# Presentation: 438680

## Gas Metrology and Classical Methods

- Franklin R. Guenther
- NIST
- 100 Bureau Drive
- Gaithersburg MD 20899-8393

## NIST Gas NTRM Meeting

**Agenda:**
- 	1:30	Welcome
- 	1:45	Summarizing the first 8 years of the gas NTRM Program (Bill Dorko)
- 	2:30	Proposal for new gas NTRM certification program
- 	3:00	Discussion
- 	3:45	ISO TC158 Discussion
- 	4:30	Adjourn

## NIST Gas SRM Status

**NIST Gas SRM Status**

## NIST Gas SRM Status

**NIST Gas SRM Status**

## Gas Standards Survey

## CCQM Intercomparisons

- BTX – ongoing
- Ethanol
- CO,CO2, Propane
- Future
- Global Warming
- Low Conc NO, SO2
- Ozone
- Others?

## Group Structure

- Classical Methods
- 4 Scientists
- STRS Support – 30%
- SRM support – 60 %

- Gas Metrology
- 7 Scientists
- 4 Technicians
- STRS Support – 27 %
- OA Support – 6 %
- Standards Activities
- SRM – 20 %
- Customer – 36 %
- Ozone Program Added in 1999

## International Activities

- Classical Methods
- CCQM
- pH, Conductivity, Purity assessment
- SIM
- pH Intercomparison
- Course
- Bilateral
- Conductivity – DFM, OMH

- Gas Metrology
- CCQM
- BTX Intercomparison
- SIM
- Auto Exhaust Intercomparison
- Course
- Bilateral
- NMi – Inorganic Gas
- NPL – Organic, IR DB

## Traceability

- Industry Requirements
- To a National Standard
- Global Economy requires global traceability
- European Directive for health monitors – just the beginning
- Specialty Gas Industry – 3 to 4 global companies

## Gas NTRM Program

- SGC Produces NTRM
- SGC Analyzes Batch
- NIST Reviews data, selects cylinders
- NIST analyzes selected cylinders
- NIST certifies batch using NIST/SGC data
- SGC retains NTRM batch for use/sale

## Program Results

- 8 years experience with program
- Steady growth to $500K annually
- Approx 80 batches
- 2500 -  3000 cylinders
- 125000 – 150000 traceable standards
- EPA Protocol Gas Standards
- Accepted by EPA
- Global Community
- Acceptance, copied

## NTRM - Future

- Effectively replace most gas SRMs
- Promote NTRM sale to end users
- Remove individual batch certification by NIST

## New Gas NTRM Program

- SGC is certified to produce gas NTRMs
- Must have successful history of NTRM production
- Accredited to ISO 17025
- Analytical systems are certified for NTRM certification
- Using *p*-NTRM certified at NIST

## New Gas NTRM Program

- SGC sends candidate *p*-NTRM to NIST
- Concentration suite to cover range
- NIST certifies *p*-NTRM against PSMs
- Best uncertainty possible
- Better than available SRMs
- Certified for 1 year only

## New Gas NTRM Program

- SGC uses *p*-NTRM to certify NTRM
- Within range of suite, using approved analytical system
- Certified value and uncertainty generated by NIST software
- Certificate generated by software
- Data sent to NIST quarterly

## New Gas NTRM Program

- NIST Quality Assurance
- Through *p*-NTRM and Software
- May call for NTRM periodically
- Will send challenge cylinder to SGC
- SGC certifies and send certificate to NIST
- Certification must agree with NIST analysis
- Within stated uncertainty

## New Gas NTRM Program

- Elimination of most gas SRMs
- Some always necessary
- NTRM Production not limited
*p*-NTRM available to SIM countries
- International Acceptance
- NIST able to turn to new gas standards

## ISO TC 158: Analysis of Gases

- No active US Participation
- Participating Members (Voting):

| Belgium | Portugal |
| --- | --- |
| Czech Republic | Russian Federation |
| Germany | Spain |
| Hungary | Sweden |
| Italy | Ukraine |
| Netherlands (S) | United Kingdom |
| Poland |  |

## Working Groups

- Terminology
- Quality assurance of gas analysis
- Gravimetric methods
- Comparison methods and certificates
- Static and dynamic volumetric methods
- Quantities of composition

## Standards	

- FDIS 6141: Requirements on certificates for gases and gas mixtures
- DIS 6142: Preparation of calibration gas mixtures – Gravimetric method
- DIS 6143.2: Determination of the composition of calibration gas mixtures – comparison methods
- DIS 6144.2: Preparation of calibration gas mixtures – static volumetric methods
- CD 6145-1: Preparation of calibration gas mixtures – Dynamic volumetric methods – methods of calibration

## Standards

- CD 6145-2: Preparation of calibration gas mixtures – Dynamic volumetric methods – Volumetric pumps
- 6145-3: Preparation of calibration gas mixtures – Dynamic volumetric methods – periodic injections into a flowing gas stream
- 6145-4: Preparation of calibration gas mixtures – Dynamic volumetric methods – continuous injection method
- 6145-5.2: Preparation of calibration gas mixtures – Dynamic volumetric methods – Capillary calibration devices
-  6145-6: Preparation of calibration gas mixtures – Dynamic volumetric methods – Critical orifices

## Standards

- 6145-7: Preparation of calibration gas mixtures – Dynamic volumetric methods – Thermal mass flow controllers
- 6145-8: Preparation of calibration gas mixtures – Dynamic volumetric methods – Diffusion
- 6145-9: Preparation of calibration gas mixtures – Dynamic volumetric methods – Saturation methods
- 6145-10: Preparation of calibration gas mixtures – Dynamic volumetric methods – Permeation methods
- 7504: Vocabulary

## Standards	

- 14166: Pure gases – Requirements for presentation of the results of gas purity analysis
- 14167: General quality assurance aspects in the use and preparation of reference gas mixtures – guidlines
- 14912: Quantities of composition
- 15796: Detection and correction of analytical bias
- 16664: Handling of calibration gases and gas mixtures - guidelines

## U.S. Participation

- ANSI
- Requires formation of Technical Activity Group (TAG)
- Freely open to all who wish to participate
- Reports to ANSI
- Requires yearly financial support to ANSI
- $3155 for TAG
- $490 per Working Group
- Must be accredited by ANSI

## Possible TAG Secretariat

- ASTM through D22
- Will they take on another ISO TG?
- NIST
- Is this a NIST Role??
- Requires support from?
- Others?