Core-Shell Diamond as a Support for Solid-Phase Extraction and High-Performance Liquid Chromatography
We report the formation of core-shell diamond particles for solid phase extraction (SPE) and high performance liquid chromatography (HPLC) made by layer-by-layer (LbL) deposition. Their synthesis begins with the amine functionalization of microdiamond by its immersion in an aqueous solution of a primary amine-containing polymer (polyallylamine (PAAm)). The amine-terminated microdiamond is then immersed in an aqueous suspension of nanodiamond, which leads to adsorption of the nanodiamond. Alternating (self-limiting) immersions in the solutions of the amine-containing polymer and the suspension of nanodiamond are continued until the desired number of nanodiamond layers is formed around the microdiamond. Finally, the core-shell particles are cross-linked with 1,2,5,6-diepoxycyclooctane or reacted with 1,2-epoxyoctadecane. Layer-by-layer deposition of PAAm and nanodiamond is also studied on planar Si/SiO2 surfaces, which were characterized by SEM, Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA). Core-shell particles are characterized by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), environmental scanning electron microscopy (ESEM), and Brunauer Emmett Teller (BET) surface area and pore size measurements. Larger (ca. 50 μm) core-shell diamond particles have much higher surface areas, and analyte loading capacities in SPE than nonporous solid diamond particles. Smaller (ca. 3 μm), normal and reversed phase, core-shell diamond particles have been used for HPLC, with 36,300 plates per meter for mesitylene in a separation of benzene and alkyl benzenes on a C18 adsorbent, and 54,800 plates per meter for diazinon in a similar separation of two pesticides.
- Research Organization:
- Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Environmental Molecular Sciences Lab. (EMSL)
- Sponsoring Organization:
- USDOE
- DOE Contract Number:
- AC05-76RL01830
- OSTI ID:
- 982950
- Report Number(s):
- PNNL-SA-72528; ISSN 1520-6882; 34739; KP1704020; TRN: US1004332
- Journal Information:
- Analytical Chemistry, 82(11):4448-4456, Vol. 82, Issue 11; ISSN 0003-2700
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ADSORPTION
AMINES
AQUEOUS SOLUTIONS
BENZENE
DEPOSITION
DIAMONDS
HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY
MESITYLENE
NUCLEAR REACTION ANALYSIS
PESTICIDES
POLYMERS
RUTHERFORD BACKSCATTERING SPECTROSCOPY
SCANNING ELECTRON MICROSCOPY
SOLAR PROTONS
SPECTROSCOPY
SURFACE AREA
SYNTHESIS
Environmental Molecular Sciences Laboratory