Ion exchange column

The speciation scheme of Batley and Florence requires eight measurements on four samples. After removing insoluble particulates by filtration, the solution is analyzed for the concentration of anodic stripping voltammetry (ASV) labile metal and the total concentration of metal. A portion of the filtered solution is passed through an ion-exchange column, and the concentrations of ASV metal and total metal are determined. A second portion of the filtered solution is irradiated with UV light, and the concentrations of ASV metal... 

Ion-exchange columns can be substituted into the general HPLC instrument shown in Eigure 12.26. The most common detector measures the conductivity of the mobile phase as it elutes from the column. The high concentration of electrolyte in the mobile phase is a problem, however, because the mobile-phase ions dominate the conductivity, for example, if a dilute solution of HCl is used as the mobile phase, the presence of large concentrations of H3O+ and Ck produces a background conductivity that may prevent the detection of analytes eluting from the column. 

The total stationary-phase volume required to process a given feed stream is proportional to the inlet concentration and volume of the feed. For example, for a typical inlet concentration of protein of 10 g/L, in a 100 L volume of feed, a column volume of at least 100 L is needed for size-exclusion chromatography. In comparison, an ion-exchange column having an adsorption capacity of 50 g/L would only require 20 L of column volume for the same feed. 

Fluorozirconate Crystallization. Repeated dissolution and fractional crystallization of potassium hexafluorozirconate was the method first used to separate hafnium and zirconium (15), potassium fluorohafnate solubility being higher. This process is used in the Prinieprovsky Chemical Plant in Dnieprodzerzhinsk, Ukraine, to produce hafnium-free zirconium. Hafnium-enriched (about 6%) zirconium hydrous oxide is precipitated from the first-stage mother Hquors, and redissolved in acid to feed ion-exchange columns to obtain pure hafnium (10). 

The degree of swelling and shrinking is important for design of ion-exchange columns, especiaUy for the location of the distributors used to disperse incoming fluids, and coUect outgoing ones, evenly over the cross-sectional area of the resin bed. Once placed, these distributors are not adjustable. The upper distributor should be above (the lower one below) the resin bed, even in the bed s swoUen form. 

Fig. 5. Fermentative production of amino acids (140). A, pure culture B, inoculation C, boiler D, air compressor E, air filter F, seed tank G, ammonia water for pH control H, fermenter I, sterilizer , culture media K, preparation tank L, centrifugal separator M, ion-exchange column N, crystallizing...

Leucrose, 6-0-(a-D-glucopyranosyl)-P-D-fmctopyranose [7158-70-5] is synthesized from sucrose usiag a dextranase enzyme from l euconostoc mesenteriodes and a small proportion of fmctose (2%). Pfeifer Langen of Germany have developed a production process for leucrose that iavolves extraction of the enzyme, treatment with 65% aqueous solution of sucrose and fmctose (1 2 wt/wt) at 25°C, separation of the product from fmctose by ion-exchange column chromatography, and crystallization. The product has not yet been launched on the market as of this writing (1996). 

A readily accessible carborane is nido-1 -(]5 i])- l- 1( 12 [I d-5], a 2witterionic species formally derived from [CB2qH23] by replacement of a by NH3. It has been shown (124) that this monocarbaborane can be obtained in excellent yield by treatment of B2QH24 with CN followed by passage through an acidic ion-exchange column (eq. 61). 

Tetramethylammonium hydroxide (5H2O) [10424-65-4 (5H2O), 75-59-2 (aq soln) ] M 181.2, m 63°, 65-68°. Freed from chloride ions by passage through an ion-exchange column (Amberlite IRA-400, prepared in its OH" form by passing 2M NaOH until the effluent was free from chloride ions, then washed with distilled H2O until neutral). A modification, to obtain carbonate-free hydroxide, uses the method of Davies and Nancollas [Nature 165 237 1950]. 

Freeboard The space provided above the resin bed in an ion-exchange column to allow for expansion of the bed during backwashing. 

Dionex Corporation - Manufacturers of liquid chromatography systems (IC and HPLC), chromatography software data systems, reversed-phase and ion-exchange columns, and accelerated solvent extraction systems... http //www.dionex.com. 

In spite of Such limitations, some examples can be found in literature. For example, a reversed-phase Cjg column has also been coupled to a weak ion-exchange column to determine gluphosinate, glyphosate and aminomethylphosphonic acid (AMPA) in environmental water (28). This method will be described further below. 

Finally,Captopril is produced. Thethioester (0.85g) isdissolved in5.5N methanolicammonia and the solution is kept at room temperature for 2 hours. The solvent is removed in vacuo and the residue Is dissolved in water, applied to an ion exchange column on the H cycle (Dowex 50, analytical grade) and eluted with water. The fractions that give positive thiol reaction are pooled and freeze dried. The residue Is crystallized from ethyl acetate-hexane, yield 0.3 g. The 1 -(3-mercapto-2-D-methylpropanoyl)-L-proline has a melting point of 103°C to 104°C. 

If the ion exchange column is loaded with several ions of similar charge, B, C, etc., elution curves may be obtained for each ion by the use of appropriate eluants. If the elution curves are sufficiently far apart, as in Fig. 7.2, a quantitative separation is possible only an incomplete separation is obtained if the elution curves overlap. Ideally the curves should approach a Gaussian (normal) distribution (Section 4.9) and excessive departure from this distribution may indicate faulty technique and/or column operating conditions. 

Ion exchange column. Prepare the Chelex-100 resin (100- 500 mesh) by digesting it with excess (about 2-3 bed-volumes) of 2M nitric acid at room temperature. Repeat this process twice and then transfer sufficient resin to fill a 1.0 cm diameter column to a depth of 8 cm. Wash the resin column with several bed-volumes of de-ionised water. 

Interfering cations, except aluminium and zirconium, can be removed by passage through an ion exchange column. In the presence of interfering anions and also aluminium and zirconium, fluoride may be separated as hydrofluorosilicic acid by distilling with dilute perchloric acid at 135 °C (temperature maintained by the addition of water) in the presence of a few glass beads. 

A very simple and elegant alternative to the use of ion-exchange columns or extraction to separate the mixture of D-amino add amide and the L-amino add has been elaborated. Addition of one equivalent of benzaldehyde (with respect to die D-amino add amide) to the enzymic hydrolysate results in the formation of a Schiff base with die D-amino add amide, which is insoluble in water and, therefore, can be easily separated. Add hydrolysis (H2SQ4, HX, HNO3, etc.) results in the formation of die D-amino add (without racemizadon). Alternatively the D-amino add amide can be hydrolysed by cell-preparations of Rhodococcus erythropolis. This biocatalyst lacks stereoselectivity. This option is very useful for amino adds which are highly soluble in die neutralised reaction mixture obtained after acid hydrolysis of the amide. 

However, the products are separated using ion-exchange columns and the starting material is a derivative rattier than a precursor of the racemic amino add, thus making the total process drcuitous since it involves several chemical steps in addition to die enzymatic resolution step. Furthermore, racemisation of the unwanted isomer is not easily accomplished. 

Workup (a) The product is isolated by passage through an ion exchange column (Dowcx AG1-X8, HCOf 100 mL) and consecutive elution with 200 mM triethylammonium bicarbonate solution. After ion exchange... 

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