Molecular sieves analysis

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. 

The separation and analysis of 1-propanol are straightforward. Gas chromatography is the principal method employed. Other iastmmental techniques, eg, nmr, ir, and classical organic quaHtative analysis, are useful. Molecular sieves (qv) have been used to separate 1-propanol from ethanol and methanol. Commercial purification is accompHshed by distillation (qv). 

The human factors audit was part of a hazard analysis which was used to recommend the degree of automation required in blowdown situations. The results of the human factors audit were mainly in terms of major errors which could affect blowdown success likelihood, and causal factors such as procedures, training, control room design, team communications, and aspects of hardware equipment. The major emphasis of the study was on improving the human interaction with the blowdown system, whether manual or automatic. Two specific platform scenarios were investigated. One was a significant gas release in the molecular sieve module (MSM) on a relatively new platform, and the other a release in the separator module (SM) on an older generation platform. 

A five-column configuration of Such an analyser system is depicted in Figure 14.6. The first event in the process is the analysis of Hj by injection of the contents of sample loop 2 (SL2) onto column 5 (a packed molecular sieve column). Hydrogen is separated from the other compounds and detected by TCD 2, where nitrogen is used as a carrier gas. The next event is the injection of the contents of sample loop 1 (SLl), which is in series with SL2, onto column 1. After the separation of compounds up to and including C5, and backflushing the contents of column 1, all compounds above C5 (Q+) are detected by TCDl. The fraction up to and including C5 is directed to column 2, where air, CO, COj, Cj, and 2= (ethene) are separated from... 

The schematic diagram of the experimental setup is shown in Fig. 2 and the experimental conditions are shown in Table 2. Each gas was controlled its flow rate by a mass flow controller and supplied to the module at a pressure sli tly higher than the atmospheric pressure. Absorbent solution was suppUed to the module by a circulation pump. A small amount of absorbent solution, which did not permeate the membrane, overflowed and then it was introduced to the upper part of the permeate side. Permeation and returning liquid fell down to the reservoir and it was recycled to the feed side. The dry gas through condenser was discharged from the vacuum pump, and its flow rate was measured by a digital soap-film flow meter. The gas composition was determined by a gas chromatograph (Yanaco, GC-2800, column Porapak Q for CO2 and (N2+O2) analysis, and molecular sieve 5A for N2 and O2 analysis). The performance of the module was calculated by the same procedure reported in our previous paper [1]. 

The recycle reactor is shown schematically in Figure 1. It consists of a catalytic or electrocatalytic reactor unit with a bypass loop, a recycle pump and a molecular sieve trap unit. The latter comprises one or two packed bed columns in parallel each containing 2-10 g of Linde 5A molecular sieve pellets. On line gas chromatography (Shimadzu 14A) was used for the analysis of CH4, O2, CO, CO2, C2H4 and C2H6 in the reactants and products. 

On-line GC analysis (Shimadzu GC 14A) was used to measure product selectivity and methane conversion. Details on the analysis procedure used for batch and continuous-flow operation are given elsewhere [12]. The molecular sieve trap was found to trap practically all ethylene, COj and HjO produced a significant, and controllable via the adsorbent mass, percentage of ethane and practically no methane, oxygen or CO, for temperatures 50-70 C. The trap was heated to -300°C in order to release all trapped products into the recirculating gas phase (in the case of batch operation), or in a slow He stream (in the case of continuous flow operation). 

Catalytic activity tests have been performed in a quartz microreactor (I.D.=0.8 cm) filled with 0.45 g of fine catalyst powders (dp=0 1 micron). The reactor has been fed with lean fiiel/air mixtures (1.3% of CO, 1.3% of H2 and 1% of CH4 in air resp ively) and has been operated at atmospheric pressure and with GHSV= 54000 Ncc/gcath The inlet and outlet gas compositions were determined by on-line Gas Chromatography. A 4 m column (I D. =5mm) filled with Porapak QS was used to separate CH4, CO2 and H2O with He as carrier gas. Two molecular sieves (5 A) columns (I D.=5 mm) 3m length, with He and Ar as carrier gases, were used for the separation and analysis of CO, N2, O2, CH4, and H2, N2, O2 respectively... 

A reliable chromatographic method has been developed for the quantitative aneilysis of hydrophobic impurities in water-soluble polymeric dyes. The method utilizes both the molecular sieve effect of normal gel permeation chromatography and solute-column packing interaction, modified by solvent composition. This method eliminates the need to extract the impurities from the polymeric dye with 100 extraction efficiency, as would be required for an ordinary liquid chromatographic analysis. 

Since the ketene will copolymerize with cyclopropanone, excess ketene was removed by addition of 3A molecular sieves followed by evacuation at 1 mm Hg for 2-3 hours at -70°C. The amount of ketene was monitored by FTIR analysis. Ketene has a distinct strong absorption between 2130 and 2150 cm-1 (5,6). The solution FTIR spectrum of cyclopropanone in Figure 1 was taken before ketene removal. 

The mesoporous molecular sieve SBA-15 has been functionalized with aminopropyl moieties via grafting. Further treatment of the 3-aminopropyl-modified material with glutardialdehyde (GA) results in GA-ATS-SBA-15. The modified silica materials were characterized by NMR and IR spectroscopy as well elemental analysis confirming the successful modification. Furthermore, the elemental analysis suggests that two of three amino moieties of the 3-aminopropyl modified material react further with... 

The composition of the gas stream before and after contact with the catalyst was monitored by subjecting aliquots to gas chromatographic analysis using a Ohkura Model 701 gas chromatograph and two columns. For N2 and O2, a 1 meter molecular sieve 5A column operating at 65°C was employed for N2O, a 2 meter Porapak Q column operating at 89°C was used. 

Reactions were carried out in a glass vessel closed with a septum cap. Neither molecular sieve nor drying gas was used. The glycosyl donor (0.41 mmol, 1 equiv) in CH2C12 (3 ml) was treated with Ph3P (3 equiv) and CBr4 (3 mol equiv) and stirred for 3h at room temperature. Then, the N,N-tetra-methylurea (300 pi) and the glycosyl acceptor (3 equiv) were added and stirred at room temperature. The reaction was monitored by TLC analysis until the bromide donor was... 

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