Balanced density slurry, column

Slurry packing techniques are required for the preparation of efficient columns with rigid particles of less than 20 micrometers in diameter. The same general packing apparatus. Figure 4.8, can be used to pack columns by the balanced-density slurry, liquid slurry, or the viscous slurry techniques. Down-fill slurry packing is the method of choice for small bore columns and packed capillary columns. 

Because the halogenated hydrocarbons that have to be used for this are both toxic and expensive, the use of balanced density slurries for packing columns is declining. 

The two main methods of packing columns for HPLC are dry packing, which is suitable for particles of diameter > 30 jim, and balanced-density slurry packing which is best for small particles of diameter 5-30 jum. 

Columns consisting of particles of less than 30-50 jum in diameter are prepared most efAciently by slurry packing. Balanced-density slurry packing [11,12] is the most successful of such methods. In this technique, a supporting liquid is used which has the same density as that of the particles. This eliminates sedimentation problems. A typical balanced-density slurry-packing apparatus is shown in Fig.3.42. For the preparation of a... 

Chromatography. I. Packing of columns Balanced density slurry method was employed and the quality of packed columns was tested chromatographically in methylene chloride. Benzene was injected as testing solute. Columns which gave satisfactory results [l.e., symmetrical elution curve, relative band broadening of 50 ym at linear velocity of 5 mm/sec, and permeability better than 1.10 -9 cm 2] were used for further experiments. 

An HPLC (39) method was developed for determination of the drug and its metabolites in human and rat bile. A stainless-steel column (15 cm X 4.6 mm I.D.) packed with UChrosorb RP-8 (Pore size 5pm) or Nucleasil Ci8 (pore size 5pm) was used. The columns were packed by means of a balanced density slurry method specially developed for the ammonia elution system. Gradient elution was performed with water (0.005 M ammonia) to which methanol was added, according to the desired programme. The final elution was usually effected with 100% methanol. Flow rate was Iml/min. A wavelength of 235 nm was found suitable for the detection of drug and its metabolites. 

A necessary component of the balanced-density slurry solvent was tetra-bromoethane, which has a density higher than that of silica. However, it decomposes easily and its toxidty is a major drawback, espedally for commercial column production. Therefore alternatives were sou t quickly. In 1972, Kirkland (4) described a technique in which silica particles were suspended in an aqueous ammonium hydroxide solution, and in 1974 Asshauer and Haliisz (S) reported success with slurries based on high-viscosity solvents. 

All analytical HPLC columns with particles < 20 pm (usually 5 or 10 pm) are packed by the slurry technique [19], which can be further classified into the high-viscosity technique and the balanced-density technique. In the latter, the particles are suspended in a fluid that has a density similar to theirs, so particle segregation by sedimentation decreases. In both techniques, the suspending fluid must be chosen in such a way that particle dispersion is maintained without aggregation and particle agglomeration is avoided by proper selection of the polarity of the sluiTy [19], [24]. 

Balanced slurry packing a slurry of the solid support in a liquid with a density identical with that of the solid support is pumped into the column. As a result of the very stable slurry, a homogeneous dense column packing is then... 

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