The National Institute of Standards and Technology (NIST) recently began to develop standard mixtures of greenhouse gases as part of a broad program mandated by the 2009 United States Congress to support research in climate change. To this end, NIST developed suites of gravimetrically assigned primary standard mixtures (PSMs) comprising carbon dioxide (CO2), methane (CH4), and nitrous oxide (N2O) in a dry-natural air balance at ambient mole fraction levels. In parallel, the National Oceanic and Atmospheric Administration (NOAA) in Boulder, Colorado, charged 30 aluminum gas cylinders with northern hemisphere air at Niwot Ridge, Colorado. These mixtures, which constitute NIST Standard Reference Material (SRM) 1720 Northern Continental Air, were certified by NIST for ambient mole fractions of CO2, CH4, and N2O relative to NIST PSMs. NOAA-assigned values are also provided as information in support of the World Meteorological Organization (WMO) Global Atmosphere Watch (GAW) Program for CO2, CH4, and N2O, since NOAA serves as the WMO Central Calibration Laboratory (CCL) for CO2, CH4, and N2O. Relative expanded uncertainties at the 95% confidence interval are <±0.06% of the certified values for CO2 and N2O and <0.2% for CH4, which represents the smallest relative uncertainties specified to date for a gaseous SRM produced by NIST. Agreement between the NOAA (WMO/GAW) and NIST values based on their respective calibration standards suites is within 0.05%, 0.13%, and 0.06% for CO2, CH4, and N2O, respectively. This collaborative development effort also represents the first of its kind for a gaseous SRM developed by NIST.
The Gas Metrology Group at the National Institute of Standards and Technology was tasked, by a congressional climate change act, to support the atmospheric measurement community through standards development of key greenhouse gases. This paper discusses the development of a methane (CH(4)) primary standard gas mixture (PSM) suite to support CH(4) measurement needs over a large amount-of-substance fraction range 0.3-20,000 μmol mol(-1), but with emphasis at the atmospheric level 300-4000 nmol mol(-1). Thirty-six CH(4) in dry air PSMs were prepared in 5.9 L high-pressure aluminum cylinders with use of a time-tested gravimetric technique. Ultimately 14 of these 36 PSMs define a CH(4) standard suite covering the nominal ambient atmospheric range of 300-4000 nmol mol(-1). Starting materials of pure CH(4) and cylinders of dry air were exhaustively analyzed to determine the purity and air composition. Gas chromatography with flame-ionization detection (GC-FID) was used to determine a CH(4) response for each of the 14 PSMs where the reproducibility of average measurement ratios as a standard error was typically (0.04-0.26) %. An ISO 6134-compliant generalized least-squares regression (GenLine) program was used to analyze the consistency of the CH(4) suite. All 14 PSMs passed the u-test with residuals between the gravimetric and the GenLine solution values being between -0.74 and 1.31 nmol mol(-1); (0.00-0.16)% relative absolute. One of the 14 PSMs, FF4288 at 1836.16 ± 0.75 nmol mol(-1) (k = 1) amount-of-substance fraction, was sent to the Korea Research Institute of Standards and Science (KRISS), the Republic of Korea's National Metrology Institute, for comparison. The same PSM was subsequently sent to the National Oceanic and Atmospheric Administration (NOAA) for analysis to their standards. Results show agreement between KRISS-NIST of +0.13% relative (+2.3 nmol mol(-1)) and NOAA-NIST of -0.14% relative (-2.54 nmol mol(-1)).
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