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1Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 1
Calibration and Measurement Capability of Gas Analysis
Calibration and Measurement Calibration and Measurement Capability of Gas AnalysisCapability of Gas Analysis
ByBy
Ratirat Ratirat SinweeruthaiSinweeruthai
Gas Analysis Laboratory
Department of Chemical Metrology and Biometry
National Institute of Metrology (Thailand)
May 25, 2009
NIMT, Thailand
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 2
Gas Analysis LaboratoryGas Analysis LaboratoryGas Analysis Laboratory
As of May 2009
2Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 3
Gas Analysis SectionGas Analysis SectionGas Analysis Section
GC : TCD, FID
SO2 Analyzer
FT-IR
Nox Analyzer
O2 Analyzer
CO Analyzer
ND-IR Analyzer
Micro GC
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 4
Gas Weighing SectionGas Weighing SectionGas Weighing Section
3Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 5
Gas Filling SectionGas Filling SectionGas Filling Section
Cleaning System for Gas CylinderCleaning System for Gas Cylinder Gas Filling System Gas Filling System
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 6
11stst stage of traceability scheme on calibration at NIMTstage of traceability scheme on calibration at NIMTSI
CERI
Japan Gas
Company
NIMT
JapaneseUsers
Thai Gas Companiesor Users
NMIJ
primary
Secondary
calibration
calibration
Certification(Relative Uncertainty1%2%)
Transfer
Secondary
Working
High-purity gasCRM
comparison
(Firstly, for O2/N2 mixtures around 20% and CO/N2 mixtures 5 ppm 100 ppm)
jcss Certification, within 1%
JCSS Certification, 1%2% Working
calibration
Accreditation of ISO/IEC 17025
Secondary
Working
Working
4Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 7
Certified Standard Gas and CalibrationCertified Standard Gas and CalibrationCertified Standard Gas and Calibration
Uncertainty : within 1%
CR
M
WR
M
WR
M
RM
O2 Analyzer
CO Analyzer
High Accuracy Low Accuracy
Uncertainty : within 1%
It is developing the method for reducing the uncertainty
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 8
Method for Certified Standard GasMethod for Certified Standard GasMethod for Certified Standard Gas
Uncertainty : within 1%
CR
M
QC
cyl
ind
er
WR
M(s
am
ple
)
QC
cyl
ind
er
QC
cyl
ind
er
5Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 9
Accreditation ScopeFor Certify and Calibration
Accreditation ScopeAccreditation ScopeFor Certify and CalibrationFor Certify and Calibration
Calibration O2 Analyzer and Certified O2 in N2
Range: 0.05 - 0.30 mol/mol
Uncertainty (k=2) : 0.25 % relative
WR
M
N2
99
.99
5%
O2 Analyzer
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 10
Accreditation ScopeFor Certify and Calibration
Accreditation ScopeAccreditation ScopeFor Certify and CalibrationFor Certify and Calibration
Calibration CO Analyzer and Certified CO in N2
Range: 5 - 25 mol/molUncertainty (k=2) : 0.80 % relative
Range: 25 - 100 mol/molUncertainty (k=2) : 0.45 % relative
WR
M
N2
99
.99
5%
CO Analyzer
6Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 11
Quality Systems that need to be fulfilled according to Gas Analysis Laboratory
Quality Systems that need to be fulfilled Quality Systems that need to be fulfilled according to Gas Analysis Laboratoryaccording to Gas Analysis Laboratory
Quality System ISO/IEC 17025:2005
Gas Analysis Production according to ISO 6143
Analysis SectionAnalysis SectionAnalysis Section
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 12
Service Route for O2 in N2 Service Route for OService Route for O22 in Nin N2 2
First Stage:First Stage:Service Type: Calibration and Certified Gas Mixture (CRM)Range: 0.05 mol/mol to 0.30 mol/mol Analysis Technique: Paramagnetic Oxygen AnalyzerService Time: April 2008Certified Reference Materials: CERI (u(x)= 0.2%rel)Bilateral Comparison: NMIJ, August 2008 (Draft B)Accreditation Body: IA Japan (In Process)
Degrees of equivalence plot
7Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 13
Service Route for O2 in N2Service Route for OService Route for O22 in Nin N22Second Stage:Second Stage:
Service Type: Preparation Primary Reference Mixture (PRM)Certified Gas Mixture (CRM)Calibration
Range: 100 mol/mol to 0.30 mol/molAnalysis Technique: GC-TCD & Paramagnetic Oxygen AnalyzerService Time: within 2009
Third Stage:Third Stage:Service Type: Preparation Primary Reference Mixture (PRM)
Certified Gas Mixture (CRM)Calibration
Range: 1 mol/mol to 100 mol/mol Analysis Technique: GC-PDHIDComparison : NMiService Time: May 2010
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 14
Service Route for CO2 in N2 Service Route for COService Route for CO22 in Nin N2 2 First Stage:First Stage:
Service Type: Preparation Primary Reference Mixture (PRM)Certified Gas Mixture (CRM) Calibration
Range: 100 mol/mol to 0.14 mol/mol Analysis Technique: GC-FID with MethanizerService Time: 2010
Second Stage:Second Stage:Service Type: Preparation Primary Reference Mixture (PRM)
Certified Gas Mixture (CRM)Calibration
Range: 1 mol/mol to 100 mol/mol Analysis Technique: GC-FID with MethanizerComparison : NMiService Time: 2011
8Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 15
Service Route for CO in N2Service Route for CO in NService Route for CO in N22 First Stage:
Service Type: Calibration and Certified Gas Mixture (CRM)Range: 5 mol/mol to 100 mol/molAnalysis Technique: ND-IR & GC-FID with MethanizerService Time: April 2008Inter-comparison: CCQM
Second Stage:Service Type : Preparation Primary Reference Mixture (PRM)
Certified Gas Mixture (CRM)Calibration
Range: 100 mol/mol to 0.14 mol/mol Analysis Technique: ND-IR & GC-FID with MethanizerBilateral Comparison: NMiService: 2011
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 16
First Stage: Inter-comparison CO in N2
Range: 5 mol/molAnalysis Technique: ND-IR Period: May 2008Certified Reference Material: CERIOrganization: CCQM Status: Draft AAccreditation Body: IA Japan Status: In Process
NIMT
Degrees of equivalence plotGC-FID ND-IR FT-IR
9Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 17
Calibration ServicesCalibration Services CO AnalyzerCO Analyzer OO22 AnalyzerAnalyzer
Certified Reference MaterialsCertified Reference Materials CO in NCO in N22 OO2 2 in Nin N22
Training CourseTraining Course Planning to open in 2009Planning to open in 2009
Calibration, Certification and TrainingCalibration, Certification and TrainingCalibration, Certification and Training
Primary reference materials Primary reference materials O2 in N2 in range of 1 % to 25 % O2 in N2 in range of 1 % to 25 %
Planning to sell within 2009Planning to sell within 2009
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 18
22ndnd stage of traceability scheme on calibration at NIMTstage of traceability scheme on calibration at NIMT(planned)(planned)SI
Japan Gas
Company
NIMT
JapaneseUsers
Thai Users
NMIJ
Preparation/Calibration
Secondary
Secondary
Working
High-purityCRM
Thai Gas
Company
Working
Primary Gas prepared by NIMT
calibration
CERI primary
Secondary
calibrationcomparison
jcss Certification, within 1%
JCSS Certification, 1%2%
Secondary
NIMT Certification
Gas Manufacture Certification
Transfer
calibration
Accreditation of ISO Guide 34
WorkingWorking
comparison
NMIs
10
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 19
GAS Reference MaterialsGAS Reference MaterialsGAS Reference Materials
Vehicle emission gas
Stack emission gas
Plan to produce in 2009-2012
Natural Gas
Ethanol in N2
Plan to produce in 201x
Plan to produce in 2011-201x
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 20
Quality Systems that need to be fulfilled according to Gas Analysis Laboratory
Quality Systems that need to be fulfilled Quality Systems that need to be fulfilled according to Gas Analysis Laboratoryaccording to Gas Analysis Laboratory
Quality System ISO/IEC 17025:2005
Gas Analysis Production according to ISO 6142 and ISO 6143
Production of Reference Material according to ISO Guide 34
11
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 21
33rdrd stage of traceability scheme on calibration at NIMTstage of traceability scheme on calibration at NIMT(planned)(planned)SI
CERI
Japanese Gas
Company
NIMT
JapaneseUsers
Thai Users
NMIJ
primary
Secondary
calibration
Secondary
Secondary
Working
High-purity gasCRM
Thai Gas
CompanyWorking
primary
calibration
SI
High-purity gas, the purity (impurities) is determined by NIMT
comparison
comparison
jcss Certification, within 1%
JCSS Certification, 1%2%
NIMT Certification
Gas Manufacture Certification
calibration
Preparation/Calibration
Accreditation of ISO Guide 34
WorkingWorking
Secondary
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 22
Mile-stoneMileMile--stonestone
-2008 ?Calibration using jcss secondary mixturesCertify Working standard gas (ISO/IEC 17025)
-2010 ?Accreditation of ISO Guide 34Preparation of Primary/Secondary gas mixtures by NIMT
-201x ? NIMT prepare High-purity gas, Primary/Secondary gas mixtures.
1st stage
2nd stage
3rd stage
12
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 23
AcknowledgementAcknowledgementAcknowledgement
How to certified gases accurately.
How to calibrate gas analyzers accurately
How to prepare PRM by using gravimetric method for binary mixture.
How to estimate uncertainty following ISO 6143
How to manage the quality system ISO/IEC 17025
National Metrology Institute of Japan (NMIJ)
National Metrology Institute of Japan National Metrology Institute of Japan (NMIJ)(NMIJ)
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 24
13
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 25
NMIJ FacilitiesNMIJ FacilitiesNMIJ Facilities
Gravimetric Method
( ISO 6142 )
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 26
AcknowledgementAcknowledgementAcknowledgement
How to prepare PRM by using gravimetric method (ISO 6142). Binary Mixture Multi component mixture
Natural gas mixture Emission gas mixture
Ethanol gas mixture How to analysis impurity in purity gases or reagent.
FT-IR GC-PDHID Moisture Analyzer (Cavity ring down technique) Karl Ficher
Safety principle for preparing PRM Principle for dynamic dilution mixing ISO 6145
Dutch Metrology Institute (VSL)Dutch Metrology Institute (VSL)Dutch Metrology Institute (VSL)
14
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 27
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 28
PRM by VSLPRM by VSLPRM by VSL
15
Chemical Metrology and Biometry Department, National Institute of Metrology (Thailand) 29
VSL FacilitiesVSL FacilitiesVSL Facilities
Gravimetric Method
( ISO 6142 )
Dynamic Volumetric Method
( ISO 6145 )