DART 이온 소스 및 고분해능 질량분석방법에 의한 탄소계 나노물질의 성분 분석법
최원석·최재원†
K-water 수질분석연구센터

Development of Analyical Methods of Carbon Nanomaterials
by Direct Analysis in Real Time (DART) Ion Source
with High Resolution Full Scanning Mass Spectrometry
Wonseok Choi and Jaewon Choi†
Water Analysis & Research Center, K water, Daejeon 306-711, Korea
Received November 13, 2012/Revised November 27, 2012/Accepted December 6, 2012

Concerns on the production, use and occurences in the environment of nanomaterial are increasing. Fast
determination of nanomaterial from various environmental matrices are requiring to understand their fates in
water, soil and biological tissues. In this study, ambient ionization technique with mass spectrometry was used
as a fast identification tools for fullerenes C60, C72 C84 and single (SW), double (DW), multi (MW) wall carbon
nanotubes (CNTs). For this performance, direct analysis in real time (DART) with Orbitrap high resolution
mass spectrometer was applied. For DART, optimized condition for ionization temperature and time were set
at 400~500oC and 1 min. Resolution, mass scan range and accuracy of Orbitrap MS were operated at 50,000,
100~1,100 amu and 5 ppm, calculated parts per million unit of monoisotope, respectively. Standard fullerene
C60, C72 and C84 were successfully ionized by DART source at high temperature. Molecular and their isotopes
were detected with high mass accuracy for 0.55~1.77 ppm. Fullerenes were not found in sludge samples from
drinking water treatment plants. For CNTs, specific m/z ions were not differentiated among SW, DW and MWCNT
standards and 36 sludges. After background mass removal, major 60 m/z ions were used for statistical
analysis. Cluster between SW, DW, MW-CNT standard and sludges were separated in principal component
analysis (PCA). Further, scanning electron microscopy (SEM) was used to supplement the qualitative method
above. There was no similarities between CNT standard samples and sludges. This methodology suggesting
very fast and accurate ionization and identification method for carbon nano-materials. Further, this is the first
report of desorption ionization technique to carbon nanotube analysis for identification.

Key words: DART, Orbitrap MS, Fullerene, CNT, Nano material