[논문]Development of nitrogen and oxygen certified reference materials in 10 μmol/mol for the purity evaluation

Ahn, Byung Soo; Moon, Dong Min; Lee, Jin Bok; Kim, Jin Seog; Lee, Jin-Hong; Hong, Kiryong

doi:10.5806/ast.2020.33.2.68

Development of nitrogen and oxygen certified reference materials in 10 μmol/mol for the purity evaluation 원문보기

분석과학 = Analytical science & technology, v.33 no.2, 2020년, pp.68 - 75

Ahn, Byung Soo (Center for Gas Analysis, Korea Research Institute of Standards and Science) , Moon, Dong Min (Center for Gas Analysis, Korea Research Institute of Standards and Science) , Lee, Jin Bok (Center for Gas Analysis, Korea Research Institute of Standards and Science) , Kim, Jin Seog (Center for Gas Analysis, Korea Research Institute of Standards and Science) , Lee, Jin-Hong (Department of Environmental Engineering, Chungnam National University) , Hong, Kiryong (Center for Gas Analysis, Korea Research Institute of Standards and Science)

Abstract ▼ AI-Helper

We have developed 10 μmol/mol nitrogen and oxygen certified reference materials (CRMs) in helium, as a SI-traceable gas standard for a quantifying of impurities in pure gases for the first time in Korea. The standard gas mixtures of nitrogen and oxygen were prepared in 5000 μmol/mol and sequentially were diluted to 250 μmol/mol and 10 μmol/mol according to the gravimetric preparation. In each dilution step, two cylinders of CRMs were prepared. The verification of internal consistency among the prepared gas mixtures was performed by using GC-TCD. The amount fractions and those expanded uncertainties (k = 2) of nitrogen and oxygen in the standard gas mixtures were (10.12 ± 0.08) μmol/mol and (10.18 ± 0.08) μmol/mol for nitrogen, and (9.88 ± 0.06) μmol/mol and (9.94 ± 0.06) μmol/mol for oxygen, respectively. We have conducted a purity assessment of two commercial helium gases using developed CRMs. As the results of the purity assessment, nitrogen and oxygen were detected by (1.66 ± 0.03) μmol/mol and (0.31 ± 0.02) μmol/mol, respectively, as the impurities in one of the pure helium.

주제어

표/그림 (7)

그림 Fig. 1. Schematic diagram of workflow for the CRM preparation and dilution steps.
그림 Fig. 2. Schematic diagram of the modified GC-TCD system that lowered the detection limit.
표 Table 1. The experimental conditions of GC-TCD for analyzing the 10 μmol/mol CRM
그림 Fig. 3. The verification results for gravimetrically prepared CRMs.
그림 Fig. 4. Chromatograms of two commercial helium resulted from the purity assessment using 10 μmol/mol CRM.
$Table 2. Amount-of-substance fractions and those expanded uncertainties (k = 2) of gravimetrically prepared CRMs$ 표 Table 2. Amount-of-substance fractions and those expanded uncertainties (k = 2) of gravimetrically prepared CRMs
$Table 3. The amount fractions and those expanded uncertainties (k = 2) of N<sub>2</sub> and O<sub>2</sub> impurities in the commercial He gases$ 표 Table 3. The amount fractions and those expanded uncertainties (k = 2) of N₂ and O₂ impurities in the commercial He gases

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제안 방법

To minimize the influence of these fluctuations, the mass of the cylinder was comparatively weighed. An empty Al cylinder, which is nearly identical to the cylinder used for the preparation of CRM, was used as a tare cylinder, and the mass of the tare cylinder was measured while measuring the mass of the sample cylinders to correct the buoyancy effect. The tare cylinder (T) and the sample cylinders (S and S') were alternated in the sequence of S-T-S' in the weighing process.
The developed CRMs were prepared based on the gravimetric method,17 so-called “primary preparation method” to link the CRMs to the SI traceability.

대상 데이터

For the CRM preparation, high purity N₂(99.9999%), O₂(99.999 %), and He (99.9999 %) gases were used. Aluminum (Al) cylinders (Luxfer, UK) with an internal volume of 10.

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