Department of Energy - doe.gov.ph · Document Masterlist, Review and Revision Status . Manual on Systems Procedures . Document Code Document Title Issue Date Review Status Revision

Department of Energy

ERTLS – Geoscientific Research & Fuel Testing Laboratory

MANAGEMENT SYSTEM

Issue Date: 01 – 2018

Page 1 of 6

Rev No.: 11

Code: DMRRS-SP

Document Masterlist, Review and Revision Status

Manual on Systems Procedures

Document Code

Document Title

Issue Date

Review Status Revision Status

Review No. Date Reviewed Revision No. Date Revised SP Systems Procedures on Quality 11-2015 2 03-2017 3 11-2015

SP1.1 Flow of Samples and Documents (One Loop) 11-2015 2 03-2017 4 11-2015

SP1.1a Receipt of Additional Test Parameters for External Customer 11-2015 2 03-2017 2 11-2015

SP1.1b Receipt of Additional Test Parameters for Internal Customer 11-2015 2 03-2017 2 11-2015

SP2.1 Monthly Maintenance Program of Analytical Balances 11-2015 2 03-2017 1 11-2015

SP2.2 Monthly Maintenance Program of Ovens and Furnaces 11-2015 2 03-2017 3 11-2015

SP2.3 Monthly Maintenance Program of Calorimeters, CHN and Sulfur Analyzers

11-2015 2 03-2017 3 11-2015

SP2.4 Recording of Ambient Temperature and Humidity 05-2017 2 03-2017 4 05-2017

SP2.5.1 External Calibration of Laboratory Equipment and Apparatus 11-2015 2 03-2017 2 11-2015

SP2.5.1.1 Monitoring of External Calibration of Equipment 01-2016 1 03-2017

SP2.5.2 Calibration of Laboratory Equipment/ Furnaces and TGA-1000 01-2016 2 03-2017 1 01-2016



MANAGEMENT SYSTEM


Page 2 of 6

Rev No.: 11

Code: DMRRS-SP



Document Code

Document Title

Issue Date


Review No. Date Reviewed Revision No. Date Revised

SP2.5.3 Calibration of Laboratory Equipment/ Parr 6200 Isoperibol Calorimeter 01-2016 2 03-2017 1 01-2016

SP2.5.4 Calibration of Laboratory Equipment/ SC 432 DR Sulfur Analyzer 01-2016 2 03-2017 1 01-2016

SP2.5.5 Calibration of Laboratory Equipment/ Leco Truspec CHN Analyzer 01-2016 2 03-2017 1 01-2016

SP3.1 Preparation of Final Test Results 01-2016 2 03-2017 2 01-2016

SP4.1 Release of Test Report to Internal Customer 01-2016 2 03-2017 3 01-2016

SP4.2 Release of Test Report to External Customer 01-2016 2 03-2017 3 01-2016

SP4.3 Release of Test Report to External Customer Through Electronic Mail 01-2016 2 03-2017 1 01-2016

SP5.1 Wastes Treatment and Storage 01-2016 2 03-2017 1 01-2016

SP5.2 Storage and Disposal of Heavy Metals 01-2016 2 03-2017 1 01-2016

SP5.3 Handling of Coal Wastes from Sample Preparation 01-2016 2 03-2017 2 01-2016

SP5.4 Retention and Disposal of Coal File and Analysis Samples 05-2017 2 03-2017 2 05-2017



MANAGEMENT SYSTEM


Page 3 of 6

Rev No.: 11

Code: DMRRS-SP



Document Code

Document Title

Issue Date



SP6.1 Management Review of Laboratory Quality Systems 01-2016 2 03-2017 2 01-2016

SP6.2 Maintaining Records of Management Review 01-2016 2 03-2017 2 01-2016

SP6.3 Submission and Approval of Documents on Quality (Internal Laboratory)

01-2016 2 03-2017 2 01-2016

SP6.4 Submission and Approval of Documents on Quality (External Communication)

01-2016 2 03-2017 2 01-2016

SP6.5 Conduct of Preventive Maintenance for Laboratory Equipment 01-2016 2 03-2017 2 01-2016

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

SP7.2 Reflecting Changes in Existing Document in Hard and Soft Copy 01-2016 2 03-2017 2 01-2016

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

SP8.1 Entering Into and Review of MOA/MOU 01-2016 2 03-2017 2 01-2016



MANAGEMENT SYSTEM


Page 4 of 6

Rev No.: 11

Code: DMRRS-SP



Document Code

Document Title

Issue Date


Review No. Date Reviewed Revision No. Date Revised SP9.1 Inventory of Chemicals and Supplies 01-2016 2 03-2017 1 01-2016

SP9.2 Request for Purchase of Chemicals and Other Supplies 01-2016 2 03-2017 1 01-2016

SP9.3 Procurement of Equipment that Provides New Capability for the Laboratory

01-2016 2 03-2017 1 01-2016

SP9.4 Purchase of Replacement of Equipment/Other Apparatus 01-2016 2 03-2017 1 01-2016

SP9.5 Bidding Procedure on Procurement and Repair 01-2016 2 03-2017 1 01-2016

SP9.6 Reception and Storage of Purchased Reagents and Other Laboratory Consumable Materials

10-2015 2 03-2017 1 10-2015

SP10.1 Obtaining Test Results Outside Repeatability Range 10-2017 2 03-2017 3 10-2017

SP10.2 Addressing Nonconformance in the Laboratory Quality System/Others 10-2015 2 03-2017 3 10-2015

SP10.3 Control/Prevention of Non-conforming Work on Coal Analysis 01-2016 2 03-2017 3 01-2016

SP10.4 Resolution of Complaint 01-2016 2 03-2017 3 01-2016



MANAGEMENT SYSTEM


Page 5 of 6

Rev No.: 11

Code: DMRRS-SP



Document Code

Document Title

Issue Date



SP10.5 Preventive/Corrective Action on Quality Control Failure 05-2017 2 03-2017 4 05-2017

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

SP11.1 Quantifying Uncertainty for Proximate Analysis (Using ISO Method) 05-2017 2 03-2017 2 05-2017

SP11.2 Quantifying Uncertainty for Calorific Value, Sulfur, Carbon, Hydrogen and Nitrogen

01-2016 2 03-2017 1 01-2016

SP12.1 Cleaning of Glassware 01-2016 2 03-2017 1 01-2016

SP13.1 Monitoring Accuracy of Test Results on Coal Analysis 01-2016 2 03-2017 3 01-2016

SP14.1 Identifying Training Needs 10-2015 2 03-2017 1 10-2015

SP14.2 Providing Training To Personnel/ Nomination and Selection 01-2016 2 03-2017 3 01-2016

SP14.3 Evaluation of Effectiveness of Training Provided to Newly-Hired/Newly-Assigned Personnel

01-2016 2 03-2017 1 01-2016



MANAGEMENT SYSTEM


Page 6 of 6

Rev No.: 11

Code: DMRRS-SP



Document Code

Document Title

Issue Date



SP14.4 Evaluation of Effectiveness of Training Received by Laboratory Personnel

01-2016 2 03-2017 2 01-2016

SP14.5 Request for Leave of Absence/Sick Leave 01-2016 2 03-2017 3 01-2016

Department of Energy ERTLS – Geoscientific

Research & Fuel Testing Laboratory

MANAGEMENT SYSTEM

Issue Date: 01- 2018

Page 1 of 1

Rev No.: 7

Code: DMRRS-CP Document Masterlist, Review and Revision Status

Procedures on Sample Preparation and Coal Analysis

Document Code

Document Title

Issue Date

Review Status Revision Status Review

No. Date

Reviewed Revision

No. Date

Revised

CP1a Collection of Channel Samples of Coal From Coal Seam/ Adopted from ASTM D 4596-99

11-2015 2 03-2017 1 11-2015

CP1b Preparation of Coal Secondary Standard 11-2015 2 03-2017 1 11-2015

CP1 Preparation of Coal Samples for Analysis/ Adopted from ISO 5069 01-2016 2 03-2017 1 01-2016

CP2 Performing Sieve Analysis of Coal and Designating Coal Size/ Adopted from ASTM D 4749

01-2016 2 03-2017 1 01-2016

CP3 Determination of Moisture Content/ Adopted from ISO 5068/ Indirect Gravimetric Method

01-2018 2 03-2017 2 01-2018

CP4 Determination of Volatile Combustible Matter/ Adopted from ISO 562

11-2015 2 03-2017 1 11-2015

CP5 Determination of Ash/ Adopted from ISO 1171 11-2015 2 03-2017 1 11-2015

CP6 Determination of Fixed Carbon/ Using ISO 17246:2010 11-2015 2 03-2017 1 11-2015

CP7 Determination of Calorific Value/ Adopted from ASTM D 5865 - 04 11-2015 2 03-2017 1 11-2015

CP8 Determination of Forms of Sulfur in Coal/ Adopted from ASTM D 2492

01-2016 2 03-2017 1 01-2016

CP9a Determination of Total Sulfur by IR Method/ Adopted from ASTM D 4239 – 05 using SC 432 DR

01-2016 2 03-2017 1 01-2016

CP9b Determination of Total Sulfur by IR Method/ Adopted from ASTM D 4239 – 05 using TruSpec S

01-2016 1 03-2017

CP10 Sulfur Determination by Eschka and Bomb Washing Methods/ Adopted from ASTM D 3177

01-2016 2 03-2017 1 01-2016

CP11 Carbon, Hydrogen and Nitrogen (CHN) Analysis/ Adopted from ASTM D 5373 - 02

11-2015 2 03-2017 1 11-2015

Department of Energy ERTLS – Geoscientific Research & Fuel Testing Laboratory

MANAGEMENT SYSTEM

Issue Date: 01– 2018

Page 1 of 5

Rev No.: 11

Code: DMRRS-F


Forms

Form # Document

Code Document

Title Issue Date


Review No. Date Reviewed Revision No. Date Revised CF1 RLS1 Request for Laboratory Services

(External Customer) 05-2015 2 03-2017 3 05-2015

CF2 RLS2 Request for Laboratory Services (Internal Customer) 11-2015 2 03-2017 2 11-2015

CF3 LWO Laboratory work Order 04-2017 2 03-2017 4 03-2017 CF4 LWO1 Coal Analysis/Laboratory Work

Order -1 (Sample Preparation) 10-2017 2 03-2017 3 10-2017

CF5 LWO2 Coal Analysis/Laboratory Work Order - 2 (Required Analysis) 11-2015 2 03-2017 2 11-2015

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 LATR ODC

to OD (a)

Laboratory Analysis Test Report -RLS No- From Coal Unit to ODC to OD with PAB Endorsement

01-2016 2 03-2017 6 01-2016

CF8b LATR ODC to OD (b)

Laboratory Analysis Test Report -RLS No- From Coal Unit to ODC to OD without PAB Endorsement

11-2015 1 03-2017

CF9a LATR

Internal (a)

Laboratory Analysis/Test Report - LWO - From Coal Unit to ODC to OD to Internal Customer with PAB Endorsement

01-2016 2 03-2017 5 01-2016

CF9b LATR

Internal (b)

Laboratory Analysis/Test Report - LWO - From Coal Unit to ODC to OD to Internal Customer without PAB Endorsement

11-2015 1 03-2017



MANAGEMENT SYSTEM


Page 2 of 5

Rev No.: 11

Code: DMRRS-F


Forms

Form # Document

Code Document

Title Issue Date


Review No. Date Reviewed Revision No. Date Revised CF10a LATR

OD to External (a)

Laboratory Analysis/Test Report - From OD to External Customer with PAB Endorsement

01-2016 2 03-2017 6 01-2016

CF10b LATR OD to

External (b)

Laboratory Analysis/Test Report - From OD to External Customer without PAB Endorsement

10-2015 1 03-2017

CF11 COR Complaint Report 11-2015 2 03-2017 2 11-2015

CF12a CRa Customer Rating (Submission of Sample) 05-2017 2 03-2017 3 05-2017

CF12b CRb Customer Rating (Submission of Sample) 05-2017 1 03-2017 1 05-2017

CF13 NCAR Non Conformance and Action Report 05-2017 2 03-2017 3 05-2017

CF14 PR Proficiency Rating 11-2015 2 03-2017 3 11-2015 CF15 DICN Document Issuance/Change

Notice 10-2015 2 03-2017 2 10-2015

CF16 AMR Ambient Monitoring Report 01-2016 2 03-2017 2 01-2016 CF19a

& CF19b

EMPCoal- Bal Acculab

Monthly Equipment Maintenance Program/ Acculab Analytical Balance

01-2017 2 03-2017 3 01-2017

CF20a &

CF20b

EMPCoal- Bal Leco

250

Monthly Equipment Maintenance Program/ Leco 250 Analytical Balance

01-2017 2 03-2017 3 01-2017


MANAGEMENT SYSTEM


Page 3 of 5

Rev No.: 11

Code: DMRRS-F


Forms

Form # Document

Code Document

Title Issue Date


Review No. Date Reviewed Revision No. Date Revised CF22a & CF22b

EMPCoal- Bal

Sartorius

Monthly Equipment Maintenance Program/ Sartorius Analytical Balance

01-2017 2 03-2017 3 01-2017

CF23a & CF23b

EMPCoal- Calo Leco

AC 350

Monthly Equipment Maintenance Program/ Leco AC 350 Isoperibol Calorimeter

01-2017 2 03-2017 3 01-2017

CF24a & CF24b

EMPCoal- Calo Parr

6200

Monthly Equipment Maintenance Program/ Parr 6200 Isoperibol Calorimeter

01-2017 2 03-2017 3 01-2017

CF25a & CF25b

EMPCoal- CHNS Leco

Tru

Monthly Equipment Maintenance Program/ Leco Truspec CHNS Analyzer

01-2017 2 03-2017 3 01-2017

CF26a & CF26b

EMPCoal- Furnace Prufer 1

Monthly Equipment Maintenance Program/ Prufer Furnace I 01-2017 2 03-2017 3 01-2017

CF27a & CF27b

EMPCoal-Furnace Prufer 2

Monthly Equipment Maintenance Program/ Prufer Furnace II 01-2017 2 03-2017 3 01-2017

CF28a & CF28b EMPCoal –

MA2000

Monthly Equipment Maintenance Program/ MA-2000 Mercury Analyzer

01-2017 2 03-2017 3 01-2017


MANAGEMENT SYSTEM


Page 4 of 5

Rev No.: 11

Code: DMRRS-F


Forms

Form # Document

Code Document

Title Issue Date



EMPCoal - Oven Air Drying

Monthly Equipment Maintenance Program/ Coal Air Drying Oven 01-2017 2 03-2017 3 01-2017

CF30 EMPCoal – Oven Jouan

Monthly Equipment Maintenance Program/ Jouan Oven 01-2016 2 03-2017 2 01-2016


Oven MFS

Monthly Equipment Maintenance Program/ Carbolite Minimum Free Space Oven

01-2017 2 03-2017 3 01-2017

CF32a & CF32b

EMPCoal - Sulfur SC 432 DR

Monthly Equipment Maintenance Program/ Leco SC 432 DR Sulfur Analyzer

01-2017 2 03-2017 3 01-2017


TGA1000

Monthly Equipment Maintenance Program/ Las Navas TGA-1000 Thermogravimetric Analyzer

01-2017 2 03-2017 3 01-2017

CF35a & CF35b MHP Monthly Housekeeping Program 01-2017 2 03-2017 3 01-2017

CF36 DR Document Review 01-2016 2 03-2017 1 01-2016 CF37a & CF37b

EMPCoal – Bal Kern

Monthly Equipment Maintenance Program/ Kern Analytical Balance 01-2017 2 03-2017 2 01-2017


MANAGEMENT SYSTEM


Page 5 of 5

Rev No.: 11

Code: DMRRS-F


Forms

Form # Document

Code Document

Title Issue Date



EMPCoal – Furnace Carbolite

AAF

Monthly Equipment Maintenance Program/ Carbolite Ashing Furnace AAF 1100 01-2017 2 03-2017 2 01-2017

CF39a & CF39b

EMPCoal – Furnace Carbolite

VMF

Monthly Equipment Maintenance Program/ Carbolite Vol. Matter Furnace VMF 1000 01-2017 2 03-2017 2 01-2017

CF40 TE Training Evaluation 11-2015 2 03-2017 1 11-2015 CF41 IQA

Checklist Internal Quality Audit Checklist 08-2016 1 03-2017



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015

Page 1 of 1 Rev No.:

3

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.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

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 rom

Start

Examine the sample/s.

If sample/s are not coal (but belong to “other related samples”) & may have problem/s on sample preparation/other equipment, OD Personnel will ask advice from Geo-Coal’s Lab Tech/Analysts/ Supervisor

Determine the nature & approximate mass of the sample/s.

A

Recommends that customer submit another sample.

OD Personnel ODC Personnel Senior SRS OD Personnel/ Senior SRS

Test requirements of customer.

From External Customer Customer proceeds to

OD. Customer discusses

his test requirements. From Internal Customer Customer proceeds to

the ODC to get RLS. Customer proceeds to

Geo-Coal & discusses his test requirements.

No

Yes



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

Code: SP 1.1


Procedure Responsible Personnel Details/Emphasis

A

OD Personnel OD Personnel ERTLS Director OD Personnel Senior SRS Geo-Coal Supervisor Laboratory Technician ODC Personnel Division Chief ODC Personnel Division Chief ODC Personnel

Correct information written in RLS Form. RLS Form 1 (photocopy copy) is retained at ODC while a copy of RLS Form 2 is transmitted to Geo-Coal together with the LWO for internal customers.

Accept the sample External customer fills in

the RLS Form 1. Internal customer fills in

the RLS Form 2.

External Customer Check information in RLS Form 1. Sign RLS Form 1. Transmit RLS Form 1 to

ODC.

Internal Customer Check information in RLS Form 2 & sign. Check & sign RLS Form 2. Transmit RLS Form 2 to

ODC.

External Customer Receive RLS Form 1.

Internal Customer

Check information in RLS Form 2 & sign.

Prepare LWO. Sign LWO. Issue LWO to Geo-Coal.

B



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

Code: SP 1.1


Recording of Sample/s --------------------------------- Procedure Responsible Personnel Details/Emphasis

B

Receive RLS/LWO & coal sample/s.

Determine if sample

preparation is

necessary.

Issue LWO-1 to Laboratory Technician.

No

Yes

Assign laboratory number to coal sample/s.

Record the date Geo-Coal receives the sample, RLS number, laboratory number, sample description & analysis required in coal Sample Tracer.

C

DC

Geo-Coal Supervisor Senior SRS Laboratory Technician Senior SRS Senior SRS

A designated table near sample tracer is provided for the purpose of receiving sample/s. Laboratory number as laboratory code for each sample.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

Code: SP 1.1



C

Receive the sample/s. 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.

Submit vial/s to Senior SRS.

E

Laboratory Technician Laboratory Technician



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

Code: SP 1.1


Recording & Analysis of Sample/s (Sample Preparation Included) ---------------------------------------------------------------------------------------- Procedure Responsible Personnel Details/Emphasis

D

Prepare sample according to CP1.

Receive the sample/s 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.

Submit prepared sample/s to Senior SRS.

E

Laboratory Technician Laboratory Technician Laboratory Technician



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

Code: SP 1.1



E

Issue prepared sample/s and LWO-2 to analyst/s.

Perform analysis of required parameters using coal standard/s 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 basis &

determine if values are

within range.

No

Yes

F

Senior SRS Analysts Senior SRS

Certified Reference Material/ secondary standard is used. Values in the Certificate of Analysis or values obtained for secondary standards after homogeneity & stability tests.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

Code: SP 1.1


Preparation & Release of Test Report ---------------------------------------------------


F

Issue PTR form to analyst/s.

Write test results in the PTR form.

Check test results in 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.

Check CF8/CF9 & sign.

G

Senior SRS Analyst/s Senior SRS Analysts/Senior SRS/Supervising SRS

Analyzed By/Checked By/Noted By



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


4

Code: SP 1.1



G

Transmit test report to ODC.

Check test report & sign.

For internal customers Signs test report.

Transmit test report to OD.

For external customers Transfer test results

using CF10. Transmit to ODC. Transmit test report to

Geo-Coal. Check & sign test

report.

Transmit to OD. Sign test report.

Release test report.

End

Transmit to ODC. Check & sign test

report.

Laboratory Technician Division Chief

ODC Personnel

OD Personnel OD Personnel ODC Personnel Supervising SRS Laboratory Technician Division Chief ODC Personnel Director OD Personnel

Director is the final signatory.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015

Page 1of 1 Rev No.:

1

Code: SP 2.1

ANALYSIS OF SAMPLE/S

Monthly Maintenance Program of Analytical Balances


SRS II / Senior SRS SRS II / Senior SRS SRS II / Senior SRS SRS II / Senior SRS Geo-Coal Supervisor

Start

Perform monthly maintenance of analytical balances.

Monthly maintenance is conducted every end of the month on top of the internal calibration being done during sample analysis. Refer to the User’s Manual for the procedure of internal calibration. Check for off center errors by weighing the 1-g standard mass at the center of the pan and at the back, front, left and right portions.

Clean the weighing chamber and pan with brush and soft cloth/paper towel.

Check dessicant and replace if necessary.

Level the balance such that the bubble is in the middle of the circle.

Go through internal calibration.

Calibrate against a calibrated 1-g standard mass.

Record the reading. Fill out the equipment

maintenance program form provided for each balance.

Check accomplished form.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015


3

Code: SP 2.2


Monthly Maintenance Program of Ovens and Furnaces

(Coal Air-Drying Oven, Jouan Oven, MFS Oven, Prufer Furnace I and II)


SRS II / Senior SRS SRS II / Senior SRS

Start

Perform monthly maintenance of ovens and furnaces.

Monthly maintenance is conducted every end of the month.

Ovens Check if the unit is

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



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 – 2015


3

Code: SP 2.2


Monthly Maintenance Program of Ovens and Furnaces

(Coal Air-Drying Oven, Jouan Oven, MFS Oven, Prufer Furnace I and II)


A

Furnaces Check if the unit is

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.

End

SRS II / Senior SRS Geo-Coal Supervisor

Check accomplished equipment maintenance program form.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

05 - 2017

Page 1of 1 Rev No.:

4

Code: SP 2.4


Recording of Ambient temperature and Humidity

Procedure Responsible Personnel Details/emphasis

Start

Turn on the hygrometer before the start of analysis on moisture, volatile matter, ash, calorific value, sulfur, carbon, hydrogen and nitrogen

Record the temperature and relative humidity in the logbook at 9:00 am to 2:00 pm.

SRS II / Senior SRS Reading and recording is made every hour for the first year to third year to establish trends/ seasonality/pattern.

End

SRS II



SYSTEMS PROCEDURE

MANUAL

Issue Date:

11 - 2015

Page 1of 1 Rev No.:

2

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

Receive/log request for calibration.

Inform ODC of the status of request, including the winning bidder.

SRS II, Lab. Tech. GSD Senior SRS, SRS II

Periodic calibration of equipment at least once a year.

Solicit quotations from ISO accredited calibration facilities. Prepare RFS and submit to the office of the Division Chief and office of the Director for signature.

Set schedule for the calibration. Attend/check quality of work rendered by the service provider. File calibration certificate and apply necessary adjustment.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

Code: SP 2.5.1.1


Monitoring of Calibrated Laboratory Equipment and Apparatus


Start

Receive/log request for calibration.

Inform ODC of the status of request, and follow up status.

Sr. SRS, SRS II, Lab. Tech. Sr. SRS Senior SRS

RFS to LATL-Calibration Section to conduct intermediate checks to maintain confidence once a year in between date calibrated and due date

Prepare RFS and submit to the office of the Division Chief and office of the Director for signature.

Set schedule for the calibration. Attend/check quality of work rendered by the service provider. File calibration certificate and apply necessary adjustment.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016


1

Code: SP 2.5.2


Calibration of Laboratory Equipment

Calibration of furnaces and TGA-1000 using certified reference materials Procedure Responsible Personnel Details/Emphasis No Yes

Perform at least two trials using proximate coal standard.

Read/observe test results on volatile matter and ash.

A

Determine if values are within repeatability and

reproducibility range indicated in the Certificate

of Analysis.

B

Senior SRS, SRS II Senior SRS, SRS II

Periodic calibration of furnaces and TGA once a year using proximate coal standard.

Start



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 3 Rev No.:

1

Code: SP 2.5.2




A

Consider the results and record/update calibration logbook.

For TGA-1000 use the results in the analysis of samples.

End

SRS II, Senior SRS



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 3of 3 Rev No.:

1

Code: SP 2.5.2



Procedure Responsible Personnel Details/Emphasis No No Yes

Perform another trial.

Consider the results and record/update calibration logbook.

For TGA-1000 use the results in the analysis of samples.

End

Check the new value if within the

repeatability/ reproducibility

limits.

B

Repeat B

SRS II, Senior SRS

SRS II, Senior SRS



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 3 Rev No.:

1

Code: SP 2.5.3


Calibration of Parr 6200 Isoperibol Calorimeter


SRS I / SRS II / Senior SRS SRS I / SRS II / Senior SRS SRS I / SRS II / Senior SRS

Start

Perform initial standardization for each set of bomb and bucket.

Make at least 10 runs of benzoic acid pellets for each set.

Compute for the mean energy equivalent, standard deviation and percent relative standard deviation (%rsd) for each set of bomb and bucket using the 10 runs.

Check the repeatability of results.

No

Yes

Perform additional runs until 10 repeatable results are obtained.

A

Initial standardization is done after the equipment is installed prior to sample analysis to establish the energy equivalent for each bomb. For 10 new runs, the range of results is +/- 12.0 cal/°C and the standard deviation must not exceed 6.5 cal/°C.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 3 Rev No.:

1

Code: SP 2.5.3




SRS I / SRS II / Senior SRS SRS I / SRS II / Senior SRS

A

Check if the %rsd does not exceed

0.15%.

No

Yes

Perform additional runs until the condition is met.

Input the mean energy equivalent for 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

The relative standard deviation of ten acceptable runs shall be 0.15% or less of the mean energy equivalent.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 3of 3 Rev No.:

1

Code: SP 2.5.3




B

After the initial 10 runs, monthly standardization is carried out to update the EE value, standard deviation and %rsd.

Perform one run for each set.

Remove the first/oldest data then include the new one (completing 10 runs).

Compute for the new mean EE value, standard deviation and %rsd.

End

SRS I / SRS II / Senior SRS

For monthly standardizations, the single new run shall not differ from the existing EE value by more than +/- 4 cal/°C. If this condition is not met, an additional run shall be made. The difference between the two runs shall not exceed +/-5.0 cal/°C and their average shall not differ from the existing EE value by more than +/-3.0 cal/°C. If such conditions are not met, 2 more runs shall be made. The difference between the four runs shall not exceed +/-8.0 cal/°C and their average shall not differ from the existing EE value by more 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 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.)



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 2 Rev No.:

1

Code: SP 2.5.4


Calibration of SC 432 DR Sulfur Analyzer


Start

Select and define the standard to be used for calibration by inputting the ID code (Part #) and the %S value.

Select the appropriate method from the method menu. (low or high sulfur).

Analyze 6 standard samples at different weights (single point calibration).

Perform the calibration in the standard calibration menu by including/excluding results to obtain linear calibration curve.

Determine whether

calibration is acceptable

or not.

No

Yes

A

Add more standard runs until calibration is acceptable

SRS II / Senior SRS SRS II / Senior SRS SRS II / Senior SRS

The standard to be used should have a sulfur value slightly higher than the range of samples to be analyzed. Low sulfur method is to be used for samples with below 4% sulfur content. For 4% and higher sulfur values, High sulfur method is most appropriate. Weights of standard to be used should be 0.09 g, 0.10 g, 0.11 g, 0.12 g, 0.13 g and 0.14 g. In including/excluding results, there must be a minimum of at least 3 runs in the linear curve. It should be based on the true value of the standard with the allowable tolerance. For a calibration to be acceptable, the fit of the curve should be approaching zero.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 2 Rev No.:

1

Code: SP 2.5.4


Calibration of SC 432 DR Sulfur Analyzer


A

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



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 3 Rev No.:

1

Code: SP 2.5.5


Calibration of Leco Truspec CHN Analyzer


Start

Blank Calibration Analyze at least

three acceptable runs of blank.

Perform blank calibration to compute for the system blank.

Standard Calibration Analyze standard

samples according to the method selected.

Perform calibration 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

Senior SRS Senior SRS

Blank calibration is done before every analysis. Standard calibration is on a semi-annual basis. Analyze one standard for single-point calibration. At least three standard samples for multi-point.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016


1

Code: SP 2.5.5




A

Determine whether

calibration is acceptable

or not.

Add more standard runs until calibration is acceptable

No

Yes

Accept and save 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

correction before every analysis to adjust the original calibration response to match the current instrument response.

Analyze 2-3 standard samples.

B

Senior SRS Senior SRS Senior SRS

The curve fit by means of root mean square must be approaching zero. The drift standard is automatically selected by the software as indicated by X mark.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016


1

Code: SP 2.5.5




B

Determine whether

results are acceptable

or not.

Select last 2 results and perform drift correction in the configuration menu.

Analyze standard as check sample.

Value obtained must be within the acceptable range. If not, perform minor troubleshooting.

End

No

Yes

Senior SRS Senior SRS

The software will automatically calculate the drift correction of the system.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

2

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.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

3

Code: SP 4.1

RELEASE OF TEST REPORTS TO CUSTOMER

Release of Test Report to Internal Customer




SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

3

Code: SP 4.2


Release of Test Report to External Customer




SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

1

Code: SP 4.3


Release of Test Report to External Customer Through Electronic Mail


Start

Check/confirm the identity, authority, and rationale of the requesting party.

Approve request.

End

Request should be made via fax or electronic mail to the OD.

Transmit test report electronically

Keep documents of transaction on file

EA

Director of ERTLS



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 – 2016

Page 1of 2 Rev No.:

1

Code: SP 5.1

MANAGEMENT OF LABORATORY WASTES

Wastes Treatment and Storage

Procedure Responsible Personnel Details/Emphasis No Yes

Start

Conduct analysis. Bring the chemical

wastes to the lavatory.

Sort the wastes/ select the acidic and basic wastes and heavy metals.

Transfer the wastes to respective containers.

Check the volume of the neutralization container, i.e., if it needs emptying.

A

Senior SRS/ SRS II Laboratory Technician

Sorting is segregating the wastes to acid, base or heavy metals. Acid & base wastes go to neutralization container, while heavy metals go to the 5-gal amber bottle.

A

BB



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016


1

Code: SP 5.1


Wastes Treatment and Storage

Procedure Responsible Personnel Details/Emphasis Yes No

A

Determine the pH of the accumulated

wastes in the neutralization

container.

Add lime.

Dispose the wastes through the sink.

B

End

Senior SRS Senior SRS/Laboratory Technician Laboratory Technician

The pH of the accumulated wastes should be within 6.5 to 6.9 (DENR recommended limits). pH should fall within 6.5 to 6.9.



SYSTEMS PROCEDURE

MANUAL


Page 1of 1 Rev No.:

1

Code: SP 5.2


STORAGE AND DISPOSAL OF HEAVY METALS


Start

After transferring the 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

Laboratory Technician



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

2

Code: SP 5.3


Handling of Coal Wastes From Sample Preparation


Start

Waste After Passing the Riffle

Crush coal into small

sizes Pass into a riffle. Set aside the mass on

the front of the riffle for further crushing and 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 Sample).

Gather the remaining mass and dispose.

End


These coal wastes go directly to drum/container for disposal (Note: Coal is not hazardous as per DENR-EMB R.A. 6969 and can be disposed like any municipal waste). Coal wastes are disposed in designated container, e.g. drum. Coal wastes are disposed in designated container, e.g. drum.

Waste After Quartering Create a round shape

of the pulverized coal mass.

Divide into 4. Scoop some and put

inside a 50-gram plastic vial from two opposite quarters.

Gather the remaining coal and dispose.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

05 - 2017 Page 1of 1

Rev No.: 2

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).

Hand in to analyst. Dispose of the

remaining coal from the four quarters.

End


Coal wastes are disposed in designated container, e.g. drum. Six (6) months retention time after the release of test results is implemented. As coal disposal takes place every end-month, a checking by the Geo-Coal Supervisor will be performed during the first week of succeeding month. Coal wastes are disposed in designated container, e.g. drum.

Monitoring & Disposal of Analysis and File

Samples

Dispose of file sample with the remaining sample from analysis after the specified retention time.

Update coal waste logbook and record the sample disposed (lab #, mass and date of disposal should be reflected).



SYSTEMS PROCEDURE

MANUAL

Issue Date: 01 - 2016

Page 1of 1 Rev No.:

2

Code: SP 6.1

IMPLEMENTATION OF LABORATORY MANAGEMENT SYSTEM

Management Review of Laboratory Management System


Start

Prepare areas for review.

Propose appropriate improvement/s.

Review areas and the

proposed improvement/s.

Discuss with the Quality Manager/ others the possible courses of actions.

Select a course of action.

The Top Management, Quality Manager and Assistant Quality Manager conduct meeting every second semester of the year.

Geo-Coal Personnel Top Management Quality Manager

Plan and implement necessary activities.

Monitor effectiveness.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

2

Code: SP 6.2


Maintaining Records of Management Review


Start

Jot down discussion on the review of the laboratory management system.

Affix initials/signature on

the review’s final output. Transmit the document to

the ODC and OD for review and approval.

Affix signature on the

review’s final output. Transmit the document

back to the Quality Manager.

Implement/disseminate information.

Keep record of review.

Assistant Quality Manager

DC/Quality Manager Laboratory Technician DC/Quality Manager Director/Top Management DC/Quality Manager Document Control Officer

End



SYSTEMS

PROCEDURE MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

2

Code: SP 6.3


Submission and Approval of Documents on Quality

(Internal of Laboratory)


Start

All management system documents should bear the initial/signature of the Quality Manager and DC of GRFTL.

Prepare/submit draft management system documents to the Quality Manager.

Review draft and

make necessary corrections.

Transmit back the document to the Quality Manager.

Finalize the document.

Affix initial/signature. Transmit revised

document to the ODC

Assistant Quality Manager DC/Quality Manager Clerk IV DC/Quality Manager Laboratory Technician DC/Quality Manager Clerk IV

Approve/affix signature on the revised document.

Transmit the document back to the Geo-Coal Section.

End



SYSTEMS

PROCEDURE MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

2

Code: SP 6.4


Submission and Approval of Documents on Quality

(External Communication)


Start

All management system documents should bear the initial/signature of the Quality Manager and/or Head of Geo-Coal, DC of GRFTL and Director. Copies of outgoing documents shall be provided to the Document Control Officer.

Prepare/submit draft management system documents to the ODC.

Review draft and make necessary corrections.

Transmit document to the Quality Manager.

Finalize the document. Affix initial/signature. Transmit revised

document to the ODC.

Assistant Quality Manager DC/Quality Manager Clerk IV Quality Manager Laboratory Technician DC/Quality Manager Clerk IV Director EA

Approve/affix signature on the revised document.

Transmit the document to the OD.

Approve/affix signature.

Transmit the document back to the ODC/external party.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

2

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 PM.

Inform ODC of the status of request, including the winning bidder.

GSD Senior SRS SRS II

Set schedule for the preventive maintenance.

Attend/check quality of work rendered by the service provider, including the scope as stipulated in the contract.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 – 2016 Page 1 of 2 Rev No.:

1

Code: SP 6.6


Internal Quality Audit


Start

Prepare memorandum for Quality Manager to request for approval of schedule and selection of auditors for the conduct of IQA.

Select auditors and approve schedule of IQA.

Internal quality audit is conducted once every third quarter of the year.

Senior Science Research Specialist Quality Manager Senior Science Research Specialist Auditors

Prepare IQA plan. Provide checklist and

reference documents (manuals, reports, etc.) to auditors.

A

Provide program of audit, including timetable and auditors’ assigned areas to be assessed.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016 Page 2 of 2 Rev No.:

1

Code: SP 6.6

IMPLEMENTATION OF LABORATORY MANAGEMENT SYSTEMS

Internal Quality Audit


End

Implement and submit corrective action report, at an agreed timeframe with the auditors.

A

Conduct IQA: - Document review - Pre-audit meeting - Audit interviews - Post-audit meeting

Prepare report and obtain acceptance of findings.

Internal quality audit is conducted once every third quarter of the year.

Auditors Auditors

Distribute report.

Are the findings accepted?

Yes

Incorporate agreed comments in report.

No

Confirm the clearance of non-conformities.

Prepare a final report of the internal quality audit.

Auditee Quality Manager Senior SRS



SYSTEMS

PROCEDURES MANUAL


Page 1 of 2

Rev No.:

2 Code: SP7.1 CONTROL OF DOCUMENTS

Document Issuance and Distribution


Identify the need for a new document

Formalize request by filling out a DICN form

Document Requester/Originator All documents must be prepared with a Document Issuance / Change Notice Form Document Requester/Originator Affected Personnel Document Requester/Originator Quality Manager

Start

Route the accomplished DICN form to the affected personnel for review/signature

Submit the request to the Quality Manager for approval

Determine if request

is approved

Transmit back to the requester

Yes

A



SYSTEMS

PROCEDURES MANUAL


Page 2 of 2

Rev No.:


Document Issuance and Distribution


A

Approve/affix signature on the DICN form

Proceed to create the new document

Submit the new document with the DICN to the Quality Manager for signature

End

Quality Manager Document Requester/Originator Indicate issue date while the revision number is left blank (for new and not yet revised documents) Quality Manager Document Control Officer Refer to the Document Distribution List for the recipients Recipients must affix their signatures on the DICN form.

Approve/affix signature on the new document

Transmit document to the Document Control Officer

Mark the document “CONTROLLED”

Update soft and hard copies of the document masterlist 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



SYSTEMS PROCEDURE

MANUAL


Page 1of 2 Rev No.:

1

Code: SP 7.3

CONTROL OF DOCUMENTS

Handling of Obsolete Documents

Procedure Responsible Personnel Details No Yes

Start

● Sort documents. ● Label the folder/envelope of the documents.

A

Determine the need to channel

obsolete documents to

the GSID

● Store the documents in the opposite end of the staff room.

Formalize requisition to transfer obsolete document.

Transmit requisition to the Office of the Division Chief.

Document Control Officer

Assistant Quality Manager

Refer to the Retention and Disposition Schedule Of Quality Documents The policy of the DOE is to channel the obsolete documents to the GSID

Include in labeling the section, division, title of the documents and date coverage



SYSTEMS PROCEDURE

MANUAL


Page 2of 2 Rev No.:

1

Code: SP 7.3

CONTROL OF DOCUMENTS

Handling of Obsolete Documents

Procedure Responsible Personnel Details

A

Office of the Division Chief

Approve the request. Transmit the request

to the Document Control Officer.

End

Coordinate with GISD.

Make necessary actions.

Transfer obsolete documents.

Division Chief Clerk

Documentation Control Officer



SYSTEMS

PROCEDURES MANUAL


Page 1 of 3

Rev No.:


Review of Documents


Assign document for review

Acknowledge receipt of assigned document for review

Assistant Quality Manager All document reviews must be done with a Sr. SRS / SRS II Document Review Form Sr. SRS / SRS II Sr. SRS / SRS II Relevant Personnel Sr. SRS / SRS II

Start

Fill out the Document Review Form

Review document Discuss with

concerned personnel if the policies and procedures stated in the document are still suitable or need revision. Reflect signature

Does the document

need revision?

A

Yes

No

B



SYSTEMS

PROCEDURES MANUAL


Page 2 of 3

Rev No.:


Review of Documents


A

Specify in the “Remarks” portion of the Document Review Form that revision is necessary.

Sign in the “Reviewed By:”

Sign in the “Noted By:”

File the accomplished Document Review Form and update review status in the Document Masterlist

Proceed with the revision of the document.

Follow the procedure in SP7.2

Sr. SRS / SRS II Sr. SRS / SRS II Assistant Quality Manager Document Control Officer After document review, the Document

Masterlist, Review and Revision Status is updated.

End



SYSTEMS

PROCEDURES MANUAL


Page 3 of 3

Rev No.:


Review of Documents


B

Specify in the “Remarks” portion of the Document Review Form that the document has been reviewed and found suitable

Sign in the “Reviewed By:”

Sign in the “Noted By:”

File the accomplished Document Review Form and update review status in the Document Masterlist

Sr. SRS / SRS II Sr. SRS / SRS II Assistant Quality Manager Document Control Officer After document review, the Document

Masterlist, Review and Revision Status is updated.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 3 Rev No.:

2

Code: SP 8.1

CONTRACTING COAL LABORATORY SERVICES

Entering Into and Review of MOA/MOU


Start

Customer coordinates with the Office of the Director.

He writes/makes letter of intent.

A

Make known his/her intention to collaborate with the Geo-Coal on specific project.

Determine if the proposal

is a worthwhile endeavor/ consult DC

Disregard the proposal Inform the customer

Inform the customer to make a draft of MOA/MOU.

Upon receipt, review the draft.

The project should contribute to national research and growth as well as serve the interest of customer.

Director

Director



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 3 Rev No.:

2

Code: SP 8.1




A

Forward the MOA/MOU to the Legal Services.

Review/provide comments to the contract.

Transmit the contract to OD

Consult DC. Inform the customer

about the comments in the contract.

DOE’s Legal Services will review and give comments.

Director EA

Director EA

B



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 3of 3 Rev No.:

2

Code: SP 8.1




B

Determine if MOA/MOU

is acceptable.

Advise the party to make necessary actions.

Inform the customer.

Yes

Director

End No



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1

Rev No.: 1

Code: SP 9.1

PROCUREMENT OF EQUIPMENT AND SUPPLIES

Inventory of Chemicals and Supplies


Start

Conduct inventory. Take note and mark

chemicals and other supplies that are nearly depleted.

Submit the inventory file to the Senior SRS of the section.

End

Laboratory Technician Senior SRS Laboratory Technician

Inventory should be done every January and July of the year

Check and sign the inventory file.

Transmit back the inventory file to the Laboratory Technician.

Keep the inventory file for everybody’s use



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

1

Code: SP 9.2


Request for Purchase of Chemicals and Other Supplies


Start

Inform the Supervisor and Laboratory Technician of the depleting item.

Countercheck the item in the inventory.

Fill in purchase request.

Submit request to the Supervisor.

Approve and sign the request.

Transmit request to the GSD.

End

Senior SRS/SRS II Laboratory Technician DC Clerk

The concerned Analysts should inform Laboratory Technician about the depleting item. Bidding procedure applies when necessary



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

1

Code: SP 9.3


Procurement of Equipment that Provides New Capability for the Laboratory


Start

Gather additional information such as brochure about the equipment.

Make strong recommendation/ justification for the need to purchase.

Endorse the recommendation to the OD.

Source out budget for the purchase of the equipment

Transmit request to the BD

Upon budget allocation, succeeding steps follow the bidding process of the GSD.

SRS II, Senior SRS Supervising SRS DC Director

Knowledge on the new technology can be obtained through attendance to seminars, referrals and researches through internet and the likes.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 2 Rev No.:

1

Code: SP 9.4


Purchase of Replacement of Equipment/Other Apparatus

Procedure Responsible Personnel Details/Emphasis Yes No

Start

Report breakdown of the equipment.

Solicit quotations for repair.

B

Determine if the cause of breakdown is reparable

Solicit certificate of obsolescence.

A

Senior SRS or SRS II Service Engineer

SRS I Supervising SRS

Affected analysis is suspended until equipment is repaired or replacement equipment becomes available.

Certificate of Obsolescence is an attachment in making strong recommendation/ justification for buying replacement of equipment.

Make strong recommendation/

justification for the need to purchase the equipment.

Transmit papers/documents to the ODC.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 2 Rev No.:

1

Code: SP 9.4


Purchase of Replacement of Equipment/Other Apparatus

Procedure Responsible Personnel Details/Emphasis Yes

A

Endorse the recommendation to the Office of the Director.

End

Upon budget allocation, follow bidding procedure of the GSD.

B

Follow procedures to process papers for equipment repair.

End

DC Director SRS I SRS I

Source out budget for this purpose.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 2 Rev No.:

1

Code: SP 9.5


Bidding Procedure on Procurement and Repair


Start

Submit PR/RFS to ODC

A

Approve and endorse the request to the OD.

Sign the request Transmit to the Budget

Division.

Allocate funds for the purchase.

Transmit request to the GSD.

Receive/log the purchase request.

Transmit the request to the ITD.

Supervising SRS DC Director Clerk

Upon submission attachments include at least three (3) quotations for budget estimate and justification.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 2 Rev No.:

1

Code: SP 9.5


BIDDING PROCEDURE ON PROCUREMENT OF EQUIPMENT


A

End

Certify the correctness of the information/ specification.

Determine fund availability and completeness of the documents.

Provide copy to the chairperson of the committee.

Set schedule of bidding.

Conduct public bidding.

Award the procurement of the equipment to the qualified bidder.

Schedule of bidding will be published through leading newspaper for seven (7) consecutive days so that the public may know



SYSTEMS PROCEDURE

MANUAL

Issue Date:

10 - 2017

Page 1of 2 Rev No.:

3

Code: SP 10.1

IMPLEMENTING CORRECTIVE ACTION

Obtaining Test Results Outside Repeatability Range


Start

Analyze sample using applicable test method (2 – 3 trials).

Read and record test results.

Compare the results

Take average of the test results.

Fill in preliminary test results form.

Affix signature. Submit preliminary

report to the Senior SRS.

Are the results

repeatable? B

End

SRS II

SRS II

Start



SYSTEMS PROCEDURE

MANUAL

Issue Date:

10 - 2017

Page 2of 2 Rev No.:

3

Code: SP 10.1


Obtaining Test Results Outside Repeatability Range


B

Discard the test results.

Repeat applicable test method. This time, analyze 5 trials.

Record test results. Fill in preliminary

test result form, indicating any observation, including the characteristic of the sample.

Affix signature and submit preliminary test result.

SRS II

No

The results are reported as: on test report under Summary of Results, the phrase, “Successive five (5) runs not repeatable”, is indicated and under Remarks/ Attachments are any observation and the specific values of the five runs/trials.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

10 - 2015

Page 1of 2 Rev No.:

3

Code: SP 10.2


Addressing Non-conformance in the Laboratory Management System/Others


Start

Observe/detect any non-conformance.

Conduct complete staff work. Confirm/discuss/clarify

events that lead to non-conformance, its root cause and impact to customers.

A

Identify corrective actions and select the most appropriate.

Prepare/submit report to the Quality Manager.

The Top Management/ Director of ERTLS, Division Chief/Quality Manager, Assistant Quality Manager/Geo-Coal Supervisor or any of the Geo-Coal members can detect and report non-conformity in the laboratory management system. The customer shall be notified through the Office of the Director to inform the customer personally or by phone or letter. On the other hand, the test report is retrieved through a letter to the customer.

Possible corrective actions are recommended.

Determine applicability of the corrective action

All Assistant Quality Manager/Geo-Coal Supervisor Division Chief/Quality Manager Assistant Quality Manager/Geo-Coal Supervisor

B

Yes

No

In case non-conformance results to suspension of work or specific service/s, notify the customer.

If non-conformance results to any change in the test report, retrieve the test report.

Assistant Quality Manager/Geo-Coal Supervisor



SYSTEMS PROCEDURE

MANUAL

Issue Date:

10 - 2015

Page 2of 2 Rev No.:

3

Code: SP 10.2


Addressing Non-conformance in the Laboratory Management System/Others

Procedure Responsible Personnel Details/Emphasis Yes

A

Approve/ implement the corrective action.

Monitor the effectiveness of the corrective action.

Resume work/service/s.

End

B

Monitoring should be done at least one month after the implementation of the corrective action.

Division Chief/Quality Manager

Audit immediately the areas affected by the implementation of the corrective action.

Internal Quality Auditors

Re-submit another proposal of possible corrective action/s.


C

C



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 2 Rev No.:

3

Code: SP 10.3


Control/Prevention of Nonconforming Work on Coal Analysis


Start

Observe the laboratory policies and systems procedures as imbedded in the ERTLS Laboratory Manual for Coal Analysis.

Detect potential/on-going nonconforming work.

Inform the authorized personnel regarding the matter.

Call a meeting. Decide for final

intervention.

The system involves only the flow of activities for coal analysis .

Geo-Coal Member Coal Unit Member


A

Need to report to DC

Yes

B No



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 2 Rev No.:

3

Code: SP 10.3


Control/Prevention of Nonconforming Work on Coal Analysis


End

Approve corrective action/direct to another option.

Transmit back to Geo-Coal.

Communicate to the members of the Coal Unit for effective implementation.

Give DC feedback on effectiveness of implementation.

Coal Unit Member

Yes

A

B No

DC Assistant Quality Manager/ Geo-Coal Supervisor



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

3

Code: SP 10.4

IMPLEMETING CORRECTIVE ACTION

Resolution of Complaint


Start

Customer fills in a Complaint Report form and submits to the OD.

Call for a meeting. Identify causes and

possible solutions. Choose the most

applicable intervention. 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 customer of the action.

OD Personnel DC, Supervising SRS Supervising SRS Geo-Coal Personnel

Involved personnel clarify/discuss the complaint Appropriate/delegated personnel will be the one to contact the customer.

Receive the report. Investigate and inform

the DC/DC relays & delegates to Supervising SRS.

End



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 – 2016 Page 1of 4 Rev No.:

4

Code: SP 10.6


Analysis of Customer’s Feedback


Start

Office of the Director Distribute feedback

form to a customer. Customer ticks

applicable factors in the feedback form.

OD Staff Laboratory Technician

Feedback form is handed in to internal & external customers who submit samples, inquire on laboratory testing capabilities/other relevant concerns and pick test results/request explanation of test results. A summary is prepared at the end of month.

Customer drops filled-up form at the DROP

box.

A

Near the lobby guard

Collect feedback forms. Compile in a folder. Summarize

feedbacks.

At OD

B



SYSTEMS PROCEDURE

MANUAL



4

Code: SP 10.6




C

Yes

Need improvement? No corrective action

needed.

No

Analyze feedback summary.

B Assistant Quality Manager Assistant Quality Manager

An average rating of 9 and above is excellent/does not need corrective action. An average rating of less than 9 needs improvement/ corrective action.



SYSTEMS PROCEDURE

MANUAL



4

Code: SP 10.6




A

Lobby guard DROP BOX: Collect feedback

forms. Transmit to OD.

HRMD Staff OD Staff

Provide photocopy to Geo-Coal Section.

Applicable to laboratory – testing/personnel/others.

B



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 – 2016 Page 4 of 4 Rev No.:

4

Code: SP 10.6




Assistant Quality Manager Assistant Quality Manager Quality Manager/ Assistant Quality Manager Assistant Quality Manager Senior SRS

Raise feedback to Quality Manager when necessary and formulate corrective action/s.

C

Approve corrective action/s.

Implement corrective action/s.

End

Major or Minor?

Major

Minor Formulate corrective

action/s.

Applicable to laboratory – testing/personnel/others. Minor concerns are those involving the attitude of the attending employee which are detailed in items 1-3 of CF12, while major factors include that of the laboratory’s technical competence in terms of items 3.1.1 – 4.



SYSTEMS PROCEDURE

MANUAL


Page 1of 2 Rev No.:

1

Code: SP 10.7


Root Cause Analysis


Start

Define the problem.

Identify the true root cause associated with the defined problem.

Use of the RCA tools and techniques using flow charts, records, documents, interviews, five whys, cause and effects, diagramming, and checklists. Refer to page 2. Use of the decision making tools and techniques using gantt chart or tree diagram Do the countermeasure Confirm the effectiveness Act and establish

Asst. Quality Manager, Geo-Coal member/s Geo-Coal member/s Asst. Quality Manager, Geo-Coal member/s Asst. Quality Manager, Geo-Coal member/s Asst. Quality Manager, Geo-Coal member/s Asst. Quality Manager Asst. Quality Manager

Implement the corrective action(s).

End

Gather data/evidence.

Identify corrective action(s) that will prevent recurrence of the problem.

Observe the corrective actions to ensure effectiveness.

If necessary, reexamine the RCA.



SYSTEMS PROCEDURE MANUAL


Page 2 of 2

Rev No.: 1

Code: SP 10.7


Root Cause Analysis



SYSTEMS PROCEDURE

MANUAL

Issue Date:

05 - 2017 Page 1of 1 Rev No.:

2

Code: SP 11.1

MEASUREMENT OF UNCERTAINTY

Quantifying Uncertainty for Proximate Analysis (Using ISO Method)


Start

Perform analysis. Record results in the

template for the computation of uncertainty of measurement for moisture determination.

Specify measurands. Identify uncertainty

sources for each measurand.

Simplify grouping sources covered by existing data.

Quantify uncertainty sources.

Compute standard deviation for each measurand.

Compute total standard deviation.

Multiply the value by 2. Record the value as

expanded uncertainty for moisture.

Perform above procedure for volatile matter and ash.

Senior SRS / SRS II Senior SRS

Senior SRS

Analysis is performed using ISO Method. Template is available for the computation of uncertainty of measurement for proximate analysis. Guide to the Expression of Uncertainty in Measurement and EURACHEM/CITAC Guide CG4 are used as references. Measurands consist of moisture, volatile combustible matter and ash. Sources of uncertainty include analytical balance, ovens and furnaces (translated to mass, temperature and/or repeatability).

Total standard deviation is the sum of standard deviations contributed by all sources of uncertainty. Multiplier 2 can be used on the basis of 95 percent confidence level. Revalidation of uncertainty value can be done when necessary/ preferably 2-3 years after.

End

Prepare computation & final value & sign.

Review the value & submit for approval.

Senior SRS Geo-Coal Supervisor Division Chief



SYSTEMS PROCEDURE

MANUAL


Page 1of 1 Rev No.:

1

Code: SP 11.2

MEASUREMENT OF UNCERTAINTY

Quantifying Uncertainty for Calorific Value, Sulfur and Carbon, Hydrogen &

Nitrogen Determinations Procedure Responsible Personnel Details/Emphasis

Start

Perform analysis. Record results in the

template for the computation of uncertainty of measurement for calorific value determination.

Specify measurands. Identify uncertainty

sources for each measurand.

Simplify grouping sources covered by existing data (type A or B).

Quantify uncertainty sources.

Compute standard uncertainty for each measurand.

Compute combined standard uncertainty.

Multiply the value by 2. Record the value as

expanded uncertainty for calorific value.

Perform above procedure for sulfur, carbon, hydrogen and nitrogen.

Senior SRS SRS II

Senior SRS SRS II

Analyses are performed using ASTM methods. Templates are available for the computation of uncertainty of measurement for the above analyses. Guide to the Expression of Uncertainty in Measurement and EURACHEM/CITAC Guide CG4 are used as references. Measurands consist of calorific value, sulfur, carbon, hydrogen and nitrogen. Sources of uncertainty include analytical balance, equipment and certified reference materials (translated to mass, temperature and/or repeatability).

Combined standard uncertainty is the sum of standard uncertainties contributed by all sources of uncertainty. Multiplier 2 can be used on the basis of 95 percent confidence level. Revalidation of uncertainty value can be done when necessary/ preferably 2-3 years after.

End



SYSTEMS

PROCEDURE MANUAL

Issue Date:

01 - 2006

Page 1of 1 Rev No.:

1

Code: SP 12.1

HOUSEKEEPING IN THE LABORATORY

Cleaning of Glassware


Start

After segregation of the wastes produced during analysis, clean the glassware and other materials.

Dry the glassware. Place the glassware in

the stock cabinet or drawer.

End

Laboratory Technician Washing glassware is done twice a day am and pm.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 2 Rev No.:

3

Code: SP 13.1

PARTICIPATION IN INTERLABORATORY PROFICIENCY TESTING

Monitoring Accuracy of Test Results on Coal Analysis


Start

Plan activities Meet Geo-Coal

members to inform of the plan.

Solicit comments and suggestions.

Revise/finalize the plan. Submit proposal/plan to

DC.

A

Approve proposal/plan.

Plan includes timetable, participating organizations and the attending Geo-Coal staff and their roles.

Coordinate with the participating organizations.

Organize/conduct meeting.

Participating organizations include representatives from laboratories of government, power plants and private laboratories.

Geo-Coal Supervisor

DC Geo-Coal Supervisor



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 2of 2 Rev No.:

3

Code: SP 13.1

PARTICIPATION IN INTERLABORATORY PROFICIENCY TESTING

Monitoring Accuracy of Test Results on Coal Analysis


A

Finalize schedule of proficiency testing and deadline of submission of test. results

End

Prepare sample. Inform participating

laboratories to pick up the sample.

Pick up sample. Conduct analysis. Transmit/submit

results of analysis.

Consolidate results of analysis.

Perform statistical evaluation .

Inform the participants about the result of testing.

Geo-Coal Supervisor

Laboratory Technician/ Geo-Coal Supervisor Representatives of participating laboratories Geo-Coal Supervisor

As much as possible, the testing on coal analysis by the laboratories will be done simultaneously.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

10 – 2015

Page 1of 1 Rev No.:

1

Code: SP 14.1

DEVELOPMENT OF LABORATORY PERSONNEL

Identifying Training Needs


Start

Solicit training requirements from laboratory personnel.

List down specific training needs.

Submit to the Head of Geo-coal Section.

Assess training needs of each laboratory personnel.

Submit list of recommendation to the DC.

Supervising SRS

Geo-Coal Member/s Supervising SRS

End

Laboratory personnel know their skill/training inadequacy in performing their functions

Assessment/evaluation is based on current work assignments and the performance of such assignments.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016


3

Code: SP 14.2


Providing Training to Personnel/Nomination and Selection


Start

HRMD routes to the Director of every bureaus/services memorandum inviting nominees for specific course.

A

Receive/log the memorandum in the logbook.

Route the memorandum to DC.

Receive the memo Collaborate with the

Director Route the memo to

supervisor of each section

The memorandum specifies the details of the training including title, date, venue, sponsor, and training requirements

EA

DC



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016


3

Code: SP 14.2




A

Identify nominee/s from the Geo-Coal

Justify nomination Submit justification/letter

to the DC

Receive/log request for nomination.

Approve nomination Route request for

nomination to the OD.


Approve nomination. Route request for

nomination to HRMD

B

Supervising SRS

DC

Executive Assistant Director

Selection of candidate must be based on applicability/requirements of his/her current job.



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 3of 3 Rev No.:

3

Code: SP 14.2




B


Select candidate for training.

Inform the candidate to submit supporting documents.

Transmit training documents to the sponsoring agency.

Inform the candidate of his/her selection to participate in the training.

Submit additional training documents.

Participate in the training course.

Submit training report. Perform echo seminar.

End

Geo-Coal Member /Participant

Selection of candidates/ nominees from other bureaus/ services will be subjected to deliberation by PDC.

Training report should be submitted 1-3 working days upon reporting to work .



SYSTEMS PROCEDURE

MANUAL

Issue Date:

01 - 2016

Page 1of 1 Rev No.:

3

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 up LOA form.

Submit form to Head of Geo-coal section.

Approve the request for leave of absence

Approve/sign the form. Submit the request to

the ODC.

Approve the request. Route the request to

the HRDD.

End

Geo-Coal Member

Geo-Coal Supervisor

DC



COAL PROCEDURES

MANUAL

Issue Date:

01 - 2016 Page 1 of 5

Rev No.: 1

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:



COAL PROCEDURES

MANUAL

Issue Date:

01 - 2016 Page 2 of 5 Rev No.:

1

Code: CP1

SAMPLE PREPARATION


Adopted from ISO 5069 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.



COAL PROCEDURES

MANUAL

Issue Date:

01 - 2016 Page 3 of 5

Rev No.: 1

Code: CP1

SAMPLE PREPARATION


Adopted from ISO 5069 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.



PROCEDURES MANUAL

Issue Date:

01 - 2016 Page 4 of 5

Rev No.: 1

Code: CP1

SAMPLE PREPARATION


Adopted from ISO 5069 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.



COAL PROCEDURES

MANUAL

Issue Date:

01 - 2016 Page 5 of 5

Rev No.: 1

Code: CP1

SAMPLE PREPARATION


Adopted from ISO 5069

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



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015

Page 1 of 2

Rev No.: 1

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



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015


1

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.



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015 Page 1 of 2

Rev No.: 1

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.

http://www.random.org/integer



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015 Page 2 of 2

Rev No.: 1

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.



COAL

PROCEDURES MANUAL



1

Code: CP2

SIEVE ANALYSIS

Performing the Sieve Analysis of Coal and Designating Coal Size

Adopted from ASTM D 4749

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.



COAL

PROCEDURES MANUAL



1

Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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.



COAL

PROCEDURES MANUAL



1

Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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.



COAL

PROCEDURES MANUAL



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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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)



COAL

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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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.



COAL

PROCEDURES MANUAL



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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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.



COAL

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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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 40o 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.



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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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%.



COAL

PROCEDURES MANUAL



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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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”).



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PROCEDURES MANUAL



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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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

Size of Round-Hole Openings in 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%.



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PROCEDURES MANUAL



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Code: CP2

SIEVE ANALYSIS


Adopted from ASTM D 4749 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



COAL PROCEDURES

MANUAL

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01 - 2018 Page 1 of 2

Rev No.: 2

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 110C for 1 hour. Note:

The nitrogen oven reaches 110C 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.



COAL PROCEDURES

MANUAL

Issue Date:

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Rev No.: 2

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



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015

Page 1 of 2

Rev No.: 1

Code: CP4

PROXIMATE ANALYSIS

Determination of Volatile Matter

Adopted from ISO 562 1 Apparatus and Materials

Balance (Accurate to 1 mg) Muffle furnace, maintained at a constant and uniform temperature of

900C +/- 5C 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 900C +/-

5C 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 900C +/- 5C in the furnace for 7 minutes. 2.8 Remove from the furnace.



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MANUAL

Issue Date:

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Page 2 of 2

Rev No.: 1

Code: CP4

PROXIMATE ANALYSIS

Determination of Volatile Matter

Adopted from ISO 562 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

2.11 Check precision of test results. Please see Table 1.

Table 1 Maximum Allowable Difference for Test Results

Test Conducted Repeatability Reproducibility < 10% 0.3% absolute 0.5% absolute 10% and over 3.0% of mean

result 0.5% absolute or 4.0% of mean result whichever is greater



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015


1

Code: CP5

PROXIMATE ANALYSIS

Determination of Ash

Adopted from ISO 1171

1 Apparatus and Materials

Balance (Accurate to 1 mg) Ash furnace, maintained at constant and uniform temperature of 815C

+/- 5C 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.



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015

Page 2 of 2

Rev No.: 1

Code: CP5

PROXIMATE ANALYSIS

Determination of Ash

Adopted from ISO 1171 2.11 Compute % ash. Formula: %Ash={(Weight after ignition–Weight of empty crucible)/Weight of sample}*100 2.12 Check precision of test results. Please see Table 1.

Table 1 Maximum Allowable Difference for Test Results Test Conducted Repeatability Reproducibility

< 10% 0.2% absolute 0.3% absolute 10% and over 2.0% of mean result 3.0% of mean result



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015

Page 1 of 1

Rev No.: 1

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)



COAL PROCEDURES

MANUAL

Issue Date:

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1

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

Issue Date:

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Code: CP7

CALORIFIC VALUE


Adopted from ASTM D 5865 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.



COAL PROCEDURES

MANUAL

Issue Date:

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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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CALORIFIC VALUE



5.6 Compute results and check precision of test results. Please see Table 1.

Table 1 Maximum Allowable Differences for Results Test Conducted Repeatability Reproducibility

Calorific Value 29 cal/g 72 cal/g 6. References 6.1 ASTM Standards

D 121 Terminology of Coal and Coke D 346 Practice for Collection and Preparation of Coke Samples for

Laboratory Analysis D 1193 Specification for Reagent Water D 2013 Method of Preparing Coal Samples for Analysis 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



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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.



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FORMS OF SULFUR

Determination of Forms of Sulfur in Coal

Adopted from ASTM D 2492 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 1193 Specification for Reagent Water 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 3180 Practice for Calculating Coal and Coke Analyses from As-

Determined to Different Bases 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



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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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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

Value Range

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

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.

Comment [RU1]:



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Using LECO SC 432 DR Adopted from ASTM 4239 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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Using LECO SC 432 DR Adopted from ASTM 4239 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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Using LECO SC 432 DR Adopted from ASTM 4239 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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Using LECO SC 432 DR Adopted from ASTM 4239 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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Using LECO SC 432 DR Adopted from ASTM 4239 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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Using LECO SC 432 DR Adopted from ASTM 4239 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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Using LECO SC 432 DR Adopted from ASTM 4239 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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Using Leco TruSpec S Adopted from ASTM D 4239 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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Using Leco TruSpec S Adopted from ASTM D 4239 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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Using Leco TruSpec S Adopted from ASTM D 4239 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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Using Leco TruSpec S Adopted from ASTM D 4239 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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Code: CP9b

TOTAL SULFUR



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.



COAL PROCEDURES

MANUAL



Code: CP9b

TOTAL SULFUR



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.



COAL

PROCEDURES MANUAL



1

Code: CP10

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.



COAL

PROCEDURES MANUAL



1

Code: CP10



Adopted from ASTM D 3177 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 815C for about an hour and then weigh. 3.14 Ignite the filter paper in a weighed crucible, partially covered, at 815C 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.



COAL

PROCEDURES MANUAL



1

Code: CP10



Adopted from ASTM D 3177 3.15 Check precision of test results. Please see Table 1. 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

D 346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis

D 1193 Specification for Reagent Water D 2013 Method of Preparing Coal Samples for 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 3180 Practice for Calculating Coal and Coke Analyses from As-

Determined to Different Bases 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



COAL PROCEDURES

MANUAL

Issue Date:

11 - 2015 Page 1 of 12 Rev No.:

1

Code: CP11

CARBON, HYDROGEN AND NITROGEN (CHN) ANALYSIS

Carbon, Hydrogen and Nitrogen (CHN) Analysis

(For C & H – by IR & For N – By Thermal Conductivity) Adopted from ASTM D 5373 - 02

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).



COAL PROCEDURES

MANUAL



1

Co de: CP11

CARBON, HYDRGEN AND NITROGEN (CHN) ANALYSIS


(For C & H – by IR & For N – By Thermal Conductivity) 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.



COAL PROCEDURES

MANUAL



1

Code: CP11




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



COAL PROCEDURES

MANUAL



1

Code: CP11




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.



COAL PROCEDURES

MANUAL



1

Code: CP11




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.



COAL PROCEDURES

MANUAL



1

Code: CP11




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.



COAL PROCEDURES

MANUAL



1

Code: CP11




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.



COAL PROCEDURES

MANUAL



1

Code: CP11




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.



COAL PROCEDURES

MANUAL



1

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.



COAL PROCEDURES

MANUAL



1

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.



COAL PROCEDURES

MANUAL



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.



COAL PROCEDURES

MANUAL



1

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 (2-3 trials in

gram)

Check Standard (2-3 trials in

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

11110e 0.10 0.10

COKE-Single point up to 93%C

AR 742 B 0.06 – 0.08 0.06 – 0.08

RLS Form 1

DEPARTMENT OF ENERGY Energy Compound, Merritt Road, Fort Bonifacio, Taguig, Metro Manila Telephone No.: Trunkline 4792900 Local 372 Direct Line 840-2093

RLS No.Date:

REQUEST FOR LABORATORY SERVICES

Phone/Fax No.

Sample(s)LabLabel CustomerLabel Qty Unit Analysis

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

Energy Research & Testing Laboratory ServicesDirector

Name & Signature of Person Submitting Sample

Addressee of Invoice and Results of Analysis

Name of Company/Agency/Organization

Address of Company/Agency/Organization

AmountDescription

External

Form #: CF1 Date of Issue: May 2015 Revision #: 3 Approved By: QM

Page 1 of 1

RLS Form 2

DEPARTMENT OF ENERGYEnergy Research & Testing Laboratory ServicesGeoscientific Research & Fuel Testing Laboratory

LWO No.

REQUEST FOR LABORATORY SERVICES [RLS]Name & Sig. of Person Submitting Sample

Name & Sig. of Head of Requesting Div/Unit

Section Chief Signature

Division Chief Signature

Special Instructions from Customer (if any) / Remarks

Noted By: Date

Phone/Local

Sample Received/Logged By: Date

Test Requested Area / Locality

Internal Customer

RLS Received By: Date

Requesting Division/Unit

Lab Code (for GRTL

use only)Sample DescriptionSample Label

Form #: CF2 Date of Issue: Nov. 2015 Revision #: 2 Approved By: QM

Page 1 of 1

Page 1 of 1

DEPARTMENT OF ENERGY Energy Research & Testing Laboratory Services Geoscientific Research & Fuel Testing Laboratory 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 Code/Label Description Tests

Requested Special Instruction

(If Any)

Date Sample Received By ERTLS : Date Sample Received By GRFTL : Date Reported : Approved By : _V. S. LLAMO____ , Division Chief

Form #: CF3 Date of Issue: Apr. 2017 Revision #: 4 Approved By: QM

Page 1 of 1

DEPARTMENT OF ENERGY Energy Research & Testing Laboratory Services Geoscientific Research & Fuel Testing Laboratory

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:__________________________________________

Form #: CF4 Date of Issue: Oct. 2017 Revision #: 3 Approved By: QM

Page 1 of 1


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


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


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

No.

Results

______________________________ Signature of Analyst(s)


Page 1 of 1


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 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 BTU/lb

ASTM D 5865-04

__________________________________________________________________________ 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:

Form #: CF8a Date of Issue: Jan. 2016 Revision #: 6 Approved By: QM

PAB ACCREDITED

TESTING LABORATORY PNS ISO/IEC 17025:2005

LA-2009-152B

Page 1 of 1


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 BTU/lb

ASTM D 5865-04

__________________________________________________________________________ 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: Analyzed By: Checked By: Noted By:

Form #: CF8b Date of Issue: Nov. 2015 Revision #: Approved By: QM

Page 1 of 1

Republic of the Philippines DEPATMENT OF ENERGY Energy Research and Testing Laboratory Services

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 BTU/lb

ASTM D 5865-04

___________________________________________________________________________________________________________ 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: Basis:

Amelia M. de Guzman Director

Form #: CF10b Date of Issue: Oct. 2015 Revision #: Approved By: QM

Page 1 of 1


COMPLAINT REPORT

Date:_______________ Reference No. :_____________________________ To :_____________________________ Director, ERTLS From :_____________________________ Name of Customer/Organization Details of Incident: Suggested Corrective Action: __________________ Signature



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):

Excellent 4 - Poor8 - Good 2 - Very Poor6 - Satisfactory

1. Courtesy - Polite, kind and thoughtful behavior toward co- 8 6 4 2 employee/ public/customer in manner of speech and actuation.

2. Readiness for service - Punctual, not engaging in unofficial 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 8 6 4 2 the customer; contentment level of customer on services provided (other criteria considered).

CUSTOMER RATING

10

10

Comments/Suggestions

10 -

10

Form #: CF12a Date of Issue: May 2017 Revision #: 3 Approved By: QM

Page 1 of 1


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/clarifiedcustomer's sample and/or purpose clearly 8- One (1) question not answeredanswered or clarified. 6- Two (2) questions not answered

4- Three (3) questions not answered2- More than three (3) questions not

answered

1.2. Test report contains all relevant information on 10- All requested information reportedthe test/s requested, i.e., test parameter, sample 8- One (1) item missinglabel, test method, basis and other technical 6- Two (2) items missingremark/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 explained6- Two (2) test results not explained4- Three (3) test results not explained2- More than three (3) test results

not explained2. 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 late4- Three (3) days late2- More than three (3) days late

CUSTOMER RATING

Form #: CF12b Date of Issue: May 2017 Revision #: 1

Approved By: QM

Page 1 of 1

Page 1 of 1


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: ________________________________ Auditor/Customer/Lab. Personnel/Others

Acknowledged by: ___________________________ 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:

Form #: CF13 Date of Issue: May 2017 Revision #: 3 Approved By: QM

Page 1 of 1


Document Originator:_________________ Date:__________

Type FromTitleDoc. CodeEffectivityDistribution 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:___________________________________________________________________________________________

Revision

DOCUMENT ISSUANCE / CHANGE NOTICE

New

Form #: CF15 Date of Issue: Oct. 2015 Revision #: 2 Approved By: QM

Page 1 of 1


TIMEDATE LOGGED BY

%RH T, °C %RH T, °C %RH T, °C123456789

10111213141516171819202122232425262728293031

REMARKS:

AMBIENT MONITORING REPORTSERIAL No.________________________

FOR THE MONTH/YEAR OF________________

Reading (%RH) / Temp (°C)9:00 AM 2:00 PM AVERAGE

Form #: CF16 Date of Issue: Jan. 2016 Revision #: 2 Approved By: QM

Page 1 of 1


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




Acculab - Analytical Balance

Serial No. 19190040

Year JUL AUG SEP OCT NOV DEC





B. Routine check








REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 1 of 1

Form #: CF19b Date of Issue: Jan. 2017 Revision #: 3 Approved By: QM



Leco 250 - Analytical Balance

Serial No.

Year

JAN FEB MAR APR MAY JUN





B. Routine check








REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 1 of 1




Leco 250 - Analytical Balance

Serial No.

Year

JUL AUG SEP OCT NOV DECA. Care and Maintenance




B. Routine check








REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 1 of 1


DEPARTMENT OF ENERGY Energy Research & Testing Laboratory Services Geoscientific Research & Fuel Testing laboratory


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.


B. Equipment

1. Check all wirings for nicks and cuts.

2. Clean the equipment with soft cloth.


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.


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.


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.


F. Calibration (Quarterly)

1. Perform calibration using Benzoic Acid Pellets.

2. Update calibration logbook and file print-out.


G. Others

1. Make sure that standardized Sodium Carbonate solution is available at all times.

2. Ensure that equipment area is clean.


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2

DEPARTMENT OF ENERGY Energy Research & Testing Laboratory Services Geoscientific Research & Fuel Testing laboratory


LECO AC 350 ISOPERIBOL CALORIMETER

Serial No. 3355

Year

JUL AUG SEP OCT NOV DEC





4. Check and make sure that the Matsunaga AVR is properly working.


B. Equipment




C. Bomb Assembly




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.



Page 1 of 2


E. Water Cooling Sytem






F. Calibration (Quarterly)




G. Others




REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2



PARR 6200 ISOPERIBOL CALORIMETER

Serial No. M15674

Year






4. Check and make sure that the Powercom UPS and Battery are properly working.


B. Equipment




C. Bomb Assembly




D. Printer

1. Ckeck if the unit is functioning. Replace rebbon if necessary. Make sure that reserve ribbon and printer paper are available at all times.



Page 1 of 2


E. Water Handling System





F. Calibration (Monthly)




G. Others




REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



PARR 6200 ISOPERIBOL CALORIMETER

Serial No. M15674

Year






4. Check and make sure that the Powercom UPS and Battery are properly working.


B. Equipment




C. Bomb Assembly




D. Printer

1. Ckeck if the unit is functioning. Replace rebbon if necessary. Make sure that reserve ribbon and printer paper are available at all times.



Page 1 of 2


E. Water Handling System





F. Calibration (Monthly)




G. Others




REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2

DEPARTMENT OF ENERGY Energy Research & Testing Laboaratory Services Geoscientific Research & Fuel Testing Laboratory


LECO TRUSPEC CHNS ANALYZER

Serial No. 3672 / 4118


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 1. Check the equipment display by going through the pre-set parameters, i.e., furnace temp & IR cell value.

2. Check the periodic maintenance counter especially 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 1. Check if the unit is functioning properly.

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.

Year_____________________

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)


Add-on Sulfur Analyzer 1. Perform system check.



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

DEPARTMENT OF ENERGY Energy Research & Testing Laboaratory Services Geoscientific Research & Fuel Testing Laboratory


LECO TRUSPEC CHNS ANALYZER

Serial No. 3672 / 4118


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.


Add-on Sulfur Analyzer 1. Check the equipment display by going through the pre-set parameters, i.e., furnace temp & IR cell value.

2. Check the periodic maintenance counter especially 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 1. Check if the unit is functioning properly.

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.

Year_____________________

Page 1 of 2


D. Calibration CHN Analyzer 1. Perform leak check test.

2. Perform system check.



5. Perform standard calibration.(Quarterly)


Add-on Sulfur Analyzer 1. Perform system check.



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



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


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


C. Calibration

1. Have the furnace calibrated annually

2. Update calibration logbook and index

3. File calibration certificate


D. Care

1. Clean the interior of the furnace

2. Clean the exterior and casing with a damp cloth


Page 1 of 2


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



PRUFER FURNACE I


Year


A. Operation




B. Routine check




C. Calibration





D. Care




Page 1 of 2


REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2



PRUFER FURNACE II


Year


A. Operation




B. Routine check




C. Calibration





D. Care




Page 1 of 2


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



PRUFER FURNACE II


Year


A. Operation




B. Routine check




C. Calibration





D. Care




Page 1 of 2


REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2



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.




B. Balance



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.


C. Computer

1. Check if the MA2000win program is working.




D. Printer


2. Check all wirings or nicks and cuts.

3. Clean the printer with soft cloth and dust brush.



Page 1 of 2

E. Calibration

1. Perform calibration using Hg standard solutions.



F. Others

1. Ensure that the unit is clean.

2. Check supplies and materials. Inform lab. tech. of any need.


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



MA-2000 MERCURY ANALYZER

Serial No. P/N JE-HE-03-1149


A. Equipment

1. Check if the boat changer is functioning properly. Clean if necessary.




B. Balance



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.


C. Computer

1. Check if the MA2000win program is working.




D. Printer


2. Check all wirings or nicks and cuts.

3. Clean the printer with soft cloth and dust brush.



Page 1 of 2

E. Calibration

1. Perform calibration using Hg standard solutions.



F. Others


2. Check supplies and materials. Inform lab. tech. of any need.


REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2



COAL - AIR DRYING OVEN

SERIAL No.

Year

JAN FEB MAR APR MAY JUNI. 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




COAL - AIR DRYING OVEN

SERIAL No.

Year

JUL AUG SEP OCT NOV DECI. 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




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, ifnecessary

C. Periodic Maintenance (Indicate date conducted)

1. Lubricate the mechanical parts of the doorhinges 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



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

2. Check and make sure that the gas regulator 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


B. Calibration - Annually


2. Update calibration logbook



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


Page 1 of 2


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



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

2. Check and make sure that the gas regulator 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


B. Calibration - Annually


2. Update calibration logbook



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


Page 1 of 2


REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2



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



5. Check and make sure that the AFA AVR output is 220v


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.


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.


D. Calibration

1. Calibrate the instrument using coal standard.



E. Others


2. Ensure that the instrument area is clean.


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



LEC0 SC 432 DR - SULFUR ANALYZER

Serial No. 3388 / 3331

Year



1. Check the gases (O2 and Comp. Air). Make sure that there is enough supply and spare cylinders are available at all times






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.


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.


D. Calibration

1. Calibrate the instrument using coal standard.



E. Others


2. Ensure that the instrument area is clean.


REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2



LAS NAVAS TGA-1000 THERMOGRAVIMETRIC ANALYZER

Serial No. 000202



1. Check the gases (N2,O2 and Comp. Air). Make sure that there is enough supply and spare cylinders are available at all times






B. Carousel, Balance and FurnaceNote: 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.


Page 1 of 2


C. Printer


2. Replace ink if necessary. Make sure that a spare is available at all times


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


E. Care and Maintenance

1. Ensure that the instrument is free from dust

2. Ensure that the monitor, cpu and printer are clean

3. Make sure that the area is clean4. Cover the instrument and the computer set with plastic


REMARKS:JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



LAS NAVAS TGA-1000 THERMOGRAVIMETRIC ANALYZER

Serial No. 000202



1. Check the gases (N2,O2 and Comp. Air). Make sure that there is enough supply and spare cylinders are available at all times






B. Carousel, Balance and FurnaceNote: 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.


Page 1 of 2


C. Printer


2. Replace ink if necessary. Make sure that a spare is available at all times


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


E. Care and Maintenance

1. Ensure that the instrument is free from dust

2. Ensure that the monitor, cpu and printer are clean

3. Make sure that the area is clean4. Cover the instrument and the computer set with plastic


REMARKS:JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2


MONTHLY HOUSEKEEPING PROGRAM

(Laboratory Technician)

Year _________

Sample Preparation Room JAN FEB MAR APR MAY JUN1. 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 use2. 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 Rooms1. 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 wk3. Ensure that gas cylinders (for calorimeter and XRF only) are properly chained in place. 2. Ensure that all equipment units, light switches airconditioners and fans are turned off; windows, doors and faucets are closed before leaving the area after office hours daily

Remarks:Jan

Feb

Mar

Apr

May

Jun

Date and Signature


Page 1 of 1


MONTHLY HOUSEKEEPING PROGRAM

(Laboratory Technician)

Year _________

Sample Preparation Room JUL AUG SEP OCT NOV DEC1. 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 use2. 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 Rooms1. 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 wk3. Ensure that gas cylinders (for calorimeter and XRF only) are properly chained in place. 2. Ensure that all equipment units, light switches airconditioners and fans are turned off; windows, doors and faucets are closed before leaving the area after office hours daily

Remarks:Jul

Aug

Sep

Oct

Nov

Dec

Date and Signature


Page 1 of 1


Document Originator:_________________ Date:__________

TypeTitleDoc. CodeEffectivityDistribution List

Remarks:____________________________________________________________________________________________

Reviewed By:_________________ Noted By:______________

Discussed with relevant personnel? yes no

Signature of affected personnel:

Review

DOCUMENT REVIEW


Page 1 of 1



Kern - Analytical Balance

Model: ABS 220-4N

Serial No. WB13AR0151






B. Routine check








REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 1 of 1




Kern - Analytical Balance

Model: ABS 220-4N

Serial No. WB13AR0151






B. Routine check








REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 1 of 1




CARBOLITE FURNACE

Model : AAF 1100

Serial No. 21-400256

Year


A. Operation




B. Routine check




C. Calibration





D. Care




Page 1 of 2


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



CARBOLITE FURNACE

Model : AAF 1100


Year


A. Operation




B. Routine check




C. Calibration





D. Care




Page 1 of 2


REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2



CARBOLITE FURNACE

Model : VMF 1000


Year


A. Operation




B. Routine check




C. Calibration





D. Care




Page 1 of 2


REMARKS:

JAN

FEB

MAR

APR

MAY

JUN

Page 2 of 2



CARBOLITE FURNACE

Model : VMF 1000


Year


A. Operation




B. Routine check




C. Calibration





D. Care




Page 1 of 2


REMARKS:

JUL

AUG

SEP

OCT

NOV

DEC

Page 2 of 2


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 #: CF40 Date of Issue: Nov. 2015

Revision #: 1 Approved By: QM

INTERNAL QUALITY AUDIT CHECKLIST

PNS ISO/IEC 17025

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Department of Energy Energy Research & Testing Laboratory Services

Geoscientific Research & Fuel Testing Laboratory

Geothermal-Coal Section

Form #: CF41 Date of Issue: Aug. 2016 Revision #: Approved By: QM

Clause Requirement for Accreditation Reference to Laboratory

Document (To be completed by the laboratory)

Remarks

4 4 Management Requirements

4.1 Organization 4.1.1 Legal identity

an entity that can be held legally responsible

4.1.2 Responsibility

Carry out testing or calibration activities to meet requirements of the standard, its customers, regulatory authorities or accreditation bodies

4.1.3 Scope of management system

ensure management system covers activities in the laboratory’s permanent facility, sites away from its permanent facilities, or in associated temporary or mobile facilities

4.1.4 Conflict of interest

when part of an organization performing activities other than testing and/or calibration, ensure the laboratory defines the responsibilities of key personnel to identify potential conflicts of interest

4.1.5a Managerial and technical personnel

have managerial and technical personnel, irrespective of other responsibilities, with authority and 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 Undue pressure

ensure arrangements for managerial and technical personnel 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 Customer confidentiality

ensure there are policies and procedures related to customer’s confidentiality of information and proprietary rights, including electronic storage and transmission of results.


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Remarks

4.1.5d Operational integrity

ensure laboratory has policies and procedures to avoid involvement in activities that would diminish confidence in its competence, impartiality, judgement or operational integrity

4.1.5e Organization chart

define organization and management structure including relationships between quality management, technical operations , support services and parent organization (if applicable)

4.1.5f Responsibility and authority

specify the responsibility, authority and interrelationships of all personnel who manage, perform or verify work affecting the quality of the tests and/or calibrations

4.1.5g Laboratory supervision

provide adequate supervision by appropriate personnel of all staff involved in calibration and testing activities, including trainees

4.1.5h Technical management

identify technical management that has overall responsibility for technical operations and provision of resources

4.1.5i Quality manager

appoint a member of staff, with direct access to senior 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 Managerial deputies

appoint deputies for key managerial personnel, where practical

4.1.5.k Importance of roles

ensure personnel are aware of relevance and importance of their activities and how they contribute to the objectives of the management system

4.1.6 Appropriate communication

appropriate communication processes established within the laboratory and include the effectiveness of the management system


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Remarks

4.2 Management system

4.2.1 Policies and procedures

Establish, implement and maintain management system appropriate to 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 Quality policy statement

ensure the quality policy statement is issued under the authority of top 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, 4.2.6 Quality manual

Maintain a quality manual that: - defines management system

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 Commitment to management system

Evidence of commitment to development, implementation and continual improvement of the management system must be available.


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Remarks

4.2.4 Customer requirements

importance of meeting customer, statutory and regulatory requirements must be communicated

4.2.7 Changes to management system

integrity of the management system must be maintained when changes are made.

4.3 Document control 4.3.1 Procedures

ensure procedures to control all documentation included in the management system are established and maintained

4.3.2.1 Approval and issue

ensure documents are reviewed and approved by authorized personnel prior to issue, and are included on a master list which identifies the revision status and distribution.

4.3.2.2 Availability

ensure all necessary quality documentation is available where required, reviewed and revised to maintain suitability

4.3.2.2 Obsolete documents

ensure documents are removed when obsolete and suitably marked if retained for either legal or knowledge preservation purposes

4.3.2.3 Identification

all management system documents 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 Document changes

ensure changes to documents are reviewed and approved by the same function that performed the original review, or a designate

4.3.3.2 Altered or new text

ensure where practical, the altered or new text is identified in the document or the appropriate attachments

4.3.3.3 Handwritten amendments

ensure if hand written amendments are allowed, defined procedures are available, which include authorities, clear marking, initialing, dating, and formal re-issue


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Remarks

4.3.3.4 Electronic documents

establish procedures to describe how changes in documents maintained electronically are made and controlled

4.4 Review of requests, tenders and contracts 4.4.1, 4.4.3 Policies and procedures

ensure policies and procedures related to review of requests, 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 Records of review

maintain records of reviews, including any significant discussions and/or changes throughout the contract

4.4.4 Notification of customer

ensure customer is informed of any deviation from the contract

4.4.5 Changes to contracts

ensure same contract review process is repeated if a contract 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 Competency

ensure that subcontractors are competent (e.g. accredited laboratory) and records are maintained of subcontractors used and their competency (e.g. terms of accreditation)

4.5.2 Customer approval

ensure customer is advised in writing and approval gained, where appropriate

4.5.3 Responsibility

unless customer or a regulatory authority specifies subcontractor, laboratory is responsible for subcontractors' work


PNS ISO/IEC 17025

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Remarks

4.6 Purchasing services and supplies


document policy and procedures for selection, purchasing, reception and storage of relevant services and supplies

4.6.2 Verification

ensure all purchased supplies that 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 Purchasing documents

ensure purchasing documents for items affecting the quality of work are reviewed and approved for technical content prior to release

4.6.4 Approved suppliers

maintain list and records of the evaluations and all approved suppliers

4.7 Service to the customer

4.7.1 Cooperation

Cooperate with customers to clarity requests and monitor laboratory's performance provided laboratory’s ensure confidentiality to other customers

4.7.2 Feedback

feedback must be sought and used to improve the laboratory’s activities

4.8 Complaints


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4.8 Policy, procedure and records

document policy and procedure for the resolution of complaints from customers or other parties and ensure records of the complaints, investigations and corrective actions (4.11) are maintained

4.9 Control of nonconforming testing and/or calibration work


ensure policy and procedures are implemented when work or results 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 Recurrence

Corrective action procedures (4.11) 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 Effectiveness

continually improve the effectiveness of the management system

4.11 Corrective action

4.11 Policies and procedures

establish policy and procedures, and designate appropriate authorities for implementing corrective actions which include: - cause analysis to determine the

root cause (4.11.2) - selection, implementation and


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Remarks

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 Identification and action

ensure needed improvements and potential sources of nonconformities 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 Procedures

establish and maintain 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 Record integrity

ensure all records are: - 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 Technical records

ensure laboratory retains technical records of: - original observations - derived data - sufficient information to establish


PNS ISO/IEC 17025

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Remarks

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 Recording

ensure observations, data and calculations are recorded at the time they are made and are identifiable to the specific task

4.13.2.3 Corrections to records

ensure any changes to the original records (including electronic) are 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 Requirements

- internal audits shall be conducted 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 Corrective action and notification of

where validity of results has been questioned, timely corrective action must be taken and customers notified in writing if it is shown that


PNS ISO/IEC 17025

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Remarks

customers laboratory results have been affected

4.14.3 Records

records of area audited, the audit findings and corrective actions must be retained

4.14.4 Follow-up audits

follow-up audit shall verify and record implementation and effectiveness of corrective action

4.15 Management reviews 4.15.1 Objectives

ensure the laboratory's 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 Contents

ensure the review includes: - 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 Actions and records

ensure findings and actions are recorded and carried out within an appropriate and agreed timescale

5 Technical Requirements

5.1 General

5.2 Personnel


PNS ISO/IEC 17025

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Remarks

5.2.1 Competence

ensure personnel performing 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 Training policy

policy and procedures must be implemented for identifying training needs, providing training and evaluating its effectiveness

5.2.3 Employees

ensure personnel are employed or contracted by the laboratory, and ensure contracted personnel are

supervised, competent and work in accordance with the management system

5.2.4 Job descriptions

maintain current job descriptions for managerial, technical and key support staff

5.2.5 Authorized personnel

Ensure management has authorized specific personnel to: - 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 Facility

ensure the laboratory or off-site facility(ies) and environmental conditions do not compromise the quality of results and that the


PNS ISO/IEC 17025

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Remarks

technical requirements for critical accommodation and environmental conditions are documented

5.3.2 Monitoring

ensure laboratory monitors, controls 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 Incompatible activities

ensure there is effective separation between areas of incompatible activities.

5.3.4 Access

ensure access to office and laboratory areas are controlled

5.3.5 Housekeeping

ensure housekeeping measures are adequate

5.4 Test and calibration methods and method validation

5.4.1 Methods and procedures

ensure laboratory uses appropriate methods and procedures for all 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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Remarks

Method deviations

calibration methods are: - documented - technically justified - authorized - accepted by the customer

5.4.2 Method selection

ensure laboratory selects and uses test and/or calibration methods, 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 Inappropriate methods

ensure laboratory informs the customer if method proposed by the customer is inappropriate or out of date

5.4.3, 5.4.4 Laboratory-developed methods and non-standard methods

ensure introduction of these methods is planned and assigned to qualified personnel with adequate resources and that plans are updated as development proceeds and communicated as necessary - when methods are used that are

not covered by standard methods,


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Remarks

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 Method validation

laboratory must validate: o non-standard methods 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 Range and accuracy

ensure the range and accuracy of the values obtainable from validated 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 Uncertainty of measurement

calibration laboratories or testing laboratories performing their own 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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Remarks

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 Calculations and data transfers

ensure calculations and data transfers are checked in a systematic manner

5.4.7.2 Computers and automated equipment

Ensure when computers or automated equipment are used for the acquisition, processing, 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

Operation Ensure all equipment and its 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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Remarks

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 Records

ensure records of equipment are 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 Procedures

ensure procedures for measuring 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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Remarks

updated 5.5.7 Out-of-service

ensure equipment subjected to 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 Calibration status

ensure equipment calibration status is identified, where 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 Return to service

ensure when equipment goes outside the direct control of the laboratory, that the function and calibration status are checked before the equipment is returned to service

5.5.12 Adjustments

ensure equipment, both hardware and software is safeguarded from adjustments which could invalidate the test and/or calibration results

5.6 Measurement Traceability

5.6.1 Calibration program

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

5.6.2.1 Calibration laboratories

must ensure the program for calibration of equipment is shall be designed and operated so that calibrations and measurements are traceable to the International System of Units (SI units), however


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Remarks

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 Testing laboratories

the requirements given in 5.6.2.1 apply for measuring and test 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 Reference standards

o program and procedure for calibration of reference 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 Reference materials

where possible, reference materials must be traceable to SI units or certified reference materials internal reference materials must be checked as far as is technically and economically practicable

5.6.3.3 Intermediate checks

procedures and schedules must be available to carry out intermediate checks on reference, primary, transfer or working standards and reference materials to maintain confidence in the calibration status

5.6.3.4 Transport and storage

procedures for safe handling, transport, storage and use of reference standards and materials must be available

5.7 Sampling


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Remarks

5.7.1 Procedures and plan

ensure procedures for sampling are available at sampling location 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 Deviations

ensure customer -requested deviations, additions or exclusions from the documented sampling procedures are recorded communicated to the appropriate personnel

5.7.3 Records

ensure laboratory has procedures 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 Procedures

document procedures for test 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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Remarks

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 Deficiencies

o ensure abnormalities or 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 Facilities

ensure laboratory has procedures 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 Quality control

ensure laboratory has quality 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 Action on quality control

Analyse and take appropriate action on quality control data that falls outside pre-defined criteria


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Remarks

data

5.10 Reporting the results

5.10.1, 5.10.8 Test reports and calibration certificates

o results of tests and calibrations must be reported accurately, clearly, unambiguously and 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 Test report

o test reports must include the 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 Calibration

o calibration certificates must include the information listed in


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Remarks

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 Opinions and interpretations

o must document the basis the opinions and interpretations are made

o must be clearly marked in a test report

5.10.6 Testing and calibration results obtained from subcontractors

o results of tests performed by subcontractors must be clearly identified

o where calibration work has been subcontracted, the laboratory performing the work shall issue the calibration certificate to the contracting laboratory

5.10.7 Where results are transmitted


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Remarks

Electronic transmission of results

electronically or electromagnetically the requirements set out in the Standard must be met

5.10.9 Amendments to test reports and calibration certificates

o amendments to a test report or calibration certificate after issue must be made in the form of a further document, or data transfer 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