward the Director DOE’s Legal

MOA/MOU to the EA Services will review
Legal Services.
and give comments.
 Review/provide
comments to the
contract.
 Transmit the contract
to OD
 Consult DC. Director

 Inform the customer EA
about the comments in
the contract.
B
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 8.1
Determine if
MOA/MOU Yes Director
is
acceptable.
 Inform the
customer.
No End
 Advise the party to

make necessary
actions.
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 9.1
PROCUREMENT OF EQUIPMENT AND SUPPLIES
Inventory of Chemicals and Supplies
Start
 Conduct inventory. Inventory should be

 Take note and mark done every January and
chemicals and other July of the year
supplies that are
nearly depleted.
 Submit the inventory
file to the Senior SRS
of the section.
 Check and sign the Senior SRS

inventory file.
 Transmit back the
inventory file to the
Laboratory Technician.
 Keep the inventory file Laboratory Technician

for everybody’s use
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 9.2
Request for Purchase of Chemicals and Other Supplies
Start
The concerned Analysts

 Inform the Supervisor Senior SRS/SRS II
should inform Laboratory
and Laboratory
Technician about the
Technician of the
depleting item.
depleting item.
 Countercheck the Laboratory Technician
item in the inventory.
 Fill in purchase
request.
 Submit request to the
Supervisor.
Bidding procedure
 Approve and sign the DC
applies when necessary
request.
 Transmit request to Clerk
the GSD.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 9.3
Procurement of Equipment that Provides New Capability for the Laboratory
Start
 Gather additional SRS II, Senior SRS Knowledge on the new

information such as Supervising SRS technology can be
brochure about the obtained through
equipment. attendance to seminars,
 Make strong referrals and researches
recommendation/ through internet and the
justification for the need likes.
to purchase.
 Endorse the DC
recommendation to the
OD.
 Source out budget for Director

the purchase of the
equipment
 Transmit request to
the BD
Upon budget allocation,

succeeding steps follow
the bidding process of
the GSD.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 9.4
Purchase of Replacement of Equipment/Other Apparatus
Start
 Report breakdown Senior SRS or Affected analysis is

of the equipment. SRS II suspended until
 Solicit quotations equipment is repaired
for repair. or replacement
equipment becomes
available.
Service Engineer
Determine if Yes
the cause of
breakdown B
is reparable
No
 Solicit certificate of SRS I

obsolescence.
 Make strong Supervising SRS Certificate of

recommendation/ Obsolescence is an
justification for the attachment in
need to purchase making strong
the equipment. recommendation/
 Transmit justification for buying
papers/documents replacement of
to the ODC. equipment.
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 9.4
Purchase of Replacement of Equipment/Other Apparatus
 Endorse the DC
recommendation to
the Office of the
Director.
 Source out budget for Director

this purpose.
 Upon budget SRS I

allocation, follow
bidding procedure of
the GSD.
End
Yes
 Follow procedures to SRS I

process papers for
equipment repair.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 9.5
Bidding Procedure on Procurement and Repair
Start
 Submit PR/RFS to Supervising SRS Upon submission

ODC attachments include
at least three (3)
quotations for budget
estimate and
 Approve and endorse DC justification.
the request to the OD.
 Sign the request Director

 Transmit to the Budget
Division.
 Allocate funds for the

purchase.
 Transmit request to the
GSD.
 Receive/log the Clerk

purchase request.
 Transmit the request to
the ITD.
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 9.5
BIDDING PROCEDURE ON PROCUREMENT OF EQUIPMENT
 Certify the
correctness of the
information/
specification.
 Determine fund Schedule of bidding

availability and will be published
completeness of through leading
the documents. newspaper for seven
 Provide copy to (7) consecutive days
the chairperson of so that the public
the committee. may know
 Set schedule of
bidding.
 Conduct public
bidding.
 Award the
procurement of
the equipment to
the qualified
bidder.
End
Issue Date:
PROCEDURE 10 - 2017
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 10.1
IMPLEMENTING CORRECTIVE ACTION
Obtaining Test Results Outside Repeatability Range
Start
 Analyze sample using SRS II

applicable test method
(2 – 3 trials).
 Read and record test
results.
 Compare the results
Are the
results No
repeatable? B
Yes
 Take average of the

test results.
 Fill in preliminary test
results form. SRS II
 Affix signature.
 Submit preliminary
report to the Senior
SRS.
End
Issue Date:
PROCEDURE 10 - 2017
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 10.1
Obtaining Test Results Outside Repeatability Range
No
 Discard the test SRS II The results are reported as: on

results. test report under Summary of
 Repeat applicable Results, the phrase, “Successive
test method. This five (5) runs not repeatable”, is
time, analyze 5 indicated and under Remarks/
trials. Attachments are any observation
 Record test results. and the specific values of the five
 Fill in preliminary runs/trials.
test result form,
indicating any
observation,
including the
characteristic of the
sample.
 Affix signature and
submit preliminary
test result.
End
Issue Date:
PROCEDURE 10 - 2015
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 10.2
Addressing Non-conformance in the Laboratory Management System/Others
Start
The Top Management/ Director

All
 Observe/detect any non- of ERTLS, Division Chief/Quality
conformance. Manager, Assistant Quality
 Conduct complete staff work. Manager/Geo-Coal Supervisor or
Assistant Quality
 Confirm/discuss/clarify any of the Geo-Coal members
Manager/Geo-Coal
events that lead to non- can detect and report non-
Supervisor
conformance, its root cause conformity in the laboratory
and impact to customers. management system.
 In case non-conformance Division Chief/Quality

The customer shall be notified
results to suspension of work Manager
through the Office of the Director
or specific service/s, notify
to inform the customer
the customer.
personally or by phone or letter.
 If non-conformance results to
On the other hand, the test
any change in the test report,
report is retrieved through a
retrieve the test report.
letter to the customer.
 Identify corrective actions Assistant Quality Possible corrective actions

and select the most Manager/Geo-Coal are recommended.
appropriate. Supervisor
 Prepare/submit report to the
Quality Manager.
Assistant Quality
Manager/Geo-Coal
Supervisor
Determine
applicability No
of the B
corrective
action
Yes
A
Issue Date:
PROCEDURE 10 - 2015
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 10.2
Addressing Non-conformance in the Laboratory Management System/Others
C
Yes
 Approve/ Division Chief/Quality Monitoring should be

implement the Manager done at least one
corrective action. month after the
 Monitor the implementation of the
effectiveness of the corrective action.
corrective action.
 Resume
work/service/s.
 Audit immediately Internal Quality Auditors

the areas affected
by the
implementation of
the corrective
action.
End
 Re-submit another Assistant Quality

proposal of Manager/Geo-Coal
possible corrective Supervisor
action/s.
C
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 10.3
Control/Prevention of Nonconforming Work on Coal Analysis
Start
 Observe the laboratory Geo-Coal Member

policies and systems
procedures as
imbedded in the
ERTLS Laboratory
Manual for Coal
Analysis.
 Detect potential/on-
going nonconforming Coal Unit Member
work.
 Inform the authorized
personnel regarding
the matter.
 Call a meeting. Assistant Quality The system involves only the

 Decide for final Manager/Geo-Coal flow of activities for coal
intervention. Supervisor analysis .
Need to No
report to DC
B
Yes
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 10.3
Control/Prevention of Nonconforming Work on Coal Analysis
Yes
 Approve corrective DC
action/direct to another
option.
 Transmit back to Geo-
Coal.
No
B
 Communicate to the Assistant Quality Manager/

members of the Coal Geo-Coal Supervisor
Unit for effective
implementation.
 Give DC feedback on
effectiveness of
implementation.
Coal Unit Member
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 10.4
IMPLEMETING CORRECTIVE ACTION
Resolution of Complaint
Start
 Customer fills in a
Complaint Report form
and submits to the OD.
 Receive the report. OD Personnel

 Investigate and inform
the DC/DC relays & DC, Supervising SRS
delegates to
Supervising SRS.
 Call for a meeting. Supervising SRS

 Identify causes and
possible solutions. Geo-Coal Personnel Involved personnel
 Choose the most clarify/discuss the
applicable intervention. complaint
 When necessary,
inform the DC/OD
personnel of the action
to be undertaken.
 Instruct immediate
implementation of the
intervention by the
Geo-Coal.
 Check and monitor
implementation.
 Report the progress to
the DC/OD.
 Contact/notify the Appropriate/delegated
customer of the action. personnel will be the one
to contact the customer.
End
Issue Date:
MANUAL Rev No.:
Research & Fuel
4
Testing Laboratory
Code: SP 10.6
Analysis of Customer’s Feedback
Start
Office of the Director Feedback form is handed in

to internal & external
 Distribute feedback customers who submit
form to a customer. OD Staff samples, inquire on
laboratory testing
 Customer ticks
capabilities/other relevant
applicable factors in
concerns and pick test
the feedback form.
results/request explanation
of test results.
Customer Near the lobby guard

drops filled-
up form at A
the DROP
box.
At OD
A summary is prepared at
Collect feedback forms. Laboratory Technician the end of month.
 Compile in a folder.
 Summarize
feedbacks.
B
Issue Date:
MANUAL Rev No.:
Research & Fuel
4
Testing Laboratory
Code: SP 10.6
 Analyze feedback An average rating of 9 and

Assistant Quality Manager above is excellent/does not
summary.
need corrective action.
Assistant Quality Manager

An average rating of less
Need No
 No corrective action than 9 needs improvement/
improvement?
needed. corrective action.
Yes
C
Issue Date:
MANUAL Rev No.:
Research & Fuel
4
Testing Laboratory
Code: SP 10.6
Lobby guard DROP

BOX:
 Collect feedback HRMD Staff Applicable to laboratory –
forms. testing/personnel/others.
 Transmit to OD.
 Provide photocopy to OD Staff

Geo-Coal Section.
B
Issue Date:
MANUAL Rev No.:
Research & Fuel
4
Testing Laboratory
Code: SP 10.6
Assistant Quality Manager Applicable to laboratory –

testing/personnel/others.
Minor
Major or  Formulate corrective Minor concerns are those
Minor? action/s. involving the attitude of the
attending employee which
are detailed in items 1-3 of
CF12, while major factors
Major
include that of the
laboratory’s technical
 Raise feedback to Assistant Quality Manager competence in terms of
Quality Manager items 3.1.1 – 4.
when necessary and
formulate corrective
action/s.
 Approve corrective Quality Manager/

action/s. Assistant Quality Manager
 Implement corrective Assistant Quality Manager

action/s. Senior SRS
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 10.7
Root Cause Analysis
Start
Define the problem. Asst. Quality Manager, Use of the RCA tools
Geo-Coal member/s and techniques using
flow charts, records,
documents, interviews,
Gather data/evidence. Geo-Coal member/s five whys, cause and
effects, diagramming,
and checklists. Refer
Identify the true root cause to page 2.
associated with the defined Asst. Quality Manager,
problem. Geo-Coal member/s
Identify corrective action(s)

that will prevent recurrence of Asst. Quality Manager, Use of the decision
the problem. Geo-Coal member/s making tools and
techniques using gantt
chart or tree diagram
Implement the corrective

action(s). Asst. Quality Manager, Do the
Geo-Coal member/s countermeasure
Observe the corrective actions

to ensure effectiveness. Asst. Quality Manager Confirm the
effectiveness
If necessary, reexamine the Asst. Quality Manager Act and establish

RCA.
End
Issue Date:
Department of Energy SYSTEMS PROCEDURE 01 – 2016
Page 2 of 2
ERTLS – Geoscientific Research & Fuel Testing MANUAL Rev No.:
Laboratory 1
Code: SP 10.7
Root Cause Analysis

Issue Date:
PROCEDURE 05 - 2017
MANUAL Rev No.:
Research & Fuel
2
Testing Laboratory
Code: SP 11.1
MEASUREMENT OF UNCERTAINTY
Quantifying Uncertainty for Proximate Analysis (Using ISO Method)
Start
 Perform analysis. Senior SRS / SRS II Analysis is performed using

ISO Method. Template is
 Record results in the Senior SRS available for the computation of
template for the uncertainty of measurement for
computation of proximate analysis. Guide to
uncertainty of the Expression of Uncertainty
in Measurement and
measurement for
EURACHEM/CITAC Guide
moisture CG4 are used as references.
determination.
 Specify measurands. Senior SRS Measurands consist of

moisture, volatile combustible
 Identify uncertainty matter and ash.
sources for each
measurand. Sources of uncertainty include
 Simplify grouping analytical balance, ovens and
sources covered by furnaces (translated to mass,
temperature and/or
existing data. repeatability).
 Quantify uncertainty
sources.
 Compute standard
deviation for each Total standard deviation is the
measurand. sum of standard deviations
 Compute total contributed by all sources of
standard deviation. uncertainty.
 Multiply the value by 2. Multiplier 2 can be used on the
 Record the value as basis of 95 percent confidence
expanded uncertainty level.
for moisture.
Revalidation of uncertainty value
 Perform above can be done when necessary/
procedure for volatile preferably 2-3 years after.
matter and ash.
 Prepare computation &

final value & sign. Senior SRS
 Review the value &
submit for approval. Geo-Coal Supervisor
Division Chief
End
Issue Date:
PROCEDURE
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 11.2
MEASUREMENT OF UNCERTAINTY
Quantifying Uncertainty for Calorific Value, Sulfur and Carbon, Hydrogen &
Nitrogen Determinations
Start
 Perform analysis. Analyses are performed using

 Record results in the ASTM methods. Templates are
available for the computation of
template for the Senior SRS uncertainty of measurement for
computation of SRS II the above analyses. Guide to
uncertainty of the Expression of Uncertainty
measurement for in Measurement and
EURACHEM/CITAC Guide
calorific value CG4 are used as references.
determination.
Measurands consist of calorific

 Specify measurands. value, sulfur, carbon, hydrogen
 Identify uncertainty and nitrogen.
sources for each
measurand. Sources of uncertainty include
analytical balance, equipment
 Simplify grouping and certified reference
sources covered by materials (translated to mass,
existing data (type A or temperature and/or
B). repeatability).
Senior SRS
 Quantify uncertainty SRS II
sources. Combined standard uncertainty is
 Compute standard the sum of standard uncertainties
uncertainty for each contributed by all sources of
measurand. uncertainty.
 Compute combined Multiplier 2 can be used on the
standard uncertainty. basis of 95 percent confidence
 Multiply the value by 2. level.
 Record the value as
Revalidation of uncertainty value
expanded uncertainty can be done when necessary/
for calorific value. preferably 2-3 years after.
 Perform above
procedure for sulfur,
carbon, hydrogen and
nitrogen.
End
Issue Date:
1
Testing Laboratory
Code: SP 12.1
HOUSEKEEPING IN THE LABORATORY
Cleaning of Glassware
Start
 After segregation of Laboratory Technician Washing glassware is

the wastes produced done twice a day am and
during analysis, clean pm.
the glassware and
other materials.
 Dry the glassware.
 Place the glassware in
the stock cabinet or
drawer.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 13.1
PARTICIPATION IN INTERLABORATORY PROFICIENCY TESTING
Monitoring Accuracy of Test Results on Coal Analysis
Start
 Plan activities Geo-Coal Supervisor Plan includes timetable,

 Meet Geo-Coal participating
members to inform of organizations and the
the plan. attending Geo-Coal staff
 Solicit comments and and their roles.
suggestions.
 Revise/finalize the plan.
 Submit proposal/plan to
DC.
 Approve proposal/plan. DC
 Coordinate with the Geo-Coal Supervisor Participating organizations

participating include representatives
organizations. from laboratories of
 Organize/conduct government, power plants
meeting. and private laboratories.
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 13.1
PARTICIPATION IN INTERLABORATORY PROFICIENCY TESTING
Monitoring Accuracy of Test Results on Coal Analysis
 Finalize schedule Geo-Coal Supervisor

of proficiency
testing and
deadline of
submission of test.
results
 Prepare sample. Laboratory Technician/

 Inform participating Geo-Coal Supervisor
laboratories to pick
up the sample.
Representatives of As much as possible,

 Pick up sample.
participating the testing on coal
 Conduct analysis.
laboratories analysis by the
 Transmit/submit
laboratories will be
results of analysis.
done simultaneously.
 Consolidate results
Geo-Coal Supervisor
of analysis.
 Perform statistical
evaluation .
 Inform the
participants about
the result of testing.
End
Issue Date:
MANUAL Rev No.:
Research & Fuel
1
Testing Laboratory
Code: SP 14.1
DEVELOPMENT OF LABORATORY PERSONNEL
Identifying Training Needs
Start
Laboratory personnel know

 Solicit training Supervising SRS their skill/training
requirements from inadequacy in performing
laboratory personnel. their functions
 List down specific Geo-Coal Member/s

training needs.
 Submit to the Head of
Geo-coal Section.
 Assess training needs Supervising SRS Assessment/evaluation

of each laboratory is based on current work
personnel. assignments and the
 Submit list of performance of such
recommendation to the assignments.
DC.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 14.2
Providing Training to Personnel/Nomination and Selection
Start
The memorandum
 HRMD routes to the
specifies the details of
Director of every
the training including
bureaus/services
title, date, venue,
memorandum inviting
sponsor, and training
nominees for specific
requirements
course.
 Receive/log the EA
memorandum in the
logbook.
 Route the
memorandum to DC.
 Receive the memo DC

 Collaborate with the
Director
 Route the memo to
supervisor of each
section
A
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 14.2
 Identify nominee/s from Supervising SRS Selection of candidate

the Geo-Coal must be based on
 Justify nomination applicability/requirements
 Submit justification/letter of his/her current job.
to the DC
 Receive/log request for DC

nomination.
 Approve nomination
 Route request for
nomination to the OD.
 Receive/log request for Executive Assistant

nomination.
 Approve nomination. Director
 Route request for
nomination to HRMD
B
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 14.2
 Receive/log request for

nomination.
 Select candidate for Selection of candidates/
training. nominees from other
 Inform the candidate to bureaus/ services will be
submit supporting subjected to deliberation
documents. by PDC.
 Transmit training
documents to the
sponsoring agency.
 Inform the candidate of
his/her selection to
participate in the training.
 Submit additional training Geo-Coal Member Training report should be

documents. /Participant submitted 1-3 working
 Participate in the training days upon reporting to
course. work .
 Submit training report.
 Perform echo seminar.
End
Issue Date:
PROCEDURE 01 - 2016
MANUAL Rev No.:
Research & Fuel
3
Testing Laboratory
Code: SP 14.5
APPLYING FOR LOA BY LABORATORY PERSONNEL
Request for Leave of Absence/Sick Leave
Start
 Call up or text a
message to inform
Supervising/Senior
SRS reason for LOA.
 When back to work, fill Geo-Coal Member
up LOA form.
 Submit form to Head
of Geo-coal section.
 Approve the request Geo-Coal Supervisor

for leave of absence
 Approve/sign the form.
 Submit the request to
the ODC.
 Approve the request. DC

 Route the request to
the HRDD.
End
Issue Date:
Department of Energy COAL 01 - 2016
MANUAL
1
Testing Laboratory
Code: CP1
SAMPLE PREPARATION
Preparation of Coal Sample/s for Analysis

Adopted from ISO 5069
1 Preparation of Laboratory Sample
1.1 The sample for analysis for residual moisture, volatile matter and ash; sulfur;
mercury; carbon, hydrogen and nitrogen; and calorific value, not including HGI,
shall be milled to below 0.212 mm (212 um or sieve size No. 70.
2. Apparatus
2.1 Air-drying
2.1.1 Air drying oven. A device for passing slightly heated air over the sample. The
oven shall be capable of maintaining a temperature of 100C to 150C above room
temperature with a maximum oven temperature of 400C, unless ambient
temperature is above 400C, in which case ambient temperature shall be used. In
case of easily oxidized coals, the temperature shall not be over 100C above room
temperature. Air changes shall be at the rate of 1 to 4 per minute.
2.1.2 Drying floor. A smooth clean floor in a room free of dust and excessive air
currents.
2.1.3 Drying pans. Non-corroding metal pans of sufficient size so that the sample may
be spread to a depth of not more than 25 mm with sides not more than 38 mm
high.
2.1.4 Gross sample scale. A scale of sufficient capacity and sensitive to 0.025 kg in
50.00 kg.
2.1.5 Laboratory sample balance. A balance of sufficient capacity to weigh the

sample and container with a sensitivity of 0.5 g in 1000 g.
2.2 Crushing and Grinding
2.2.1 Jaw, cone, rotary crusher, hammer mill or other suitable crusher may be used to
reduce the sample to pass the sieve size in 1.1. Hard steel, chilled iron plate
with tamper, sledge or hand bar may be used for preliminary crushing of any
large lumps in the sample before feeding into the crusher.
2.3 Pulverizing or Milling
2.3.1 For final reduction of laboratory sample to pass 212 um (sieve size No. 70),
milling equipment may be used:
Issue Date:
Code: CP1
SAMPLE PREPARATION

2.3.1.1 Hammer mill. This should be completely enclosed to avoid loss of dust or
moisture.
2.3.1.2 Porcelain jar ball mill. This mill shall be approximately 230 mm in diameter and
250 mm in height with smooth, hard, well rounded, flint pebbles or equivalent,
which do not appreciably increase the ash content of the sample.
2.4 Refining
2.4.1 Bucking board (chrome steel) or mortar (agate or equivalent) and pestle. For
reducing the small fractions of the sample that do not pass no. 70 sieve after
pulverization.
2.5 Dividing
2.5.1 Mechanical divider. A mechanical sample divider using a reciprocating or

rotating cutter, a rotating hopper and spout, a rotating slotted cone, or other
acceptable devices for dividing the sample.
2.5.2 Riffle. A manual sample divider that splits the coal stream into a number of
alternate elements. Riffle divisions should be at least three times the top size
of coal being divided. It is preferable that feed chutes and enclosed riffles be
used. The slope of feed chutes and riffles must be at least 600.
2.5.2.1 Feed scoop. A feed scoop or pan having straight sides and equal to the
effective width of the riffle shall be used to feed the stand-type riffle.
2.5.2.2 Feed chute. The discharge opening of the feed chute shall be the same
width as the riffle opening.
2.6 Mixing
2.6.1 Mixing wheel. One type of a mechanical device used for mixing the analysis
sample. In this device, the samples are in closed containers attached to the rim
of a wheel at an angle of 450 with the horizontal wheel shaft. The wheel
provides space for a number of containers depending on its diameter and is
turned slowly by a small motor and reduction gear. The wheel should be
rotated at a speed so that the particles fall gently from top to bottom of the
container, mixing the sample thoroughly. The container should be about half
full and never more than two thirds full in order to obtain good mixing of the
sample.
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP1
SAMPLE PREPARATION

2.7 Sizing or Sieving
2.7.1 A sieve of 212 um aperture is used.
2.8 Packaging
2.8.1 Heavy vapor-impervious bags, properly sealed, or non-corroding cans such as

those with an airtight, friction top or screw top sealed with a rubber gasket and
pressure-sensitive tape may be used to store and transport the laboratory
sample. Glass containers, sealed with rubber gaskets, may be used, too, but
care must be taken to avoid breakage during transport.
3 Precautions
3.1 The preparation of the gross or divided sample shall be done by trained and
experienced personnel. The sample preparation operation should be performed
in an enclosed space, roofed, cool and free from excessive air movements.
3.2 Before preparing the gross or divided sample, the number and nature of the
analysis and tests should be considered. A separate moisture laboratory sample
may be required, and portions may be required for grindability and other tests.
Also, a reserve sample may be desired in case a check analysis or test is
required.
3.3 Since most coals oxidize on exposure to air, the air-drying procedure should not
be prolonged past the time necessary to bring the temperature of the moisture to
equilibrium with the air in the room in which further reduction and division are to
be made. The sample shall be allowed to attain room temperature before
weighing and further reduction.
3.4 In collecting, handling, reducing and dividing the sample, all operations shall be
done rapidly and in as few operations as possible since moisture loss depends on
several factors other than total moisture content such as time required for
crushing, atmospheric temperature and humidity and type of crushing equipment.
3.5 While awaiting preparation, the uncrushed gross or divided sample shall be
protected from moisture change due to exposure to rain, wind, and sun or contact
with absorbent materials.
3.6 Whenever sub-samples are stored or transported, the containers and sub-sample
shall be weighed, equilibrated to the new atmosphere by air-drying and the weight
loss or gain shall be used in the calculation of moisture content.
Issue Date:
Department of Energy 01 - 2016
ERTLS – Geoscientific PROCEDURES
Page 4 of 5
1
Testing Laboratory
Code: CP1
SAMPLE PREPARATION

3.7 Whenever a distinct change of humidity occurs during the course of the
preparation of an air-dried sub-sample, the sub-sample should be weighed and
its moisture equilibrated with the new atmosphere and the weight loss or gain
shall be used in the calculation of moisture content.
4 Procedure
4.1 Weighing
4.1.1 The minimum allowable weight of the sample at any stage depends on the size
consist, the variability of the constituent sought, and the degree of precision
desired.
4.2 Air Drying
4.2.1 Gross or Divided Sample
4.2.1.1 Weigh and spread the sample in pans. The coal may be stirred, without loss
of particles, to speed up air-drying.
4.2.1.2 Continue air-drying until the loss in weight of the total gross or divided sample
is not more than 0.1% per hour. Avoid excessive drying time.
4.2.2 Laboratory Sample
4.2.2.1 Weigh the sample, plus pan, plus container, if one is used. Spread the sample
in the pan to a depth not to exceed 25 mm.
4.2.2.2 Place the pan in the oven, together with the container and air-dry until the loss
in weight is not more than 0.1% per hour. Avoid excessive drying.
4.2.2.3 If an oven is not available, the sample may be air-dried in a room free from
dust & excessive air currents. Stirring at intervals will lessen air-drying time.
4.2.3 Reduction and Division
4.2.3.1 Samples may require air-drying in order to feed properly through the reduction
and dividing equipment.
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP1
SAMPLE PREPARATION

4.2.3.2 Manual Rifling
Divide the crushed sample by using a large riffle. Riffles properly used will
reduce sample variability but cannot eliminate it. Pass the coal through the
riffle from a feed scoop, feed bucket, or riffle pan having a lip or opening the
full width of a riffle. When using any of the above containers to feed the riffle,
spread the coal evenly in the container, rinse the container, and hold it with its
front edge resting on top of the feed chute, then slowly tilt it so that the coal
flows in a uniform stream through the hopper straight down over the center of
the riffle into all the slots, thence into the riffle pans, one-half of the sample
being collected in a pan. Under no circumstances shovel the sample into the
riffle, or dribble into the riffle from a small-mouthed container. Do not allow
the coal to build up in or above the riffle slots. If it does not flow freely
through the slots, shake or vibrate the riffle to facilitate even flow.
4.2.3.3 With suitable pulverizing equipment, reduce the sieve size sub-sample to
lower than No. 70 (212-um) sieve size. Divide the ground sub-sample until a
minimum of 50 g is obtained.
5 Calculation of Air-Drying Loss (ADL)
Calculate ADL, in % mass fraction, as follows:
ADL = {(b1 - bf)/b1} x 100
Where: b1 = mass of sample before drying, in grams

bf = mass of sample after constant drying, in grams
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP1a
COAL SAMPLING
Collection of Channel Samples of Coal From Coal Seam

Adopted from ASTM D 4596-99
1. Apparatus and Materials
 Measuring device, not less than 3 meters long

 Miner’s pick or similar tool, with file for sharpening
 Brush or broom, for removing loose particles on the coal face
 Chalk
 Sample containers with cover
 Ground cloth- canvas tarpaulin or heavy-duty plastic sheet about 3X3
meters
 Tags and pen, for sample identification and marking
 Shovel
 Notebook and pencil, or other means for record keeping.
2. Procedure
2.1 At each sampling site, survey the condition of the coal face and the rock
above the coal (if exposed).
2.2 With a miner’s pick, remove weathered coal from the face area to be sampled,
to the depth (but at least 3 cm) required in the plan of sampling. True up to the
face to leave a straight surface normal to the bedding and free of extraneous
matter.
2.3 Describe and record observations on the character of layers in the coal seam
to the extent required by the sampling plan.
2.4 Mark the sides of the channel with chalk and mark any mineral partings or
other parts of the seam that are to be discarded.
2.5 Clear and smooth the floor adjacent to the sample area and spread a ground
cloth on the floor with one edge at the coal face.
2.6 Cut away with a miner’s pick (or other tool) a channel from top to bottom (or
bottom to top) of the coal seam. If a saw is used at the sides of the channel,
exercise care that fines generated by the saw do not become part of the
sample. Ensure that all material from the channel that is to be sampled
according to the plan of sampling falls on the ground cloth and that any
material matter to be discarded does not contaminate the coal
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP1a
COAL SAMPLING
Collection of Channel Samples of Coal From Coal Seam

Adopted from ASTM D 4596-99
sample. Cut the channel to a uniform width and depth in a rectangular cross
section, to ensure that representative volumes of material are obtained from
every part of the coal seam.
2.7 As quickly as possible, transfer the material on the ground cloth to a sample
container and seal and then label the container.
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP1b
SECONDARY STANDARD
Preparation of Coal Secondary Standard
1 Collection of Bulk Sample
1.1 Collect 5-10 kg of coal according to Coal Sampling Procedure (Collection of

Channel Samples of Coal from Coal Seam Adopted from ASTM D 4596-99/CP
1a).
2 Preparation of Sample
2.1 Prepare the sample according to Preparation of Coal Sample for Analysis
Adopted from ISO 5069 (CP1). For every five (5) kg of sample to be
prepared, fill fifty (50) vials to about three fourths each.
2.2 Assign label for each vial of sample prepared.
2.3 Fill each vial of prepared sample with nitrogen gas and store inside
dessicator/dessicabinet to minimize oxidation.
2.4 Perform randomization of the 50 vials using random function in MS Excel or

the random sequence generator at www.random.org/integer for no duplicate
samples.
2.5 As a preliminary check, choose 2-3 vials of the prepared sample and analyze
for volatile combustible matter content.
Compare and evaluate the results obtained to check if sample is sparking or

not. Sample is sparking if there is ash deposit present outside the walls of the
crucible and its cover and if the results obtained show significant difference
between replicates (results are not repeatable). Sparking coal sample is not
recommended for secondary standard.
3 Homogeneity Test
3.1 Determine the suitability of the sample for the test method and check if the
sample is sufficiently homogenous by performing homogeneity test.
Please refer to Appendix XI: Test for Homogeneity according to ASTM D

6796-02 Standard Practice for Production of Coal, Coke and Coal
Combustion Samples for Intelaboratory Studies, Annual Book of ASTM
Standards 2006 and/or to the Manual written by Dr. Rudy H. Tan,
Understanding Proficiency Testing Schemes for Coal, pages 27-29.
For this procedure, analyze five (5) vials of the prepared sample for proximate
total sulfur and/or heating value.
Issue Date:
Code: CP1b
SECONDARY STANDARD
Preparation of Coal Secondary Standard
3.2 If sample is homogenous, proceed to analysis of required parameters.
3.3 If sample is not homogenous, remix sample from all prepared vials to make it
homogenous and repeat 3.1.
4 Analysis
4.1 Analyze three (3) vials of the prepared sample (10 trials for each vial) for
residual moisture, volatile combustible matter, ash content and other desired
parameter/s.
4.2 Check for repeatability and reproducibility.
4.3 Compute for the average and standard deviation of all the results (30 trial
runs) obtained.
4.4 Calculate for the minimum and maximum tolerance using formula 2 x
standard deviation.
5 Stability Check
5.1 Perform stability check to ensure that no changes occur in the coal secondary
sample.
Please refer to the Manual written by Dr. Rudy H. Tan, Understanding

Proficiency Testing Schemes for Coal, page 30 – Stability Check for
Proficiency Testing Samples.
As much as possible analyze all the parameters determined during

homogeneity test. Evaluate results of analysis.
5.2 If the sample is stable, continue using the secondary standard.
5.3 If the sample is not stable, discard and prepare new secondary standard.
Issue Date:
Department of Energy COAL 01 – 2016
MANUAL
Code: CP2
SIEVE ANALYSIS
Performing the Sieve Analysis of Coal and Designating Coal Size

1 Scope
Raw and prepared (crushed, cleaned or screened) coals can be tested by this
method. The test method is not applicable for determining the sieve analysis nor
for designating the size of pulverized coal. Size fractions down to and including
38 um can be treated under this method.
2 Sieve Analysis of Coal
2.1 Apparatus and Materials
 Sieves - Available are 2 in. (50.8 mm), 1.5 in. (38.1 mm), 1 in. (25.4 mm),
3/8 in. (9.5 mm), 4.75 (#4), 2.36 (#8)
 Mechanical sieve shaker
2.2 Weight of Gross Sample
2.2.1 The weight of the gross sample shall be 10 kg.
2.2.2 In order to divide the gross sample into test samples, do sample division in
accordance with ASTM D 2013.
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

01.3.1.1 Samples may be

divided according to the following schedule:
 Coal Larger than 25 mm (1 in.) Round – Sieve without mixing or dividing

 Coal Smaller than 25 mm (1 in.) Round – Divide in amount to not less than
56.6 kg (125 lb) by riffling or by arranging the sample in a long, flat pile and
successively halving it or quartering it by the alternate-shovel method as
follows: Starting at one end of the long pile, take successive shovelfuls
from the long pile using a flat, straight-edged shovel (advancing a distance
equal to the width of the shovel for each shovelful), and retain alternate
shovenfuls or every fourth shovelful for the sample.
 Coal Smaller than 12.5 mm (1/2 in.) Round – Divide to not less than 11.4
kg (25 lb) by passing through a riffle or equally accurate dividing device, or
by the alternate-shovel method.
 Coal Smaller than 4.75 mm (No. 4) Sieve – Divide to not less than 1000 g
(2 lb) by riffling.
 For anthracitic coal, the laboratory samples for sieving shall consist of the
following min. amounts:
Pea (passing-21mm, 13/16 in. & retained on-14 mm, 9/16 in.) – 22.7 kg/
50 lb
Buckwheat #1 (14 mm, 9/16 in. & 8 mm, 5/16 in.) – 11.3 kg/25 lb
Buckwheat #2/rice (8 mm, 5/16 in. & 4.8 mm, 3/16) – 4.5 kg/10 lb
 For sizes larger than pea & smaller than buckwheat # 2 (rice), use the ff.:
Run-of-mine coal – Not < 1,800 kg (4,000 lb)

Screened coal w/ upper limit larger than 100 mm (4 in.) round – Not <
1,800 kg (4,000 lb)
Coal smaller than 100 mm (4 in.) round – Not < 900 kg (2,000 lb)
Coal smaller than 50 mm (2 in.) round – Not < 450 kg (1,000 lb)
Coal smaller than 25 mm (1 in.) round – Not < 215 kg (500 lb)
Coal smaller than 12.5 mm (1/2 in.) round – Not < 45 kg (100 lb)
Coal smaller than 2.36 mm (No. 8 mesh, USA Standard) – Not < 4.5 kg (10 lb)
Coal smaller than 600 um (No. 30 mesh, USA Standard – Not < 0.5 kg
(1lb)
01.3 Procedure
2.3.1 General Considerations
2.3.1.1 Accurately weigh the test sample before sieving. Weigh with a precision equal
to or better than 0.5% of the fraction being weighed.
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

2.3.1.2 Start with the sieve having the largest required aperture (for an exception,
please see 2.3.1.8).
2.3.1.3 Limit the portion of coal used for each sieving so that all coal particles will be in
direct contact with the aperture at the completion of sieving on each successive
sieve.
2.3.1.4 Sieve until all portions of the sample are used. Combine all separately sieved
material representing a particular size-fraction but obtained from sieving
separate portions of the same sample.
2.3.1.5 Whenever sieving through a series of sieves and the larger particles have been
sieved from the test sample and the weight of the smaller sieve fraction(s)
exceeds the weight for that fractions(s) as given in 2.2.2.1, it is permissible to
divide the remaining portion of the test sample (the smaller sieve size) to not
less than that weight given in 2.2.2.1 before sieving at the smaller sieve sizes.
2.3.1.6 Continue sieving with successive sieves having the desired size apertures until
the sieve having the smallest desired size aperture is used.
2.3.1.7 Sieving can be done by grouping sieves having the desired size apertures, thus
accomplishing the sieving in one operation known as nesting.
2.3.1.8 When utilizing smaller mesh sieves, especially when wet-sieving, use the
smallest sieve first in order to remove clays and other extremely small materials
that may blind and clog the largest mesh sieves, that is, when both 150 um
(No. 100) and 75 um (No. 200) sieves are used, use the latter first in order to
facilitate sieving. Additionally, where larger particles are present that can
adversely affect the size of the sieve openings, use a cover sieve (protective
sieve of a larger mesh) to keep coarse particles off the finer sieves.
2.3.1.9 Where possible, use sieve covers on sieve apparatus to limit dust & particle loss.
2.3.1.10 Weigh each size fraction of sieved coal with a precision equal to or better than
0.5% of the fraction being weighed.
2.3.1.11 Note that the objective of shaking, either manually or mechanically, is to place
all of the pieces of a given size on the appropriate sieve and to avoid size
degradation. Coal particles greater than 600 um (No. 30) are particularly
susceptible to attrition: therefore, avoid excessive sieving time and amplitude.
Please see 2.3.3.4.
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

2.3.2 Hand Sieving
2.3.2.1 Hand sieve with a reciprocating, horizontal motion so that a particle travels over
a distance of not more than 200 mm (about 8 in.). The maximum particle size
travel distance shall be 100 mm (4in.) or less for 203-mm (8-in.) diameter sieves
and 37.5 mm (1.5 in.) or less for 75-mm (3-in.) diameter sieves. Take care to
prevent any of the coal particles from fracturing upon impact with the sieve frame
or with other coal particles.
2.3.2.2 Manual (hand) sieving is performed slightly differently depending on the size of
the particles.
2.3.2.3 For coal larger than 63 mm (2 ½ in.) round – Manipulate pieces of coal not
passing readily through sieves 63-mm (2 ½ in.) round and larger to see if they
will pass through the opening in any position. Do not shake sieves (63-mm (2 ½
in.) round and larger except for whatever jiggling may be necessary to clear the
sieves of fine coal.
2.3.2.4 For coal smaller than 63 mm (2 ½ in.) round but larger than 6.3 mm (1/4 in.)
round – Test coal passing the 63-mm (2 ½ in.) round sieve with sieves down to
and including 6.3 mm (1/4 in.) round as follows: Move the sieve horizontally a
distance of about 200 mm (8 in.0 at just a sufficient rate to cause the pieces of
coal to tumble or roll the sieve. Stop the motion of the sieve without the impact.
After ten such shakes (five in each direction), sieving of the increment is
complete.
2.3.2.5 For coal particles smaller than 6.3-mm (1/4-in.) round – Use wire cloth sieves
with square openings (see Table 1). Place the test sample on a clean dry sieve
with the pan attached. Make, or at least, complete, the test on one sieve at a
time (11.2.7). While holding the uncovered sieve and pan in both hands, sieve
with a gentle rotary motion until most of the finer material has passed through
and the residue looks fairly free of finer particles. This operation usually takes
only 1 or 2 min for sieves coarser than 150 um (No. 100) and 3 or 4 min for
sieves 150 um (No. 100) and finer. (4.75 #4 and 2.36 #8)
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

2.3.2.6 When the residue appears to be free of finer particles, replace the cover on
the sieve and carefully separate the sieve from the pan. Place the sieve onto
a second pan that is clean and dry. Temporarily cover and move the original
pan with contents aside. Hold the sieve, cover and pan firmly in one hand,
gently tap the side of the sieve with the handle of the brush used for cleaning
sieves. Dust adhering to the sieve and particles in the mesh will be
dislodged by this action. Brush the underside of the sieve. Note: Particles
could be lost while inverting the sieve or be trapped or broken. As an
alternate procedure, the underside can be brushed by tilting the sieve to
about a 30o angle.
2.3.2.7 Replace the empty can onto the sieve and restore the assembly to an upright
position. Tap the cover lightly and carefully remove the cover. Replace onto
the sieve any coarse material remaining in the cover. Set the cover aside.
2.3.2.8 Continue the sieving without the cover, as described in 2.3.2.5 and 2.3.2.6,
until not more than 1 mass percent of the material passes any sieve during 1
min of sieving operation. Combine any additional pan residue to the
contents of the original pan temporarily set aside in 11.2.5.1 as product for
eventual weighing. The gentle sieving motion involves no danger of spilling
the residue, which is to be kept well distributed on the sieve. Continuously
rotate the sieve during the sieving.
2.3.2.8.1 To determine when sieving is completed, perform the following End-Point

Test: 20o from the horizontal. Move the sieve up and down in the plane of
inclination at the rate of about 150 times per minute and strike the sieve
against the palm of the other hand at the top of each stroke. To avoid losing
particles that pass between the lid and the sieve, perform the sieving over a
light-colored surface that will allow these particles to be seen and recovered.
Return any material collecting on the surface to the sieve.
2.3.2.8.2 After every 25 strokes, turn the sieve one sixth of a revolution in the same
direction. As an aid to proper sieve rotation, mark the sieve cover with three
straight lines, intersecting at 60o through the center, with one of the lines
marked with an arrowhead to indicate the starting point.
2.3.2.8.3 Continue the sieving operation until the additional material, which passes
through in 1 min of continuous sieving fails to change by more than 10% the
amount of material on that sieve. Remove material from the sieve as
described in 11.2.5.1. Weigh and record the masses of these final sieve and
pan products.
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

2.3.2.8.4 Hand sieving is the original basic method of making sieve analysis and can
be used to check (calibrate) mechanical sieving results. In hand sieving, the
tests are made, or at least completed on one sieve at a time, that is, when a
nest or stack of sieves is used initially, the test must still end with each
individual sieve being treated in the manner prescribed in 2.3.2.8.3.
2.3.2.8.5 Consistency importat to hand sieving - The operator should try to be

consistent with the hand sieving method to always reproduce the same
circular motion and tapping action.
2.3.3 Mechanical Dry Sieving
2.3.3.1 When sieving with the assistance of a mechanical sieve shaker, adhere to
the general considerations given in 2.3.1.
2.3.3.1.1 When using mechanical sieve shakers, determine the length of sieving time
best suited to the type of coal being tested, and, for shakers with variable
controls, determine and establish the exact setting of the controller for best
results, based on repeatability and completeness of serving without
degradation. Please see 2.3.3.4.
2.3.3.2 For routine plant control tests, 3 to 5 min is usually sufficient to give the
desired result, while for other materials a sieving time of from 10 to 30 min is
necessary. Avoid prolonged sieving time when testing friable materials
subject to degradation. Please see 2.3.3.4.
2.3.3.3 To determine the sieving time necessary to produce acceptable analytical

results, use the following procedure: from a gross sample; with the use of a
sample divider, select four sub-samples of a suitable mass or volume for the
test. Sieve one of these samples for 4 min, a second for 10 min, a third for
15 min, and a fourth for 20 min. Tabulate the results of these tests by the
percentages retained on each sieve, and the length of sieving result will be
readily apparent and can be established.
2.3.3.4 For most tests, a satisfactory time has been used when an additional 1 min
of sieving fails to change by more than 1.0% the mass on any of the sieves
used.
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MANUAL
Code: CP2
SIEVE ANALYSIS

2.3.3.5 Sieve tests where the ultimate in precision is desired can be set up on the basis
of shaking the nest of sieves until not more than 0.5% of the material on the
finest sieve passes that sieve in a 5-mm period. This is a good technique to
follow when no control can be made on the type of mechanical sieve shaker to
be used, or when hand and mechanical serving are used interchangeably.
2.3.4 Wet Sieving
2.3.4.1 Generally, do test sieving on air-dried (dry) material; however, if difficulty is

encountered in obtaining reproducible results on materials below 600 um (No.
30 USA Standard) and if the material is not altered physically in water, more
accurate tests can be made by the wet method.
2.3.4.2 Wet sieving is required in any of the following circumstances:
2.3.4.3 The material to be sieved cannot be dried because of expected deterioration or

agglomeration.
2.3.4.4 The material is extremely fine and static electricity does not allow the material
to be effectively dry-sieved.
2.3.4.5 Fine particles cling to coarse particles and the fine particles cannot be
accurately sized with dry-sieving.
2.3.4.6 Clays are present.
2.3.4.7 In preparing for a wet sieve test, dry the sample to a constant mass at a
temperature not to exceed 40oF (104oF). Avoid sample degradation that can
be caused by oven-drying. Weigh the residue to the nearest 0.1 g. When the
material readily mixes with water, place the test sample on the finest sieve, and
wash it back and forth with a gentle stream from a hose in such a way that
there is no loss by rising dust or splashing. For some coals, it may be
necessary to use a wetting agent, such as isopropyl alcohol. When the water
passing through the sieve is clear, dry the sieve containing the residue in an
oven, if possible, to a constant mass and temperature not to exceed 40 o C
(104o F). Avoid sample degradation that can be caused by over drying. Weigh
the residue to the nearest 0.1 g. Then, repeat this procedure on the coarsest
sieve and then again on each sieve in descending size until the finest sieve
again is reached. Combine the two segments passing the finest sieve.
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

2.3.4.8 This drying time will vary with the size of the sample and the characteristics of
the coal and should be established by a series of weighing checks at intervals
until no significant change occurs less than 0.1% of previous weight. Please
see Method D 2014.
2.3.4.9 When the material does not mix well with water, first place the dried, accurately
weighed sample into an appropriate container and fill the container about three
quarters-full of water. Shake contents vigorously to mix the material with the
water. Pour this mixture onto the sieve and perform the washing process as
described above. The use of a wetting agent, such as isopropyl alcohol,
providing said reagent causes no interference with sieving, can avoid this
operation.
2.3.4.10 It is possible to perform wet sieving with a nest of sieves with a mechanical
sieve shaker by equipping the shaker so that a small stream of water can be
received through the top and drained from the bottom pan after passing
through the nest.
2.3.4.11 When wet sieving, adhere to the general considerations given in 2.3.1.
2.3.5 Combined Wet and Dry Sieving
2.3.5.1 When a sieve analysis to be made with a nest of sieves cannot be done on a
dry basis because of the presence of fine particles which either agglomerate,
adhere to the coarser particles, or cause blinding to the sieve openings,
remove the fine particles first by wet sieving and then perform the rest of the
analysis on a dry basis.
2.3.5.2 In the combined wet and dry method, in order to remove clays and other
materials that blind or clog the larger mesh sieves, test the sample first on the
finest sieve using the wet method as described in 2.3.4.7 (use a protective
sieve of larger mesh above the finest sieve to prevent damage to the finest
sieve). Dry the coarse residue and sieve while dry in accordance with the
appropriate method in 2.3.2 & 2.3.3. Express percentage results in terms of
the original dry mass of the test sample before wet testing.
2.3.6 Calculation
2.3.6.1 Calculate the sum of the size fraction masses from 2.3.1.9 and call the sum the
combined mass.
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MANUAL
Code: CP2
SIEVE ANALYSIS

2.3.6.2 Convert all masses to the same units before calculation that is, kilograms,
grams.
2.3.6.3 Convert and utilize the masses of the size fraction by both multiplying and
making proper use of significant figures. For example, if a size fraction weighed
11.35 kg, another 204 g, and another 148 g determine all the masses to the
nearest 0.01 kg (since 11.25 kg is reported to the nearest 0.01 kg) before
proceeding with calculations, as: 11.25 kg + 0.20 kg + 0.15 kg = 11.60 kg.
2.3.6.4 If the percentage mass loss or gain is over 2%, reject the analysis and make
another test. The formula for the calculation of the percentage mass loss or gain
is as follows:
{( Mf - M i ) /M i } 100 = % M
Where: Mf = combined air-dried mass of the size fractions, g (oz);

M i = air-dried mass of gross sample prior to sieving, g (oz) and
% M = % mass loss or gain upon sieving, g (oz)
A mass gain will result in a positive percent while a mass loss will result in a
negative percent. For sub-bituminous coals, incorporate inherent moisture into
these calculations if required.
2.3.6.5 If the variation is greater than the above tolerance of 2%, recheck the figures for
possible errors in determining mass, calculating, blinding of the sieve apertures
or accidental spillage. If calculation, transcription, or other error is detected and
correctable, correct the error. If the resulting variation from initial sample weight
is within the 2% tolerance, accept and report the corrected results. If the source
of error is not detected or if it is detected but uncorrectable, repeat the test.
Note: In wet sieving, there is often a high volume of water-coal-mineral slurry
passing through the finest sieve. In some cases, where it is appropriate,
flocculants can be added to the material passing the finest sieve during wet-
sieving to facilitate settling of those solids. Note: When working with small
samples or when using 75-mm (3-in.) sieves, it is desirable to determine a tare
mass for each sieve and pan.
2.3.6.6 Convert the mass (in 2.3.1.10) of an individual size fraction to a percentage
basis by dividing the mass of that portion by the combined fractional masses, or
by the original mass and multiplying by 100. Calculate each mass (weight)
percent to the nearest 0.01% and then round to the nearest 0.1%.
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

3 Designation of the Size of Coal from Sieve Analysis Data
3.1 Size Designation
3.1.1 The size designation result applies only to natural continuous range of sizes as
produced by mining, handling, crushing, screening and beneficiation.
3.1.2 The designation shall indicate the range of the size by giving the upper and
lower limiting sieves (top-size and bottom-size) between which 805 or more of
the sample is retained as determined by the actual test data.
3.1.3 The sieve defining the upper limit shall be the smallest sieve of the series upon
which is retained a total of less than 5% of the sample.
3.1.4 The sieve defining the lower limit shall be at the largest sieve through which
passes a total of less than 155 of the sample. Note: By contractual agreement,
the percents used to designate top-size and bottom-size may be changed to
meet specific requirements.
3.1.5 The terms for defining sizes shall be written with the upper limiting sieve first,
followed by an “X” and finally the lower limiting sieve. The abbreviation “mm” or
“in” shall follow the lower limiting sieve but may be omitted after the upper
limiting sieve. For sieves of the USA Standard or Tyler sieve series (No. 4 and
smaller), the abbreviation “No.” or the word “mesh,” respectively, shall be used
each time a sieve is indicated. Note: Care must be taken to designate the
standard source of the sieve, for example, Tyler or U.S. A. standard, in order to
correlate the sieve number with the diameter of the openings.
3.1.6 When the total retained on the 200-mm 98-in.0 sieve is 5% or greater, the size
shall be designated by reporting the lower limiting sieve preceded by “200 mm (8
in.) x” and followed by an expression in parentheses giving the percentage over
200 mm (8in.) to the nearest 1%.
3.1.7 The size fraction of material which passes through the smallest sieve of a series,
or of material which has been crushed to a certain top-size, shall be designated
by the word „minus‟ preceding its top-size (for example “minus 28 mesh, Tyler
sieve series.” This size fraction can also be referred to synonymously as “-28
mesh, Tyler,” “28 mesh x 0, Tyler “ or “28 mesh by zero, Tyler”).
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

3.1.8 The size fraction of material retained on the largest sieve of a series, or of
material retained on any sieve in a series and all larger particles shall be
designated by the word "plus" preceding the size designation; for example, "plus
No. 30 U. S. A. Standard sieve series" refers to all material incapable of passing
the No. 30 sieve, This size fraction can also be referred to as "+No. 30, USA.
Standard" or "+No. 30").
3.1.9 The type of perforated plate opening used for sizes of 6.3 mm (1/4 in.) and larger
shall be designated "rd" or "sq' to indicate round (rd) or square (sq) openings,
respectively. This abbreviation of rd or sq shall follow the lower limiting sieve but
may be omitted after the upper limiting sieve in a series where both sieves are
round or square, for example, 75 mm x 12.5 mm sq. These examples illustrate
the system of size designation:
 200 mm x 12.5 mm sq (10% over 200 mm) { 8 in. x 1/2 in. sq (10% over 8 in.)}
 200 mm x 100 mm rd (24% over 200 mm){8 in. x 4 in. rd (24% over 8 in.)}
 100 mm x 50 mm sq (4 in. x 2 in. sq)
 75 mm x 12.5 mm sq (3 in. x 1/2 in. sq.)
 50 mm sq x No. 4 (2 in. sq x No. 4)
 100 x 200 mesh, Tyler
 No. 4 x No. 30 USA Standard
 25.0 mm sq x No. 50 (1 in. sq x No. 50)
3.1.10 Additionally, for anthracitic coal, size designation of the typically double screened
product can be defined by a descriptive, one-word term, as given in Table 1.
Table 1 Size Designation, Anthracitic Coal

Size of Round-Hole Openings in
Size Testing Sieves, mm (in.)
Passing Retained On
Egg 83 (3 1/4) 62 (2 7/16)
Stove 62 (2 7/16) 41 (1 5/8)
Chestnut 41 (1 5/8) 21 (13/16)
Pea 21 (13/16) 14 (9/16)
Buckwheat #1 14 (9/16) 8 (5/16)
Buckwheat #2 (Rice) 8 (5/16) 4.8 (3/16)
Buckwheat #3 (Barley) 4.8 (3/16) 2.4 (3/32)
Buckwheat #4 2.4 (3/32) 1.2 (3/64)
3.2 Using the percentages calculated in 2.3.6, report the results to the nearest 0.1%.
Issue Date:
MANUAL
Code: CP2
SIEVE ANALYSIS

4 References
4.1 ASTM Standards
 D 197 Test Methods for Sampling & Fineness Test of Pulverized Coal
 D 346 Practice for Collection and Preparation of Coke Samples for
Laboratory Analysis
 D 388 Classification of Coals by Rank
 D 2013 Method of Preparing Coal Samples for Analysis
 D 2234 Test Methods for Collection of a Gross Sample of Coal
 D 4371 Test Method for Determining the Washability Characteristics of
Coal
 E 11 Specification for Wire-Cloth Sieves for Testing Purposes
 E 323 Specification for Perforated-Plate Sieves for Testing Purposes
4.2 Other Document
 Specification C-80 Commonwealth of Pennsylvania, Department of

General Services, Bureau of Purchases, Specification for Coal: Anthracite
Issue Date:
MANUAL
2
Testing Laboratory
Code: CP3
PROXIMATE ANALYSIS
Determination of Moisture Content

Adopted from ISO 5068/Indirect Gravimetric Method
1 Apparatus and Materials
 Balance (Accurate to 1 mg)

 Nitrogen oven
 Weighing vessel, shallow, silica, glass or aluminum with well-fitting lid,
diameter of about 0.36 cm
 Non-corrodible tray
 Desiccator
 Silica gel (Self-indicating desiccant)
 Nitrogen gas, dry and containing less than 30 ppm of oxygen
2 Procedure
2.1 Weigh 1.0 gram of sample into a clean, dry weighing vessel with cover.
2.2 Place it in a non-corrodible tray.
2.3 Uncover the vessel and then place together in the nitrogen oven.
2.4 Open fully the nitrogen gas cylinder valve.
2.5 Slowly open the nitrogen gas regulator valve until 0.4 bar pressure is reached.
2.6 Open fully the gate valve.
2.7 Adjust the nitrogen gas flow to 300 cc/min.
2.8 Flush the sample inside the oven with nitrogen gas for 30 minutes.
2.9 Switch on the nitrogen oven and dry the sample at 110C for 1 hour. Note:
The nitrogen oven reaches 110C 30 min. after it is put on as indicated by the
green light indicator.
2.10 Switch off the nitrogen oven and remove the non-corrodible tray with the
vessel from the oven.
2.11 Cover the vessel.
2.12 Cool in a desiccator for about 15 minutes and weigh.

Issue Date:
MANUAL
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Testing Laboratory
Code: CP3
PROXIMATE ANALYSIS
Determination of Moisture Content

Adopted from ISO 5068/Indirect Gravimetric Method
2.13 Close the nitrogen gas cylinder valve, followed by the closure of the regulator
valve and the gate valve.
2.14 Compute % moisture.
Formula:
% Moisture = (Loss in weight/Weight of sample)*100
2.15 Check precision of test results. Please see Table 1.
Table 1 Maximum Allowable Difference for Test Results

Test Repeatability Limit
Residual Moisture 0.4% absolute
Issue Date:
MANUAL
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Testing Laboratory
Code: CP4
PROXIMATE ANALYSIS
Determination of Volatile Matter


 Muffle furnace, maintained at a constant and uniform temperature of
900C +/- 5C
 Quartz crucible, with matching cover, cylindrical (Approximately 22 mm
ID, 25 mm OD and 38 mm in height)
 Crucible stand, steel wire, heat resistant
 Tong
 Desiccator
 Silica gel (Self-indicating desiccant)
 Spatula
 Timer
2 Procedure
2.1 Switch on main electrical line.
2.2 Switch on power for the muffle furnace.
2.3 Temper the quartz crucible and cover by heating in the furnace at 900C +/-
5C for about 7 minutes using the steel wire, heat resistant stand.
2.4 Remove from the furnace, allow the crucible and cover to cool in a metal slab
and finally in a desiccator for about 15 minutes.
2.5 Weigh 1.0 g of sample into the previously cooled and weighed quartz crucible
and cover.
2.6 With the crucible cover on, place it in the steel wire, heat resistant stand.
2.7 Heat the crucible at 900C +/- 5C in the furnace for 7 minutes.
2.8 Remove from the furnace.

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MANUAL
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Testing Laboratory
Code: CP4
PROXIMATE ANALYSIS
Determination of Volatile Matter

2.9 Let it cool in a metal slab and finally in the desiccator for about 15 minutes and
weigh.
2.10 Compute % volatile combustible matter.
Formula:
% VCM = {(Loss in weight/Weight of sample)*100} - % Moisture

Test Conducted Repeatability Reproducibility
< 10% 0.3% absolute 0.5% absolute
10% and over 3.0% of mean 0.5% absolute or 4.0% of
result mean result whichever is
greater
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MANUAL
1
Testing Laboratory
Code: CP5
PROXIMATE ANALYSIS
Determination of Ash

 Ash furnace, maintained at constant and uniform temperature of 815C
+/- 5C
 Dish of silica, porcelain or platinum, 10 to 15 mm deep
 Insulating plate
 Tong
 Desiccator
 Silica gel, or any self-indicating desiccant
 Spatula
 Timer
2 Procedure
2.1 Temper the porcelain crucible at 815ºC for at least an hour prior to use.
2.2 Let it cool in a metal slab and then in the desiccator for about 15 minutes.
2.3 Weigh the clean, dry porcelain crucible.
2.4 Spread 1.0 g of the sample evenly in the crucible and weigh.
2.5 Place the uncovered crucible with sample on the insulating plate.
2.6 Put inside the cold ash furnace.
2.7 Switch on main electrical line.
2.8 Leave the sample inside the furnace for 4 hours.
2.9 Remove the crucible from the furnace and allow to cool in a metal slab and
then in the desiccator for 15 minutes.
2.10 Weigh the crucible.

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MANUAL
1
Testing Laboratory
Code: CP5
PROXIMATE ANALYSIS
Determination of Ash
2.11 Compute % ash.
Formula:
%Ash={(Weight after ignition–Weight of empty crucible)/Weight of sample}*100

< 10% 0.2% absolute 0.3% absolute
10% and over 2.0% of mean result 3.0% of mean result
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP6
PROXIMATE ANALYSIS
Determination of Fixed Carbon

Using ISO 17246:2010
1 Procedure/Calculations
1.1 Calculate % fixed carbon using the percentages of moisture, volatile matter and
ash.
Formula:
% Fixed carbon = 100 – (% Moisture + % VM + % Ash)

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MANUAL
1
Testing Laboratory
Code: CP7
CALORIFIC VALUE
Determination of Calorific Value

1 Reagents and Materials
 Standard sodium carbonate solution for acid correction

 Fuse wire
 Distilled water
 Benzoic acid pellet
 Methyl orange indicator
 Oxygen gas – 99.9%
2 Apparatus
 Balance accurate to 1 mg
 Parr 6200 calorimeter with the following accessories
o Oxygen combustion bomb
o Calorimeter bucket
o Oxygen tank, fitted with pressure gauges and oxygen filling
connections
o Printer
o Parr 6510 water handling system
o Combustion capsule
o UPS with built-in AVR
 Automatic burette, 50 ml capacity
3 Preparation of Sample
3.1 Weigh approximately 0.8 g of coal sample (0.5 g in case of high heating
value samples e.g. bunker fuel, diesel) into the combustion capsule. Record
the exact weight.
3.2 Place the capsule in the wire loop connected to the bomb head.
3.3 Attach a 10 cm fuse wire to the loop.
3.4 Put approximately 1 ml of distilled water in the bomb to saturate the oxygen
moisture.
3.5 Replace the bomb head in the bomb cylinder and close by setting the screw
cap on the cylinder and turning it down firmly by hand
3.6 Open the oxygen tank valve and adjust delivery pressure to 450 psig.
Attach the filling hose to the bomb inlet valve then press the O2 Fill key on
the calorimeter operation menu.
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MANUAL
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Testing Laboratory
Code: CP7
CALORIFIC VALUE

4 Operating the Calorimeter
4.1 Plug the Powercom UPS to the 220 volt outlet.
4.2 Check the water level at Parr 6510 water handling system. Use distilled
water to adjust the water level to 4 inches from the top of the reservoir.
4.3 Turn ON the following power switches:

a. UPS
b. Water handling system
c. Parr 6200 calorimeter
d. Printer
4.4 Activate the pump and heater by pressing the PUMP AND HEATER key on
the calorimeter operation menu. Allow at least 20 minutes for the calorimeter
to warm-up and the jacket temperature to reach 30 ºC (+/-0.5) and stays
there for approximately 10 minutes.
NOTE: During the warm-up period, the START key is in disable mode until
the stabilization is complete.
4.5 Fill the automatic pipette with distilled water coming from the reservoir then
drain it to the bucket. Set the bucket inside the calorimeter jacket. Use the
lifting handle to lower the bomb in the water with its feet spanning the circular
boss in the bottom of the bucket. Push the two ignition lead wires into the
terminal sockets on the bomb head.
4.6 Close the calorimeter cover.
4.7 Select DETERMINATION or STANDARDIZATION as appropriate by

toggling the operating mode key. Press START key to initiate the test. The
calorimeter will prompt the operator for Bomb ID, Sample ID, Sample
Weight and Spike Weight (if necessary).
4.8 The calorimeter will now take over and conduct the test. During the analysis
period, it establishes initial equilibrium (PREPERIOD will be displayed on the
status bar). Before it fires the bomb, it will sound a series of short beeps to
warn the operator to move away from the calorimeter. Once the bomb has
been fired, it will display POSTPERIOD on the status bar.
Issue Date:
Code: CP7
CALORIFIC VALUE

4.9 The calorimeter will then signal the operator if the test is completed and
preliminary results will be printed automatically by the connected printer.
4.10 Open the cover and remove the bomb and bucket. Water in the bucket is
returned to the water handling system. The calorimeter is again ready for the
next test.
4.11 Open the knurled valve knob on the bomb head to release the residual gas.
This should be done slowly over a period of not less than one minute to avoid
entrainment losses.
4.12 Remove all unburned pieces of fuse wire form the bomb electrodes.
Straighten them and measure their combined length in centimeter. Subtract
this length from the initial of 10 cm to obtain the fuse wire correction to be
entered.
4.13 Wash all interior surfaces of the bomb with distilled water and collect the
washing in a beaker. Titrate the bomb washing with a standard sodium
carbonate solution using methyl orange as indicator.
4.14 At the end of the testing period, turn off all power switches (pls. see #3) and
unplug the UPS power cord.
5. Generation of Final Report
5.1 Press REPORT key.
5.2 Press SELECT FROM LIST key.
5.3 Choose the file to be corrected using the UP and DOWN arrow keys. Press
SELECT to enter selection.
5.4 Press DISPLAY key. This will display the corrections to be done in case of
preliminary report. Otherwise, final reports will be displayed.
5.5 Enter the following data (press ENTER key after every data entered)
a. Fuse – enter the fuse wire correction in centimeter (fuse

multiplier is set to 2.3 cal/cm)
b. Acid – enter acid correction in calories
c. Sulfur – enter sulfur correction in %
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MANUAL
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Testing Laboratory
Code: CP7
CALORIFIC VALUE

5.6 Compute results and check precision of test results. Please see Table 1.
Table 1 Maximum Allowable Differences for Results

Calorific Value 29 cal/g 72 cal/g
6. References
6.1 ASTM Standards
 D 121 Terminology of Coal and Coke

Laboratory Analysis
 D 1193 Specification for Reagent Water
 D 3173 Test Method for Moisture in the Analysis Sample of Coal and
Coke
 D 3177 Test Methods for Total Sulfur in the Analysis Sample of Coal and
Coke
 D 3180 Practice for Calculating Coal and Coke Analyses from As-
Determined to Different Bases
 D 4239 Test Method for Sulfur in the Analysis Sample of Coal and Coke
Using High Temperature Tube Furnace Combustion Methods
 E 1 Specification for ASTM Thermometers
 E 144 Recommended Practice for Safe Use of Oxygen Combustion
Bombs
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP8
FORMS OF SULFUR
Determination of Forms of Sulfur in Coal

1 Reagents
 4.8 N HCl (2+3)

 1.5 N NH4OH (1+10)
 Ethanol
 Bromine water
 BaCl2 solution – 100 g BaCl2 H2O in 1 L of H2O
 Methyl orange indicator – 0.02 g in 100 mL hot water
2 Procedure
2.1 Weigh 2-5 g sample in a 250-mL beaker.
2.2 Add 50 mL of 4.8 HCl in small increments while stirring.
2.3 Add few drops of ethanol to facilitate the wetting process.
2.4 Boil gently for ½ hours.
2.5 Filter using #40 filter paper. Wash thoroughly with hot water. Return the filter
paper with residue to the beaker and reserve for pyritic determination.
2.6 Add 5 mL of bromine water and boil for at least 5 minutes or until all the
bromine had been given off. Cool to room temperature.
2.7 Precipitate Fe by adding NH4OH solution slowly. Add 5 mL excess. Filter and
wash thoroughly with hot water.
2.8 Add methyl range indicator and neutralize with HCl. Add 1 mL excess.
2.9 Heat to boiling. Add 20 mL BaCl2 solution drop wise while stirring. Boil for 10-
15 minutes. Let it stand for overnight.
2.10 Prepare a blank by doing the same above procedure.
2.11 Filter using #42 filter paper. Wash thoroughly with hot water.
2.12 Ignite in a tared crucible.

Issue Date:
Code: CP8
FORMS OF SULFUR
Determination of Forms of Sulfur in Coal

3. Computations
% SO4S = {(S-Cm) – (B-CB)} x 13.735 / W
Where: SO4S = Sulfate sulfur

S = Weight of sample crucible plus ignited BaSO4 precipitate
Cm = Weight of sample crucible
B = Weight f blank crucible plus ignited sulfate blank
CB = Weight of blank crucible
W = Weight of test specimen used
4. References
4.1 ASTM Standards

 D 2013 Method for preparing Coal Samples for Analysis
 D 3173 Test Method for Moisture in the Analysis Sample f Coal and Coke
 D 3177 Test Methods for Total Sulfur in the Analysis Sample of Coal and
Coke
 D 4239 Test Methods for Sulfur in the Analysis Sample of Coal and Coke
Using High Temperature Tube Furnace Combustion Methods
 E 832 Specification for Laboratory Filter Papers
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP9a
TOTAL SULFUR
Determination of Total Sulfur by IR Method

Using LECO SC 432 DR Adopted from ASTM D 4239
1 Theory of Operation
The SC-432 Sulfur Analyzer is a non-dispersing, infrared, digitally controlled

instrument designed to measure the sulfur content in a wide variety of organic
materials, including soil, cement and limestone.
Analysis begins by weighing out a sample into a combustion boat. When

ANALYZE is touched, the sample is placed in the combustion system, which is
typically regulated at 1,350°C, in a pure oxygen environment. The combination of
furnace temperature and analysis flow causes the sample to combust. All the
sample, which is contained in the combustion boat, goes through an oxidative
reduction process that causes sulfur-bearing compounds to break down freeing the
sulfur. The sulfur oxidizes to form SO2. The design of the combustion system
prevents atmosphere from entering the combustion zone. After a specific period of
time, oxygen begins to flow through the lance to accelerate the combustion of
hard-to-combust materials and the sulfur, as SO2, is released into the carrier flow
as sample gas.
The sample gas is swept through the boat stop to the back of the inner
combustion tube, then forward between the inner and outer combustion tubes,
effectively allowing the sample gas to remain in the high temperature zone for a
longer period, permitting efficient oxidation.
From the combustion system, the gas flows through two Anhydrone tubes to
remove moisture through a flow controller, which sets the flow of sample gas to 3.5
l/min, then through the infrared detection cell.
The cell measures the concentration of sulfur dioxide gas present. The software in
the instrument takes into account the sample weight, calibration and known
moisture value and converts the concentration value to a percentage (in parts per
million or ppm).
2 Operation
2.1 Initial Power - up
2.1.1 The power switch in front of the analyzer should be turned off, while the furnace
section’s switch is turned on.
2.1.2 Turn on the gas supplies and set the delivery pressures to 40 psi.
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MANUAL
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Testing Laboratory
Code: CP9a
TOTAL SULFUR

Using LECO SC 432 DR Adopted from ASTM 4239
2.1.3 Turn on the power switch to automatically turn on the furnace. Note: From this
point on, if the system needs to be reset, simultaneously press Ctrl Alt Delete on
the keyboard.
2.1.4 The instrument boots up and displays the main screen.
2.2 System Check
2.2.1 Note: The gas supplies are on and the regulator is set at 40 psi. Access the
Ambient Monitor procedure by touching MAINTENACE, then press AMBIENT
MONITOR
2.2.2 Check that the temperatures, voltages and pressure used in the system fall within
prescribed range limits. Please see Table 1.
Table 1 System Parameters

Variable Nominal Range
Value
Oven Temperature, oC 45 44 - 46
Furnace Temperature, oC Variable Nominal
Flow Presure, psi* 10 >5
Back Pressure, mm Hg 760 +2% of set
barometric pressure
Sulfur IR Cell, volts 8.5 -
*psi is 0 if flow pressure is turned off
2.2.3 To check the stability of a monitored value, touch the  or  arrow to highlight the Comment [RU1]:
point for observation.
2.2.4 The minimum and maximum values for the highlighted point are also displayed.
To reset these values, touch RESET MIN/MAX.
2.2.5 To receive a printout of the parameters, and the minimum, maximum and current
values, touch PRINT TABLE.
2.2.6 To further check the stability of a monitored value, touch the  or  arrow. The
arrow highlights the point for observation. Then touch PLOT PARAMETER to
display a graphic plot of the value over time. The plot indicates stability over time.
Issue Date:
MANUAL
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Testing Laboratory
Code: CP9a
TOTAL SULFUR

2.2.7 To receive a printout of the plotted parameter, touch PRINT PLOT.
2.2.8 To start plotting again, touch RESET PLOT.
2.2.9 To return to the table format, touch DISPLAY TABLE.
2.2.10 If any values are out of range, refer to the Electronic Adjustments in the Service
section or the System Configuration for adjustment procedures.
2.2.11 Touch ESC to exit.
2.3 System Setup
2.3.1 Note: The procedures are all located under Setup in the Maintenance menu. To
access, touch the MAINTENANCE icon, then the SETUP icon to display the setup
procedure. Touch the procedure icon to open each procedure. When all
procedures in the System Setup have been completed, install all the side panels.
2.4 System Configuration
2.4.1 This part allows the operator to set the system operating conditions used for
analyzing, displaying results, printing results and calibrating. Refer to the
definitions in the Manual, then touch  to highlight the parameter to be edited.
There are three types of edit windows that will be displayed on the right as each
parameter is highlighted.
2.4.2 If the parameter has multiple but limited options, a bullet box is displayed. To
change the value, touch the desired option.
2.4.3 If the parameter has a numerical value, the keypad will be displayed.
2.4.4 If the parameter has an alphanumeric value, the edit box will be displayed. Enter
the new value, then touch OK to save the change or CANCEL to abort the change.
2.4.5 Once a parameter has been edited, the next parameter becomes highlighted.
2.4.6 The list of parameters is longer than what fits on the screen. Keep touching  to
view the rest of the parameters.
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MANUAL
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Code: CP9a
TOTAL SULFUR

2.4.7 Touch PRINT to receive a printout of all the parameters. Save the printout for
future reference.
2.5 System Calibration
2.5.1 Note: Calibration, which can be performed through Standard Calibration or Edit
Calibration, allows the operator to calibrate the system based upon previously
analyzed standards. Check system calibration daily for accuracy. It is most
accurate when minimum of five standard results are used.
2.5.2 Prior to performing the standard calibration procedure, define the standard to be
used for calibration, then select the defined standard ID when performing
analyses, and analyze the number of standards to be used in calculating the new
calibration. Note: Defining the standards allows the operator to input and maintain
a list of ID codes with pertinent information on the standards that will be used in
calibration. This procedure only needs to be performed once for each standard
that will be used, unless information changes.
2.5.3 Touch the CALIBRATE icon, then touch DEFINE STANDARDS to open the
procedure.
2.5.4 Touch  or  to move the cursor up or down one line at a time.
2.5.5 Touch ADD STANDARD and a pop-up window is displayed allowing entry of a
new standard ID code, lot #, sulfur standard and sigma. When the values are all
entered, touch OK to add the standard to the list or CANCEL to abort the addition
and return to the initial Define Standards screen.
2.5.6 To edit an existing standard, touch  or  to highlight the standard, then touch
MODIFY STANDARD. A pop-up window displays the standard ID code for editing.
After editing, touch OK to apply the edits to the highlighted standard or CANCEL
to abort the edit procedure and return to the initial Define Standards screen.
2.5.7 Note: For most accurate calibration, analyze three to five standard samples with
the appropriate combustion aids before performing standard calibration.
Calibration can be performed through Standard Calibration, Edit Calibration, or
Data Base Calibration menus. Touch the CALIBRATION icon, then the
STANDARD CALIBRATION to open the procedure.
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MANUAL
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Testing Laboratory
Code: CP9a
TOTAL SULFUR

2.5.8 Touch  or  to change cursor direction or move the cursor up or down one
line.
2.5.9 Touch Pg Up or Pg Dn to display another screen of standards. The box at the

right indicates the relative position of the cursor within the list.
2.5.10 The standard results may not be within standard value range, however, unless the
value is out of range by a factor of two or more, the results is still valid.
2.5.11 To view additional answer information before selecting, touch NEXT FIELD to view
the following information: # .ID Code, Sulfur, Method, Moisture, Time & Date of
ID Code, Weight, Sulfur, Method, Time & Date #, ID Code, Operator, ID Code 2,
ID Code 3.
2.5.12 Touch INCLUDE RESULTS to highlight the line marked by the cursor and move
the cursor one line in the direction specified on screen. Choose values that fall
within the overall deviation of the material. For example, if the standard deviation
is equal to  0.01, the lowest and highest results must be within 0.02 to be
acceptable.
2.5.13 Touch EXCLUDE RESULT to remove the highlight from the line marked by the
cursor and move the cursor one line in the direction specified on screen.
2.5.14 Touch PROCESS RESULTS and the instrument will calculate the new calibration
based on the included results. If an included sample is not defined, a pop-up
window is displayed allowing the operator to define or exclude the sample(s). If
the operator has security access to the Define Standards procedure, the newly
defined standard will be added to the standards list. Only operators with Define
Standards access may define standards.
2.5.15 Touch  or  to move the cursor up or down one line in the list of chosen results
on the left.
2.5.16 Touch NEXT FIELD to toggle the third column in the standards list between %
Error, Peak Area and Weight. When these fields are displayed, the chart shows
these points, where the X-axis is always going to space the selected points
evenly and the Y-axis will display the % Error, Peak Area or Weight.
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MANUAL
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Testing Laboratory
Code: CP9a
TOTAL SULFUR

2.5.17 Touch EXCLUDE RESULT to ghost-out the result marked by the arrow and cross
hairs. This allows the operator to exclude results that seem to deviate
significantly from the calibration curve. To help identify erratic points, touch
NEXT FIELD until the % Error is shown on the plot.
2.5.18 Touch INCLUDE RESULT to put an excluded result back in the list and on the
chart.
2.5.19 Note that the results used to calculate the new calibration have not changed.
Refer to Recalculate Results to update these and any other results.
2.5.20 When exiting this procedure, a pop-up window displays to confirm the calibration.
If YES is touched, the calibration is saved and the screen is printed out
automatically. Note: Save the Calibration printout sheet. If an Edit Calibration
needs to be performed, the operator will need to use the printout. Edit
Calibration should only be used to enter a previous calibration that has been
lost.
2.6 Analysis of Sample
2.6.1 Refer to the original manual of SC-432 DR.
2.6.2 To access the analyze procedures, touch the ANALYZE menu icon.
2.6.3 To place a lab sample ID code in memory, touch ADD ID CODE. Enter the new ID
Code, then press ENTER to move the cursor to enter additional ID code
information, such as ID Code 2, ID Code 3, and Moisture. After entering the ID
Code, touch OK to save the ID code or CANCEL to abort the addition and return
to the initial Sample Log-in screen. The ID code will remain in memory unless
deleted.
2.6.4 To select either a standard or lab sample ID code already in memory touch either
 or  to move the highlight block to the ID code to be used and touch ESC. The
instrument returns to the Analyze screen and the highlighted ID code is displayed
on the Log-in Sample line of the Sample Weights box.
2.6.5 When an ID code is no longer needed in memory use the arrow keys to
highlight the ID code and touch DELETE ID code.
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MANUAL
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Testing Laboratory
Code: CP9a
TOTAL SULFUR

2.6.6 The weights can now be entered into the Sample Weights list. Refer to the
Sample Weight Entry section for more information. Additional samples can
continue to be logged-in without returning to the Select ID Code procedure,
unless a different ID code is used.
2.6.7 The default sample weight is o.350 g. The system accepts sample weights
ranging from 0.0001 - 9.9999 g.
2.6.8 Two factors are used to determine the appropriate sample weight: 1) the rate of
sulfur released must be below the cell saturation point as noted by a flat-topped
peak area in the sample plot; and (2) the ability of the sample to combust and
provide good precision as noted in the sample results.
2.6.9 Place the boat on the balance pan and press TARE on the balance or touch
BALANCE TARE on the screen.
2.6.10 Add sample materials. When the balance stabilizes, touch ENTER WEIGHT to
store the weight and sample log-in information in the Sample Weights list.
2.6.11 Analysis by automatic loading follows this procedure: Remove the autoloader
rack, load the sample boat(s) onto the rack as they are logged-in and weighed.
Boat should be placed next to each other without leaving blank slots. Place the
loaded rack in the autoloader. Note: Boats should be placed in the furnace's
rounded end first. Boats can be scraped clean and reused up to four times,
unless samples are analyzed using vanadium, in which case the boats can only
be used once. Result will be more consistent if the sample is spread evenly in
the boat before analyzing.
2.6.12 Touch the ANALYZE icon.
2.6.13 Use the arrow keys to highlight the starting position on the rack illustration. Give
attention that position number one is the top outside slot when the rack is in
place. Note: The instrument analyzes until the Sample Weights list is empty or
the autoloader reaches position 36, whichever comes first.
2.6.14 Touch the ANALYZE icon to save the starting position and begin the analyses.
The analyzer assigns rack position numbers to each sample in the list, starting
with the number entered in #2.6.2.13. The autoloader loads the sample boats,
performs the analysis, then unload the samples and drops into the bucket.
Make sure the bucket is installed and that there is enough room in the bucket
for the number of boats loaded.
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2.6.15 The analysis is complete when both Result Window borders are thick lines,
ABORT ANALYSIS returns to ANALYZE, and the printer prints the results.
After each analysis, the results is placed at the end of the Results list and final
results appears in the Result Window. Note: RESET ANALYSIS, if sample has
not been placed in the furnace, to stop the analysis, then remove the sample.
The weight will be stored to the top of the Sample Weights list. ABORT
ANALYSIS, if the sample has been placed in the furnace; to stop analysis of the
current sample. The sample weight is removed from the Weight list and the
results of the aborted analysis is displayed and saved. The result will be
incomplete.
2.6.16 If the instrument remains idle for the amount of time specified in Screen Timeout,
the operator is logged-off and the furnace drops to Standby Temperature.
2.7 Reporting Results of Analysis
2.7.1 Touch the REPORTS icon, then touch RESULTS to open the procedure.
2.7.2 Touch Pg Up or Pg Dn to scroll through screens of answers.
2.7.3 Touch  or  to change cursor direction or move the cursor up or down one line
at a time.
2.7.4 To view additional answer information before selecting, touch NEXT FIELD to
view the following information: #, ID Code, Sulfur, Method, Moisture, Time &
Date ID Code, Weight, Sulfur, Method, Time and Date #, ID Code, Operator, ID
Code 2, ID Code 3.
2.7.5 Touch INCLUDE RESULTS to highlight the line marked by the cursor for
transfer, transmission printing or deletion. The cursor moves one line in the
direction specified on screen.
2.7.6 Touch EXCLUDE RESULTS to remove the highlight from the line marked by
the cursor. The cursor moves one line in the direction specified on screen.
2.7.7 After selecting analysis results, touch PROCESS RESULTS.

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2.8 Recalculation of Results
2.8.1 Recalculation of results allows the operator to update results to reflect the current
calibration. Touch the CALIBRATION icon, then RECALCULATE RESULTS to
access this procedure.
2.8.2 Touch Pg Up or Pg Dn to scroll through screens of results. The arrow cursor

on the left will remain in its current position.
2.8.3 Touch  or  to move the cursor up or down one line at a time.
2.8.4 Touch INCLUDE RESULT to highlight the line marked by the arrow cursor.
2.8.5 Touch EXCLUDE RESULT to remove the highlight from the line marked by the
arrow cursor.
2.8.6 To recalculate all included results, touch PROCESS RESULTS. The Analyzer
performs the recalculations, then displays a pop-up window. Touch the
appropriate option to save the results of the new calibration, print the chosen
results with the new calibration and save the changes, or cancel the changes and
revert the results to the previously saved values.
2.9 Checking of Precision of Test Results (Please see Table 2)
Table 2. Precision Test for Sulfur

Sulfur Content Repeatability
Low sulfur 0.03%
High sulfur 0.05%
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Using Leco TruSpec S Adopted from ASTM D 4239
1 Analytical Balance
1.1 Check if the bubble is centered within the circle of level indicator.
Adjust if necessary. Please refer to page 10 of Sartorius operating instruction.
1.2 Plug the power cord into wall outlet and turn ON the balance. Balance
must be warmed up for 30 minutes before using.
1.3 Perform internal calibration Please refer to page 16 of Sartorius operating
instruction.
2 Gase/s This can be done before or right after switching on the unit.
2.1 Fully open the gas cylinder valves. Set/Check delivery pressures of
the following:
Oxygen – 38 psi
2.2 Record initial and final readings (before and after every analysis or
calibration) for every cylinder in the Sulfur TruSpec s logbook.
3 CHNS Analyzer / Computer / Printer
Initial Power-Up
1 Turn On automatic voltage regulator (AVR). Delay time is less than 1

minute.
2 Turn On the CHNS unit first and wait for at least 5 minutes before turning
On the CPU.
3 Turn ON the CPU, monitor, and printer (if needed).

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Equipment Stabilization. It is advisable to let the equipment stabilize for at

least 2 hours before performing system check and sample analysis.
1 From the main screen menu, double click the TruSpec software icon.
CHN and S analyses spreadsheet will automatically appear. To use S
analyzer only, access the CHN spreadsheet, click DIAGNOSTICS,
select furnace then click STOP buttons on the combustion and
afterburner furnace settings
2 On the S spreadsheet, click DIAGNOSTICS and select FURNACE.
3 Set or check the following temperature settings:
Combustion furnace – 1350ºC
4 Click RESTART button to activate the heater of the combustion tube.
5 The operator can view the ambient monitor display after turning ON
the unit and compare parameter values on page 8-6 of instructions
manual. Click DIAGNOSTICS menu and click AMBIENT CHART.
Verify that there are no alarms indicated by an exclamation mark in a
yellow box to the left of the list of parameters.
6 Click the check box of the parameter to be monitored and the graph
will automatically appear.
7 Click CLOSE to exit ambient chart menu.

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System Check: This is a quick way to determine if major systems in the instrument are
operating properly.
1. Click DIAGNOSTICS and select SYSTEM CHECK.
2. Click START. All circles on the left system names should be filled in green
and “PASSED” mark will appear in the results column. If in any case, red X
or “FAILED” mark appeared, stabilize the equipment for additional hour(s) or
perform troubleshooting for the system that failed during the system check.
Please refer to error messages on pages 5-89 up to 5-98 of the instructions
manual.
3. Again, perform system check and wait for the “PASSED” mark to appear.
4. To exit DIAGNOSTICS menu, click close.
Sample ID, position and method log-In
Sample ID
1. From the SAMPLES menu, click LOG-IN and the sample dialog box
will appear.
2. Enter the sample name and other information required/needed in the

selection box.
If sample name has already been listed just click on the last row of the
name column and select the sample name from the list on the drop
down window.
3. Click OK to log-in the sample.

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4 Method
Creation:
1. From the CONFIGURATION menu, click METHOD. The method dialog
box will appear.
2. Click ADD and a row will be added at the bottom of the spreadsheet or
click an empty row and enter a method name.
3. From the method dialog box, click PROPERTIES and enter the desired
ANALYSIS PARAMETERS values to each parameter. Refer to Method
Parameter Definitions on page 4-34.
4. Click OK when finished.
Selection: This procedure can be done when the method to be used has already been
created.
1. From the main screen menu, double click on the last row of the method
column and select method to be used from the list on the drop down box.
5 Analysis
Analyze sample:
- From the SAMPLES menu, click ANALYZE or F5 button.
The unit will automatically analyze all the samples encoded sequentially. After analysis, the
sample plot will appear in the window below the spreadsheet. The result of the analysis will
appear in the spreadsheet and plot window.
Abort analysis
- From the SAMPLES menu, click ABORT. The analysis in progress will be aborted.
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Delay/Pause/Resume analysis:
- Select where in the sample list to delay or pause analysis
- From the sample menu, click PAUSE. The pause/delay dialog box will
appear prompting the operator to enter the time to delay and/or restart he
analysis.
- Click OK to apply time delay and when to restart analysis.
This procedure permits the operator to delay /pause and resume an analysis either manually or
at a pre-set time. A clock symbol will appear in the spreadsheet next to the sample that will be
analyzed after the pause.
Conditioner Analysis:
1. Weigh 1-2 conditioning samples (~0.17 gram of any coal sample).

2. Analyze the samples following analysis procedure.
Blank Analysis:
1. From the main screen menu, click NAME select BLANK.
2. From the CONFIGURATION menu, click METHOD and choose the

method to be used.
3. Press ANALYZE or F5. The weight is automatically set to 1.000 gram

during blank analysis.
Perform at least 3-5 blank analyses or check the standard deviation (SD) of the last
three runs if it is < 0.001% proceed to blank calibration
4. To check standard deviation – from the spreadsheet select from the

sample grid menu and highlight rows of the blank runs. Statistical data
will automatically appear in the dashboard area of the main screen
display.
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Blank Calibration: Perform blank calibration before every calibration/analysis.
1. Highlight the blank results of analysis from the spreadsheet to be

calibrated.
2. Click CONFIGURATION and select BLANK.
3. Click a row to select the element(s) and then click INCLUDE or

EXCLUDE an element to be included/excluded in blank calibration.
4. Click OK to calculate the system blank based on the blank analysis

results obtained and the software will automatically compute for the
system blank.
Standard Calibration:
1. Weigh and analyze standard samples according to the method to be used.
2. Select/highlight the results to be included in calibration.
3. Click CONFIGURATION and select CALIBRATION.
4. From the fly-out menu that will appear, click the arrow in the drop down
box of the following:
a.) Cell – to select a cell (element) to calibrate.
b.)
b.) Curve type – to select a curve type to be applied for each cell.
5. View the curve displayed in the graph. As much as possible the graph
should intersect the black squares which represent the values for the
standard analyzed. Evaluate the curve fit by means of Root Mean Square
(RMS) error; the lower the value (approaching zero) the better.
6. Click OK to calibrate the selected cell.
7. Click Print to print a copy of the calculated calibration
8. Click OK to exit the calibration procedure and save the calibration curve.
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Drift Correction: Perform drift correction before every analysis to adjust the original
calibration response to match the current instrument response.
1. Weigh 2-3 standard samples. The software will automatically or the

operator can manually select what sample and its weight can be used as
drift standard sample as indicated by X mark.
2. Analyze the sample.
3. Compare the results obtained from the true value. If the results obtained
are within the allowable range proceed to the check standard procedure; if
not, select last two (2) data from the results of standard analysis in the
spreadsheet.
4. Click CONFIGURATION and from the fly-out menu select DRIFT
5. From the table same as below that will appear on the screen, click a row
to select the element(s) and click INCLUDE or EXCLUDE element(s) to be
included/excluded in drift correction.
6. Click OK to calculate the drift based on the analysis obtained. The

software will automatically compute for the drift correction of the system.
Just in case that the operator will shift from one method to another, it is necessary to perform
blank calibration and drift correction separately.
Check Standard: Perform check standard after every drift correction or standard
calibration
1. Weigh and analyze at least two trials of coal standard.
2. Check if the values obtained are within the acceptable range for specific
coal standard. If acceptable, proceed with the analysis of unknown
sample(s); if not, consider/perform minor troubleshooting.
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Sample Analysis:
1. Weigh approximately 0.17 gram of the unknown sample. Please refer to

manual sample preparation.
2. Encode or select the ID code or part number, method, and weight of the
sample in the spreadsheet. Encoding can be done one at a time, i.e., for every
weighing or all at one time to save time.
3. Click F5 or ANALYZE.
Print Results:
1. From the SAMPLES menu, click PRINT. The Report Settings screen will
automatically appear.
2. Click the following selection: REPORT, FIELDS, FONT and ELEMENT

and configure print formats.
REPORT- report format, plot height, statistics, heading text
3. Click OK to save changes and print the selected results.
Shutdown:
A. Total shutdown
1. Close all the gas cylinder valves but do not pull the relief valves to release
gases.
2. From the spreadsheet menu, click DIAGNOSTICS and then select

FURNACE.
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3. From the furnace diagnostics screen that will automatically appear on the
screen, click STOP to deactivate heaters of the following: combustion
furnace. Wait until the temperature reaches 500°C or lower
(approximately 30 minutes).
4. Click CLOSE to exit from the DIAGNOSTICS menu.
5. Click DATABASE and select EXIT. The software will automatically close.
6. From the main screen menu click START and select SHUTDOWN. (This
is the usual procedure how to switch off a computer.)
7. Switch OFF the CHNS analyzer unit and AVR.
Failure to cool the furnace prior to turning the power switch off will result in overheating
of the loading head assembly and possible damage to the instrument.
B: Standby mode
1. Perform steps 1 and 2 in A.
2. From the CONFIGURATION menu, click SYSTEM. The System

Configuration dialog box will appear.
3. Enter the desired furnace standby temperature (preferably 200°C).
4. Click OK to close the system configuration dialog box.
In this case the operator can switch off the computer monitor but not the CPU.
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Maintenance. In order to obtain the best possible results of analysis periodic

maintenance must be performed.
Maintenance counter is list of components and assemblies, within the instrument, that have been
determined to require periodic maintenance. An analysis counter will determine when periodic
maintenance is needed and alert the operator. Please refer to Chapter 6 – Maintenance pages 6-
2 to 6-49 of the TruSpec CHN analyzer operating manual on periodic maintenance schedule and
how to perform specific replacement of consumables.
1. From the configuration menu, click COUNTERS and the dialog box will
appear.
2. Click ADD to define a maintenance counter.
3. Enter the information required in the dialog box. Please refer to

maintenance counter definitions on page 6-15 of the TruSpec S operating
manual for additional information.
4. Reset the count data once replacement of consumables listed has been
performed.
5. Click OK to exit the procedure.
Please refer to error message definitions on page 5-73 of the TruSpec S operating
manual for corrective actions and other troubleshooting concerns.
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SULFUR DETERMINATION
Sulfur Determination by Eschka and Bomb Washing Methods

1 Reagents and Materials
 Saturated NH4OH solution, of density = 0.88g/mL

 Saturated HCl solution, of density = 1.18 g/mL
 BaCl2 solution, 20% solution
 Saturated Bromine water
 Methyl orange indicator
 #40 and 42 Whatman filter paper
 pH paper (optional)
 Silver nitrate solution (optional)
2 Apparatus
 400 ml beaker
 Funnel
 Stirring rods, rubber policeman
 Wash bottle
 Pt or tempered silica crucibles
 Hot plate
 Furnace or bunsen burner
 Tong
 Filtering stand
 Watch glass
 Hot hand
 Aspirator
3 Procedure
3.1 Weigh 0.7 – 1.0-gram sample and form into pellet.
3.2 Ignite inside a bomb calorimeter.
3.3 Remove bomb from the calorimeter and connect a tygon tubing into the exhaust
valve. Dip the other end of the tubing to a one-inch deep distilled water in a 400
mL beaker. Slowly release the exhaust valve of the bomb until the bomb is at
atmospheric pressure.
3.4 Wash the inside of the bomb, tygon tubing and the exhaust valve thoroughly,
catching the washing into the beaker.
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3.5 Add indicator, then titrate the washing with standardized Na2CO3.
3.6 Make the solution basic by adding NH4OH drop by drop. Cover the beaker with
watch glass and then let the solution boil.
3.7 While still hot filter the solution through Whatman #40 filter paper. Then, discard
the filter paper.
3.8 Add indicator to the solution if it turned colorless; if not, continue by adjusting the
acidity of the filtrate by adding HCl, with 2 to 3 drops in excess of base. The
solution will change its color from yellow to red or pink.
3.9 Add 5 ml Bromine water.
3.10 Boil the solution without the watch glass to expel Bromine. The solution will turn
colorless. Note: An alternative test is by adding the indicator to the solution. If it
turns pinkish, the process is complete.
3.11 Add 25 ml of 20% BaCl2 solution to precipitate the sulfate. Let it stand overnight.
3.12 Filter the solution through #42 Whatman filter paper with hot distilled water. To
test if washing is completed, add a few drops of AgNO3 solution to the filtrate. If
the solution turns cloudy in appearance, continue washing until the filtrate does
not change in color anymore.
3.13 Temper silica crucibles at 815C for about an hour and then weigh.
3.14 Ignite the filter paper in a weighed crucible, partially covered, at 815C for about
an hour and compute %S using the formula below:
Formula:
%S = (Weight of the precipitate*13.734)/Weight of the sample
Note: Perform the operation including blank and coal standards. For
unknown sample(s), use three (3) trials each.
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Table 1 Maximum Allowable Differences of Results

Repeatability Reproducibility
Coal
< 2% sulfur 0.05 0.10
> 2% sulfur 0.10 0.20
Coke 0.03 0.05
4 References
4.1 ASTM Standards

Laboratory Analysis
 D 2015 Test Methods for Gross Calorific Value of Coal and Coke by
the Adiabatic Bomb Calorimeter
 D 3173 Test Method for Moisture in the Analysis Sample of Coal and
Coke
 D 3176 Practice for Ultimate Analysis of Coal and Coke
 D 3286 Test Method for Gross Calorific Value of Coal and Coke by
the Isoperibol Bomb Calorimeter
 E 144 Practice for Safe Use of Oxygen Combustion Bombs
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CARBON, HYDROGEN AND NITROGEN (CHN) ANALYSIS
Carbon, Hydrogen and Nitrogen (CHN) Analysis

(For C & H – by IR & For N – By Thermal Conductivity)
1 Analytical Balance
1.1 Check if the bubble is centered within the circle of level indicator.
Adjust if necessary. Please refer to page 10 of Sartorius operating
instruction.
1.2 Plug the power cord into wall outlet and turn ON the balance.
Balance must be warmed up for 30 minutes before using.
1.3 Perform internal calibration Please refer to page 16 of Sartorius operating
instruction.
2 Gases This can be done before or right after switching on the unit.
2.1 Fully open the gas cylinder valves. Set/Check delivery pressures
of the following:
Helium – 35 psi
Oxygen – 35 psi
Compressed Air – 45 psi
2.2 Record initial and final readings (before and after every analysis or
calibration) for every cylinder in the CHN analysis logbook labeled
GC Log4: Coal-CHN.
3 CHN Analyzer / Computer / Printer
Initial Power-Up
1 Turn On automatic voltage regulator (AVR). Delay time is less than 1

minute.
2 Turn On the CHN unit first and wait for at least 5 minutes before
turning On the CPU.
3 Turn ON the CPU, monitor, and printer (if needed).

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CARBON, HYDRGEN AND NITROGEN (CHN) ANALYSIS

Adopted from ASTM D 5373 – 02
Equipment Stabilization. It is advisable to turn ON and let the unit in its

standby mode preferably 200-650ºC a day prior to use. This will lessen the
equipment stabilization period on same day analysis.
1 From the main screen menu, double click the TruSpec software
icon. CHN and S analyses spreadsheet will automatically appear.
This means that CHN and S analyzers can be used
simultaneously. To use CHN analyzer only, access the S
spreadsheet and click DATABASE and click EXIT on the fly-out
menu.
2 On the CHN spreadsheet, click DIAGNOSTICS and select

FURNACE.
3 Set or check the following temperature settings:
Combustion furnace – 950ºC

Afterburner furnace – 850°C
4 Click RESTART buttons to activate heaters of the following:

combustion and after burner furnace, reduction tube, and ballast
oven.
5 The operator can view the ambient monitor display by at least two
(2) hours after turning ON the unit and compare parameter values
on pages 8-9 of instructions manual. Click DIAGNOSTICS menu
and click AMBIET CHART. Verify that there are no alarms
indicated by an exclamation mark in a yellow box to the left of the
list of parameters.
6 Click the check box of the parameter to be monitored and the

graph will automatically appear.
7 Click CLOSE to exit ambient chart menu.

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Leak Check Test: This procedure automatically checks the entire/section of

the combustion (oxygen) and/or measurement (helium) system of the
instrument for a gas leak.
Perform leak check when the furnace has stabilized. Additional 30 minutes
stabilization period at pre-set temperature is required before performing any of the
following:
Whole O2 – before every analysis

Whole Helium – Helium gas cylinder and TC cell replacement only
Segmented O2 or He Aliquot loop- if the whole system leak check failed.
A. Whole O2 or Helium:
1. Click DIAGNOSTICS and select LEAK CHECK.
2. Click WHOLE O2 or He and click START. Wait for the green indicator
on the left of the list ambient parameters or the “PASSED” on the
results column.
3. Click CLOSE to exit diagnostics menu.
B. Segmented O2 or He Aliquot Loop: This should be done if the whole O2 or He

leak check failed in order to determine/isolate which section of the system is leaking.
1. Click SEGMENTED O2 or He ALIQUOT LOOP and click START.
2. Wait for the red indicator on the left of list of instrument section or
“FAILED” mark on the results column.
3. Refer to error messages on pages 5-89 to5-98 TruSpec CHN

Instruction Manual and perform possible troubleshooting.
4. Again, perform whole O2 or He leak. Check and wait for the

“PASSED” mark to appear.
5. Click CLOSE to exit diagnostics menu

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System Check: This is a quick way to determine if major systems in the instrument
are operating properly.
1. Click DIAGNOSTICS and select SYSTEM CHECK.
2. Click START. All circles on the left system names should be filled in green
and “PASSED” mark will appear in the results column. If in any case, red
X or “FAILED” mark appeared, stabilize the equipment for additional
hour(s) or perform troubleshooting for the system that failed during the
system check. Please refer to error messages on pages 5-89 up to 5-98 of
the instructions manual.
3. Again, perform system check and wait for the “PASSED” mark to appear.
4. To exit FURNACE menu, click close.
Let the unit undergo additional 2-4 hours stabilization period before performing
analysis.
4 Sample Preparation
1. Place the sample cup holder on the analytical balance pan.
2. Place tin foil cup on the sample cup holder and tare the balance.
3. Add approximately 0.17 gram of unknown sample or refer to table for

weight selection of samples/standards according to what method to be
used.
4. Remove the tin foil from the sample cup holder. Carefully twist the foil
to seal and at the same time expel the air present during sample
loading.
5. Re-weigh the twisted/sealed tin foil and take note of the weight of the
sample.
6. Place the weighed sample and take note of each position in the
carousel/loading head.
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Sample ID, position and method log-In
Sample ID
1. From the SAMPLES menu, click LOG-IN and the sample dialog box
will appear.
2. Enter the sample name and other information required/needed in

the selection box.
If sample name has already been listed just click on the last row of
the name column and select the sample name from the list on the
drop down window.
3. Click OK to log-in the sample.
Position
1. Double click on the position column and encode the number of the
corresponding position in the carousel for each sample.
Encoding can be done all at one time or after every analysis. Just in case that the operator
wishes to change the default position, a dialog box will appear confirming the change(s) in the
position.
5 Analysis
Analyze sample:
- From the SAMPLES menu, click ANALYZE or F5 button.
The unit will automatically analyze all the samples encoded sequentially. After analysis, the
sample plot will appear in the window below the spreadsheet. The result of the analysis will
appear in the spreadsheet under each element name.
Abort analysis
- From the SAMPLES menu, click ABORT. The analysis in progress will be
aborted.
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Delay/Pause/Resume analysis:
- Select where in the sample list to delay or pause analysis
- From the sample menu, click PAUSE. The pause/delay dialog box will
appear prompting the operator to enter the time to delay and/or restart
he analysis.
- Click OK to apply time delay and when to restart analysis.
This procedure permits the operator to delay /pause and resume an analysis either manually
or at a pre-set time. A clock symbol will appear in the spreadsheet next to the sample that will
be analyzed after the pause.
5 Method
Creation:
1. From the CONFIGURATION menu, click METHOD. The method dialog
box will appear.
2. Click ADD and a row will be added at the bottom of the spreadsheet or
click an empty row and enter a method name.
3. From the method dialog box, click PROPERTIES and enter the desired
ANALYSIS PARAMETERS, ELEMENT PARAMETERS, BURN
PROFILE and MACRO BALLAST PARAMETERS values to
parameters.
4. Click OK when finished.
Selection: This procedure can be done when the method to be used has already been
created.
1. From the main screen menu, double click on the last row of the method
column and select method to be used from the list on the drop down
box.
Conditioner Analysis:
1. Weigh 3-5 blank conditioning samples (~0.15 gram EDTA standard).

Please refer to manual sample preparation.
2. Analyze the samples following analysis procedure.

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Blank Analysis:
1. From the main screen menu, click NAME select BLANK.
2. From the CONFIGURATION menu, click METHOD and choose the

method to be used.
3. Press ANALYZE or F5. The weight is automatically set to 1.000

gram during blank analysis.
Perform at least 3-5 blank analyses or check the standard deviation (SD) of the
last three runs if it is < 0.001% proceed to blank calibration
4. To check standard deviation – from the spreadsheet select from the

sample grid menu and highlight rows of the blank runs. Statistical
data will automatically appear in the dashboard area of the main
screen display.
Blank Calibration: Perform blank calibration before every calibration/analysis.
1. Highlight the blank results of analysis from the spreadsheet to be

calibrated.
2. Click CONFIGURATION and select BLANK.
3. From the table same as below that will appear on the screen, click a
row to select the element(s) and then click INCLUDE or EXCLUDE
an element to be included/excluded in blank calibration.
4. Click OK to calculate the system blank based on the blank analysis

results obtained and the software will automatically compute for the
system blank.
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Standard Calibration:
1. Weigh and analyze standard samples according to the method to be

used.
Please refer to manual sample preparation, weight, sample and method selection.
2. Select/highlight the results to be included in calibration.
3. Click CONFIGURATION and select CALIBRATION.
4. From the fly-out menu that will appear same as below, click the arrow in
the drop down box of the following:
a.) Cell – to select a cell (element) to calibrate. Each cell (element) should
be calibrated separately.
b.) Curve type – to select a curve type to be applied for each cell.
5. View the curve displayed in the graph. As much as possible the graph
should intersect the black squares which represent the values for the
standard analyzed. Evaluate the curve fit by means of Root Mean
Square (RMS) error; the lower the value (approaching zero) the better.
6. Click OK to calibrate the selected cell. One or more cells can be selected.
7. Repeat procedures 4-5 to calibrate other cells.
8. Click OK to exit the calibration procedure and save the calibration curve.
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP11

Drift Correction: Perform drift correction before every analysis to adjust the original
calibration response to match the current instrument response.
1. Weigh 2-3 standard samples. The software will automatically or the

operator can manually select what sample and its weight can be used
as drift standard sample as indicated by X mark.
2. Analyze the sample.
3. Compare the results obtained from the true value. If the results
obtained are within the allowable range proceed to the check standard
procedure; if not select last two (2) data from the results of standard
analysis in the spreadsheet.
4. Click CONFIGURATION and from the fly-out menu select DRIFT
5. From the table same as below that will appear on the screen, click a
row to select the element(s) and click INCLUDE or EXCLUDE
element(s) to be included/excluded in drift correction.
6. Click OK to calculate the drift based on the analysis obtained. The

software will automatically compute for the drift correction of the
system.
Just in case that the operator will shift from one method to another, it is necessary to perform
blank calibration and drift correction separately.
Check Standard: Perform check standard after every drift correction or standard
calibration
1. Weigh and analyze at least two trials of coal standard. Please refer to
table for weight selection of coal standards according to the method to be used for
analysis.
2. Check if the values obtained are within the acceptable range for
specific coal standard. If acceptable, proceed with the analysis of
unknown sample(s); if not, consider/perform minor troubleshooting.
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP11

Sample Analysis:
1. Weigh approximately 0.17 gram of the unknown sample. Please refer to

manual sample preparation.
2. Place the sample in the carousel. Take note of the corresponding

number/position in the carousel.
3. Encode or select the ID code or part number, method, weight and

position in the carousel of the sample in the spreadsheet. Encoding can
be done one at a time, i.e., for every weighing or all at one time to save time.
4. Click F5 or ANALYZE.
Print Results:
1. From the SAMPLES menu, click PRINT. The Report Settings screen
will automatically appear.
2. Click the following selection: REPORT, FIELDS, FONT and ELEMENT

and configure print formats.
REPORT- report format, plot height, statistics, heading text
3. Click OK to save changes and print the selected results.
Shutdown:
A. Total shutdown
1. Close all the gas cylinder valves but do not pull the relief valves to
release gases.
2. From the spreadsheet menu, click DIAGNOSTICS and then select

FURNACE.
Issue Date:
MANUAL
Testing Laboratory
Code: CP11

3. From the furnace diagnostics screen that will automatically appear on

the screen, click STOP to deactivate heaters of the following:
combustion furnace, afterburner furnace, reduction tube, and ballast
oven. Wait until the temperature reaches 500°C or lower
(approximately 30 minutes).
4. Click CLOSE to exit from the DIAGNOSTICS menu.
5. Click DATABASE and select EXIT. The software will automatically

close.
6. From the main screen menu click START and select SHUTDOWN.
(This is the usual procedure how to switch off a computer.)
7. Switch OFF the CHN analyzer unit and AVR.
Failure to cool the furnace prior to turning the power switch off will result in
overheating of the loading head assembly and possible damage to the instrument.
B: Standby mode
1. Perform steps 1 and 2 in case 1
2. From the CONFIGURATION menu, click SYSTEM. The System

Configuration dialog box will appear.
3. Enter the desired furnace standby temperature (preferably 200°C).
4. Click OK to close the system configuration dialog box.
In this case the operator can switch off the computer monitor but not the CPU.
Issue Date:
MANUAL
1
Testing Laboratory
Code: CP11

Maintenance. In order to obtain the best possible results of analysis periodic

maintenance must be performed.
Maintenance counter is list of components and assemblies, within the instrument, that have
been determined to require periodic maintenance. An analysis counter will determine when
periodic maintenance is needed and alert the operator. Please refer to Chapter 6 –
Maintenance pages 6-2 to 6-49 of the TruSpec CHN analyzer operating manual on periodic
maintenance schedule and how to perform specific replacement of consumables.
1. From the configuration menu, click COUNTERS and the dialog box will
appear.
2. Click ADD to define a maintenance counter.
3. Enter the information required in the dialog box. Please refer to

maintenance counter definitions on page 6-47 of the TruSpec CHN
analyzer operating manual for additional information.
4. Reset the count data (encircled column from the table below) once
replacement of consumables listed has been performed.
5. Click OK to exit the procedure.
Please refer to error message definitions on page 5-90 of the TruSpec CHN
Analyzer operating manual for corrective actions and other troubleshooting
concerns.
Weight selection for standard sample:
Data below will vary depending on part number and lot number of standard(s) to be to be
analyzed.
Method Standard Sample Drift Correction Check Standard

(2-3 trials in (2-3 trials in
gram) gram)
EDTA EDTA 0.10 0.17
Single point up to 83%C 502-443 0.09 – 0.10 0.09 – 0.10
Multipoint up to 80%C GBW 11105c or GBW 0.10 0.10
11110e
COKE-Single point up to AR 742 B 0.06 – 0.08 0.06 – 0.08
93%C
RLS Form 1 External
DEPARTMENT OF ENERGY
Energy Compound, Merritt Road, Fort Bonifacio, Taguig, Metro Manila Form #: CF1
Date of Issue: May 2015
Telephone No.: Trunkline 4792900 Local 372 Revision #: 3
Approved By: QM
Direct Line 840-2093
RLS No.
Date:
REQUEST FOR LABORATORY SERVICES
Name & Signature of Person Submitting Sample
Addressee of Invoice and Results of Analysis
Name of Company/Agency/Organization
Address of Company/Agency/Organization
Phone/Fax No.
Sample(s)
LabLabel CustomerLabel Description Qty Unit Analysis Amount
Estimated Cost of Laboratory Services (In Words): Php

* Full payment is required upon submission of sample to the laboratory.
Please pay to the cashier of the Department of Energy and present your Official Receipt in claiming the corresponding
report for analysis/testing from us. This form also serves as your billing statement.
Note : Please make check payment payable to the Department of Energy

Sample/s Received By:
Approved By:
AMELIA M. DE GUZMAN
Director
Energy Research & Testing Laboratory Services
Page 1 of 1
RLS Form 2 Internal Customer
DEPARTMENT OF ENERGY Form #: CF2
Date of Issue: Nov. 2015
Energy Research & Testing Laboratory Services Revision #: 2
Geoscientific Research & Fuel Testing Laboratory Approved By: QM
LWO No.
REQUEST FOR LABORATORY SERVICES [RLS]

Name & Sig. of Person Submitting Sample
Requesting Division/Unit
Phone/Local
Name & Sig. of Head of Requesting Div/Unit
Lab Code (for GRTL

Sample Label Sample Description Test Requested Area / Locality
use only)
Sample Received/Logged By: Date
RLS Received By: Date

Section Chief Signature
Noted By: Date

Division Chief Signature
Special Instructions from Customer (if any) / Remarks
Page 1 of 1
Energy Research & Testing Laboratory Services Apr. 2017
Date of Issue:
Geoscientific Research & Fuel Testing Laboratory Revision #: 4

Approved By: QM
LABORATORY WORK ORDER
Date:
To :
From :
Subject :
External Internal
Reference : RLS No.: LWO No.:
Please analyze the following sample/s for particular test described below:
Sample Tests Special Instruction

Description
Code/Label Requested (If Any)
Date Sample Received By ERTLS :

Date Sample Received By GRFTL :
Date Reported :
Approved By : _V. S. LLAMO____ , Division Chief
Page 1 of 1
Oct. 2017
Date of Issue:
COAL ANALYSIS
Laboratory Work Order-1
Date :_____________________
Reference No. :_____________________
Laboratory Sample No.:____________________________________________________
Customer Sample Description:_______________________________________________
_______________________________________________
Assigned To: ______________________
Sample/s Received By:_______________
Date Sample/s Received:_____________
Sample Preparation Required

Ref. No./ ADL 72 mesh Ashing at Cone Prep’n. Sampling Pellet
Lab. No. (Routine 500oC for AFT of Ash to Prep’n.
Coal Pass 200 For XRF
Analysis) Mesh (XRF)
Ref. No./
Lab. No.
HGI
Determination
Analysis Required:
______________________________________________________________________________
______________________________________________________________________________
Difficulties Encountered:
______________________________________________________________________________
______________________________________________________________________________
Date Prepared Sample/s Submitted:________________________

Received By:__________________________________________
Page 1 of 1
Energy Research & Testing Laboratory Services Nov. 2015
Date of Issue:

Approved By: QM
COAL ANALYSIS
Laboratory Work Order-2
Date :_____________________
Reference No. :_____________________
Laboratory Sample No. :___________________________
Customer Sample Description:__________________________________________________
__________________________________________________
Analysis Required: (Please check the applicable boxes)
Assigned To:
sisylanA etamixorP ‫ٱ‬
)NHC( sisylanA etamitlU ‫ٱ‬
eulaV cifirolaC ‫ٱ‬
rufluS ‫ٱ‬
hsA fo sisylanA lareniM ‫ٱ‬
rufluS fo smroF ‫ٱ‬
erutarepmeT noisuF hsA ‫ٱ‬
gnizidixO ‫ٱ‬
gnicudeR ‫ٱ‬
tseT kniS taolF ‫ٱ‬
)yficepS( srehtO ‫ٱ‬
Prepared Sample/s Received By: __________________________

Date Received: ________________________________________
XRF Pellets Received By:_______________________________ Date: _________________

Ash Cones Received By :_______________________________ Date: _________________
Report Required:
sisaB devieceR sA ‫ٱ‬
riA ‫ٱ‬-dried Basis
sisaB yrD ‫ٱ‬
Draft Report Due Date:____________________
Page 1 of 1
Date of Issue:

Approved By: QM
AIR-DRYING LOSS
RLS No. _________________
Lab. No. _________________
Date : _________________
Time: _________________
Weight of tray (a) + sample (b1) ________________ Final ADL = (b1-bf) x 100%
Weight of tray (a) ________________ b1
Weight of sample (b1) ________________ Final ADL = ________ %
*Acceptable limit of change = Loss in weight < 0.1% per hour

1 2 3 4
Date/Time
a+b1
-a
b
(bn+1-bn) x 100%
b1
5 6 7 8
Date/Time
a+b1
-a
b
(bn+1-bn) x 100%
b1
9 10 11 12
Date/Time
a+b1
-a
b
(bn+1-bn) x 100%
b1
Submitted By: _______________________ Received By: ________________

Date : ________________
Page 1 of 1
Date of Issue:
Approved By: QM
PRELIMINARY TEST RESULTS
Date : ________________________________
Ref. No. : ________________________________
No. of Samples : ________________________________
Description : ________________________________________________________
Prepared By : ________________________________________________________
Analysis/es Required : ________________________________________________________
Analyst(s) : ________________________________________________________
Basis : sA ‫ٱ‬-received
riA ‫ٱ‬-dried
yrD ‫ٱ‬
______________________________________________ : yficepS :srehtO ‫ٱ‬
Date/Time Started : ________________________________
Date/Time Finished : ________________________________
Remarks: _______________________________________________________________
________________________________________________________________
Sample No. Trial Results

No.
______________________________
Signature of Analyst(s)
Page 1 of 1
DEPARTMENT OF ENERGY
Geoscientific Research & Fuel Testing Laboratory
PAB ACCREDITED
TESTING LABORATORY
PNS ISO/IEC 17025:2005
LA-2009-152B
Laboratory Analysis/Test Report Form #: CF8a
Jan. 2016
Date of Issue:
Date : Revision #: 6
RLS No. : Approved By: QM
Sample Description :
Date Received :
Date Test Completed:
Basis :
Summary of Results:
Analysis Method Sample Marked
Air Drying Loss*, % mass fraction ISO 5068-1:2007

Residual Moisture*, % mass fraction ISO 5068-1983
Volatile Matter, % mass fraction ISO 562:2010
Ash, % mass fraction ISO 1171:2010
Fixed Carbon*, % mass fraction ISO 17246:2010
Carbon*, weight % ASTM D 5373-02
Hydrogen*, weight % ASTM D 5373-02
Nitrogen*, weight % ASTM D 5373-02
Sulfur*, weight % ASTM D 4239-05
Method B
Gross Calorific Value*, cal/g ASTM D 5865-04
BTU/lb
__________________________________________________________________________
The test results presented in this report relate only to the item/s tested. This report is submitted for the exclusive use of the customer to
whom it is addressed. No part of this test report shall be quoted or used for promotional purposes without the written approval of the
Department of Energy.
Remarks/Attachments:
* Test outside the laboratory’s scope of accreditation.
Analyzed By:
Checked By:
Noted By:
Page 1 of 1
DEPARTMENT OF ENERGY Form #: CF8b
Date of Issue:
Revision #:
Approved By: QM
Laboratory Analysis/Test Report
Date :
RLS No. :
Sample Description :
Date Received :
Date Test Completed:
Basis :
Summary of Results:
Analysis Method Sample Marked
Air Drying Loss, % mass fraction ISO 5068-1:2007

Fixed Carbon, % mass fraction ISO 17246:2010
Carbon, weight % ASTM D 5373-02
Hydrogen, weight % ASTM D 5373-02
Nitrogen, weight % ASTM D 5373-02
Sulfur, weight % ASTM D 4239-05
Method B
Gross Calorific Value, cal/g ASTM D 5865-04
BTU/lb
__________________________________________________________________________
Analyzed By:
Checked By:
Noted By:
Page 1 of 1
Republic of the Philippines Form #: CF10b
DEPATMENT OF ENERGY Oct. 2015
Date of Issue:
Revision #:
Energy Research and Testing Laboratory Services Approved By: QM
Date
RLS No.
Company
Address
Phone Number:
Fax Number :
LABORATORY ANALYSIS / TEST REPORT

Sample/s Test / Analysis Method Results
Air Drying Loss, % mass fraction ISO 5068-1:2007
Fixed Carbon, % mass fraction ISO 17246:2010
Carbon, weight % ASTM D 5373-02
Hydrogen, weight % ASTM D 5373-02
Nitrogen, weight % ASTM D 5373-02
Sulfur, weight % ASTM D 4239-05
Method B
Gross Calorific Value, cal/g ASTM D 5865-04
BTU/lb
___________________________________________________________________________________________________________
Basis:
Amelia M. de Guzman
Director
Page 1 of 1
Date of Issue:

Approved By: QM
COMPLAINT REPORT
Date:_______________
Reference No. :_____________________________
To :_____________________________
Director, ERTLS
From :_____________________________
Name of Customer/Organization
Details of Incident:
Suggested Corrective Action:
__________________
Signature
Page 1 of 1
DEPARTMENT OF ENERGY Form #: CF12a
Energy Research & Testing Laboratory Services May 2017
Date of Issue:
Approved By: QM
CUSTOMER RATING
Please accomplish this form and drop at the box near the lobby guard (Or drop at the feedback DROP BOX at the Office of the Director, ERTLS)
To be filled up by attending employee:

Type of Sample: Petroleum products Geothermal/mineral water Coal Gas Rock Others, please specify:__________
Name of attending employee: Date:

Position: Division/Services:
To be filled up by customer:
Name of Customer: Signature:
Company: Address/Tel.No.:
Purpose: Inquire Submit sample Pick up test report Others, please specify:
Please rate the laboratory/attending employee on the following factors (if applicable):
Comments/Suggestions
10 - Excellent 4 - Poor
8 - Good 2 - Very Poor
6 - Satisfactory
1. Courtesy - Polite, kind and thoughtful behavior toward co- 10 8 6 4 2

employee/ public/customer in manner of speech and actuation.
2. Readiness for service - Punctual, not engaging in unofficial 10 8 6 4 2

matters, like chatting, eating, telephoning, etc. while customer is
waiting or watching.
3. Satisfaction (overall) - Ability to fulfill the needs/requirements of 10 8 6 4 2

the customer; contentment level of customer on services provided
(other criteria considered).
Page 1 of 1
Date of Issue:
Approved By: QM
CUSTOMER RATING
Please accomplish this form and drop at the box near the lobby guard (Or drop at the feedback DROP BOX at the Office of the Director, ERTLS)
To be filled up by attending employee:
Type of Sample: Petroleum products Geothermal/mineral water Coal Gas Rock Others, please specify:__________
Name of attending employee: Date:
Position: Division/Services:
To be filled up by customer:
Name of Customer: Signature:
Company: Address/Tel.No.:
Purpose: Inquire Submit sample Pick up test report Others, please specify:
Please rate the laboratory/attending employee on the following factors (if applicable): Comments/Suggestions
1. Satisfaction relating to technical competence - Ability to
address the needs/requirements of the customer related to
sample testing/research.
1.1. Inquiry on type of analysis appropriate to the 10- All inquiry clearly answered/clarified
customer's sample and/or purpose clearly 8- One (1) question not answered
answered or clarified. 6- Two (2) questions not answered
4- Three (3) questions not answered
2- More than three (3) questions not
answered
1.2. Test report contains all relevant information on 10- All requested information reported
the test/s requested, i.e., test parameter, sample 8- One (1) item missing
label, test method, basis and other technical 6- Two (2) items missing
remark/s. 4- Three (3) items missing
2- More than three (3) items missing
1.3. When requested, test results are explained 10- All test results explained fully
fully and understood by the customer. 8- One (1) test result not explained
6- Two (2) test results not explained
4- Three (3) test results not explained
2- More than three (3) test results
not explained
2. Availability of test result/s - Meets scheduled date of release of 10- On-time
test report (ten working days from receipt of sample). 8- One (1) day late
6- Two (2) days late
4- Three (3) days late
2- More than three (3) days late
Page 1 of 1
Date of Issue:

Approved By: QM
NON CONFORMANCE AND ACTION REPORT
NCR No. Date Raised:

Issued To: Ref. to ISO/IEC 17025 Clause/s:
Section: Geothermal-Coal Doc. Ref.
Found: During Audit ( ) Outside Audit ( )
Complaint ( ) Quality objectives/systems ( )
Equipment ( ) Others ( )
Type: Significant Non-Conformity ( ) Minor Non-Conformity ( ) Observation ( )
Description (Use separate sheet if necessary):
Raised by: Acknowledged by:

________________________________ ___________________________
Auditor/Customer/Lab. Personnel/Others Auditor/Customer/Lab. Personnel
Root Causes Identified: (Root cause analysis)
Corrective/Preventive Action (1) ( ) Cleared

( ) Not Cleared
Remarks:
___________________________
Auditor/Customer/Lab.
Personnel/Others
_________________
Date
Corrective/Preventive Action (2) ( ) Cleared
( ) Not Cleared
Remarks:
______________________________
Auditor/Customer/Lab.
Personnel/Others
_________________
Date
Follow-up Effectiveness
Verified by (Asst. QM): Noted by (QM): Date of Close Out:

Page 1 of 1
Page 1 of 1
Oct. 2015
Date of Issue:
DOCUMENT ISSUANCE / CHANGE NOTICE
Document Originator:_________________ Date:__________
New Revision
Type From
Title
Doc. Code
Effectivity
Distribution List
To
Reason/s for revision/s:__________________________________________________________________________________________
Prepared By:_________________ Approved By:______________
Discussed with relevant personnel? yes no
Signature of affected personnel:
Issued to relevant personnel and retrieved the obsolete? yes no
Signature of recepients:
REMARKS:___________________________________________________________________________________________
Page 1 of 1
Energy Research & Testing Laboratory Services Jan. 2016
Date of Issue:
Revision #: 2
AMBIENT MONITORING REPORT

SERIAL No.________________________
FOR THE MONTH/YEAR OF________________
TIME Reading (%RH) / Temp (°C)

DATE 9:00 AM 2:00 PM AVERAGE LOGGED BY
%RH T, °C %RH T, °C %RH T, °C
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
REMARKS:
Page 1 of 1
Date of Issue:
Revision #: 3
MONTHLY EQUIPMENT MAINTENANCE PROGRAM

Acculab - Analytical Balance
Serial No. 19190040
Year
JAN FEB MAR APR MAY JUN
A. Care and Maintenance
1. Remove the residues from the weighing chamber using a
small brush.
2. Clean the weighing pan and housing with soft cloth.
3. Check dessicant and replace if necessary.
B. Routine check
1. Check and ensure that the balance is leveled such

that the bubble is in the middle of the circle.
2. Check that the unit is working.
a. Go through internal calibration
C. Calibration against a standard weight

1. Calibrate against standard 1-gram weight.
2. Record the reading for 1-gram weight.
Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 1 of 1
Date of Issue:
Revision #: 3

Acculab - Analytical Balance
Serial No. 19190040
Year
JUL AUG SEP OCT NOV DEC
small brush.
B. Routine check


Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 1 of 1
DEPARTMENT OF ENERGY Form #:CF20a
Date of Issue:
Revision #: 3

Leco 250 - Analytical Balance
Serial No.
Year
small brush.
B. Routine check

Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 1 of 1
DEPARTMENT OF ENERGY Form #:CF20b
Date of Issue:
Revision #: 3

Leco 250 - Analytical Balance
Serial No.
Year

small brush.
B. Routine check

Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 1 of 1
Date of Issue:
Revision #: 3
Geoscientific Research & Fuel Testing laboratory
Approved By: QM

LECO AC 350 ISOPERIBOL CALORIMETER
Serial No. 3355
Year

A. Oxygen gas supply
1. Check the oxygen gas supply. Replace the
cylinder if O2 supply is < 450 psi.
2. Check and make sure that the gas regulator

is properly working.
3. Check and make sure that all gas hoses are

free from leak
4. Check and make sure that the Matsunaga

AVR is properly working.
Conducted by:
Date Conducted:
B. Equipment
1. Check all wirings for nicks and cuts.
2. Clean the equipment with soft cloth.
Conducted by:
Date Conducted:
C. Bomb Assembly
1. Check for gas bubbles released from any point
on the bomb if submerged in water during firing.
2. Check for any sign(s) of weakness or

deterioration.
Conducted by:
Date Conducted:
D. Printer
1. Ckeck if the unit is functioning. Replace ribbon
if necessary. Make sure that reserve ribbon and
printer paper are available at all times.
2. Check all wirings for nick and cuts.
Conducted by:
Date Conducted:
Page 1 of 2
E. Water Cooling Sytem
1. Check if the unit is functioning.
2. Check the water level if it is 4 inches from the top

of the reservoir. Fill it up with distilled water if necessary.
4. Clean the unit with soft cloth and dust brush.
Conducted by:
Date Conducted:
F. Calibration (Quarterly)
1. Perform calibration using Benzoic Acid Pellets.
2. Update calibration logbook and file print-out.
Conducted by:
Date Conducted:
G. Others
1. Make sure that standardized Sodium Carbonate

solution is available at all times.
2. Ensure that equipment area is clean.
Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3
Geoscientific Research & Fuel Testing laboratory
Approved By: QM

LECO AC 350 ISOPERIBOL CALORIMETER
Serial No. 3355
Year



free from leak
4. Check and make sure that the Matsunaga

AVR is properly working.
Conducted by:
Date Conducted:
B. Equipment
Conducted by:
Date Conducted:
C. Bomb Assembly

deterioration.
Conducted by:
Date Conducted:
D. Printer
1. Ckeck if the unit is functioning. Replace ribbon
Conducted by:
Date Conducted:
Page 1 of 2
E. Water Cooling Sytem

of the reservoir. Fill it up with distilled water if necessary.
Conducted by:
Date Conducted:
F. Calibration (Quarterly)
Conducted by:
Date Conducted:
G. Others

Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 3

PARR 6200 ISOPERIBOL CALORIMETER
Serial No. M15674
Year


free from leak
4. Check and make sure that the Powercom
UPS and Battery are properly working.
Conducted by:
Date Conducted:
B. Equipment

Conducted by:
Date Conducted:
C. Bomb Assembly

deterioration.
Conducted by:
Date Conducted:
D. Printer
1. Ckeck if the unit is functioning. Replace rebbon

Conducted by:
Date Conducted:
Page 1 of 2
E. Water Handling System

of the reservoir. Fill it up with distilled water if
necessary.
Conducted by:
Date Conducted:
F. Calibration (Monthly)

Conducted by:
Date Conducted:
G. Others

Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3

PARR 6200 ISOPERIBOL CALORIMETER
Serial No. M15674
Year


free from leak
4. Check and make sure that the Powercom
UPS and Battery are properly working.
Conducted by:
Date Conducted:
B. Equipment

Conducted by:
Date Conducted:
C. Bomb Assembly

deterioration.
Conducted by:
Date Conducted:
D. Printer
1. Ckeck if the unit is functioning. Replace rebbon

Conducted by:
Date Conducted:
Page 1 of 2
E. Water Handling System

of the reservoir. Fill it up with distilled water if
necessary.
Conducted by:
Date Conducted:
F. Calibration (Monthly)

Conducted by:
Date Conducted:
G. Others

Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Energy Research & Testing Laboaratory Services Jan. 2017
Date of Issue:
Revision #: 3

LECO TRUSPEC CHNS ANALYZER
Serial No. 3672 / 4118
Year_____________________
A. Gases
1. Check gas supplies: a. Oxygen ( CHN )
b. Compressed Air
c. Helium
d. Oxygen ( Add-on S)
( Inform laboratory technician to procure or prepare
for petty cash advance if applicable)
2. Check and make sure that all gas regulators are working
properly
3. Check and make sure that all gas hoses are free
from leak.
4. Check and make sure that exhaust gas tubings are
free flowing.
B. Equipment
CHN Analyzer
1. Check the equipment display by going through the
pre-set parameters, i.e., furnace temp, IR and TC
cell values.
2. Check the periodic maintenance counter especially
for crucible and reagents. Replace if necessary.
3. Clean the equipment with soft cloth
Add-on Sulfur Analyzer

pre-set parameters, i.e., furnace temp & IR cell value.
for anhydrone or filter. Replace if necessary.
C. Computer and Printer

Computer
1. Check if the unit is functioning properly.
3. Clean the unit with soft cloth
Printer
2. Check print-outs. Replace ribbon if necessary.
(Make sure that reserve ribbon and printer paper
are available at all times)

4. Clean the unit with soft cloth.
Page 1 of 2
D. Calibration
CHN Analyzer
1. Perform leak check test.
2. Perform system check.
3. Perform blank calibration.
4. Analyze standard sample as check standard. Apply
drift correction if needed. (Monthly)
5. Perform standard calibration.(Quarterly)

4. Perform standard calibration. (Quarterly)
E. Others
1. Ensure that instrument area is clean.
2. Check supplies and materials.
(Inform laboratory technician of any need)
Conducted by:
Date:
Remarks:
Page 2 of 2
Energy Research & Testing Laboaratory Services Jan. 2017
Date of Issue:
Revision #: 3

LECO TRUSPEC CHNS ANALYZER
Serial No. 3672 / 4118
Year_____________________
A. Gases
1. Check gas supplies: a. Oxygen ( CHN )
b. Compressed Air
c. Helium
d. Oxygen ( Add-on S)
( Inform laboratory technician to procure or prepare
for petty cash advance if applicable)
2. Check and make sure that all gas regulators are working
properly
3. Check and make sure that all gas hoses are free
from leak.
4. Check and make sure that exhaust gas tubings are
free flowing.
B. Equipment
CHN Analyzer
pre-set parameters, i.e., furnace temp, IR and TC
cell values.
for crucible and reagents. Replace if necessary.

pre-set parameters, i.e., furnace temp & IR cell value.
for anhydrone or filter. Replace if necessary.
C. Computer and Printer

Computer
3. Clean the unit with soft cloth
Printer
2. Check print-outs. Replace ribbon if necessary.
(Make sure that reserve ribbon and printer paper
are available at all times)

4. Clean the unit with soft cloth.
Page 1 of 2
D. Calibration
CHN Analyzer
1. Perform leak check test.
5. Perform standard calibration.(Quarterly)

4. Perform standard calibration. (Quarterly)
E. Others
1. Ensure that instrument area is clean.
(Inform laboratory technician of any need)
Conducted by:
Date:
Remarks:
Page 2 of 2
Date of Issue:
Revision #: 3

PRUFER FURNACE I
Serial No. P/N LE-EQ-000773
Year
A. Operation
1. Check if the unit is working
2. For the thermocouple, check if the temperature

will rise at its set point
Conducted by:
Date Conducted:
B. Routine check
1. Check and ensure tight closing of the door
2. Check and make sure that the air inlet located

at the top of the furnace is free from clog
Conducted by:
Date Conducted:
C. Calibration
1. Have the furnace calibrated annually
2. Update calibration logbook and index
3. File calibration certificate
Conducted by:
Date Conducted:
D. Care
1. Clean the interior of the furnace
2. Clean the exterior and casing with a damp cloth
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3

PRUFER FURNACE I
Year
A. Operation

Conducted by:
Date Conducted:
B. Routine check

Conducted by:
Date Conducted:
C. Calibration
Conducted by:
Date Conducted:
D. Care
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 3

PRUFER FURNACE II
Year
A. Operation

Conducted by:
Date Conducted:
B. Routine check

Conducted by:
Date Conducted:
C. Calibration
Conducted by:
Date Conducted:
D. Care
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3

PRUFER FURNACE II
Year
A. Operation

Conducted by:
Date Conducted:
B. Routine check

Conducted by:
Date Conducted:
C. Calibration
Conducted by:
Date Conducted:
D. Care
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 3

MA-2000 MERCURY ANALYZER
Serial No. P/N JE-HE-03-1149
Year

A. Equipment
1. Check if the boat changer is functioning properly.
Clean if necessary.
Conducted by:
Date Conducted:
B. Balance
1. Check and ensure that the balance is leveled such that
the bubble is in the middle of the circle.
3. Calibrate against standard 200 grams.

(100g, 50g, 2pcs-20g, 10g external weights)
4. Brush out/Wipe up any spills on the balance.
5. Clean the weighing pan and housing with a soft cloth.
Conducted by:
Date Conducted:
C. Computer
1. Check if the MA2000win program is working.
Conducted by:
Date Conducted:
D. Printer
2. Check all wirings or nicks and cuts.
3. Clean the printer with soft cloth and dust brush.
Conducted by:
Date Conducted:
Page 1 of 2
E. Calibration
1. Perform calibration using Hg standard solutions.
Conducted by:
Date Conducted:
F. Others
1. Ensure that the unit is clean.

Inform lab. tech. of any need.
Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3

MA-2000 MERCURY ANALYZER
Serial No. P/N JE-HE-03-1149
Year
A. Equipment
1. Check if the boat changer is functioning properly.
Clean if necessary.
Conducted by:
Date Conducted:
B. Balance
1. Check and ensure that the balance is leveled such that
the bubble is in the middle of the circle.
3. Calibrate against standard 200 grams.

(100g, 50g, 2pcs-20g, 10g external weights)
4. Brush out/Wipe up any spills on the balance.
5. Clean the weighing pan and housing with a soft cloth.
Conducted by:
Date Conducted:
C. Computer
1. Check if the MA2000win program is working.
Conducted by:
Date Conducted:
D. Printer
2. Check all wirings or nicks and cuts.
3. Clean the printer with soft cloth and dust brush.
Conducted by:
Date Conducted:
Page 1 of 2
E. Calibration
1. Perform calibration using Hg standard solutions.
Conducted by:
Date Conducted:
F. Others

Inform lab. tech. of any need.
Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 3

COAL - AIR DRYING OVEN
SERIAL No.
Year

I. OPERATION
1. Check that the unit is working
2. Check that the blower is working properly
II. ROUTINE CHECK
1. Check the temperature setting against digital thermometer reading

2. Check the temperature reading using calibrated thermometers
3. Update logbook
III. CARE AND MAINTENANCE
1. Check that thermometers are tightly mounted
2. Check that the air inlet/outlet holes are free from clogs
3. Check the unit for any sign of deterioration
4. Lubricate mechanical parts of the door hinges and

movable parts of the door lock if necessary
5. Clean the unit using vacuum cleaner

and soft cloth.
IV. CALIBRATION - ANNUALLY
1. Have the oven calibrated annually
2. Have the thermometers calibrated annually
3. File calibration certificates
Conducted By:
Date:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 1 of 1
Date of Issue:
Revision #: 3

COAL - AIR DRYING OVEN
SERIAL No.
Year

I. OPERATION
2. Check that the blower is working properly
II. ROUTINE CHECK
1. Check the temperature setting against digital thermometer reading

2. Check the temperature reading using calibrated thermometers
3. Update logbook
III. CARE AND MAINTENANCE
1. Check that thermometers are tightly mounted
2. Check that the air inlet/outlet holes are free from clogs
3. Check the unit for any sign of deterioration
4. Lubricate mechanical parts of the door hinges and

movable parts of the door lock if necessary
5. Clean the unit using vacuum cleaner

and soft cloth.
IV. CALIBRATION - ANNUALLY
2. Have the thermometers calibrated annually
3. File calibration certificates
Conducted By:
Date:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 1 of 1
Date of Issue:
Revision #: 2

JOUAN OVEN
Serial No. 39508380
Year
JAN. FEB. MAR. APR. MAY JUN. JUL. AUG. SEPT.OCT. NOV. DEC.
A. Operation
B. Routine Checks
1. Check thermostat scale setting against

temperature reading.
Readjust the thermostat, if necessary
2. Check and ensure tight closing of the door.

Adjust the hinge or the locking plate, if
necessary
C. Periodic Maintenance (Indicate date conducted)
1. Lubricate the mechanical parts of the door

hinges and movable parts of the door lock
(annually)
D. Care
1. Clean the interior of the oven
2. Clean the exterior and casing of the oven with

soft cloth using dilute liquid detergent solution
REMARKS :
JAN.
FEB.
MAR.
APR.
MAY.
Page 1 of 2
JUN.
JUL.
AUG.
SEPT.
OCT.
NOV.
DEC.
JAN. FEB. MAR. APR. MAY JUN. JUL. AUG. SEPT.OCT. NOV. DEC.
Conducted By :
Date :
Page 2 of 2
Date of Issue:
Revision #: 3

CARBOLITE MINIMUM FREE SPACE OVEN
Serial No. 1038
Year

A. Gas Supply, Lines and Accessories
1. Check if there is enough supply of N2
gas. Make sure that a spare cylinder is available
at all times

is properly working
3. Check and make sure that the gas hose from

the gas tank to the unit is free from leak
4. Check and make sure that the exhaust gas

tubing is free flowing
5. Check the anhydrone. Replace if necessary
6. Check and make sure that the gas output

flow meter is free from moisture
Conducted by:
Date Conducted:
B. Calibration - Annually
2. Update calibration logbook
Conducted by:
Date Conducted:
C. Care and Maintenance

1. Ensure that the unit is free from dust
2. Make sure that the area is clean
3. Cover the unit with plastic
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3

CARBOLITE MINIMUM FREE SPACE OVEN
Serial No. 1038
Year

A. Gas Supply, Lines and Accessories
1. Check if there is enough supply of N2
gas. Make sure that a spare cylinder is available
at all times

is properly working
3. Check and make sure that the gas hose from

the gas tank to the unit is free from leak

5. Check the anhydrone. Replace if necessary
6. Check and make sure that the gas output

flow meter is free from moisture
Conducted by:
Date Conducted:
B. Calibration - Annually
2. Update calibration logbook
Conducted by:
Date Conducted:
C. Care and Maintenance

1. Ensure that the unit is free from dust
3. Cover the unit with plastic
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 3

LEC0 SC 432 DR - SULFUR ANALYZER
Serial No. 3388 / 3331
Year
A. Gas Supplies, Lines and Accessories
1. Check the gases (O2 and Comp. Air).

Make sure that there is enough supply and
spare cylinders are available at all times
2. Check and make sure that all gas regulators

are properly working

free from leak

5. Check and make sure that the AFA AVR

output is 220v
Conducted by:
Date Conducted:
B. Furnace, Autoloader and Monitor
1. Fan filters located a the top of the unit and at the

back of the furnace - if dirt is visible, wash with soap
and water. Shake out excess water before replacing it.
2. Anhydrone or Magnesium Perchlorate - replace when

warning alarm displays or whenever the reagent
becomes caked or moistened.
3. Reagent tube - wash with soap and water. Let it dry

before placing glass wool and anhydrone.
4. Heating element - check if the temperature will rise at

its set point.
Conducted by:
Date Conducted:
Page 1 of 2
C. Printer
1. Check if the unit is working.
2. Replace ribbon if necessary. Make sure that a spare

ribbon and printer paper are available at all times.
Conducted by:
Date Conducted:
D. Calibration
1. Calibrate the instrument using coal standard.
Conducted by:
Date Conducted:
E. Others
2. Ensure that the instrument area is clean.
Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3

LEC0 SC 432 DR - SULFUR ANALYZER
Serial No. 3388 / 3331
Year
1. Check the gases (O2 and Comp. Air).



free from leak


output is 220v
Conducted by:
Date Conducted:
B. Furnace, Autoloader and Monitor
1. Fan filters located a the top of the unit and at the

back of the furnace - if dirt is visible, wash with soap
and water. Shake out excess water before replacing it.
2. Anhydrone or Magnesium Perchlorate - replace when

warning alarm displays or whenever the reagent
becomes caked or moistened.
3. Reagent tube - wash with soap and water. Let it dry

before placing glass wool and anhydrone.
4. Heating element - check if the temperature will rise at

its set point.
Conducted by:
Date Conducted:
Page 1 of 2
C. Printer
1. Check if the unit is working.
2. Replace ribbon if necessary. Make sure that a spare

ribbon and printer paper are available at all times.
Conducted by:
Date Conducted:
D. Calibration
1. Calibrate the instrument using coal standard.
Conducted by:
Date Conducted:
E. Others
2. Ensure that the instrument area is clean.
Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 3

LAS NAVAS TGA-1000 THERMOGRAVIMETRIC ANALYZER
Serial No. 000202
Year
1. Check the gases (N2,O2 and Comp. Air).

free from leak
output is 220v
Conducted by:
Date Conducted:
B. Carousel, Balance and Furnace

Note: From the main menu of TGA-FAST, access "DIAGNOSTICS"
in the "OPTIONS" menu to check the carousel, balance and
furnace.
1. Check the carousel elevation. Make sure that there
is a 2-3 mm distance between the pedestal and the
crucible if the carousel is in "up" position.
2. Check the carousel position by sending a carousel
position #. Make sure that the carousel follows the
position entered.
3. Check and make sure that the balance reading being
displayed in the "diagnostics" window coincides with
the one being displayed by the balance inside the
instrument
4. Verify balance performance by weighing a 1-g weight.
(+/-0.005 g)
5. Check and make sure that the temperature reading

being displayed in the "diagnostics" window is the
same as the one being displayed by the temperature
controller inside the instrument
6. For the furnace thermocouple, check if the temperature
will rise at its set point.
Conducted by:
Date Conducted:
Page 1 of 2
C. Printer

2. Replace ink if necessary. Make sure that a spare
is available at all times
Conducted by:
Date Conducted:
D. Calibration
1. Have the furnace calibrated once a year.
2. Calibrate the instrument using coal standards
This is done once a year
3. Update calibration factors in the linearization
spreadsheet (TGA-FAST)
4. Update calibration logbook and calibration chart
5. File print-out
Conducted by:
Date Conducted:
E. Care and Maintenance

1. Ensure that the instrument is free from dust
2. Ensure that the monitor, cpu and printer are clean
4. Cover the instrument and the computer set with
plastic
Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 3

LAS NAVAS TGA-1000 THERMOGRAVIMETRIC ANALYZER
Serial No. 000202
Year
1. Check the gases (N2,O2 and Comp. Air).

free from leak
output is 220v
Conducted by:
Date Conducted:
B. Carousel, Balance and Furnace

Note: From the main menu of TGA-FAST, access "DIAGNOSTICS"
in the "OPTIONS" menu to check the carousel, balance and
furnace.
1. Check the carousel elevation. Make sure that there
is a 2-3 mm distance between the pedestal and the
crucible if the carousel is in "up" position.
2. Check the carousel position by sending a carousel
position #. Make sure that the carousel follows the
position entered.
3. Check and make sure that the balance reading being
displayed in the "diagnostics" window coincides with
the one being displayed by the balance inside the
instrument
4. Verify balance performance by weighing a 1-g weight.
(+/-0.005 g)
5. Check and make sure that the temperature reading

being displayed in the "diagnostics" window is the
same as the one being displayed by the temperature
controller inside the instrument
6. For the furnace thermocouple, check if the temperature
will rise at its set point.
Conducted by:
Date Conducted:
Page 1 of 2
C. Printer

2. Replace ink if necessary. Make sure that a spare
is available at all times
Conducted by:
Date Conducted:
D. Calibration
1. Have the furnace calibrated once a year.
2. Calibrate the instrument using coal standards
This is done once a year
3. Update calibration factors in the linearization
spreadsheet (TGA-FAST)
4. Update calibration logbook and calibration chart
5. File print-out
Conducted by:
Date Conducted:
E. Care and Maintenance

1. Ensure that the instrument is free from dust
2. Ensure that the monitor, cpu and printer are clean
4. Cover the instrument and the computer set with
plastic
Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 3
MONTHLY HOUSEKEEPING PROGRAM

(Laboratory Technician)
Year _________
Sample Preparation Room JAN FEB MAR APR MAY JUN

1. Ensure that the area is clean.
2. Clean equipment units in the area using soft
cloth and mild detergent. Perform minor
troubleshooting if necessary. Place covers when not in use
2. Wash/clean glassware, crucibles and
laboratory materials (sieves, trays, vials, etc.)
after every use and store in proper place.
3. Store coal samples in the racks and dispose
as scheduled. Update coal waste logbook.
4. Ensure that gas cylinders are properly
chained in place and labeled (if empty or the
date of delivery).
5. Ensure that all equipment units, light switches
and fans are turned off; windows and doors
are closed before leaving the area after office hours daily.
Wet Laboratory, Calorimeter, XRF, Mercury

and Instrument Rooms
1. Clean the area every first day of the week. 1st wk
Clean every housing/casing of equipment 2nd wk
units using soft cloth and mild detergent. 3rd wk
Place cover when not in use. 4th wk
3. Ensure that gas cylinders (for calorimeter
and XRF only) are properly chained in place.
airconditioners and fans are turned off;
windows, doors and faucets are closed before
leaving the area after office hours daily
Date and Signature
Remarks:
Jan
Feb
Mar
Apr
May
Jun
Page 1 of 1
Date of Issue:
Revision #: 3
MONTHLY HOUSEKEEPING PROGRAM

(Laboratory Technician)
Year _________
Sample Preparation Room JUL AUG SEP OCT NOV DEC

1. Ensure that the area is clean.
2. Clean equipment units in the area using soft
cloth and mild detergent. Perform minor
troubleshooting if necessary. Place covers when not in use
2. Wash/clean glassware, crucibles and
laboratory materials (sieves, trays, vials, etc.)
after every use and store in proper place.
3. Store coal samples in the racks and dispose
as scheduled. Update coal waste logbook.
4. Ensure that gas cylinders are properly
chained in place and labeled (if empty or the
date of delivery).
and fans are turned off; windows and doors
are closed before leaving the area after office hours daily.
Wet Laboratory, Calorimeter, XRF, Mercury

and Instrument Rooms
1. Clean the area every first day of the week. 1st wk
Clean every housing/casing of equipment 2nd wk
units using soft cloth and mild detergent. 3rd wk
Place cover when not in use. 4th wk
3. Ensure that gas cylinders (for calorimeter
and XRF only) are properly chained in place.
airconditioners and fans are turned off;
windows, doors and faucets are closed before
leaving the area after office hours daily
Date and Signature
Remarks:
Jul
Aug
Sep
Oct
Nov
Dec
Page 1 of 1
Jan. 2016
Date of Issue:
DOCUMENT REVIEW
Document Originator:_________________ Date:__________
Review
Type
Title
Doc. Code
Effectivity
Distribution List
Remarks:____________________________________________________________________________________________
Reviewed By:_________________ Noted By:______________
Discussed with relevant personnel? yes no
Signature of affected personnel:
Page 1 of 1
Date of Issue:
Revision #: 2

Kern - Analytical Balance
Model: ABS 220-4N
Serial No. WB13AR0151
Year
small brush.
B. Routine check


Conducted by:
Date Conducted:
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 1 of 1
Date of Issue:
Revision #: 2

Kern - Analytical Balance
Model: ABS 220-4N
Serial No. WB13AR0151
Year
small brush.
B. Routine check


Conducted by:
Date Conducted:
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 1 of 1
Date of Issue:
Revision #: 2

CARBOLITE FURNACE
Model : AAF 1100
Serial No. 21-400256
Year
A. Operation

Conducted by:
Date Conducted:
B. Routine check

Conducted by:
Date Conducted:
C. Calibration
Conducted by:
Date Conducted:
D. Care
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 2

CARBOLITE FURNACE
Model : AAF 1100
Year
A. Operation

Conducted by:
Date Conducted:
B. Routine check

Conducted by:
Date Conducted:
C. Calibration
Conducted by:
Date Conducted:
D. Care
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:
Revision #: 2

CARBOLITE FURNACE
Model : VMF 1000
Year
A. Operation

Conducted by:
Date Conducted:
B. Routine check

Conducted by:
Date Conducted:
C. Calibration
Conducted by:
Date Conducted:
D. Care
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JAN
FEB
MAR
APR
MAY
JUN
Page 2 of 2
Date of Issue:
Revision #: 2

CARBOLITE FURNACE
Model : VMF 1000
Year
A. Operation

Conducted by:
Date Conducted:
B. Routine check

Conducted by:
Date Conducted:
C. Calibration
Conducted by:
Date Conducted:
D. Care
Conducted by:
Date Conducted:
Page 1 of 2
REMARKS:
JUL
AUG
SEP
OCT
NOV
DEC
Page 2 of 2
Date of Issue:

Approved By: QM
TRAINING EVALUATION FORM

(Applies to Trainings Other Than Equipment Training)
Name of Trainee: ____________________________________________________
Section/Position: _____________________________________________________
Title of the Training: __________________________________________________
Duration: ___________________________________________________________
Direction: Please check appropriate box.
Low High
1 2 3 4 5
How adequately did the training

meet the objectives of GRFTL?
To what extent did the training

enrich the knowledge of the trainee?
How useful were the topics of the

training to the trainee in relation to
his work?
Was the training duration sufficient

enough to enrich trainee’s
knowledge?
Evaluated by: ______________________________________________________

Name / Signature of Supervisor
Form #: CF41
Department of Energy Aug. 2016
Date of Issue:
Energy Research & Testing Laboratory Services Revision #:
Approved By: QM
Geothermal-Coal Section
INTERNAL QUALITY AUDIT CHECKLIST

PNS ISO/IEC 17025
Reference to Laboratory
Clause Requirement for Accreditation Document Remarks
(To be completed by the laboratory)
4 4 Management Requirements
4.1 Organization
4.1.1 Legal an entity that can be held legally
identity responsible
4.1.2 Carry out testing or calibration
Responsibility activities to meet requirements of
the standard, its customers,
regulatory authorities or
accreditation bodies
4.1.3 ensure management system covers
Scope of activities in the laboratory’s
management permanent facility, sites away from
system its permanent facilities, or in
associated temporary or mobile
facilities
4.1.4 when part of an organization
Conflict of performing activities other than
interest testing and/or calibration, ensure
the laboratory defines the
responsibilities of key personnel to
identify potential conflicts of interest
4.1.5a have managerial and technical

Managerial and personnel, irrespective of other
technical responsibilities, with authority and
personnel resources to carry out their duties
including implementation,
maintenance and improvement of
the management system; and to
identify occurrence of departures
from management system or from
tests or calibration procedures
4.1.5b ensure arrangements for
Undue managerial and technical personnel
pressure to make them free from any undue
internal and external commercial,
financial and other pressures and
influences that may adversely affect
the quality of work
4.1.5c ensure there are policies and
Customer procedures related to customer’s
confidentiality confidentiality of information and
proprietary rights, including
electronic storage and transmission
of results.
Page 1 of 23
Department of Energy

PNS ISO/IEC 17025
4.1.5d ensure laboratory has policies and
Operational procedures to avoid involvement in
integrity activities that would diminish
confidence in its competence,
impartiality, judgement or
operational integrity
4.1.5e define organization and
Organization management structure including
chart relationships between quality
management, technical operations ,
support services and parent
organization (if applicable)
4.1.5f specify the responsibility, authority
Responsibility and interrelationships of all
and authority personnel who manage, perform or
verify work affecting the quality of
the tests and/or calibrations
4.1.5g provide adequate supervision by
Laboratory appropriate personnel of all staff
supervision involved in calibration and testing
activities, including trainees
4.1.5h identify technical management that
Technical has overall responsibility for
management technical operations and provision
of resources
4.1.5i appoint a member of staff, with
Quality direct access to senior
manager management, as quality manager
irrespective of other duties and
responsibilities, who has defined
responsibility and authority for
implementing and maintaining the
management system
4.1.5j appoint deputies for key managerial
Managerial personnel, where practical
deputies
4.1.5.k ensure personnel are aware of
Importance of relevance and importance of their
roles activities and how they contribute to
the objectives of the management
system
4.1.6 appropriate communication
Appropriate processes established within the
communication laboratory and include the
effectiveness of the management
system
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PNS ISO/IEC 17025
4.2 Management system

4.2.1 Establish, implement and maintain
Policies and management system appropriate to
procedures scope of activities; document
policies and procedures as a
management system to ensure
quality of all work and that they are
communicated, understood,
available to, and implemented
4.2.2 ensure the quality policy statement

Quality policy is issued under the authority of top
statement management and includes at least:
- the laboratory management’s
commitment to good professional
practice and quality of service to
customers
- statement of the laboratory’s
standard of service
- the purpose of the management
system related quality
- a requirement that all personnel
familiarize themselves with quality
documentation
- the laboratory management’s
commitment to compliance with
the Standard and to continually
improve the management system
- these overall objectives are to be
reviewed as part of management
review
4.2.2, 4.2.5, Maintain a quality manual that:
4.2.6 - defines management system
Quality manual policies and objectives
- includes or makes reference to
supporting procedures, including
technical procedures and outlines
structure of the documentation in
the management system
- defines the roles and
responsibilities of technical
management and the quality
manager
4.2.3 Evidence of commitment to
Commitment to development, implementation and
management continual improvement of the
system management system must be
available.
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PNS ISO/IEC 17025
4.2.4 importance of meeting customer,
Customer statutory and regulatory
requirements requirements must be
communicated
4.2.7 integrity of the management system
Changes to must be maintained when changes
management are made.
system
4.3 Document control
4.3.1 ensure procedures to control all
Procedures documentation included in the
management system are
established and maintained
4.3.2.1 ensure documents are reviewed
Approval and and approved by authorized
issue personnel prior to issue, and are
included on a master list which
identifies the revision status and
distribution.
4.3.2.2 ensure all necessary quality
Availability documentation is available where
required, reviewed and revised to
maintain suitability
4.3.2.2 ensure documents are removed
Obsolete when obsolete and suitably marked
documents if retained for either legal or
knowledge preservation purposes
4.3.2.3 all management system documents
Identification must be uniquely identified and
include date of issue and/or
revision, identification, page
numbering, total number of pages
or a mark to signify the end of the
document, and the issuing
authority(ies)
4.3.3.1 ensure changes to documents are
Document reviewed and approved by the
changes same function that performed the
original review, or a designate
4.3.3.2 ensure where practical, the altered
Altered or new or new text is identified in the
text document or the appropriate
attachments
4.3.3.3 ensure if hand written amendments
Handwritten are allowed, defined procedures are
amendments available, which include authorities,
clear marking, initialing, dating, and
formal re-issue
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PNS ISO/IEC 17025
4.3.3.4 establish procedures to describe
Electronic how changes in documents
documents maintained electronically are made
and controlled
4.4 Review of requests, tenders and contracts
4.4.1, 4.4.3 ensure policies and procedures
Policies and related to review of requests,
procedures tenders and contracts are
established, maintained and
include:
- defining, documenting and
understanding customer
requirements before commencing
work
- laboratory's capability and
resources
- appropriate method selection
- work that is subcontracted by the
laboratory
4.4.2 maintain records of reviews,
Records of including any significant discussions
review and/or changes throughout the
contract
4.4.4 ensure customer is informed of any
Notification of deviation from the contract
customer
4.4.5 ensure same contract review
Changes to process is repeated if a contract
contracts has to be amended after work has
commenced and that all affected
staff are advised of the amendment
4.5 Subcontracting of tests and calibrations
4.5.1, 4.5.4 ensure that subcontractors are
Competency competent (e.g. accredited
laboratory) and records are
maintained of subcontractors used
and their competency (e.g. terms of
accreditation)
4.5.2 ensure customer is advised in
Customer writing and approval gained, where
approval appropriate
4.5.3 unless customer or a regulatory

Responsibility authority specifies subcontractor,
laboratory is responsible for
subcontractors' work
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PNS ISO/IEC 17025
4.6 Purchasing services and supplies

4.6.1 document policy and procedures
Policies and for selection, purchasing, reception
procedures and storage of relevant services
and supplies
4.6.2 ensure all purchased supplies that

Verification affect the quality are not used until
verified as complying with defined
specifications, and records of the
actions taken to demonstrate
compliance are maintained
4.6.3 ensure purchasing documents for

Purchasing items affecting the quality of work
documents are reviewed and approved for
technical content prior to release
4.6.4 maintain list and records of the

Approved evaluations and all approved
suppliers suppliers
4.7 Service to the customer

4.7.1 Cooperate with customers to clarity
Cooperation requests and monitor laboratory's
performance provided laboratory’s
ensure confidentiality to other
customers
4.7.2 feedback must be sought and used

Feedback to improve the laboratory’s activities
4.8 Complaints
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PNS ISO/IEC 17025
4.8 document policy and procedure for
Policy, the resolution of complaints from
procedure and customers or other parties and
records ensure records of the complaints,
investigations and corrective
actions (4.11) are maintained
4.9 Control of nonconforming testing and/or calibration work

4.9.1 ensure policy and procedures are
Policies and implemented when work or results
procedures do not conform to own procedures
or customer requirements and
include:
- defined responsibilities,
authorities and actions
- an evaluation of the significance
of the nonconforming work
- corrective actions and decision
about the acceptability of the
nonconforming work to be taken
immediately
- notification to the customer and
work recall, if necessary
- defined responsibility for
authorizing the resumption of
work
4.9.2 Corrective action procedures (4.11)
Recurrence must be implemented when
evaluation indicates recurrence
could occur or there is doubt
regarding compliance of
laboratory's operations with own
policies and procedures
4.10 Improvement
4.10 continually improve the
Effectiveness effectiveness of the management
system
4.11 Corrective action

4.11 establish policy and procedures,
Policies and and designate appropriate
procedures authorities for implementing
corrective actions which include:
- cause analysis to determine the
root cause (4.11.2)
- selection, implementation and
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PNS ISO/IEC 17025
documentation of corrective
actions (4.11.3)
- monitoring results to ensure
effectiveness of corrective action
(4.11.4)
- areas affected are to be audited
(4.14) if nonconformities
indicate laboratory not complying
with own management system
(4.11.5)
4.12 Preventive action
4.12 ensure needed improvements and
Identification potential sources of nonconformities
and action are identified and action plans
developed, implemented and
monitored, using controls to ensure
they are effective
4.13 Control of records
4.13.1.1 establish and maintain procedures
Procedures covering aspects listed below for
control and quality and technical
records:
- identification
- collection
- indexing
- access
- filing
- storage
- maintenance
- disposal
- protect, back-up and prevent
unauthorised access to or
amendment of records stored
electronically (4.13.1.4)
4.13.1.2 ensure all records are:
Record integrity - legible
- readily retrievable
- maintained in a suitable
environment
- retained for established time
- held secure and in confidence
(4.13.1.3)
4.13.2.1 ensure laboratory retains technical
Technical records of:
records - original observations
- derived data
- sufficient information to establish
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PNS ISO/IEC 17025
an audit trail
- calibration records
- staff records
- copy of each test report or
calibration certificate issued
- identity of personnel responsible
for test/calibration
- identity of personnel responsible
for checking results
and that retained records of each
test or calibration contain sufficient
information to:
- identify factors affecting the
uncertainty
- enable the test or calibration to be
repeated using original conditions
4.13.2.2 ensure observations, data and
Recording calculations are recorded at the
time they are made and are
identifiable to the specific task
4.13.2.3 ensure any changes to the original
Corrections to records (including electronic) are
records made so that:
- original record is not obscurred
- correct value entered alongside
- alterations signed or initialled by
the person making the correction
- equivalent measures must be
taken for records stored
electronically
4.14 Internal audits
4.14.1 - internal audits shall be conducted
Requirements periodically and in accordance
with a predetermined schedule
and procedure to verify continuing
compliance with the requirements
of PAO and the management
system
- quality manager is responsible for
planning and organizing audits to
be carried out by trained and
qualified personnel independent
of activity being audited (where
resources permit)
4.14.2 where validity of results has been
Corrective questioned, timely corrective action
action and must be taken and customers
notification of notified in writing if it is shown that
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PNS ISO/IEC 17025
customers laboratory results have been
affected
4.14.3 records of area audited, the audit
Records findings and corrective actions must
be retained
4.14.4 follow-up audit shall verify and
Follow-up record implementation and
audits effectiveness of corrective action
4.15 Management reviews

4.15.1 ensure the laboratory's
Objectives management conducts a review
yearly of the management system
and testing/calibration activities,
based on a predetermined schedule
and procedure to ensure continuing
suitability and effectiveness and to
introduce necessary changes or
improvements
4.15.1 ensure the review includes:
Contents - suitability of policies and
procedures
- reports from managerial and
supervisory personnel
- outcome of recent internal audits
- corrective and preventive actions
- assessments by external bodies
- results of interlaboratory
comparisons or proficiency tests
- changes in the volume and type
of work
- customer feedback
- complaints
- recommendations for
improvement
- other relevant factors (e.g. quality
control activities, resources and
staff training)
4.15.2 ensure findings and actions are
Actions and recorded and carried out within an
records appropriate and agreed timescale
5 Technical Requirements
5.1 General
5.2 Personnel
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PNS ISO/IEC 17025
5.2.1 ensure personnel performing
Competence specific tasks are qualified on the
basis of education, training,
experience and/or demonstrated
skills and that when staff are being
trained appropriate supervision is
provided
5.2.2 policy and procedures must be
Training policy implemented for identifying training
needs, providing training and
evaluating its effectiveness
5.2.3 ensure personnel are employed or
Employees contracted by the laboratory, and
ensure contracted personnel are
supervised, competent and work in
accordance with the management
system
5.2.4 maintain current job descriptions for
Job managerial, technical and key
descriptions support staff
5.2.5 Ensure management has
Authorized authorized specific personnel to:
personnel - perform specific sampling, testing
and/or calibration activities
- issue test reports and/or
calibration certificates and that
PAO signatory approval has been
taken into consideration
- give opinions and interpretations
- operate particular types of
equipment and that records of all
technical personnel (including
contracted personnel) are
maintained for:
- relevant authorization(s) including
date on which authorization
and/or competence is confirmed
- competence
- educational and professional
qualifications
- training, skills and experience
5.3 Accommodation and environmental conditions

5.3.1 ensure the laboratory or off-site
Facility facility(ies) and environmental
conditions do not compromise the
quality of results and that the
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PNS ISO/IEC 17025
technical requirements for critical
accommodation and environmental
conditions are documented
5.3.2 ensure laboratory monitors, controls

Monitoring and records environmental
conditions, where applicable and
that tests and/or calibrations are
stopped when results are
jeopardized by the environmental
conditions
5.3.3 ensure there is effective separation

Incompatible between areas of incompatible
activities activities.
5.3.4 ensure access to office and

Access laboratory areas are controlled
5.3.5 ensure housekeeping measures are

Housekeeping adequate
5.4 Test and calibration methods and method validation

5.4.1 ensure laboratory uses appropriate
Methods and methods and procedures for all
procedures calibrations and test activities
covered by scope of accreditation
(including sampling, handling,
transport, storage and preparation
of items to be tested and/or
calibrated, and where appropriate,
an estimation of the measurement
of uncertainty as well as statistical
techniques for analysis of test
and/or calibration data) and that all
instructions, standards, manuals,
and reference data are current and
available to personnel. (instructions
on the use and operation of all
relevant equipment, on the
handling and preparation of items
for testing and/or calibration, or
both, where the absence of such
instructions could jeopardize the
result of tests and/or calibrations)
5.4.1 ensure deviations from test
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PNS ISO/IEC 17025
Method calibration methods are:
deviations - documented
- technically justified
- authorized
- accepted by the customer
5.4.2 ensure laboratory selects and uses

Method test and/or calibration methods,
selection including methods of sampling that:
- meet the needs of the customer;
and
- are appropriate for the tests
and/or calibrations
- the customer has been informed
of the method chosen (if not
specified)
- where appropriate, are based on
latest international, regional or
national standards, or by
reputable technical organizations,
or in relevant scientific texts or
journals, or as specified by the
manufacturer of the equipment
and where necessary the
standard be supplemented with
additional details to ensure
consistent approach
- laboratory developed methods or
methods adopted by the
laboratory may be used if they are
appropriate for intended use and
validated
- have been verified for use in the
laboratory, if a standard method
(if the standard method changes,
the confirmation shall be
repeated)
5.4.2 ensure laboratory informs the
Inappropriate customer if method proposed by the
methods customer is inappropriate or out of
date
5.4.3, 5.4.4 ensure introduction of these
Laboratory- methods is planned and assigned to
developed qualified personnel with adequate
methods and resources and that plans are
non-standard updated as development proceeds
methods and communicated as necessary
- when methods are used that are
not covered by standard methods,
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PNS ISO/IEC 17025
then:
o purpose of the test and/or
calibration must be identified
o method developed must be
validated before use
o customer agreement must be
obtained and include
specification of customer
requirements
5.4.5.2  laboratory must validate:

Method o non-standard methods
validation o laboratory designed/
developed methods
o standard methods outside
their intended scope
o amplifications and
modifications of standard
methods
o to confirm that the methods
are fit for the intended use
 records for method validation
must include
o results obtained
o procedure used
o statement as to whether the
method is fit for the intended
use
5.4.5.3 ensure the range and accuracy of

Range and the values obtainable from validated
accuracy methods (e.g. the uncertainty of the
results, detection limit, selectivity of
the method, linearity, limit of
repeatability and/or reproducibility,
robustness against external
influences and/or cross-sensitivity
against interference from the matrix
of the sample/test object) are
relevant to the customers’ needs
5.4.6.1 calibration laboratories or testing
Uncertainty of laboratories performing their own
measurement calibrations must have and
implement procedures for
estimating the uncertainty of
measurement for all calibrations
5.4.6.2 testing laboratories must document
and implement procedures for
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PNS ISO/IEC 17025
estimating uncertainty of
measurement
(refer to PAB Policy for application
of this clause)
5.4.6.3 all uncertainty components which
are of importance in the given
situation shall be taken into account
using appropriate methods of
analysis when estimating
uncertainty of measurement
5.4.7.1 ensure calculations and data

Calculations transfers are checked in a
and data systematic manner
transfers
5.4.7.2 Ensure when computers or
Computers and automated equipment are used for
automated the acquisition, processing,
equipment recording, reporting, storage or
retrieval of test or calibration data,
the laboratory shall ensure that:
o laboratory developed software is
sufficiently documented and
suitably validated
o procedures are established and
implemented for protecting the
data and include
o integrity and confidentiality of
data entry or collection
o data storage
o data transmission
o data processing;
o computers and automated
equipment are maintained to
ensure proper functioning
o appropriate environmental and
operating conditions are provided
5.5 Equipment
5.5.1 to 5.5.4 Ensure all equipment and its
Operation software (including that outside the
laboratory’s permanent control)
required for all testing and/or
calibration activities:
o is available and functioning
properly
o is capable of achieving the
accuracy
o comply with the specifications
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PNS ISO/IEC 17025
o has calibration program
established for the key quantities
or values
o is calibrated or checked before
being placed into service
o is checked and/or calibrated
before use (see 5.6 also)
o is operated by authorized
personnel
o has current instructions on the
use and maintenance available
o is uniquely identified, where
practicable
5.5.5 ensure records of equipment are

Records maintained and include:
o identity of the equipment and its
software
o manufacturer's name, model and
serial number or other unique
identification
o evidence that equipment complies
with the accuracy requirements
and with specification relevant to
the tests or calibrations
o current location, where
appropriate
o the manufacturer's instructions, if
available, or reference to their
location
o calibration history and due date of
next calibration
o the maintenance plan, where
appropriate, and maintenance
carried out to date
o any damage, malfunction,
modification or repair to the
equipment.
5.5.6, 5.5.11 ensure procedures for measuring

Procedures equipment are documented and
include:
o safe handling
o transport
o storage
o use
o planned maintenance
o where applicable, that copies of
correction factors are correctly
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PNS ISO/IEC 17025
updated
5.5.7 ensure equipment subjected to
Out-of-service overloading or mishandling, giving
suspect results, or shown to be
defective or outside specified limits,
is taken out of service and is:
o isolated or clearly labeled or
marked as being out of service
o examined for the effect of the
defect or departure from specified
limits on previous tests and/or
calibrations
o addressed under the "Control of
nonconforming work" procedure
(see 4.9)
5.5.8, 5.5.10 ensure equipment calibration
Calibration status is identified, where
status practicable and where intermediate
checks are needed to maintain
confidence in calibration status that
a procedure is documented to carry
out these checks
5.5.9 ensure when equipment goes

Return to outside the direct control of the
service laboratory, that the function and
calibration status are checked
before the equipment is returned to
service
5.5.12 ensure equipment, both hardware

Adjustments and software is safeguarded from
adjustments which could invalidate
the test and/or calibration results
5.6 Measurement Traceability

5.6.1 ensure all equipment used in testing
Calibration and/or calibration activities is
program calibrated before being put into
service and is included in the
equipment calibration program
5.6.2.1 must ensure the program for

Calibration calibration of equipment is shall be
laboratories designed and operated so that
calibrations and measurements are
traceable to the International
System of Units (SI units), however
Page 17 of 23

PNS ISO/IEC 17025
where traceability cannot be strictly
made in SI units, traceability can be
established by use of:
- certified reference materials
- specified methods and/or
consensus standards that are
clearly described and agreed by
all parties concerned
Participation in suitable
interlaboratory comparisons is
required where possible.
5.6.2.2 the requirements given in 5.6.2.1
Testing apply for measuring and test
laboratories equipment unless it has can be
established that the associated
contribution from the calibration
contributes little to the total
uncertainty of the test result
5.6.3.1 o program and procedure for
Reference calibration of reference standards
standards o reference standards must include
traceability as described in 5.6.2.1
o reference standards of
measurement must be used for
calibration only
o reference standards shall be
calibrated before and after any
adjustment
5.6.3.2 where possible, reference materials
Reference must be traceable to SI units or
materials certified reference materials
internal reference materials must be

checked as far as is technically and
economically practicable
5.6.3.3 procedures and schedules must be
Intermediate available to carry out intermediate
checks checks on reference, primary,
transfer or working standards and
reference materials to maintain
confidence in the calibration status
5.6.3.4 procedures for safe handling,

Transport and transport, storage and use of
storage reference standards and materials
must be available
5.7 Sampling
Page 18 of 23

PNS ISO/IEC 17025
5.7.1 ensure procedures for sampling
Procedures are available at sampling location
and plan and include:
o a sampling plan (based on
appropriate statistical methods,
wherever reasonable)
o factors to be controlled to ensure
validity of test/calibration results
5.7.2 ensure customer -requested

Deviations deviations, additions or exclusions
from the documented sampling
procedures are recorded
communicated to the appropriate
personnel
5.7.3 ensure laboratory has procedures

Records for recording sampling data and
operations and that the records
include:
o sampling procedure used
o identification of the sampler
o environmental conditions (if
relevant)
o diagrams (or equivalent) to
identify sampling location
o statistics that sampling procedure
is based on, if appropriate
5.8 Handling of test and calibration items

5.8.1 document procedures for test
Procedures and/or calibration item management
which ensure protection of integrity
of the item and the interests of the
laboratory and client and cover:
o transportation
o receipt
o handling
o protection
o storage
o retention and/or disposal
5.8.2 ensure laboratory has a system for
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PNS ISO/IEC 17025
Identification identifying test and/or calibration
items both physically and in the
records and accommodate a sub-
division of groups of items if
applicable
5.8.3 o ensure abnormalities or
Deficiencies deficiencies on item received are
recorded
o if there is doubt about the
suitability of item, or it does not
conform to description provided,
or the test or calibration required
is not specified, ensure that the
customer is contacted and that
the instructions are recorded
5.8.4 ensure laboratory has procedures
Facilities and appropriate facilities to maintain
item integrity, and the protection of
secured items and when specified
environmental conditions are
required, that these are maintained,
monitored and recorded
5.9 Assuring the quality of test and calibration results
5.9.1 ensure laboratory has quality
Quality control control procedures for monitoring
validity of tests and calibration, it
must be planned activity, reviewed
and includes:
o regular use of certified reference
materials and/or secondary
reference materials
o participation in interlaboratory
comparison or proficiency-testing
programs
o replicates using the same or
different methods
o retesting or recalibration of
retained items
o correlation of results for different
characteristics of an item
resulting data must be recorded so
as trends are detectable and
statistical techniques must be
applied to the reviewing of the
results where practicable
5.9.2 Analyse and take appropriate action
Action on on quality control data that falls
quality control outside pre-defined criteria
Page 20 of 23

PNS ISO/IEC 17025
data
5.10 Reporting the results
5.10.1, 5.10.8 o results of tests and calibrations
Test reports must be reported accurately,
and calibration clearly, unambiguously and
certificates objectively, and in accordance
with any specific instructions in
the methods
o test reports and calibration
certificates must include all
information requested by the
customer, required by the method
and necessary for the
interpretation of the test or
calibration results
o results may be reported in a
simplified way when performed for
internal customers or in the case
of a written agreement with the
customer, however, any
information not reported to the
customer, but is normally required
to be, must be readily available in
the laboratory
o test reports and calibration
certificates must be designed to
accommodate each type of test or
calibration carried out and to
minimize the possibility of
misunderstanding or misuse
o for details on the use of PAB
endorsement refer to PAB/SR11
5.10.2, 5.10.3 o test reports must include the
Test report information listed in the Standard
under 5.10.2 items (a) to (k)
o where necessary for the
interpretation of the test results,
the items included in 5.10.3.1 (a)
to (e) must be included in the test
report
o test reports containing the results
of sampling must also include the
additional requirements listed in
5.10.3.2 (a) to (k) as necessary
for the interpretation of the test
results
5.10.2, 5.10.4 o calibration certificates must
Calibration include the information listed in
Page 21 of 23

PNS ISO/IEC 17025
certificates the Standard under 5.10.2 items
(a) to (k)
o where necessary for the
interpretation of calibration
results, the requirements included
in 5.10.4.1 (a) to (c) must also be
included in the calibration
certificate
o if a statement of compliance with
a specification is made, the
clauses of the specification which
are met or not met must be
identified (5.10.4.2)
o where statement of compliance is
made omitting the measurement
results and associated
uncertainties, the laboratory must
record and retain those results
(5.10.4.2)
o the uncertainty of measurement
must be taken into account when
statements of compliance are
made (5.10.4.2)
o calibration results before and after
adjustment or repair, if available,
must be reported (5.10.4.3)
o calibration certificates or labels
must not contain any
recommendation on the
calibration interval except when
requested by the customer
(5.10.4.4)
5.10.5 o must document the basis the

Opinions and opinions and interpretations are
interpretations made
o must be clearly marked in a test
report
5.10.6 o results of tests performed by

Testing and subcontractors must be clearly
calibration identified
results o where calibration work has been
obtained from subcontracted, the laboratory
subcontractors performing the work shall issue
the calibration certificate to the
contracting laboratory
5.10.7 Where results are transmitted
Page 22 of 23

PNS ISO/IEC 17025
Electronic electronically or electromagnetically
transmission of the requirements set out in the
results Standard must be met
5.10.9 o amendments to a test report or
Amendments to calibration certificate after issue
test reports and must be made in the form of a
calibration further document, or data transfer
certificates and include reference to the
original as detailed in the
Standard
o when a complete new test report
or calibration certificate is
required, it must be uniquely
identified and include a reference
to the original it replaces
Page 23 of 23

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Available Formats

Issue Date:

Department of Energy 01 – 2018

Manual on Systems Procedures

Document Document Issue Review Status Revision Status

Manual on Systems Procedures

Document Document Issue Review Status Revision Status

Manual on Systems Procedures

Document Document Issue Review Status Revision Status

Manual on Systems Procedures

Document Document Issue Review Status Revision Status

Manual on Systems Procedures

Document Document Issue Review Status Revision Status

Manual on Systems Procedures

Document Document Issue Review Status Revision Status

Document Masterlist, Review and Revision Status

Procedures on Sample Preparation and Coal Analysis

Review Status Revision Status

Document Document Issue Review Status Revision Status

Document Document Issue Review Status Revision Status

Document Document Issue Review Status Revision Status

Document Document Issue Review Status Revision Status

Document Document Issue Review Status Revision Status

The Geo-Coal implements standard operating procedures in receiving coal samples,

The procedures are detailed in the succeeding flowcharts.

Flow of Samples and Documents (One-loop)

Receipt of Sample/s from Customer

Procedure Responsible Personnel Details/Emphasis

From Internal Customer

OD Personnel/ If sample/s are not

Procedure Responsible Personnel Details/Emphasis

 Accept the sample OD Personnel

External Customer RLS Form 1 (photocopy

Procedure Responsible Personnel Details/Emphasis

 Assign laboratory Senior SRS Laboratory number as

 Record the date Geo-

 Issue LWO-1 to Senior SRS

Procedure Responsible Personnel Details/Emphasis

 Receive the sample/s. Laboratory Technician

 Put sample/s in vial/s

Recording & Analysis of Sample/s (Sample Preparation Included)

Procedure Responsible Personnel Details/Emphasis

 Receive the sample/s Laboratory Technician

 Submit prepared Laboratory Technician

Procedure Responsible Personnel Details/Emphasis

 Issue prepared Senior SRS

Analysts Certified Reference

Preparation & Release of Test Report

Procedure Responsible Personnel Details/Emphasis

 Issue PTR form to Senior SRS

 Write test results in Analyst/s

 Check test results in Senior SRS

Procedure Responsible Personnel Details/Emphasis

 Transmit test report to Laboratory Technician

 Transmit test report to ODC Personnel

For external customers

 Transmit to ODC. Laboratory Technician

 Transmit to OD. ODC Personnel

 Release test report. OD Personnel

Monthly Maintenance Program of Analytical Balances

Procedure Responsible Personnel Details/Emphasis

 Perform monthly SRS II / Senior SRS Monthly maintenance is

 Level the balance such

 Calibrate against a Check for off center errors by