Spirit, The

When the distillation is complete, filter olT the crude orange solid (9 g.) at the pump, wash it wdth water and drain well. Recrystallise from methanol or from methylated spirits. The p-bromobiphenyl is obtained as colourless lustrous plates, m.p. 89-91 " yield, 7 g. 

Dissolve 0 3 ml. of glacial acetic acid in 2 ml. of water in a 25 ml. conical flask, and add 0 4 ml. (0 44 g.) of phenylhydrazine. Mix thoroughly to obtain a clear solution of phenylhydrazine acetate and then add 0 2 ml. (0 21 g.) of benzaldehyde. Cork the flask securely and shake the contents vigorously. A yellow crystalline mass of the hydrazone soon begins to separate. Allow to stand for 15 minutes, with occasional shaking, and then filter the solid product at the pump, wash first with very dilute acetic acid and then with water, and finally drain thoroughly. Recrystallise the material from rectified or methylated spirit, the benzaldehyde phenylhydrazone being thus obtained in fine colourless needles, m.p. 157 yield, 0 4 g. 

Mix I ml. of benzaldehyde and i ml. of aniline in a small evaporating-basin, place the latter on a boiling water-bath and stir the mixture gently with a glass rod. Globules of water soon appear on the oily layer. After about 20 minutes place the basin in ice-water, and stir the contents well, whereupon solidification should rapidly occur. (If the material does not solidify, replace the basin on the boiling water-bath for a further 10 minutes.) Break up the solid material in the basin, transfer to a conical flask, and recrystallise from rectified spirit. The benzylidene-aniline is obtained as colourless crystals, m.p, 52° yield, o-8 g. 

Dissolve I ml. of benzaldehyde and 0-4 ml. of pure acetone in 10 ml. of methylated spirit contained in a conical flask or widemouthed bottle of about 50 ml. capacity. Dilute 2 ml. of 10% aqueous sodium hydroxide solution with 8 ml. of water, and add this dilute alkali solution to the former solution. Shake the mixture vigorously in the securely corked flask for about 10 minutes (releasing the pressure from time to time if necessary) and then allow to stand for 30 minutes, with occasional shaking finally cool in ice-water for a few minutes. During the shaking, the dibenzal -acetone separates at first as a fine emulsion which then rapidly forms pale yellow crystals. Filter at the pump, wash well with water to eliminate traces of alkali, and then drain thoroughly. Recrystallise from hot methylated or rectified spirit. The dibenzal-acetone is obtained as pale yellow crystals, m.p. 112 yield, o 6 g. 

Pyridine methiodide and ethiodide. Place 2 drops of dry pyridine in a test-tube, add 2 drops of methyl iodide and mix. A vigorous reaction occurs and on cooling, a colourless crystalline mass of pyridine methiodide, CjHjN.Mel, is formed cf. p. 377) when recrystallised from methylated spirit, the methiodide has m.p. 117. ... 

Continue the passage of bromine vapour until the solution in A assumes a distinctly yellow colour (2-3 hours) the reaction is then complete. Filter the tribromoaniline on a Buchner funnel, wash it thoroughly with water to remove hydrobromic acid, and suck as dry as possible. Ilecr3 stallise from methylated (or rectified) spirit. The yield is 22 g. m.p. 120°. 

Bromo-4-aminotoluene hydrochloride. Transfer the partially dried 3-bromo-4-acetaminotoluene to a 1 5-litre round-bottomed flask, add 250 ml. of rectified spirit, and reflux on a water bath until the sohd dissolves completely. Introduce through the condenser 250 ml. of concentrated hydrochloric acid to the boihng solution and continue the refluxing for a further 3 hours. During this time crystals of 3-bromo-4-aminotoluene hydrochloride separate. Pour the hot mixture into a 1-Utre beaker and cool thoroughly. Filter the crystals of the hydrochloride at the pump through a Buchner funnel and wash rapidly with two 50 ml. portions of chilled rectified spirit. The yield of the hydrochloride is 150 g. 

Naphthyl methyl ether (nerolin). Use 36 0 g. of p-naphthol, 10-5 g. of sodium hydroxide in 150 ml. of water, and add 31 -5 g. (23 -5 ml.) of dimethyl sulphate whilst the mixture is cooled in ice. Warm for 1 hour at 70-80°, and allow to cool. Filter oflF the naphthyl methyl ether at the pump, wash with 10 per cent, sodium hydroxide solution, then liberally with water, and drain thoroughly. Recrystallise from benzene or methylated spirit. The yield is 33 g., m.p. 72°. 

In a 500 ml. wide-mouthed reagent bottle place a cold solution of 25 g. of sodium hydroxide in 250 ml. of water and 200 ml. of alcohol (1) equip the bottle with a mechanical stirrer and surround it with a bath of water. Maintain the temperature of the solution at 20-25°, stir vigorously and add one-half of a previously prepared mixture of 26-5 g. (25 -5 ml.) of purebenzaldehyde (Section IV,115) and 7 -3 g. (9-3 ml.) of A.R. acetone. A flocculent precipitate forms in 2-3 minutes. After 15 minutes add the remainder of the benzaldehyde - acetone mixture. Continue the stirring for a further 30 minutes. Filter at the pump and wash with cold water to eliminate the alkali as completely as possible. Dry the solid at room temperature upon filter paper to constant weight 27 g. of crude dibenzalacetone, m.p. 105-107°, are obtained. Recrystallise from hot ethyl acetate (2-5 ml. per gram) or from hot rectified spirit. The recovery of pure dibenzalacetone, m.p. 112°, is about 80 per cent. 

Place 10 ml. of pure benzaldehyde (Section IV,115) and 100 ml. of concentrated aininonia solution (sp. gr. 0-88) in a 250 ml. wide-mouthed reagent bottle. Cork the bottle securely, shake vigorously for 10 minutes and allow to stand with occasional shaking for 24 hours. By this time the benzaldehyde should be converted into a hard mass of hydrobenz-amide. Break up the solid mass with a spatula or a thick glass rod, filter with suction, wash with water, and drain thoroughly. RecrystalUse from absolute alcohol (or absolute methylated spirit). The yield of hydrobenzamide (colourless crystals), m.p. 101°, is 7 g. It is easily hydrolysed by cold dilute acids. 

Stir a mixture of 2-4 g. of powdered hydrazine sulphate, 18 ml. of water and 2-4 ml. of concentrated aqueous ammonia (sp. gr. 0-88), and add 4-6 g. (4 4 ml.) of benzaldehyde (free from benzoic acid) dropwise, with stirring, over a period of 30-60 minutes. Stir the mixture for a further hour, collect the solid by suction filtration and wash it with water. RecrystalUse from 8 ml. of rectified spirit. The 3 ield of benzalazine (yellow needles), m.p. 92-93°, is 3-6 g. 

Method 2. Intimately mix 99 g. of pure phthahc anhydride and 20 g. of urea, and place the mixture in a 1 litre long-necked, round-bottomed flask. Heat the flask in an oil bath at 130-135°, When the contents have melted, eflfervescence commences and graduaUy increases in vigour after 10-20 minutes, the mixture suddenly froths up to about three times the original volume (this is accompanied by a rise in temperature to 150-160°) and becomes almost sohd. Remove the flame from beneath the bath and allow to cool. Add about 80 ml. of water to disintegrate the sohd in the flask. Alter at the pump, wash with a httle water, and then dry at 100°. The yield of phthahmide, m.p. 233° (i.e., it is practically pure) is 86 g. If desired, the phthahmide may be recrystalhsed from 1200 ml. of methj lated spirit the first crop consists of 34 g. of m.p. 234°, but further quantities may be recovered from the mother hquor. 

United States Spirits. The manufacture of distiUed spirits is tightly controUed within narrow limits that are specified in reference 2. ATE regulations require that a detailed statement of the production process be submitted for approval prior to placing any process in operation. 

The analysis of individual chemical constituents in distilled spirits currently is performed using gas chromatography (gc) and high pressure Hquid chromatography (hplc). Although other types of instmmental analyses have yielded much information regarding the chemical constituency of distilled spirits, the combination of gc and hplc has allowed hundreds of different chemical components of distilled spirits to be individually identified and accurately quantified. 

The high degree of sensitivity, selectivity, and efficiency of gas chromatography allows the elucidation of a complete profile of the volatile components of distilled spirits. The wide selection of chromatographic columns and techniques, such as gc-ms, gc-ftir, and gc-ms-ftir, has allowed the chemist to routinely identify and quantify individual constituents on a parts-per-biUion level. The two most critical variables in the analysis of volatile components of distilled spirits by gas chromatography are the selection of a suitable chromatographic column and of the most appropriate detector. 

The acids are mixed in a flask (500 c.c.), and the nitrobenzene added in portions of 5—10 c.c. at a time. Heat is evolved, and the mass becomes somewhat deeper in colour. When the nitrobenzene has been added, the flask is heated for a shoit time on the water-bath. K few drops are then potiied into a test-tube of water. The dinitrobenzene should, if the reaction is complete, separate out as a hard pale yellow cake If it is semi-sohd, the heating" must be continued. The contents of the flask are then poured, whilst warm, into a large quantity of water. The dinitrobenzene, which separates out, is filteied at the punap and well washed with water. It is then dried. The yield is nearly theoretical. A few grams should be recrystallised from spirit. The remainder may be used for the next preparation without further puiification. 

A weighed portion of the AOS sample is dissolved in water and ethanol containing a small amount of n-decane and the mixture is shaken with petroleum spirit. The organic phase is subjected to GC using a 2 m x 10 mm packed column of 5% carbowax 20M on Chromorb T applying the following conditions ... 

Enterprising spirit - the confidence to seek out opportunities for success, to strive for innovation, and to accept the considered risktaking that comes with it. 

It is a pleasure for us who are friends, colleagues, and collaborators, to offer this contribution to a volume published in honor of Yngve Ohm s bS " birthday. For most of his career, Yngve has been interested in response properties of various systems to various probes, and we offer this contribution in that spirit. The Generalized Oscillator Strength, the subject of this paper, is the materials property that describes the response of a medium to swift particle, and thus, perhaps, an appropriate subject for this volume. Mostly, we are happy to take this opportunity to thank Yngve for his help, inspiration, and friendship over the years. 

Khunrath s engraving of Christ-Anthropos, the Archetype of the universe (fig. 3), initiated many of the elements later found in Fludd s prolific illustrations of the Macrocosmic Man. These included the use of the male nude, kabbalistic inscriptions, geographical compass-points, the diagrammatic structure of the Macrocosm and the motif of the dove of the Holy Spirit. The apocalyptic context of these images and their role in the Protestant Reformation of the late sixteenth and early seventeenth centuries will be considered in the following chapter. 

Like other Lutheran Spirituals such as Arndt, Franckenherg speaks in Pauline terms of the old natural and carnal man, who must be put off and crucified. Antichrist is the Reason of the Old Blind Fleshly Birth. The theological arguments aimed against the Roman Catholics are based on reason and on individual interpretations of the Scriptures. Their exponents have to be awakened to the guidance of the spirit, the Mind of Christ and to Christ himself within you. ... 

Shall our Reason judge of the Divine Oracles which the Holy Ghost hath brought forth through the Mouth of the Saints, when as Men of God spoke them not in their own Wills, but as they were led by the Spirit.. . the Holy Ghost.. . the only worker of Regeneration ... 

It is the Spirit of Christ that fills the heavens and earth through the power of his name and performs all acts of healing. His life is the light of the world. Through his Spirit the Resurrection will come about, when all things will be made new and the world will be rectified. 

In his recapitulation Franckenberg enquires as to the nature of the medicine of the wise. Answering himself, he states that it is nothing other than water, powder, or plaster derived from nature, or found by human wit. This water springs from God s Spirit, the Ruach Elohim and operates through God s Word, the name of Jesus, to heal human illness. It is also a balsam, or oil. 

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