Synthesis and characterization of dibutyltetramethyldisilazane-bonded silica phases for reversed-phase high-performance liquid chromatography
摘要:
A new sllane, dl-n-butyltetramethyldisllazane (DBTMDS), has been synthesized. Sllanizations with DBTMDS of a narrow-pore and a wide-pore silica yielded relatively high concentrations of bonded n-butyl ligands, of 4.22 and 4.09-mu-mol/m2, respectively. The chromatographic properties of the n-butyl bonded phase (C4-NH), synthesized with DBTMDS, were compared with n-butyl bonded phases (C4-CL) synthesized with n-butyldimethylchlorosilane (BDMCS) and Vydac-C4 under the same chromatographic conditions. The adsorption of basic compounds including N,N-diethylaniline (N,N-DEA), dansylarginine (Dns-Arg), and (phenylthlo)hydantoin-arginine (PTH-Arg), as well as several polypeptides and small proteins including angiotensin I, angiotensin II, and lysozyme, was shown to be less for the C4-NH sorbents than for C4-CL and Vydac-C4 sorbents. While the S value for the basic protein lysozyme was significantly lower on the wide-pore C4-NH sorbent, the S and log K0 values for a range of selected proteins were comparable to those obtained with the Vydac-C4 sorbent. The tests of hydrolytic stability of the bonded phases showed significantly greater stability for the C4-NH sorbents than for the C4-CL sorbents under isocratic mobile-phase conditions of 10 % and 40 % acetonitrile with 0.1 % TFA.
A process for cleaning a wafer having an uneven pattern at its surface. The process includes at least the steps of: cleaning the wafer with a cleaning liquid; substituting the cleaning liquid retained in recessed portions of the wafer with a water-repellent liquid chemical after cleaning; and drying the wafer, wherein the cleaning liquid contains 80 mass % or greater of a solvent having a boiling point of 55 to 200° C., and wherein the water-repellent liquid chemical supplied in the substitution step has a temperature of not lower than 40° C. and lower than a boiling point of the water-repellent liquid chemical thereby imparting water repellency at least to surfaces of the recessed portions.
Disclosed is a liquid chemical for forming a water-repellent protecting film at least on a surface of a recessed portion of an uneven pattern at the time of cleaning a wafer having a finely uneven pattern at its surface and containing silicon at least a part of the uneven pattern. This liquid chemical contains a silicon compound A represented by the general formula: R
1
a
Si(H)
b
X
4-a-b
and an acid A, the acid A being at least one selected from the group consisting of trimethylsilyl trifluoroactate, trimethylsilyl trifluoromethanesulfonate, dimethylsilyl trifluoroactate, dimethylsilyl trifluoromethanesulfonate, butyldimethylsilyl trifluoroactate, butyldimethylsilyl trifluoromethanesulfonate, hexyldimethylsilyl trifluoroacetate, hexyldimethylsilyl trifluoromethanesulfonate, octyldimethylsilyl trifluoroactate, octyldimethylsilyl trifluoromethanesulfonate, decyldimethylsilyl trifluoroacetate and decyldimethylsilyl trifluoromethanesulfonate.
A process for cleaning a wafer having an uneven pattern at its surface. The process includes at least the steps of: cleaning the wafer with a cleaning liquid; substituting the cleaning liquid retained in recessed portions of the wafer with a water-repellent liquid chemical after cleaning; and drying the wafer, wherein the cleaning liquid contains 80 mass % or greater of a solvent having a boiling point of 55 to 200° C., and wherein the water-repellent liquid chemical supplied in the substitution step has a temperature of not lower than 40° C. and lower than a boiling point of the water-repellent liquid chemical thereby imparting water repellency at least to surfaces of the recessed portions.
Disclosed is a liquid chemical for forming a water-repellent protecting film at least on a surface of a recessed portion of an uneven pattern at the time of cleaning a wafer having a finely uneven pattern at its surface and containing silicon at least a part of the uneven pattern. This liquid chemical contains a silicon compound A represented by the general formula: R1aSi(H)bX4-a-b and an acid A, the acid A being at least one selected from the group consisting of trimethylsilyl trifluoroactate, trimethylsilyl trifluoromethanesulfonate, dimethylsilyl trifluoroactate, dimethylsilyl trifluoromethanesulfonate, butyldimethylsilyl trifluoroactate, butyldimethylsilyl trifluoromethanesulfonate, hexyldimethylsilyl trifluoroacetate, hexyldimethylsilyl trifluoromethanesulfonate, octyldimethylsilyl trifluoroactate, octyldimethylsilyl trifluoromethanesulfonate, decyldimethylsilyl trifluoroacetate and decyldimethylsilyl trifluoromethanesulfonate.