Molecular sieve columns

The in vitro hydrogenase activity was determined by using a gas chromatograph (Hewlett Packard 5890 A Series II, column molecular Sieve 5 A, Mesh 60/80). As described before [Happe and Naber, 1993], methylviologen reduced by sodium dithionite was used as electron donor. One unit is defined as the amount of hydrogenase evolving 1 pmol Hi-min1 at 25°C. 

GC column molecular sieve 5A, 13X Chromosorb 102 (80/100 mesh), Carboxen 1004, Haye Sep Q, Carbosieve, Carbosphere, silica gel, activated alumina, or any other equivalent material. Fused silica nonpolar capillary column may be used for low sample volume. 

Specificity is the most important requirement in gas analysis. Techniques dependent on the physical properties of the gas molecules, such as thermal conductivity, density, viscosity, and sound velocity, generally have insufficient specificity to differentiate a single gas in a mixture of gases, and therefore must incorporate in the procedure some type of preliminary separation. Vapor phase fractionation (gas chromatography) is an example of a popular analytical technique based upon a physical property (thermal conductivity) of the gas that requires preliminary separation of the gases by means of special columns (molecular sieve, silica gel, etc.). 

Gel permeation chromatography, exclusion chromatography. gel filtration chromatography. A technique for separating the components of a mixture according to molecular volume differences. A porous solid phase (a polymer, molecular sieve) is used which can physically entrap small molecules in the pores whilst large molecules pass down the column more rapidly. A solvent pressure up to 1000 psi may be used. 

This type of analysis requires several chromatographic columns and detectors. Hydrocarbons are measured with the aid of a flame ionization detector FID, while the other gases are analyzed using a katharometer. A large number of combinations of columns is possible considering the commutations between columns and, potentially, backflushing of the carrier gas. As an example, the hydrocarbons can be separated by a column packed with silicone or alumina while O2, N2 and CO will require a molecular sieve column. H2S is a special case because this gas is fixed irreversibly on a number of chromatographic supports. Its separation can be achieved on certain kinds of supports such as Porapak which are styrene-divinylbenzene copolymers. This type of phase is also used to analyze CO2 and water. 

Fig. 16. Plots showing (a) variation of (c F/2)J. / ) with 1 for O2 (left plot, X, 0.84- 0.72 mm = 20-25 mesh Q 0.42-0.29 mm = 40-50 mesh) and N2 (right plot, on 3.2-mm pellets) in Bergbau-Forschung carbon molecular sieve and (b) variation of HETP with Hquid velocity (interstitial) for fmctose (soHd symbols), and glucose (open symbols) in a column packed with KX 2eoHte crystals. From refs. 22 and 23.

Sulfur hexafluoride may be analyzed chromatographicaHy using a molecular sieve or a Porapak QS column. Using an electron-capture detector, a sensitivity of 10 to lO " ppb is possible (51—53). 

The greater preference of molecular sieves for combining with water molecules explains why this material can be used for drying ethanol and why molecular sieves are probably the most universally useful and efficient drying agents. Percolation of ethanol with an initial water content of 0.5% through a 144 cm long column of type 4A molecular sieves reduced the water content to lOppm. Similar results have been obtained with pyridine. 

Rapid purification Pass through a column of basic alumina (Grade 1, lOg/mL of CHCI3), and either dry by standing over 4A molecular sieves, or alternatively, distil from P2O5 (3% w/v). Use immediately. 

Cyclobutanone [1191-95-3] M 70.1, b 96-97 , d 0.931, n 1.4189. Treated with dilute aqueous KMn04, dried with molecular sieves and fractionally distd. Purified via the semicarbazone, then regenerated, dried with CaS04, and distd in a spinning-band column. Alternatively, purified by preparative gas chromatography using a Carbowax 20-M column at 80°. (This treatment removes acetone). 

MgS04 or NaOH and distd under vacuum. Further dried by reaction with sodium under nitrogen, refluxed for several hours and distd. The distillate was then passed through a column of Linde type 4A molecular sieves and finally distd under nitrogen, from more molecular sieves. Fractionally distd. 

Formamide (specific conductance 2 x 10 ohnr cnr ) of low water content was dried by passage through a column of 3A molecular sieves, then deionized by treatment with a mixed-bed ion-exchange resin loaded with H" " and HCONH" ions (using sodium formamide in formamide)[Notley and Spiro J Chem Soc (B) 362 1966. ... 

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