Notes on alcohol determination [in pharm a
ceutical preparations]. R. E. Schoetzow (J. Amer.
Pharm. Assoc., 1930, 19, 1060—1062).—Alkalis, such as milk of magnesia, prevent “ bumping ” in the distillation of alcohol, when added to preparations such as tincture benzoin compound in sufficient amount to combine with the resins present. Other preparations which are subject to excessive foaming can be distilled successfully if a slight excess of calcium chloride be a d d e d ; it precipitates or combines with the foam-producing constituents. In the decolorisation of tincture of iodine with sodium thiosulphate, an excess m ust be avoided, otherwise the distillate will be acid or will contain sulphur compounds. In the determination of alcohol in spirit of nitrous ether according to the U.S.P. method, it is better first to decompose the ethyl nitrite with potassium iodide and sulphuric acid, decolorise the iodine as above with thiosulphate and sodium hydroxide, and make the necessary correction lor the extra amount of alcohol. In the removal of volatile oils from distillates by extraction with light petroleum previous to redistillation, it is advisable to use the fraction b.p. 35—80°. Some preparations do not give clear distillates, b u t if magnesium carbonate be added to the alcoholic mixture after extracting with light petroleum, after agitation, chilling, filtering, and redistilling, a clear distillate is usually obtained.
E . H . Sh a r p l e s.
Phenol-water m ixtu res. 6. J. W. F e r r y (Pharm.
•’ 1931, 126, 58).—The f.p. of the “ liquid carbolic Ji5s • m*xture proposed for the new B.P. is 3• 1° and the
“is/5 is 1-0615. The f.p. limits are suggested as a useful pharmaceutical specification. F . J. W i l k i n s .
Strychnine. II. Action of certain substances in m asking the taste of strychnine. J. C. Wa r d
and J. C. Mu x c h (.T. Amer. Pharm. Assoc., 1930, 19,
1057—1060; cf. A., 1930, 1456).—The bitter taste of strychnine may be masked by a number of chemically unrelated substances, such as salts, sucrose, and yerba santa extract and in the salts the cation is the significant factor in the masking action, the efficiency of which decreases in the o rd e r: magnesium (78%), calcium (25%), sodium (8%), potassium (2%). Addition of sodium bicarbonate increases the bitterness, and the most efficient masking action was possessed by yerba santa extract, which increased the threshold of strychnine from its normal value of 5-4 micrograms to 36-4, on the addition of 5%. No relationship was found between acuity and speed of perception of the bitter taste of strychnine. No consistent masking effect could be attributed to the anions studied. E. H . Sh a r p l e s.
Lobeline. I. Evaluation of lobeline preparations and com parison w ith lobelanine and w ith the total alkaloids of L o b elia in fla ta . M. Ni s i s i t a
(Okayama Ig. Zasshi, 1929, 39, 1985—1986).—Of the preparations examined, a fresh solution of crystalline lobeline had the greatest toxicity and the greatest effect on respiration. The emetic action, which was greatest with brownish crystals of “ lobeline sulf.”
(Merck), appears to be produced by a decomposition product of lobeline. Ch e m ic a l Ab s t r a c t s.
P o ly p o d iu m o c c id e n ta le . L. Fis c h e r and F . J.
Go o d r ic h (J. Amer. Pharm. Assoc., 1930, 19, 1063—
1071).—The rhizome (loss in air 75-44%, loss a t 110°
3-48%, acid-insoluble ash 0-26% , acid-soluble ash 2-42%, water-insoluble ash 2-06% , water-soluble ash 0-62%) of P. occidentale (licorice fern), grown on the Pacific coast, gives 41-19% of aqueous extract (on the drug dried a t 75°), and contains 13-6% of reducing sugars, 1-26% of starch, 6-22% of pentosans, 3-67% of tannins (chiefly of the pyrocatechol variety), 0-005% of volatile oil, a yellow colouring m atter (dyes silk a fast yellow), 2-36% of glycyrrhizin and ammoniated glycyr- rhizin (?). I t contains no appreciable amounts of alkaloids and is non-toxic to white rats, even in large
amounts. E. H . Sh a r p l e s.
Preparation o f C arstanjen’s com pound. A. A.
Ha rw o o d (J. Amer. Pharm. Assoc., 1930, 19, 1171—
1173).—Difficulties occurring in the preparation of this compound (potassium sulphite-thymoquinone) can be avoided by starting from freshly prepared sulphite as follows. A solution of 100 g. of potassium hydroxide in 100 c.c. of water is saturated with sulphur dioxide. An equal amount of potassium hydroxide is then added and then an equimolecular am ount of potassium bicarbonate. The solution is heated to 80°
and thymoquinone added in small amounts, with shaking, until an excess is present as indicated by the presence of an oily layer on the surface. Sulphur dioxide is then passed in until partial decolorisation occurs and, on cooling a t 0°, the compound crystallises out.
Attempts to prepare the compound from potassium bisulphite were unsuccessful owing to reduction to thymoquinol. The author, in disagreement with Carstanjen’s explanation, th a t the amounts of potassium hydroxide liberated by the repeated addition of equal quantities of thymoquinone to the potassium sulphite should be the same, finds th a t the amount of alkali used
B r i t is h C h e m ic a l A b s t r a c t s — B .
274 C l. X X .— Me d i c i n a l Su b s t a n c e s ; Es s e n t i a l Oi l s.
in converting tlie bisulphite into the normal sulphite diminishes with each increase in thymoquinone added.
E . H. Sh a r p l e s.
Stabilisation of solution of arsenious and m er
curic iodide, U .S .P . X [Donovan’s solution].
W. J. Hu s aand W. W. F. En z(J. Amer. Pharm. Assoc., 1930, 1 9 , 1228—1230).—Donovan’s solution, stabilised by various methods, after storage for 10 months in well- filled, amber-coloured bottles, showed the following percentage deterioration : control 12-4, authors’ modi
fied formula (cf. B., 1930, 585) < 1 , neutralised with potassium hydroxide 10-1, saturated with carbon dioxide 8-7, neutralised with potassium hydroxide and saturated with carbon dioxide 6-1, air replaced by hydrogen 12-5, neutralised with potassium hydroxide and air replaced by hydrogen 7-3, calcium carbonate added 6-0, terpin hydrate added 8-3. E . H. Sh a r p l e s.
A ssay of m ercurochrom e “ 220. ” G. W. Ha r r is
(Quart. J. Pharm., 1930, 3, 455—459).-—Normal mer
curochrome loses about 10% of its weight when dried a t 110° and 15 mm. A series of commercial samples gave values for bromine (peroxide method) ranging from 18 to 21-3%, and for acetic acid 1—3%. A limit of 1% is suggested for the latter, and the mercury content should approximate to 23-5% (on the determinations ; cf. White, A., 1921, i, 71). R. Ch i l d.
Tincture of capsicum . C. F. Poe, A. P. Wy s s, and B. S . Sl a t o r(J. Amer. Pharm. Assoc., 1930,19, 1188—
1190).—Analyses of the tinctures prepared with different concentrations of alcohol and with different samples of capsicum are discussed from the point of view of the detection of adulteration. E. H. Sh a r p l e s.
Capsicum tincture, B.P. W. J. Be a r d s l e y and F. J. Bo lto n (Quart. J. Pharm., 1930, 3, 427—432).—
To avoid the deposition of fatty m atter from the tincture a t low temperature it is suggested th a t the capsicum (7-5 g.) be macerated with 100 c.c. of 60% alcohol, percolated, and the marc pressed ; to the resulting liquid is added one half its volume of 90% alcohol. R. Ch i l d.
Further studies on the salvarsans and related com pounds. C. N. My e r s (J. Amer. Pharm. Assoc., 1930,1 9 ,1051—1056).—The lack of efficiency and greater need for uniformity of certain types of arsenicals, particularly neosahlarsan, is emphasised. Examination of some types of the latter product has shown th at some are essentially monosubstituted, other disubstituted;
another group was approximately half and half, and another contained 81-6% of a sulpharsphenamine-like impurity. Similarly, many commercial samples of salvarsan contain comparatively large amounts of inert, non-arsenic containing material and some require large excesses of alkali to produce the disodium s a lt ; this factor, coupled with the action of water th a t has absorbed much carbon dioxide, may be the cause of disastrous results clinically. The use of warm or hot water for the addition of the alkali leads to decomposi
tion with formation of arsenoxide. E. H. Sh a r p l e s.
Leaf oils of W ashington conifers. II. J u n ip eru s S co p u lo ru m . I I I . P in u s m o n tíco la . IV. T su ga h etero p h ylla . A. J. L e h m a n and E. V. L y n n (J. Amer.
Pharm. Assoc., 1930,19,1071—1075,1185—1187,1304^
1307 ; cf. B., 1930, 1003).—II. Steam-distillation of the j fresh leaves of J. scopulorum yielded 0 • 49% of a yellowish- green oil (<P 0-966 [?],[«]“ +41-18°, «1° 1-4856, acid value 1-52, saponif. value 11-29, ester [as bornyl acetate] 3-41%) having a balsamic odour and containing a-pinene, camphene (?), ß-pinene, terpinene, terpineol (partly as butyrate or acetate), azulene, a phenol, and unidentified oxygenated compounds.
III. Steam-distillation of the leaves of P. monticok yields 0-053% of oil [d25 0-8695, n“ 1-4724, [a]?
—17-31°, acid value 4-24, saponif. value 26-78, esters (as bornyl acetate) 7-88%] containing a- and ß-pinene, ß-phellandrene, probably camphene (total terpenes about 80%), borneol (as butyrate ?), azulene, sesqui
terpenes (6%), and a compound giving a lactone on oxidation.
IV. The oils distilled from the air-dried leaves (0-12%) and fresh leaves and twigs (0-09%) of T.
heterophylla have, respectively: d2a 0-9499, 0-8741;
< 1-4935, 1-4804; [a]25 —, —17-33°; acid value 45-74, 3-11 ; saponif. value 78-51, 16-51 ; ester as bornyl acetate 11-49%, 4-69% ; alcohol as estei 9-01%, 3-68%. A mixture of the two oils contained 65% of terpenes (a- and ß-pinene, ß-phellandrene, camphene), cadinene, benzoic acid (free and as ester) and a sesquiterpene, picene, which has been found also in the oil from Picea sitchensis. E. H. Sh a r p l e s.
E ssential oil from the fruit of Ferula Badra K em a. B. N.- Ru t o v s k i and I. V. Vinogradova
(Trans. Sei. Chem. Pharm. Inst., Moscow, 1930, No. 22, . 72—79).—The oil of Ferula galbaniflua had d%& 0-8736, g ccd -f 16-16°, Wp 1 -4765, acid value 1 • 2, ester value 19-12, ester value after acetylation 31-78; it consists chiefly of hydrocarbons. d-ß-Pinene, d-limonene, ketones (1%), and an alcohol, <Z|| 0-9801, a„ + 1 -2 °, 1 -4935, were p re sen t; camphene was not found.
Ch e m ic a l Ab s t r a c t s.
E ssen tial oil of L a s e r p itiu m h is p id u m , MB-B. N. Ru t o v s k i and N. N. Ma k a r o v a-Sem lianska
(Trans. Sei. Chem. Pharm. Inst., Moscow, 1930, No. 22, 85—94).—The oil (0-1 8 -0 -7 7 % ) had 0-8442- 0-8781, [<x]D +17-05° t o —3-8°, wg 1 -4C82—1 -4786, acid value 0-92—5-27, ester value 18-66—142-16, ester value after acetylation 17-14—151-8, alcohol content 2-43—9-28% (free), 5-13—39-12% (combined)- Geraniol (40—42%) is the most valuable constituent of the oil from the fruits ; citronello. was not found.
Ch e m ic a l Ab s t r a c t s.
Oil and cam phor content of the leaves of Lauras c a m p h o r a . B. N. R u t o v s k i and I. V . V in o g r a d o v a
(Trans. Sei. Chem. Pharm. Inst., Moscow, 1930, No. 22, 126— 129).—The finely-powdered leaves are distilled with steam and the distillate is extracted with ether, the camphor content being calculated from the m.p., f-P->
and [¡x]d of the residue. Results are tabulated.
Ch e m ic a l Ab st r a c t s.
[Characterisation of] ethereal o ils. K. Bodes- d o r f (Arch. Pharm., 1930, 2 6 8 , 486—491).—The reac
tions of anethole, woeugenol, geraniol, eugenol, geranyl acetate, citral, and citronellal with 0 • 3iY -p e r b e n z o ic
B r itis h C h e m ic a l A b s t r a c t s —B .
Cl. X X I .— P h o t o g r a p h i c M a t e r i a l s a n d P r o c e s s e s . 2 7 5
acid in chloroform a t 2 0 ° have been followed. In the first three cases the reaction is completed within a few hours, but in the others it proceeds much more slowly.
In view of the simplicity of the method, an attem pt has been made to use the oxygen number (ef. Prileshaeff, A., 1 9 1 1 , i, 255, 6 0 4 ) for the characterisation of ethereal oils. The oil is dissolved in 25 c.c. of IV-perbenzoic acid and the excess of the latter determined after 18
and 2 4 hrs. A satisfactory end-point was attained with seven oils, but not with oil of cinnamon.
H . E. E. No t t o n.
Dispersion of the optical rotation of essential oils. L. A. Tsc h u g a e v and Y. Z. Ciie sn o (Trans. Sei.
Chem. Pharm. Inst., Moscow, 1 9 2 8 , No. 19, 1 8 1 — 1 8 5 ).—
The dispersion coefficient o / / a c ( e = 6 5 6 ; / [¿ (¿ = 4 8 6 ¡xjj.)
is for a large number of substances about 1 -9 5 , b u t shows considerable deviations. A number of ketones give high values ( 2 - 0 5 — 3 - 5 0 ) . The constant serves for the characterisation of individual compounds and naturally occurring mixtures. Data for 31 oils are tabulated.
Ch e m ic a l Ab s t r a c t s.
Caution in w orking w 'th ether. No l t e. See III.
Tobacco. Ko e n ig; Hu tch e so n and Co p l e y.—See XVI.
See also A., Eeb., 187, Determ ination of m ercury in m ercuric cyanide ( C a t t e l a i n ) . 1 9 0 , Continuous extraction apparatus ( S e l f and C o p .fie l d ) . 1 9 5 ,
Automatic distillation of ether, alcohol, chloroform , etc. (L app ). 2 1 8 , Organ c com pounds of selenium
( K e im a t s u and Y o k o t a ) . 2 3 5 , Synthesis of contrast media for pyelography ( S u g ii and others). Deriva
tives of 4-phenyl-2-m ethylquinoline ( B r a h m a c h a r i
and B h a t t a c h a r y y a ) . 2 3 9 , 1-Hydroxy- and 1- am ino-derivatives of theobrom ine ( R o j a i i n s and
F e g e l e r ) . 2 4 2 , Alkaloid from A nona reticu la ta
S a n t o s ) . Alkaloids of B erb eris T h u m b e rg ii (Iv o n d o
and T o m ita ). S try c h n o s alkaloids ( L e u c h s ) . 2 4 3 ,
Oxonitin (S p ä t h and G a li n o v s k y ) . M.p. of pure yohimbine ( W a r n a t ) . Alkaloids of S in o m en in iu m and Cocculus (K o n d o and others). Identification of alkaloids ( F u l t o n ) . Detection of alkaloids in plants : cytisine ( K l e i n and F a r k a s s ) . 2 4 6 , M icro
sublimation ( C h a lm e t a ) . Determ ination of quinine • alkaloids ( P r i d e a u x and W i n f i e l d ) . 2 5 2 , T rypsin preparations for prevention of adhesions ( W a l t o n ) . 2 5 9 , M ethylglyoxaline derivatives (Su p n i e w s k i).
260, Antipyretic action of 3-am inohydrocarbo- styril, its isom erides and derivatives (Wa t a n a b e).
Isotonic soap for injection (Picou). Local anses- ti etics from piperidine ( R o s e a n d others). 2 6 6 , orU7 DC at-°-n t u '3 e r c u *‘n (M a s c h m a n n a n d K ü s t e r ) .
>. Purification and concentration of diphtheria toxin and anatoxin (S c h m id t and others). Purifi
cation of Shiga and typhoid phages ( H o s o y a and others). Bactericidal effect of ether and chloroform vapours (Y a s u d a ). Terpenes and essential oils as disinfectants (D e ; S u b r a h m a n y a n ) . 2 6 8 , H orm one of pituitary gland ( v a n D y k e and W a l l e n - L aw h e n c e) . 2 6 9 , Hormone of anterior pituitary lobe ( B i e d l ) .
Female sex hormone : a ssa y and preparation
(D A m o u r and G u s t a v s o n ) . 2 7 4 , A lkaloids from
S id a c o r d ifolia (Gnosn and D u t t ) . E ssential oil of bark of M ag n o lia o b o v a ta ( S u g ii and S h in d o ) .
Pa t e n t s.
Curing of tobacco. W . A. Pik e, H . M. Pi k e, and
W . T. He n r y (U.S.P. 1 ,7 6 8 ,1 4 2 , 2 4 .6 .3 0 . Appl.,
7 .1 1 .2 7 ).—The newly-cut tobacco leaves are subjected to hot fumes containing creosote, lignin, and acetic acid, preferably obtained from the hard woods, so th a t the fumes completely penetrate into the sap before it is evaporated by the heat. E. H . Sh a r p l e s.
Cyto-vaccine of tubercle bacilli. J. S. Ko m in z
(U.S.P. 1 ,7 6 6 ,1 3 1 , 2 4 .6 .3 0 . Appl., 2 9 .1 0 .2 3 ).—A sus
pension of live tubercle bacilli in a sterile normal saline solution is subjected to a treatm ent to kill the bacilli, the mixture is injected into a healthy mammal, and the fluctuating mass which is developed is evacuated to obtain a liquid containing the defensive anti-bodies and partly digested tubercle bacilli. This liquid is treated mechanically and/or chemically to break down capsular structures to render its absorption complete into another mammal in which it may be injected. I t may be treated with ether and triturated and, after elimination of ether, the residual dry mass triturated again and then mixed with a solution of sodium chloride to produce an emulsion. E. II. Sh a r p l e s.
Manufacture of [m ercury] products having a sterilisin g action on bacteria and/or fungi. T. W. F.
Cl a r k (B.P. 3 3 8 ,9 6 3 , 2 9 .8 .2 9 ).—Phenolphthalein or fluorescein or their homologues or halogen derivatives are treated in solution and a t raised tem perature with mercury oxycyanide or with a mixture of alkali cyanide arid mercury oxide. C. Ra n k e n.
B asic product from oleic acid (B.P. 3 1 7 ,3 2 5 ).—
See I I I . Castor oil soap (U.S.P. 1 ,7 6 7 ,0 4 1 ).—See X I I . XXL—PHOTOGRAPHIC MATERIALS AND
PROCESSES.
S om e properties of fine-grain developers for m otion picture film . H. C. Ca r l t o n and J. I. Cr a b t r e e (Kodak Res. Lab., Abridged Sci. Publ., 1 9 2 9 , 1 3 , 1 9 1 — 2 0 4 ).—Borax developer gives more emulsion speed for longer development tim e s; a maximum gamma of
1 - 4 is obtainable. The effects of varying the concentra
tion of the constituents of the developer are described and tabulated. Borax developer becomes exhausted more rapidly than other developers, bu t can be revived by adding half the original quantities of elon, quinol, and borax together with a little sodium sulphite. The developer cannot be used for more than 1 6 0 ft. of film per gal. The sludge of silver which forms does not inter
fere with successful development. Increasing sulphite content decreases graininess, bu t too much is deleterious.
1 G. per litre of hypo produces very fine-grained images.
Extensive tests indicate th a t borax developer does not produce finer-grained images th an does the standard formula (D . 1 6 ), b u t is preferable where a low degree of development is required. Eastm an motion-picture panchromatic film (type 2) was used throughout.
J. Le w k o w it s c h.
B r itis h C h em ica l A b s tr a c ts—B .
2 7 6 Cl. XXII.— Ex p l o s i t s s ; Ma t c h e s. Cl. XXIII.— Sa n i t a t i o n ; Wa t k b Pu b i f i o a t i o n.
Variation of the threshold speed of an em ulsion according to the developer and conditions of developm ent. I I I . E. R. Bu ll o c k (Kodak Res. Lab., Abridged Sei. Publ., 1929, 13 , 7—10).—The threshold speed of an emulsion passes through a maximum with increasing times of development. The “ maximum threshold speed ” varies with the composition of the developer. The time of development, for a given emulsion and developer, required to obtain the maximum threshold speed is called the “ optimum development time.” The treatm ent of an emulsion with dilute silver nitrate solution between exposure and development (cf.Wightman and Quirk, B ., 1927, 268) was investigated, and it was found th a t (1) the maximum threshold speed and optimum development time are increased ; (2) dry
ing and keeping of the emulsion after treatm ent causes continuously increasing latent fog ; (3) short treatm ent (e.g., 0-02% AgNOs for 5 min.) has a distinct anti- fogging efiect; (4) if a sulphite-free alkaline developer or ferrous oxalate is used, immediate fogging occurs, bu t may be obviated by washing in water, or bathing in very dilute potassium bromide solution, before develop
ment. This latter treatm ent does not alter effects (1)
and (3). J. Le w k o w it s c h.
C hem istry of selenium toning. A. Se y e w e t z
(Brit. J. Phot., 1930, 77, 718—719).—Silver images toned to completion with (a) sodium selenosulphate in excess of sodium sulphite and (b) sodium selenosulphide showed an almost quantitative convertion into silver selenide. The mechanism of the chemical reactions is
suggested. J. W. Gl a s s e t t.
See also A., Feb., 180, N ew photochem ical effect on “ celloidin ” paper (Me w e s).
Pa t e n t s.
Production of photographic silver-salt em ul
sio n s. G . Sc h w a r z (B.P. 339,769,22.11.29).—An inner compartment containing a solution of a colloid is separated by collodion or chromated gelatin diaphragms, on one side from a silver salt solution containing the anode, and on the other from a solution of a halide compound containing the cathode. By electrolysis a silver halide emulsion free from the salts of double decomposition is formed in the inner' compartment.
Details of the apparatus are given. J. W. Gl a s s e t t.
Dye-carrying layer for photographic film s and the like. S . E. Sh e p p a r d and J. G. McNa l l y (U S P 1,768,795, 1.7.30. Appl., 1.3.29).—The rear side of the emulsion support is coated with a layer of polyvinyl alcohol containing an anti-halation dye which will act as a desensitiser in solution. J. W. Gl a s s e t t.
Manufacture of sensitised b ases for photographic purposes. H. D. Mu r r a y, D. A. Sp e n c e r, and Colo ur Ph o t o g r a p h s ( Br it. & Fo r e ig n), Lt d. ( B .P . 337,868, 24.8.29).—A water-impermeable support, e.g., nitro
cellulose, cellulose acetate, or “ celastoid,” is superfici
ally de-esterified to render the surface water-absorbent, and is then impregnated with a light-sensitive
diazon-ium salt or a silver or iron compound. Suitable de- esterifying agents are suggested for each type of support.
J. W. Gl a ss e t t.
Printing of colour photographs. Am ir a Trust
(B.P. 340,044, 26.9,29. Ger., 1.10.28).—Auxiliary dyes, which are readily removed after exposure, are added to the coloured positive films in order to equalise the exposures required by each particular film under its corresponding colour-separation negative.
J. W. Gl a s s e t t.
Production of photographs in colour. W. W.
Tr ig g s. From Mu l t ic o l o r Fil m s, In c. (B.P. 339,323, 4.6.29).—Two colour-separation negatives, taken undei green-blue and orange-red filters, are printed simul
taneously in register upon opposite sides of a double
coated film, which is developed, fixed, washed, and passed through an iron toning bath so th a t one side only, i.e., the orange-red filter positive, is toned blue.
The film is then totally immersed in a solution of a basic red dye (a mixture of basic magenta and auramine, which is not mordanted by the iron bath) and finally passed through a uranium mordanting and toning bath, which fixes the orange-red image. The film is then fixed, washed, and diied. Suitable iron toning and uranium mordanting baths are described.
J. W. Gl a s s e t t.
P hotography of X -ray im a g es. K. Sc h in z e l(B.P.
339,996, 9.7.29. Austr., 9.7.28).
[W hite-light prism device for] colour photo
graphy and colour kinem atography. S. Pr i s n k b
(B.P. 341,078, 7.10.29).
XXII.—EXPLOSIVES; MATCHES.
See A., Feb., 203, N itration of cellulose (Be r l and
Ru e f f). 211, Preparation of tetryl (De s v e r g n e s).