Irradiation apparatus

The irradiations are in general performed under purified, oxygen-free nitrogen in a cylindrical irradiation apparatus with a water-cooled central sleeve into which the lamp is introduced and efficient cooling is used to keep the temperature between 10° and 0° C. Temperatures in the range of 0° to 80° do not influence the photolysis step as demonstrated in the case of a 6j -nitrite, but increase the rate of rearrangement of the nitroso derivative to the oxime. 

Irradiation apparatus, 51, 133 Irradiation, of bicyclo[2.2.1] hepta-2,5-diene to give quadricyclane, 51, 133 W-Isobutylaniline, 53, 127 Isobutyric acid, alkylation,... 

Using the triple-ion beam irradiation apparatus, the microstructural evolution of austenitic stainless steel, which is considered as a structural material for water-cooled fusion reactors... 

Figure 21 Photograph of the triple-beam irradiation apparatus.

Photolysis Reactors and Ultraviolet Sources. For 253.7-m/ irradiation, a modified irradiation apparatus purchased from Delmar Co. was used. The reactor was a 2-necked, 500-ml., round-bottomed flask. One neck was an O-ring joint, and the other was a 24/40 joint. A 4- X 1-inch coiled low pressure mercury quartz lamp was placed inside the flask through the O-ring neck, and the joint was sealed with removable O-rings. The reactor was connected directly to the mass spectrometer by the 24/40 joint. The samples were placed inside the flask and irradiated internally. The O-ring was shielded from direct radiation so as not to induce degradation. The estimated output of the lamp was 30 watts, and the ambient temperature within the reactor during irradiation was 70°C. 

A 1-L Pyrex vessel is charged with 29.5 g (0.13 mol) of (5S)-(5-0-tert-butyldimethylsiloxymethyl)furan-2(5H)-one, 23.7 g (0.13 mol) of benzophenone (Note 10) and 800 mL of methanol. The vessel is placed in a water-cooled, immersion-irradiation apparatus (Note 11), and the solution is degassed for 1 hr in a stream of nitrogen. It is then irradiated using two 125-watt, 350-nm lamps the reaction is complete after 48 hr (Note 12). The solvent is evaporated and the residue is purified by silica chromatography [1 kg of silica, 8.5-cm x 43-cm column with a gradient elution from ethyl acetate petroleum ether (1 1) to neat ethyl acetate]. This yields 18.5 g (55%) of the title compound, 18.3 g (77%) of recovered benzophenone, 3.6 g of benzpinacol,... 

Figure 7.40 Diagram of an irradiation apparatus for quantum yield measurements. F, filter B, beam splitter A, actinometer S, sample...

Figure 7. Schematic diagram of fruit irradiation apparatus...

The irradiation apparatus, consisting of a triple walled Dewar constructed of Pyrex, is charged with a solution of 25.0 g (0.277 mol) of 3-methyl-cyclohex-2-enone (5) in reagent-grade CH2C12. A gas outlet tube to an... 

The schematic diagram of the VUV irradiation apparatus is shown in Fig. 12. We used ODS-SAM as a sample. First, the sample was set in a vacuum chamber... 

According to ref. 3, nonacarbonyldiiron [Fe2(CO)g] was synthesized by photochemical dimerization of pentacarbonyliron [Fe(CO)s] in a mixture of glacial acetic acid and acetic acid anhydride (10 1) at room temperature employing a Dema irradiation apparatus with a Philips HPK 125 W or TQ 150 W medium pressure mercury lamp. The material should be stored at -25°C in a freezer and handled under an atmosphere of argon. Pentacarbonyliron [Fe(CO)s] was a gift from BASF AG, Germany and was used without further purification. 

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