Report on Co-production of CH 4 /air within ACRM framework
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1 Report on Co-production of CH 4 /air within ACRM framework 8 th APMP/TCQM Gas CRM workshop NMIJ/AIST, Tsukuba, 9~11 June 2010 By Hai Wu, NIM 1
2 Brief Introduction to ACRM ACRM Concept Asian Collaboration on CRM; Trademark Asian CRM; ** ERM: European RM IRMM, BAM, LGC provide highest quality and reliability Objective Establishing regional network for CRM; Supplying CRM of highest quality and reliability; Reducing expenses on new CRM production; Cooperation on the CRM in MRA; 2
3 Collaboration schemes within ACRM Co-characterization The property value should be derived by combining the measurement results from each partner Co-validation The property value is assigned by one NMi, and is also validated by another one or two NMi CH 4 /air co-production: ONLY example The ACRM is prepared and value-assigned by all partners. Each partner equally contributes to production of CRM. Co-production 3
4 Protocol - Project background Co-production of CRM of CH 4 /air was suggested by Dr. Jinseog Kim (KRISS), Jun. 2006; Methane is one of the key GHGs; WMO recommends to establish national standard system; Co-production of CH 4 /air can be cost-effective; Objective: co-produced CH 4 /air CRM can meet WMO requirements(~1.8ppm±0.002ppm, k=2); Discussed and approved by NMIJ, KRISS, NIM, 6th meeting of ACRM, Mar. 2007; 4
5 Protocol Coproduction Scheme Source gases (CH 4, Ar, N 2, O 2 ) By NMIJ & KRISS CRM candidate (air sample), By NIM PRM preparation By KRISS Calibration of air sample By NIM, NMIJ, and KRISS CRM of CH 4 /air ~1.8ppm, uncertainty: 0.002ppm(k=2) 5
6 Protocol Traceability of co-produced CRM mass:kg Pure material:1 IUPAC MW:g/mol Publicly accepted m j x i,j M i Standard procedure (ISO 6142) Gas PRM Purity analysis, and Subtraction method Gas CRM ISO
7 Protocol - QA/QC Human resources Qualification, Experience, Training and retraining, Knowledge Management system Conform to ISO & ISO G34, by Peer Review Pure gases above 5N, impurities checked Gravimetric preparation system validated by CCQM-P41 results Sample cylinder A6061 Al cylinder, form LUXFER, WMO recommended RM candidate preparation WMO recommended procedure, from NOAA website Certification method High precision, GC-FID is recommended Stability test: short-term and long-term 7
8 Timetable Jul 2006, proposal Mar 2007, protocol, approved Feb 2008, NIM ordered cylinder from USA Sep 2008, KRISS started PRM preparation Dec 2008, LUXFER cylinder arrived at NIM Sep 2009, RM candidate prepared by CAWAS/NIM Nov 2009, PRM distributed to each partner Dec 2009, NIM sent RM candidate to partners Dec 2009, certification of RM candidate by NIM Jul 2010, KRISS & NMIJ receive RM candidate and certify it, respectively Dec 2011, long-term stability test by each partners 8
9 Issues should be concerned Compressed gas cylinders relating issues As a special good, it takes time to do Custom Clearance in case of importing and exporting cylinders; As a pressure container, it should be officially admitted by the country; As a dangerous good, especially for large cylinder, commodity inspection may be a problem before its transportation; 9
10 Methane purity analysis, NMIJ Impurities Methods Remarks N 2 GC/PID MOLSIEVE 5A PLOT (30 m x 0.53 mm x 50 mm) O 2 GC/PID MOLSIEVE 5A PLOT (30 m x 0.53 mm x 50 mm) Ar GC/PID MOLSIEVE 5A PLOT (30 m x 0.53 mm x 50 mm) H 2 GC/PID MOLSIEVE 5A PLOT (30 m x 0.53 mm x 50 mm) CO GC/PID MOLSIEVE 5A PLOT (30 m x 0.53 mm x 50 mm) CO 2 GC/PID Carboxen 1006 PLOT (30m x 0.53 mm) C 2 H 4 - C 2 H 6 GC/FID Al 2 O 3 /KCl PLOT (50 m x 0.53 mm) C 3 H 8 ~ - H 2 O Dew pt Panametrics capacitance hygrometer 10
11 Methane purity data, NMIJ Impurities / µmol/mol Tokyo gas chemical Xi Type u(xi) remarks N 2 < normal 0.04 O 2 < rectangular 0.12 Ar < rectangular 0.07 ND H 2 < rectangular 0.10 ND CO < rectangular 0.29 ND CO 2 < rectangular 0.22 ND C 2 H 4 <0.1 C 2 H 6 < rectangular 0.32 ND C 3 H 8 ~ <0.1 H 2 O < rectangular 0.31 DP<-80 Purities / % > ( ) 11
12 Nitrogen purity data, KRISS component Analysis (10-6 mol/mol) Distribution Mole fraction (10-6 mol/mol) Uncertainty (10-6 mol/mol) H2 <0.05 Rectangular O Normal CO <0.1 Rectangular CO2 <0.01 Rectangular CH Normal Ar <0.1 Rectangular H2O 1.2 Normal N
13 Oxygen purity data, KRISS component Analysis (10-6 mol/mol) Distribution Mole fraction (10-6 mol/mol) Uncertainty (10-6 mol/mol) H2 <0.05 Rectangular Ar <1 Rectangular N2 2.8 Normal CO2 <0.01 Rectangular CH4 <0.003 Rectangular CO <0.1 Rectangular H2O 1.1 Normal THC <0.1 Rectangular O
14 Argon purity data, KRISS component Analysis (10-6 mol/mol) Distribution Mole fraction (10-6 mol/mol) Uncertainty (10-6 mol/mol) H2 <0.05 Rectangular O Normal N2 1.6 Normal CO2 <0.01 Rectangular CH4 <0.003 Rectangular CO <0.1 Rectangular H2O 1.5 Normal THC <0.1 Rectangular Ar
15 Stepwise dilution, KRISS Pure CH 4 Pure Ar Pure O 2 Pure N 2 10% CH 4 /N 2 0.7% CH 4 /N % CH 4 /N % CH 4 /N % CH % Ar % O 2 + N 2 balance ME5512#, c = µmol/mol, U = µmol/mol (k=2) PRM 15
16 RM candidate preparation, NIM/CAWAS According to WMO recommendations: Preparation and stability of standard reference air : A6061 LUXFER Al cylinder, 30Liter Cylinder was cleaned: filling ambient air up to 200PSI, and then vented it repeating for more than 3 times Filling natural air sample by pumping system Adjusting the trace gas levels Inner pressure of 2100PSI Moisture was checked and below 5ppm 16
17 Air mixtures filling system 17
18 Short-term stability of RM candidates, NIM A A CH 4 conc./ppb 11/4/09 11/5/09 11/6/09 11/7/09 11/8/09 11/9/09 11/10/09 11/11/09 11/12/09 Testing Date
19 Certifying RM candidate at NIM Repeat. No. A A Average RSD 0.14% 0.15% Instrumental: Agilent 6890N (FID) Column: HP-PLOT Al2O3 S, 60m 0.53mm 15µm Oven: 50 Spl Loop: 1mL Spl Flow Rate: 100mL/min 19
20 Uncertainty Evaluation Mathematical Model c. CRM = PRM PRM(ACRM): f rep CH4/air, µmol/mol, U=0.0010µmol/mol (k=2), U rel =0.054% Repeatability factor: c U rel (f)=0.15%/sqrt(14)=0.040% U CRM =0.068%*1.8521=0.0013µmol/mol 20
21 Summary Project is almost finished Objective: CH 4 /air, (~1.8ppm±0.002ppm, k=2); Preliminary result: CH 4 /air, (~1.8ppm±0.0013ppm, k=2); Long-term stability test, by Dec 2011? It takes about 5 years to achieve the objective. However, it explored an effective way to co-produce ACRM presently; By the project, technology, knowledge, CRM etc. are shared by all the partners. 21
22 Summary In case of inter-nmi s collaboration on cylinderpackaged gas CRM, the cylinder related issues should be well planned Admitted by the destination country, which should be clear in the protocol; Commodity inspection on the cylinder before exporting, which is requested by the carrier; Co-production scheme could be cost-effective for batch CRM production. 22
23 Thank you for your attention! 23
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