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May 24, 2012 - Anal. Chem. , 1977, 49 (12), pp 1006A–1006A. DOI: 10.1021/ac50020a728. Publication Date: October 1977. ACS Legacy Archive...
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1006 A · ANALYTICAL CHEMISTRY, VOL. 49, NO. 12, OCTOBER 1977

used to bond the stationary phase. For example, Locke et al. (10) reported the use of Grignard reagents to attach the stationary phases to the solid sup­ port. Gilpin and his coworkers (11) re­ ported an in situ bonding procedure. Unger and his group (8) recently re­ ported the incorporation of the bond­ ed phases in the silica gel matrix, a technique they termed "bulk modifi­ cation". This procedure is a promising one, since the amount of bonded phase per surface area of the support can be quite high. Most commercially available bond­ ed phases are prepared with either bior trifunctional silanes. Typically, these phases are treated further with chlorotrimethylsilane to remove resid­ ual hydroxyl groups. Presently, some manufacturers are beginning to pre­ pare phases from monofunctional silanes. A great variety of phases can be bonded to the support or synthesized on the support once a suitable starting material is bonded to it. The latter ap­ proach was described by Novotny (12). However, in practice, the most commonly used bonded phases in liq­ uid chromatography are: amine, —(CH 2 )„NH 2 ; nitrile,—(CH 2 )„CN; phenyl, —(CH 2 ) n C 6 H 5 ; octadecyl, —(CH 2 )i 7 CH 3 and various ion ex­ changers; more recently, shorter alkane chains were introduced. The most commonly used bonded phases in gas chromatography are various carbowaxes, alkanes, and polymeric organosilicones prepared from the re­ action of di- and trichlorosilanes. Calculation of Surface Coverages The amount of the stationary phase bonded to the support is an important parameter frequently needed to com­ pare column performances. This quantity can be reported in several ways. a) From the results of elemental analysis, the weight/weight percent of carbon is reported. If N, CI, etc., are part of the bonded phase, their weight/weight percent should also be given. Typical values for percent car­ bon on microparticulate silica gel hav­ ing a surface area of 300-350 m2/g are about 3-4% for a methylsilane and about 20% for octadecylsilane. It is our opinion that reporting the total per­ cent carbon content is the least desir­ able method of characterizing the bonded phase. b) By use of the elemental analysis results, the surface coverage can be re­ ported in terms of weight of bonded phase per unit surface area of the sup­ port. Along the same lines, Unger et al. (8) recommended that surface cov­ erages be reported in terms of the moles of bonded phase per specific surface area. Typical values for