Autoclave set

Fig. 9.18 Schematic representation of autoclave set-up. Reprinted with permission from [10], 2002, Society of Plastic Engineers.

There are thus groups who rely on more conventional autoclaves also for parallelized studies, but the transition to conventional zeolite synthesis are not sharply defined. At hte-company an autoclave system is used which allows larger sample volumes (Fig. 3). 16 inserts are used in one autoclave housing. These inserts can be filled by a dispensing robot and simultaneously placed in a heating unit. Centrifugation in a module, which is adapted to the autoclave set, is used for product isolation. From the centrifuge module the product is transferred to an XRD sample holder where it can automatically be analyzed. 

Figure 16 pictures a high-pressure autoclave set up as a CSTR. In this arrangement the introduction of the substrate is done using an HPLC pump. The liquid level in the reactor is kept constant using a liquid level controller (A) which is monitored by the computer. When the liquid input reaches a set level an exit valve (B) is opened to drain some of the reaction liquid to maintain the liquid level in the reactor. With such a system there is no need for a second pump to remove the product stream. 

Figure 25-6 shows a schematic autoclave set up. Sometimes the autoclave is equipped with sapphire windows permitting observation and optical measurements. A CO2 SCD equipment needs a pressure compressor and a chiller to transform CO2 vapor into CO2 liquid (or SF). 

Decontamination of wastes by autoclaving can be somewhat tricky, since the efficacy of this technique relies on the penetration of steam into every portion of the load (242), and the contact time (the time that the steam contacts all portions of the load) and the autoclave set time (the time set on the autoclave timer) are rarely equal. In fact, for large loads, it has been demonstrated that complete steam contact times can lag autoclave set times by a factor of four or more (254), resulting in incomplete sterility or decontamination. In all cases, the manufacturer s recommendations for the operation of the steam autoclave should be followed. 

Most of the textured apparel and industrial yams are woven or knitted directly into fabric. The carpet BCF yams can be tufted directly off package into loop pile or velvet constmctions. For the textured saxony constmctions, the BCF and the spun staple yams must be ply-twisted and heat-set. The heat-setting temperature for nylon-6 and nylon-6,6 is 180—220°C in hot—dry atmosphere, and 120—140°C in saturated steam. The yams are twist-set in pressurized autoclaves or continuously on the Superba and Suesson machines (121). Before setting the twist, the yam is heated and relaxed for predevelopment of the bulk. 

After the initial hydrogenation studies were completed with WVGS 13407, all other liquefaction experiments were conducted in a larger, 3.8-liter bolted-closure autoclave fitted with an electrically driven magnetic stirrer arbitrarily set to provide mixmg at 1000 rpm. A temperature controller and power supply were connected to a three-zone furnace to control reaction temperature... 

It is noteworthy that the best results could be obtained only with very pure ionic liquids and by use of an optimized reactor set-up. The contents of halide ions and water in the ionic liquid were found to be crucial parameters, since both impurities poisoned the cationic catalyst. Furthermore, the catalytic results proved to be highly dependent on all modifications influencing mass transfer of ethylene into the ionic catalyst layer. A 150 ml autoclave stirred from the top with a special stirrer... 

The pH of the medium is set around 7.0 (neutral conditions) and sterilisation is carried out by autoclaving at 121°C. CaCh HzO, MgCh.6H20 and glucose are sterilised separately. In the first two cases to prevent precipitation and in me last case to prevent caramelisation (decomposition of glucose). 

General Procedure for Batch Carbonylation of Methanol in the Absence of Methyl Iodide. A complete set of procedures appears in ref. 5 bnt the following procedure is representative of a methanol carbonylation. To a 300 mL Hastelloy C-276 autoclave was added 0.396 g (1.5 mmol) of RhCl3 3H20, 112.0 g (0.507 mol) of N-methyl pyridinium iodide, 30.0 g (0.5 mol) of acetic acid, and 64.0 g (2.0 mol) of methanol. The mixture was heated to 190°C under 250 psi (1.72 MPa) of 5% hydrogen in carbon monoxide. Upon reaching temperatnre the gas feed was switched... 

In addition to normal compression set test conditions, usually 22 hours at 70 °C in a hot air oven, pharmaceutical elastomeric closures may be subjected to compression set conditions simulating steam sterilization cycles in an autoclave for 30 minutes at 121 °C. Also, sterilizing cycles employing ETO, radiation, or dry heat are used. Comparison data between formulations are used to develop compression set values that will identify potentially acceptable compounds under these conditions. 

In a typical experiment, 50 g of NaOH flakes were first dissolved in 120 g of water. The required amount of catalyst was then wet loaded into the caustic solution and 72 g of ethanolamine added. Before heating the autoclave was closed and the air inside purged out with N2. The autoclave was then heated with the set temperature (433 K) reached after about 80 minutes. This time is taken as zero in the plots that follow. The standard operating conditions used for catalyst evaluation unless otherwise stated were as follows temperature 433 K pressure 0.9 MPa ethanolamine concentration 2.9 M NaOH concentration 6.2 M stirrer speed 80 rpm catalyst 8 g with particle size 106-211 pm. 

Syngas Homologation of Acetic Acid. To a N2-flushed liquid mix of acetic acid (50.0 gm) and methyl iodide (5.67 gm, 40 mmole), set in a glass liner is added 0.763 gm of ruthenium(IV) oxide, hydrate (4.0 mmole). The mixture is stirred to partially dissolve the ruthenium and the glass liner plus contents charged to a 450 ml rocking autoclave. The reactor is sealed, flushed... 

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