Relative elution volume

Nielson125 reports the synthesis of 7-((V-aIkylamino)- and T-(N,N-di-alkylamino)-l,3,5-triazaadamantanes by reductive alkylation of 94, which is obtained from 91 by an improved hydrogenation procedure (rhodium-charcoal catalyst, 25.5 psi). Paper chromatography54 and the Kovats indices and relative elution volumes of 1,3,5-triazaadamantane derivatives are measured.55 7-Amino-l,3,5-triazaadamantane is used as a vulcanization accelerator.127 7-(N,N-Dialkylamino)-l,3,5-triazaadamantanes are utilized as a new class of high-density fuel (DIADAM).128 Some 7-substituted 1,3,5-triazaadamantanes have bacteriostatic and fungistatic activity.129 7-Bromo-,... 

Fig. 1. Gel filtration chromatography, (a) Schematic illustration of gel filtration chromatography (b) elution diagram indicating the separation (c) a plot of relative elution volume versus the logarithm of molecular mass for known proteins, indicating how the molecular mass of an unknown can be read off when its relative elution volume is known.

Several derivatives obtained by reduction/acetylation of acidolysis monomers have been analyzed by high performance liquid chromatography (HPLC) (Kristersson and Lundquist unpubl. work 1983). The relative elution volumes for these compounds are listed in Table 6.1.1. Nonacetylated reduction products of acidolysis monomers have also been examined by HPLC (Kristersson and Lundquist unpubl. work 1983). From the results shown in Table 6.1.2, it is evident that good separation was achieved but, unfortunately, compounds 6a (threo form), 6b and 6c have very similar elution volumes. 

The relative elution volumes of the main peaks were 0.94 of Vo and 1.27 of Vo for two different electric potentials applied (100 and 150 mV, respectively). The relative elution volumes were inversely proportional to the relative velocities with respect to the average velocity of the carrier liquid and corresponded to the positions of the focused zones inside the channel. 

The molecular weight of the protein is determined by comparing its relative elution volume (Ve - Vc/Vg) to those of several standard molecules (Figure 5D). Ve is the solvent volume required for the elution of a solvent from the column. 

Both monomers and the micelles elute from the column, i.e. t less than t. The relative elution volume, Vj, Is given as ... 

The relative elution volume, v, is thus composed of two terras ... 

Pig 11. Plot of relative elution volume against reciprocal reduced concentration [48] (Redrawn with changes)... 

Liquids have relatively low compressibility compared with gases and, thus, the mobile phase velocity is sensibly constant throughout the column. As a consequence, elution volumes measured at the column exit can be used to obtain retention volume data and, unless extreme accuracy is required for special applications, there is no need for the retention volume to be corrected for pressure effects. 

The simplest mode of IGC is the infinite dilution mode , effected when the adsorbing species is present at very low concentration in a non-adsorbing carrier gas. Under such conditions, the adsorption may be assumed to be sub-monolayer, and if one assumes in addition that the surface is energetically homogeneous with respect to the adsorption (often an acceptable assumption for dispersion-force-only adsorbates), the isotherm will be linear (Henry s Law), i.e. the amount adsorbed will be linearly dependent on the partial saturation of the gas. The proportionality factor is the adsorption equilibrium constant, which is the ratio of the volume of gas adsorbed per unit area of solid to its relative saturation in the carrier. The quantity measured experimentally is the relative retention volume, Vn, for a gas sample injected into the column. It is the volume of carrier gas required to completely elute the sample, relative to the amount required to elute a non-adsorbing probe, i.e. 

Fig. 17. A schematic of the alkane line obtained by inverse gas chromatography (IGC) measurements. The relative retention volume of carrier gas required to elute a series of alkane probe gases is plotted against the molar area of the probe times the. square root of its surface tension. The slope of the plot is yielding the dispersion component of the surface energy of...

The most widely used molecular weight characterization method has been GPC, which separates compounds based on hydrodynamic volume. State-of-the-art GPC instruments are equipped with a concentration detector (e.g., differential refractometer, UV, and/or IR) in combination with viscosity or light scattering. A viscosity detector provides in-line solution viscosity data at each elution volume, which in combination with a concentration measurement can be converted to specific viscosity. Since the polymer concentration at each elution volume is quite dilute, the specific viscosity is considered a reasonable approximation for the dilute solution s intrinsic viscosity. The plot of log[r]]M versus elution volume (where [) ] is the intrinsic viscosity) provides a universal calibration curve from which absolute molecular weights of a variety of polymers can be obtained. Unfortunately, many reported analyses for phenolic oligomers and resins are simply based on polystyrene standards and only provide relative molecular weights instead of absolute numbers. 

Tsuji and Goetz24 developed a quantitative high performance liquid chromatographic method for separating and measuring erythromycins A, B, and C, their epimers and degradation products. This method uses a /iBondapak Ci 8 reverse column with acetonitrile-methanol-O.2m ammonium acetate-water (45 10 10 25) as solvent. The pH and composition of the mobile phase may be adjusted to optimize resolution and elution volume. The authors utilized the procedure on USP reference standard and report a relative standard deviation of 0.64%. 

The elution volume of a solute is determined mainly by its relative molecular mass and it has been shown that the elution volume is approximately a linear function of the logarithm of the relative molecular mass. It is possible to determine the relative molecular mass of a test molecule using a calibration curve prepared from the elution volumes of several reference substances of known relative molecular mass. This should be done using the same column and conditions (Figure 3.37) and in practice it may be possible to calibrate the column and separate the test substance at the same time by incorporating the reference compounds in the sample. Such a method is rapid and inexpensive and does not demand a highly purified sample, provided that there is a specific method for detecting the molecule in the eluate. 

Figure 3.37 Determination of relative molecular mass by gel permeation chromatography. A mixture of proteins (approximately 10 /ug of each) was separated on an UltroPak TSK SW column and the elution volume for each protein plotted against the logarithm of its relative molecular mass (RMM). 

Abstract A preconcentration method using Amberlite XAD-16 column for the enrichment of aluminum was proposed. The optimization process was carried out using fractional factorial design. The factors involved were pH, resin amount, reagent/metal mole ratio, elution volume and samphng flow rate. The absorbance was used as analytical response. Using the optimised experimental conditions, the proposed procedure allowed determination of aluminum with a detection limit (3o/s) of 6.1 ig L and a quantification limit (lOa/s) of 20.2 pg L, and a precision which was calculated as relative standard deviation (RSD) of 2.4% for aluminum concentration of 30 pg L . The preconcentration factor of 100 was obtained. These results demonstrated that this procedure could be applied for separation and preconcentration of aluminum in the presence of several matrix. 

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