Nickel filter

A methanolic solution of a V-alkyl-2-nitroaniline (13.3 mmol) was hydrogenated at 20 C and atmospheric pressure in the presence of Raney nickel, filtered and treated with coned HCI (1.32 mL, 13.3 mmol), followed by sodium dicyanimide (1.17 g, 13.1 mmol) in H20 (5 mL). The mixture was heated in an open vessel on a steam bath for 1 h, by which time most of the McOH had evaporated. The resulting suspension of a black oil was treated with a solution of picric acid (6.0 g, 26.2 mmol) in MeOH, whereupon the dipicrate of the product separated as yellow crystals. 

Unfortunately, filtering is not generally so effective. Figure 4-4a shows what can be accomplished by use of a nickel filter 0.01 mm thick oil a spectrum with intensity independent of wavelength. 

X-ray diffraction has been applied to certain AB cements. For example. Crisp et al. (1979), in a study of silicate mineral-poly(acrylic acid) cements, used the technique both to assess the purity of the powdered minerals employed and to monitor mineral decomposition in mixtures with poly(acrylic acid), in order to indicate whether or not cement formation had taken place. They employed Cu radiation passed through a nickel filter for most of the samples, a seven-hour exposure time was found to be adequate for the development of a discernible diffraction pattern. Samples were identified by reference to published powder diffraction data. 

Compression molded (150°C for 3 minutes press chilled with cold water immediately thereafter) samples of poly(trans-l,4-hexadiene) (14) and poly(5-methyl-l,4-hexadiene) were examined with a General Electric (XRD-3) X-ray unit. Transmission Laue X-ray photographs were taken using nickel filtered copper X-radiation. Samples were stretched to four times of their original lengths to obtain oriented fibers. The fiber patterns were obtained in a flat plate film holder with the specimen to film distance standardized at 5 centimeters. X-ray diffraction patterns were similarly obtained for the hydrogenated sample of poly(5-methyl-l,4-hexadiene). 

Following variant II, after treating by the modifier, the solid phase was separated by filtration and additionally washed off with 0.2 liters of water under vacuum of the water-jet pump. Further, as in variant I, one part of the product was dried at 105°C for two hours (product C), while the other was dried at 20°C until a sample mass became constant (product D). The products were investigated by the powder X-ray phase analysis (PXRD) using nickel-filtered CoKa radiation. 

X-ray diffraction (XRD) patterns for the materials were recorded on a X-ray diffractometer using nickel-filtered CuKa (0.154 nm) radiation and a liquid nitrogen-cooled germanium solid-state detector. Thermal stability of the materials was performed using a thermogravimetric analyser. The acidity of calcined samples were determined... 

Fig. 27 X-ray diffraction pattern of our Ti02 fiber. The Ti02 fiber was pulverized, and the X-ray diffraction pattern of the powder was recorded with a Rigaku X-ray diffractometer with CuKa radiation with a nickel filter...

Primary X-ray spectrum for Cu with the absorption edge of a nickel filter superimposed showing how it may be used to isolate the long wavelength emission peak. 

These data were obtained with a Norelco diffractometer using nickel-filtered copper Ka radiation. 

X-ray diffractometer with copper target, beryllium window, nickel filter, and data acquisition and processing system... 

X-Ray Powder Patterns. Samples for x-ray pattern determinations were sealed in 0.2-mm. glass capillary tubes under an atmosphere of argon. The samples were then exposed to nickel-filtered, CuKa radiation in an 11.459-cm. Debye-Scherrer camera for 18 to 20 hours. 

X-Ray Diffraction Analysis. X-ray powder diffraction data for indexing were obtained with a General Electric XRD-6 diffractometer. Samples were sealed in glass capillaries (0.5 mm o.d.) and exposed to nickel-filtered CuKa radiation. KCl or iridium was used as an internal standard. X-ray powder diffraction intensity data were obtained with a General Electric XRD-5 unit. Here,... 

Powder photographs were taken with a 57.3-mm radius Debye-Scherrer camera and nickel-filtered Cu Ka radiation (Xmean = 1.5418 A). For intensity work, the multiple-film technique was used. The lattice constant, derived from 23 reflections from 42.56° to 73.47° 20 and corrected for film shrinkage with a parallel film of a reference substance, was Oo = 15.02 A with an estimated standard deviation of 0.01 A. 

X-Ray Diffraction. All diffraction patterns were taken on powdered samples with a General Electric XRD-6 diffractometer. A copper target and nickel filter were used. 

The X-ray diffraction (XRD) patterns of the sample were measured using Rigaku D-Max. II VC X-ray diffractometer using nickel filtered Cu Ka (X= 1.5406 A) radiation. The specific BET surface area and average pore sizes were determined by N2 adsorption-desorption isotherms at 77 K using an Omnisorp-lOO. Diffuse reflectance UV-spectra were obtained using Perkin Elmer Lambda 5 spectrophotometer using mesoporous silica MCM-41 or MCM-48 as a standard. The details are already reported earlier [27]. 

The program, AXIS, was specifically designed to analyse fibre diffraction patterns similar to that shown in Figure 1, although some of the methods described in this chapter may be extended to other types of pattern if required. The fibre patterns are recorded on flat film using pinhole collimated, nickel-filtered CuKor radiation, and finely powdered calcite is dusted onto the specimen to provide a calibration ring of spacing 0.3035 nm. 

The X-ray powder diffraction (XRPD) pattern of a sample of atorvastatin calcium, Form-I, was recorded at room temperature on Bruker D8 Advance diffractometer (Karlsruhe, Germany), using nickel-filtered Cu Ka radiation. The sample was mounted in a polymethylmethacrylate sample holder, and analyzed in a continuous mode with a step size of 0.01° and a step time of 1 s over an angular range of 3-40° 26. The XRPD results are found in Fig. 1.18 and in Table 1.3, being evaluated with the DIFFRACplus EVA (version 9.0) diffraction software. 

X-Ray powder diffraction pattern The X-ray powder diffraction pattern of zaleplon powder sample was obtained using a Philips diffractometer system (model PW1710). The pattern was obtained using nickel-filtered copper radiation (=1.5405 A), and is shown in Fig. 8.1. A full data summary is provided in Table 8.2. 

The x-ray powder diffraction pattern of etodolac was obtained using a Rigaku MiniFlex powder diffraction system, equipped with a horizontal goniometer in the 0 /2-0 mode. The x-ray source was nickel-filtered K-a emission of copper (1.544056 A). A 10-mg sample was packed into an aluminum holder using a back-fill procedure, and was scanned over the range of 50 to 6 degrees 2-0, at a scan rate of 0.5 degrees 2-0/min. 

Powder X-ray diffraction (XRD) patterns were recorded using a HZG 4A2 X-ray diffractometer with nickel-filtered Cu Kx (X = 0.15418 nm) radiation with a 0.04 degree step, a step time of 2 s, and a measurement range 20= 3-85°. 

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