Dissemination of gas CRM in China

Hai Wu
wuhai@nim.ac.cn

National Institute of Metrology (NIM), China

2016/7/27

14th workshop, APMP/TCQM GAWG

Mongolia, 26-28 July 2016
Outlines

• Administration of gas CRMs in China

• Inter-lab comparison on gas CRMs
• Gas CRM used for calibration of analyzers

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1- Administration of CRMs in China
◎ Traceability system of gas measurement

MRA

Developed by NIM KC, PR

National CRM

Calibration Procedures

Calibration/Measurement Results
By testing/calibration labs
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1- Administration of CRMs in China
◎ Administration of CRMs

4
1- Administration of CRMs in China
◎ Requirements for CRMs of Level 1 and 2

CRM Level 1 (GBW XXXX) CRM Level 2(GBW(E) XXXX)

Producer Bodies qualified by AQSIQ. Bodies qualified by AQSIQ.
Typically are metrological Typically are industries,
research institutes, authority research institutes or others
labs or others
Characterization 1) By using absolute method of 1) Same techniques as used for
technique highest accuracy; CRM Level 1;
2) Two methods of different 2) Certification against CRM
principles; Level 1;
3) Multi-lab collaboration;
Stability Stable over ≥ 1 year; Stable over several months;
Applications 1) Calibration of instrument; 1) Calibration of instrument;
2) Validation of method; 2) Validation of method;
3) Validation of CRM Level 2; 3) Routine measurement ;
4) Other applications
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1- Introduction of CRMs in China
◎ Gas CRMs and producers CRM numbers: Level 1
-Level 1: ~150 NIM Other

-Level 2: ~1700
-RMP: ~150 8%

Gas CRMs of NIM

92%

24% Environment
Food
37%
Energy CRM numbers: Level 2
Safety NIM Other
3% Purity Gas
6% Medical
Forensic 6%
6% Others
6%
9%
9%

94%

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2- Inter-lab comparison on gas CRMs
• ILC is important for maintain the equivalence of gas CRMs
– RMP: 150
– CRM of level 2: 1700 kinds

• NIM’s role
– Coordinating ILC on gas
CRMs
– Link to CMC
– Sharing knowledge in order to
improve equivalence of national
CRMs

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2.1- ILC on CH4/air

– Methane alarmer subject to

compulsory verification CCQM-K82

– 0.5%mol/mol, 3%mol/mol
are the typical concentration
level at which verification
were conducted.

– En ratios of 95% of 30 CRMs within ±1

1.500 1.000

1.000

0.500

0.500
En值

En值
0.000 0.000
L0 4
L2 1
L1 0
L2 2
L0 2
L1 5
L1 2
L2 3
L2 0
L0 1
L1 6
L1 8
L2 8
L2 9
L2 7
L0 5
L2 6
L1 3
L3 0
L1 4
L0 3
L0 9
L0 7
L1 1
L0 8
L0 6
L1 9
L2 5

L15
L27
L16
L14
L22
L07
L01
L20
L24
L02
L13
L04
L19
L12
L28
L26
L18
L10
L17
L05
L09
L11
L21
L29
L30
L03
L25
L23
L06
L08
-0.500

-0.500

-1.000

-1.500 -1.000
实验室代码 实验室代码

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2.2- ILC on H2S CRMs
• H2S are typical sulfur-containing air pollutant in the air
• CRMs of (10~100)mol/mol are usually used to calibrate H2S detectors
• 12 RMP prepared CRM and sent to NIM for preparation comparison.
• En ratios of ~50% CRMs were not satisfied
– Most En ratio were below -1
– H2S adsorption effect onto cylinder surface may cause drop in concentration.

4
2
0
-2
En -4
-6 A B C D E F G H I J K
-8
-10
-12 系列1 系列2
-14
研制单位

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3- Gas CRMs establish traceability
• Mandatory verification based on Metrology Law
– Catalogue of working measurement instrument subject to compulsory
verification
• Include list of gas analyzers used in trade settlement, safety
protection, medical healthcare, and environmental monitoring
• Above analyzers be subject to periodical verification (compulsory
calibration, so called “verification”)
– MTCs (Measurement Technology Committee)
• Setting verification SOPs for each analyzer
– JJG 968 verification regulation of flue gas analyzer
stability, repeatability, indicate error(accuracy)…
• In which CRMs should be used

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3.1- CRMs establish traceability in IAQ measurement

IAQ standard Setting criteria for 13 air pollutants

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Traceability system of HCHO measurement
• HCHO standard generation system
– Basing on ISO 6145
– Dissemination range: 0-10ppm
– ACRM collaboration project:
trilateral comparison results proved
equivalence
– Used to calibrate HCHO analyzer

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Traceability system of O3 measurement

• Ozone measurement
– SRP41
• Established by NIST
• National primary standard
• Range: 0-1000ppb
• Participating in BIPM.QM-K1

– NIM O3 measurement standard

• Range 1：0-1000ppb
• Range 2：0-500ppm
(Sterilization device)
• JJG 1077-2012, verification
regulation for O3 analyzer

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3.2-Traceability system of exhaust gas measurement

• Vehicle emission measurement is mandatory

1999 GB I

2002
GB II

GB III
2005

2008 GB IV

2013
BEIJING V

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3.2-Traceability system of exhaust gas measurement

• JJG 688-2007
Calibrated parameters:
Propane, carbon monoxide, carbon dioxide
Nitrogen monoxide, oxygen

CCQM-K3
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3.3-Traceability system of flue gas measurement

• CRMs for flue gas measurement

– NO: 10-100 µmol/mol
– SO2: 20-200 µmol/mol
– CO: 10-100 µmol/mol
– CO2: 100-160 mmol/mol
– C3H8: 1-10 µmol/mol
– balance：N2

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3.4-Traceability system of exhaust gas measurement
CCQM-K23b -- i-Butane

5.0%
4.0%
3.0%

Relative deviation (%)

2.0%
1.0%
0.0%
-1.0%
-2.0%
-3.0%
-4.0%
-5.0%

BAM

GUM

KRISS
OMH
SMU

NRCCRM
NPL

NMi VSL
CMI

CENAM

CEM

NMIA

IPQ

INMETRO

NMIJ
VNIIM
Laboratory

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3.5- Gas CRM addresses industry need

 Address need from State GRID Corporation

 Setting up criteria of diagnosis for GIS based on
the measurement results.

 CRM for measuring decomposition products of GIS

SF6
 SO2
 SO2F2
 SOF4
 HF
 C3H8
 CO
 …

 CRM needed when evaluating the performance of

SF6 analyzers
summary
• Gas CRM plays important role in establishing the traceability
of calibration/measurement results
• Around 150 RMPs serve over 1800 kind of gas CRMs in
China. NIM as the NMI take the responsibility of establishing
international equivalence of gas CRMs.
• ILC is an important manner to provide external QA to the.
RMP
• Some gas analyzers of special applications are subject to
mandatory verification in China, in order to ensure the
traceability of measurement results.

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Thanks for your attention.

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