Pressure quartz tubes

A solution of 0.17 g (51) in 160 ml benzene is stirred magnetically and irradiated for 6 hr with a Hanau NK 6/20 low-pressure mercury lamp (main emission at 2537 A) placed in a central water-cooled quartz tube. Cyrstalliza-tion of the crude product gives 0.15 g (52) (88%). 

A similar unit, modified in details such as location of condenser, use of an agitator and shape of the vessel, was used by Fisher and Whitney . Further substantial modifications to permit interface location of specimens, cooling of specimens and operation under applied pressure, have been described by Fisher . Earlier laboratory test methods tried by Fisher and Whitney included exposure of specimens heated by their own electrical resistance and of tubular specimens containing a pencil-type resistance-wire heater in a quartz tube. 

Fig. 3.1.2 The apparatus used in 1956 for the methanol extraction of Cypridina luciferin. The dried Cypridina (500 g) is extracted at a temperature lower than 40°C with refluxing methanol under reduced pressure for two days. The atmosphere inside the apparatus is completely replaced with hydrogen gas that was purified by its passing through a quartz tube containing red-heated copper fragments. The temperature of the mantle heater is adjusted, the system evacuated, and then all stopcocks are closed. The extraction with refluxing methanol continues for many hours without any further adjustment. From the author s 1957 notebook.

Catalytic activity for the selective oxidation of H2S was tested by a continuous flow reaction in a fixed-bed quartz tube reactor with 0.5 inch inside diameter. Gaseous H2S, O2, H2, CO, CO2 and N2 were used without further purification. Water vapor (H2O) was introduced by passing N2 through a saturator. Reaction test was conducted at a pressure of 101 kPa and in the temperature range of 150 to 300 °C on a 0.6 gram catalyst sample. Gas flow rates were controlled by a mass flow controller (Brooks, 5850 TR) and the gas compositions were analyzed by an on-line gas chromotograph equipped with a chromosil 310 coliunn and a thermal conductivity detector. 

C05-0146. A 0.1054-g mixture of KCIO3 and a catalyst was placed in a quartz tube and heated vigorously to drive off all the oxygen as O2. The O2 was collected at 25.17 °C and a pressure of 759.2 torr. The volume of gas collected was 22.96 mL. (a) How many moles of O2 were produced (b) How many moles of KCIO3 were In the original mixture (c) What was the mass percent of KCIO3 in the original mixture ... 

Methyl radicals were produced by pyrolysis of azomethane (CH3N2CH3). Azomethane was synthesized as describe earlier [18]. It was purified periodically by fteeze-pump cycles at 77 K, and the gas purity verified by RGA. The methyl radical source was similar to that developed by Stair and coworkers. [10, 11] The source was made of a quartz tube with 3 mm OD and 1 mm ID, resistive heating was supplied by means of a 0.25 mm diameter tantalum wire wrapped outside the quartz tube. The len of the heating zone was 4 cm, recessed from the end of the tube by 1 cm. An alumina tube around the outside of the heating zone served as a radiation shield. Azomethane was admitted to the hot tube at a pressure of 1x10-8 to 1x10-7 Torr via a high-vacuum precision leak valve. The pyrolysis tube was maintained at about 1200 K, adequate to decrease the major peaks in the mass sp trum of the parent azomethane at 58 and 43 amu by at least a factor of 100. 

Some reaction results also were obtained in a conventional single-pass flow reactor oporating at atmospheric pressure. The reactor consisted of a 4 mm i.d. fiised-quartz tube. The reagent gases were mixtures of 9.9% O2 in He, 4.1% NO in He and 1.1% CH in He, all of which were obtained from Matheson. The products were analyzed by gas chromatography. 

Figure 3s UV autoclave (after Gascard and Saus /A/) a magnetic stirrer, b autoclave lid, c connection to thermostat, d = pressure-stable quartz tube, e autoclave housing, f = quartz or Pyrex tube, g - lamp, h gas entrance and sampling valve, i = gas outlet.

Atmospheric Pressure Chemical Ionization. As its name reveals, APCI[16] is a Cl carried out at atmospheric pressure instead of under vacuum, as occurs for classical Cl. As for ESI, the sample must be in a solution that is continuously flowing into the APCI source (flow rate between 0.2 and 2 ml min ). The solution passes through a pneumatic nebulizer and is desolvated in a heated quartz tube or heating block, thus producing vaporization of solvent and analyte molecules (Figure 2.4). 

Radiation is derived from a sealed quartz tube containing a few milligrams of an element or a volatile compound and neon or argon at low pressure. The discharge is produced by a microwave source via a waveguide cavity or using RF induction. The emission spectrum of the element concerned contains only the most prominent resonance lines and with intensities up to one hundred times those derived from a hollow-cathode lamp. However, the reliability of such sources has been questioned and the only ones which are currently considered successful are those for arsenic, antimony, bismuth, selenium and tellurium using RF excitation. Fortunately, these are the elements for which hollow-cathode lamps are the least successful. 

Fig. 1. Relationship between catalyst temperature and reaction time in methane partial oxidation catalyzed by Ni/Si02 (temperature of the gas phase (a) 1019 K, (b) 899 K, (c) 809 K, (d) 625 K). The reaction was carried out in a fixed-bed reactor (a quartz tube of 2 mm inside diameter) at atmospheric pressure. Before reaction, the feed gas was allowed to flow through the catalyst undergoing heating of the reactor from room temperature to 1073 K at a rate of 25 K min-1 to ignite the reaction, and then the reactant gas temperature was decreased to the selected value. Reaction conditions pressure, 1 atm catalyst mass, 0.04 g feed gas molar ratio, CH4/O2 = 2/1 GHSV, 90,000 mL (g catalyst)-1 h-1) (25).

Several radical approaches have been also used for the synthesis of 3-oxo-perhydro derivatives based on the use of trimethylstannyl chloride or tributylstannyl chloride activation in presence of 2,2 -azobisisobutyronitrile (AIBN) <1996JOC5418, 2000TL5915>. Photochemical strategies were applied to the formation of 3-oxo perhydro intermediates <1998J(P1)3577>. Compounds 348 and 349 were isolated as a 1 1 mixture after photolysis of 347 using a high-pressure mercury lamp in quartz tubes at room temperature in the presence of cr-trifluoro-acetophenone and KF (Equation 61) <2002TL7777>. 

The sample of desorbed tritide is placed inside a quartz tube that is connected to a gas-handling manifold by a TorrSeal . A quartz sleeve with Silicon Carbide (SiC) in the annular space is placed around the end of the quartz tube, surrounding the sample with microwave susceptor. The quartz tube and susceptor sleeve are thermally insulated from the rest of the microwave cavity. An internal thermocouple measures the temperature of the sample and provides the temperature signal for process control of the desired temperature. A shine block (alumina foam), attached to the thermocouple, blocks radiant heating of the TorrSeal and the upper area of the quartz tube and manifold. An IR pyrometer is used as a secondary measure of the temperature of the susceptor, and therefore of the sample. A stainless steel shield reflects microwaves from the quartz tube not in the susceptor sleeve, eliminating the production of a plasma at low pressure in the quartz tube. 

Thermolysis of H S was carried out in an open tubular reactor quartz tube with argon/HjS feed over a wide composition spectium (20-100% H S) at four temperatures (1030-1070 K). These experiments show that the reaction is essentially first order in H S partial pressure. Hydrogen yield also increases monotoiucally with feed composition at all temperatures (Adesina et al., 1995). 

Figure 1. Lamp chamber containing 66 low-pressure mercury vapor lamps encased in quartz tubes, each situated 1.27 cm from adjacent lamp.

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