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CCQM – Gas Analysis Working Group
Jin Seog Kim
KRISS
Presentation to CCQM
April 2016
CCQM
GAWG
34th Meeting (participants 47: 21 Economies+BIPM/NOAA/IAEA) – 18th-19th Apr. 2016, BIPM
• 12 comparisons in 2015-2016 – K84 (CO), K101 (oxygen/nitrogen), K90 (formaldehyde),
K111 (core KC, propane), K112 (Biogas), K113 (Noble gas),
K116 (Water vapour), K117 (ammonia), K118 (Natural gas),
K119 (LPG), K121 (terpenes), K120 (ambient CO2)
• 8 comparisons in 2017-2019 – K137 (core KC, NO), K41.2017 (H2S),
– K74.2018 (NO2), K3.2018 (automotive gases), K10.2018 (BTEX)
– K26b.2019 (SO2), K68.2019 (ambient N2O)
– Pxxx (particle number/charge concentration), Pxxx (Particle mass con.)
• 3 KC, 5 RMO KC & SC in KCDB – K94 (DMS), BIPM.QM-K1 (ISCIII, DMDM)
– APMP 2, COOMET 3 2
Summary of 2015/2016
• Draft A KC reports
• 7 planed KCs (Repeat KCs)
• Approval of strategy document of track A KC
- CMC re-review for Cycle XVIII
• Other issues
- Task group on strategy of particle/black carbon
- Task group on ozone cross section
• Next meeting
3
Today’s report
4
Core KC: CCQM-K111 Propane in Nitrogen VSL
(draft A)
APMP.QM-K111 Draft A CERI
EURAMET.QM-K111 Draft A VSL
COOMET.QM-K111 Measurement VNIIM
SIM.QM-K111 Measurement INMETRO
Page
CCQM-K111
5
CERI INMETRO KRISS NIST NMISA NPL VNIIM VSL
-15
-10
-5
0
5
10
15
diffe
renc
e (µ
mol
/mol
)
Laboratory
CCQM-K111.1 NMISA, VSL draft A
CCQM-K90 Formaldehyde 2 µmol/mol in nitrogen BIPM
(Draft A) (to support air quality regulation)
NIST could not report a value, because of instrumental problem
• Cylinder still at NIST
• Draft A report written without any measurements on cylinder attributed to
NIST Subsequent comparison (K90.1)
Set of transfer standards value assigned by BIPM
CCQM-K112 Biogas VSL
(Draft A) Component Drift - min Drift - max Homogeneity
Methane -0.12% 0.04% 0.14%
Carbon dioxide -0.09% 0.12% 0.38%
Nitrogen -0.14% 0.01% 0.52%
Hydrogen -0.24% 0.13% 0.26%
Oxygen -1.54% -1.07% 9.21%
Ethane -0.15% 0.22% 0.28%
Propane -0.66% 0.34% 0.32%
A B C D E F G H J K A
-0.05
-0.04
-0.03
-0.02
-0.01
0.00
0.01
0.02
0.03
0.04
0.05
0.06 reference value
consensus value
diffe
ren
ce
(cm
ol/m
ol)
laboratory
Degrees-of-equivalence oxygen
KCRV: Reference values
CCQM-K119 LPG
(Draft A)
CCQM-K121 Terpenes NIST
Degrees of equivalence between lab value and KCRV for each monoterpene. Error bars represent expanded
uncertainties, U Diff = sqrt(uKCRV2 + uLab
2); k = 2. Dashed lines represent uncertainties of gravimetric values, k = 2.
CCQM-K116 10 µmol/mol H2O/N2 NPL June 2015: cylinders to participants, NIM
CCQM-K117 10-30 µmol/mol NH3 in nitrogen VSL Jan. 2017: cylinders to participants
CCQM-K118 Natural gas (with H2) BAM/VSL
Jan 2017: cylinders to participants
CCQM-K120a & K120b Ambient level CO2 BIPM Nov. 2016: prepared cylinders to BIPM
On-going KCs: Measurement in 2016
CCQM-K117 Ammonia 20 µmol/mol VSL
(Protocol ready, Analytical comparison)
• 50 L aluminium cylinders with UN-stamps are available
• Gas company can be filled with an ammonia in nitrogen
mixture at 150 bar with delivery time 5 months
• But the costs associated with the cylinders are approx. € 16000
• Participant will pay € 2000 for the comparison cylinder and
after finishing of KC measurement the participants will own
the Cyl.
Terminology: analytical & preparative
Analytical comparison: Coordinator Lab prepare comparison Cyl.
Distribute Cyl. to participants
Preparative comparison: Participant prepare comparison Cyl.
Transfer Cyl to coordinator
CCQM-K137 Core KC 30-70 µmol/mol NO/N2 BIPM June 2017: prepared 2 cylinders to BIPM
CCQM-K41.2017 10 µmol/mol H2S/N2 KRISS May 2017: cylinders to participants
CCQM-K74.2017 10 µmol/mol NO2/N2 BIPM March 2018: prepared cylinders to BIPM
CCQM-K3.2018 Automobile gases VSL April 2018: cylinders to participants
CCQM-K10.2018 BTEX NIST April 2018: prepared cylinders to NIST
CCQM-K26b.2019 300 nmol/mol SO2 NIST 2019: cylinders to participants
CCQM-K68.2019 ambient N2O BIPM 2019: prepared cylinders to BIPM
Planed KCs: Measurement during 2017-2019
Outline programme
Reference No. Description Coordinating
Laboratory
Expected
Start date Status
Rational for Key
Comparison
BIPM.QM-K1 KC (Ozone at ambient level) BIPM / 20
2007 -
ongoing on-going Atmospheric and air quality
CCQM-K90 KC (Formaldehyde in air) BIPM 2015 A Atmospheric and air quality
CCQM-K111 Core KC (Propane in Nitrogen) VSL 2014 A Core mixtures
CCQM-K112 KC (Biogas) VSL 2014 A Energy gases (Renewable)
CCQM-K113 KC (Noble Gases Mixture) KRISS 2014 A New emerging requirements
CCQM-K116 KC (Water vapour 10ppm) NPL 2015 M New emerging requirements
CCQM-K117 KC (NH3) VSL&NIST 2015 P Atmospheric and air quality
CCQM-K118 KC (Natural gas) VSL & BAM 2015 P Energy gases
CCQM-K119 KC (LPG) NPL 2015 A Energy gases
CCQM-K121 KC (Monoterpenes in Nitrogen) NIST 2015 A Atmospheric and air quality
CCQM-K120a KC (Ambient CO2, 380 to 480 μmol/mol) BIPM with NIST 2016 P Atmospheric and air quality
CCQM-K120b
Core KC (Ambient CO2, 380 to 800
μmol/mol) BIPM with NIST 2016 P Atmospheric and air quality
CCQM-K137
Core KC (NO in Nitrogen, 30-70
μmol/mol) BIPM 2017
Atmospheric and air quality
(Core mixtures)
CCQM-K41.2017 KC (H2S in Nitrogen, 10 μmol/mol) KRISS 2017
Atmospheric and air quality
(Non core mixture)
CCQM-PXX
PC(Micro-scale particles, number/charge
concentration) PTB/NPL 2017 New emerging requirements
CCQM-PXX
PC(Micro-scale particles, mass
concentration) VNIIM 2017 New emerging requirements
CCQM-K74.2018 KC (NO2 in Nitrogen, 10 μmol/mol) BIPM 2018 Atmospheric and air quality
CCQM-K3.2018 KC (Automotive gases) VSL 2018 Car emission gases
CCQM-K10,2018 BTEX/VOC NIST 2018 Air Quality
CCQM-K26b.2019 KC (300 nmol/mol SO2) NPL 2019 Analytical capability
CCQM-K68.2019 KC (Ambient N2O)
BIPM with
KRISS 2019 Atmospheric and air quality
CCQM-PXX
PC (Carbon/Oxygen isotope ratios in
CO2 ) BIPM/IAEA 2019 New emerging requirements
CCQM-KXX Core KC (SO2) NIST 2020 Core mixtures
CCQM-KXX KC (New energy gas) 2020 Energy gases
CCQM-KXX KC (Nano & micro-scale particles) 2020 New emerging requirements
CCQM-KXX KC (ppb level of water vapour) 2021 New emerging requirements
CCQM-PXX PC(HCl or HF in workplace air) 2021 Atmospheric and air quality
CCQM-KXX Core KC (CO) 2022 Core mixtures
Page
Approval of GAWG strategy document on the 19th April, 2016
GAWG strategy for comparisons and CMC claims
by Paul Brewer and Adriaan van der Veen
- Strategy for selecting comparison studies for the GAWG
work programme
- Strategy for CMC claims
- Implementation of the flexible scheme to support CMCs
- Guidance for CMC claims for purity analysis
- Guidance for linking RMO comparisons to track A key
comparisons
- Annex A: Example calculations for track A (K52, K53 and
K76) and track B (K82)
Page
CMC Re-review for cycle XVIII
Re-review items: Track A (flexible scheme) components
• Evidence based on track record from previous core comparisons • Optional - can continue using existing approach
GAWG Strategy Plan (2017-2027) The task team for revision of strategic plan of GAWG
JS Kim, Robert, Paul, Adriaan, Jerry, Hanspeter
Page
Task group on Particulate Comparison
• Members:
Liu Junji (NIM), Paul Quincy (NPL), Andreas Nowak
(PTB), Hanspeter Andres (METAS), Shankar G.
Aggarwal (NPLI) and Yuri Kustikov (VNIIM)
• Strategy development:
June 2015: kick-off at ETHZ particle conference
Sep. 2015: first draft available to circulate
• Comparison protocols:
Presented at GAWG meeting (April 2016)
PS sizing: a) 2.5 / 10 mm
b) 1 – 10 nm
Draft Roadmap
2016 2018 2020 202X
size
key/parallel PS Number &
charge concentration
10 nm
500 nm
2.5 mm 10 mm
PS mass
concentration
PS number
concentration PS BC
time
*PS = pilot study
28.07.2016 METAS 20
Coordination: PTB/NPL
Host: TROPOS (WMO WCC physical aerosol measurements)
Participants: PTB, NPL, METAS, NPLI, KRISS, VINITFRI,
NMIJ(?), NIM (?), LNE (?), BAM (?), TROPOS (if WEM agrees)
Timescale: Protocol: October 2016
comparison in first quarter 2017
Draft A: October 2017
Draft B: April 2018
Comparison on number / charge concentration Repeat of EURAMET 1224 (charge conc.),1282 (number conc.)
CCQM.Pxxx Particle Comparison in 2017
1993
Room-temperature ozone cross sections at 253.65 nm
0.9 %
Task Group on Ozone Cross Section
GAWG: Joseph Hodges (NIST), Joëlle Viallon (BIPM), Robert Wielgosz (BIPM),
Sangil Lee (KRISS), Paul Brewer (NPL), Jari Walden (FMI)
Other: Christof Janssen (Paris-Jussieu) and !!!
Gas phase titration
Page
Sources of Measurement Uncertainty & Bias Relative weighting of published data will be influenced by uncertainties in: sample conditions: purity & stability (O3 molar fraction), temperature, pressure transmittance measurement pathlength type of source (Hg lamp, continuum, laser) instability in irradiance of light source
spectral contribution from other Hg lines baseline stability & stray light detector non-linearity
Will need to assess appropriate combined uncertainties of literature data
23
• Progress report Core KCs (K111 series), Protocols for New KCs • Approval of ‘Strategy Document’ for flexible CMC
application • Task team for GAWG strategy document (2017-
2027) • Next GAWG Meeting (11-14 October 2016, IPQ) 11-12 GAWG meeting 13 Workshop on Scientific results 14 Workshop on Standards and Measurements for Clean Air • 2017 Fall meeting: October 2017, VSL
Summary
24
34th GAWG Meeting, 18th-19th Apr. 2016, BIPM
Acknowledgements All member participants, Coordinators of comparisons,
and Experts who provide presentations.