88 THE ANALYST. ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOODS AND DRUGS ANALYSIS. The Determination of Glycerin in Wine. J. GI.. Gugliemetti and V. Coppetti. (Ann. de Chim. aqaaZ., 1904, ix., 11, 12.)-The following rapid method is stated to give very accurate results: Fifty C.C. of the wine are thoroughly mixed with 2.5 grammes of animal charcoal and 50 grammes of purified dry sand, and the mixture evaporated to dryness on the water-bath. The residue, after cooling, is pulverized and mixed with 5 grammes of powdered quicklime, and the gray powder heated on the water-bath with 50 C.C. of absolute alcohol (specific gravity 0.796). Tho alcoholic extract is filtered off, and the residue extracted twice more in the same way with successive portions of 25 C.C. of alcohol. The united alcoholic extracts are slowly evaporated on the water-bath to about 5 C.C.The basin is then finally rinsed with 5 G.C. of absolute alcohol, and the washing of the residue finished with 30 C.C. of sulphuric ether (specific gravity 0*720), the washings being added to the alcoholicTHE ANALYST. 89 extract, and the mixture shaken and filtered. The colourless filtrate is collected in a, weighed platinum basin, the tube being washed out twice with 5 C.C. of sulphuric ether, and the washings also passed through the filter. The basin is heated on the water-bath at about 60” to 70” C. for thirty to forty-five minutes, the drying then completed in a desiccator, and the residue of pure glycerin weighed in the covered basin, every precaution being taken to prevent the absorption of water.C. A. M. Determination of other Flours in Wheat Flour. G. Volpino. ( h i t . fh“ Untersuch. tier Nahr. zcnd Genussmittel, 1903, vi., 1089-1095.)-Two methods are described. The first depends on the quantity of gluten obtained from the sample; whilst the second is based upon the fact that foreign flours contain a considerably larger proportion of insoluble proteids, excluding gluten, than does wheat flour. If a mixture of wheat dour with rye, barley, maize, or rice meal be made into a dough, and the latter be well kneaded in a stream of water, a m&ss of gluten is obtained, approximately proportional in quantity to the amount of wheat flour present. For instance, 30 grammes of wheat flour yielded sbouf 8 grammes of gluten. A mixture consisting of 15 grammes of wheat flour and 15 grammes of either rye, barley, maize, or rice meal gave from 4 to 5 grammes of glrzten.The details of the second method are as follows : 30 grammes of the meal are formed into a lump of dough with a little water. The dough is well washed in a stream of water, being during this operation kneaded with the hands. All the wash- water is collected and strained through a piece of linen to remove small particles of gluten. The liquid is then passed through an asbestos filter, and the residue on the filter dried for one hour at 100’ C. The nitrogen is now determined in 2 grammes of this dry residue, and the amount found multiplied by 6 to give the proteide present. Pure wheat flour does not yield more than 0.2 per cent.of insoluble proteids other than gluten, whilst maize meal contains 6-5per cent., barley and rice meals 6.0 per cent., and rye meal 5.0 per cent. of these proteids. w. P. s. The “Dextrins” of Pine-Honey. 0. Haenle and A. Scholz. (Zed. fur U?ztersuch. der Nuhr. und Genussmittel, 1903, vi., 1027-1031.)-The so-called ‘ 6 dextrins ” consist of various bodies which do not readily ferment, and which may therefore be separated by fermenting the other sugars of the honey with yeast. A portion of these ‘‘ dextrins” is insoluble i s 87 per cent. alcohol, and can be precipitated from a dilute alcoholic solution as barium compounds by the addition of barium hydroxide solution. They reduce Fehling’s solution to a slight extent, but are converted by hydrolysis into st mixture containing about 30 per cent.of reducing carbohydrates. The dextrins ” themselves are strongly dextro-rotary to polarized light. w. P. s. Cocoanut Oil in Margarine. E. W. T. Jones. Chem. News, 1903, lxxxviii., 317.)-Attention is drawn to the evident occurrence of cocoanut oil in margarine. The fat of this oil has a high specific gravity, a low Valenta degree, and a refraction90 THE ANALYST. corresponding with that of genuine butter-fat ; hence -the butyro-refractometer is useless for detecting this form of admixture. Two samples examined gave the following figures : Specific gravity at 100" F. . . . ... ... 911.3 909.7 Reichert-Wollny number (5 grammes) . . . 4.3 4.5 Valenta test ... ... ... ... ... 74O c. 79" c. Refractometer number at 30" C. ... ...50.0 47.5 w. P. s. The Formation of Viridinic Acid from Caffeo-Tannic Acid. A Nestler. Zeit. fiir Untersuch, der Nahr. uud Genzusmittel, 1903, vi., 1032-1033.)-0n washing coffee-berries in a dilute solution of sodium carbonate to remove dirt, it was noticed that, after drying the berries in the open air, they became black, greyish-black, or green in colour, This coloration penetrated deeply into the interior of the berries, and was due to the oxidation of caffeo-tannic acid in the presence of alkali, viridinic acid being formed. Experiments were made, which showed that a dilute solution of any of the alkalies or alkaline carbonates produced this change in coffee-berries, and also in an aqueous extract of the latter. Another colour-reaction with coffee-berries is mentioned.On treating a section of a berry with a drop of concentrgted hydrochloric acid, after about thirty minutes a microscopical examination shows that the cell contents are coloured blue. The addition of glycerol changes the colour to bluish-green, then grey-green, and finally grey w. P. s. The Amount of Salicylic Acid in Cherries and Violets. A. Desmoulibre. (Journ. Pharm. Chim., 1904, xix., 121-125.)-Cherries of different origin examined by the author were all found to contain salicylic acid as a normal constituent. The following results were obtained by a colorimetric method of determination applied to a solution of the extracted salicylic acid : English cherries, 0.15 ; French cherries, 0.20; sour cherries, 0.15; black Bourgogne cherries, 0.10; and wild cherries, 0.21 milligramme per kilogramme.Salicylic acid was also detected in the marigold, and also in different members of the VioZace@ family, the amounts ranging from a trace in V. odoruta, etc., to 0.08 to 0.144 per cent. in V. Syrtica, tricoEor, and arvensis. The cultivated variety of V. tricoEor contained less salicylic acid than the wild plant. C. A. M. Determination of the Alcoholic Strength of Tincture and Liniment of Iodine. (Pharm. Journ., 1904, lxxii., 9.)-A convenient quantity of liquid is shaken with an excess of metallic mercury. The reaction is rapid, mercuric iodide being formed, which dissolves in the potassium iodide to a colourless solution, or nearly so, if British Pharmacopoeia spirit has been used. Should methy- lated spirit have been employed, the colour of the solution is dark yellow.After complete chemical change has been effected, a small quantity of sodium hydroxide F. H. Alcock.THE ANALYST. 91 solution is added, and the distillation proceeded with in the usual way. Unless sodium hydroxide be added, traces of merouric iodide always [pass over into the distillate. w. P. s. Determination of Morphine in Opium. P. L. Aslanoglou. (Chem. News, 1903, lxxxviii., 286, 287.)-In this process the morphine is extracted from the opium with water, the alkaloid being then precipitated from the evaporated aqueous extracts, washed with ether, dried and weighed. Ten grammes of the opium are extracted for several hours-twelve hours for the first extraction-with several successive quantities of 250 C.C.of water. The filtered extracts are evaporated, the residue is taken up with 75 C.C. of water, filtered and washed to make 100 C.C. of filtrate. Thirty C.C. of 94 per cent. alcohol are added to the latter, and, after stirring for thirty minutes, 4 C.C. of 10 per cent. ammonia solution. The mixture is set aside for twelve hours, when the precipitate is collected on a tared filter, washed with 50 C.C. of water, drained, and partially dried at 60" C. The filter and morphine are then well washed with ether, and finally dried at 75" C. and weighed. 0.1012 gramme is added to the weight of morphine found in 10 grammes of opium, to correct for solubility of the alkaloid in the quantity of solution and washings used. w. P. s. Determination of Morphine in Opium and Tincture of Opium.E. Dowzard. (Pharm. Jozmn., 1903, lxxi., 909-910.)-The author considers that the British Pharma- copaeia method is clumsy from an analytical point of view, and also objectionable because of the difficulty of obtaining the necessary 104 C.C. of filtrate; he has, there- fore, devised the following method, which is free from these objections, and at the same time requires much less opium. Eight grammes of the powdered opium are treated in a flask with 100 C.C. of water for one hour at a temperature of 80" to 90" C., the flask being closed with an india- rubber stopper and frequently shaken during this time. The contents are then cooled, 3 grammes of slaked lime added, and the mixture well agitated in the closed flask for a further two hours. The whole is now poured on a filter, 51.6 C.C.of the filtrate (equal to 4 grammes of opium) are placed in a corked flask, 5 C.C. of 90 per cent. alcohol, 30 C.C. o€ ether, and 2 grarnmes of ammonium chloride are added, and, after shaking for 30 minutes, allowed to stand for twelve hours. The whole is then filtered, when the morphine remains attached to the filter, which also retains the clear ether, whilst the aqueous portion runs through. After removing the clear ether with a pipette, the filter and its contents are washed with morphinated water until free from chlorides, then once with water, and finally with about 15 C.C. of ether, the latter being poured over the edges of the filter and rern\oved, at the end of a few minutes, with a pipette. Both filter and morphine are exposed to the air for thirty minutes, then broken up in a beaker by the aid of a glass-rod, and gently heated with 20 C.C.of & sulphuric acid solution. After cooling, the solution is titrated with & sodium hydroxide solution, using methyl orange as indicator. Each C.C. of & sulphuric acid solution is equivalent to 0.0283 gramme of anhydrous morphine, 0.05 gramme being added to the weight found, as directed in the British Pharmacopa4a.92 THE ANA&YST. In the case of the tincture, 100 C.C. are evaporated to a volume of 30 c.c., 3 grammes of slaked lime are well mixed with the residue, and the mixture trans- ferred to a, 100 C.C. flask. Water is added up to the mark, any froth being removed by the addition of a drop of ether, and the solution allowed to stand for one hour.After filtration, 50 C.C. of the filtrate (equal to 50 C.C. of the tincture) are operated on as described urlder opium. In this process 80 C.C. of tincture and 3 grammes of slaked lime are diluted to a volume of 85 c.c. The latter should be 81.9 c.c., as 3 grammes of slaked lime, together with extractive carried down with it, displace 1.9 C.C. of water. Tables are given showing percentages of morphine in both opium and the tincture for each 0.1 C.C. of $n sulphuric acid solution used, the range being from 9 to 20 C.C. in tenths of a C.C. An error in the British Pharrnacopceia method is pointed out. w. P. s. A Reaction distinguishing between Heroine and Morphine. Manseau. (Bull. Xoc. Pharm. Bordeaux; through Ann. de ChiwL. anal., 1904, ix., 22.)-0n adding a little heroine to 2 C.C.of a 10 per cent. solution of urotropine in sulphuric acid there is an immediate golden coloration, changing to saffron-yellow, and finally to deep blue. Morphine, under the same conditions, gives a purple coloration, whilst narceine gives a saffron-yellow, and narcotine a golden-yellow. The yellow colour given by heroine is intermediate between the colours given by narceine and narcotine, but any confusion can be prevented by repeating the test, using formaldehyde in place of urotropine. C. A. M. Adulterated Spike Oil. E. J. Parry and C. T. Bennett. (Chem. und Druggist, 1903, Ixiii., 1011.)-Large quantities of adulterated spike oil having appeared on the market during the last few months, most of it having apparently been specidly prepared to pass the ordinary tests to which spike oil is usually subjected, the authors record a few of the adulterants they have met with and the means adopted for their detect ion.The optical rotation of the oil should not exceed +4O. Samples with a rotation over + 5' are very suspicious. The usual solubility test in 70 per cent. alcohol is untrustworthy, but by using six volumes of 65 per cent. alcohol at 15' C. the authors find that, whilst pure oils are soluble, the addition of 5 to 10 per cent. of most adulterants affects this solubility. A fractional distilla$ion reveals practically any adulterant that is likely to be added to spike oil in sufficient quantity to be remunerative. The usual adulterants are turpentine, oil of rosemary of the commonest quality, and safrol. In a sample examined a fraction was obtained, boiling between 230' and 240' C., which had a specific gravity of 0.986, was optically inactive, and had a refractive index of 1.4980.Its odour was marked, and was sufficient to identify it as being chiefly safrol. The percentage of esters and alcohols present gives useful information should oil of rosemary be suspected. w. P. s.THE ANALYST. 93 Adulterated Citronella Oil. E. J. Parry and C. T. Bennett. (Chem. and Druggist, 1903, lxiii., 1061.)-A sample of this oil recently examined was found to contain 20 per cent. of alcohol, which had probably been added to make an already adulterated oil soluble, and thus pass 1 L Schimmel's test." This form of adulteration is readily detected on distilling the oil.w. P. s. Cod-Liver Oil and its Adulterants. E. W. Mann, (Pharm. Jouurn., 1903, lxxi., 840.)-The adulteration of cod-liver oil does not usually consist in adding a, foreign oil to it. Non-genuine oil is more often composed of a mixture of oils obtained from the livers of a whole catch of fish without discrimination-cod, haddock, coalfish, shark, and:others. To ascertain whether these various oils could be distinguished from one another, the author has carried out a number of experi- ments, the results of which are given in the following table. The samples are authentic, in most cases being actually prepared from the fish, under supervision. --- Cod-liver oil, Cod-liver oil, Norwegian .. Newfoundland Cod-liver oil, Japanese .. Whale oil ..Shark oil .. Haddock oil . . Coalfish oil . . Seal oil .. .. Dugong oil . _ Ling oil.. .. Minhaden oil . . Hoi oil .. .. Brusrner oil . . V I A 2 s o c &$ 0.9262 0'9258 0.5252 0'9192 0'9290 0'9318 0.9272 0-9275 0'9203 0.9231 0'9301 09186 0.9222 a -2 f m a 25 -4 147'79 139.25 134'96 92-35 143'50 160'00 139.10 123-40 66.60 122-80 145'80 116'60 130.11 a 4 8 2 .r( - 0.36 0.45 1 '40 2'08 6'09 2.67 1-35 2-79 2.39 0.29 2-50 0'18 0'13 8 F ; 5 nB d Z p g 1S4-1 185.4 186.7 188% 1885 191'2 186.1 194.5 197.5 181.6 186.1 164'7 180.4 7'74 9.87 7-18 7.70 5'46 2 '42 6.52 3.60 3 '74 6-73 15'06 4'92 6'44 2 -0 2'0 1 '4 0 '4 0'8 1'1 0'7 2 '5 2 '5 0.7 2'2 1.8 1'9 B.P. Sul- phuric Acid Test, Before Stirring. -- red brown, tinged violet red brown, tinged violet intense violet light brown brown orange bruwr wown, tinged violet dark brown orange violet brown brown range, tinged violet violet B.P.Sul- phuric Acid Test, After Stirring. -~ violet violet ntense violet nearly black vsndyke brown red brown brown violet intense van- dyke brown brown violet brown vivid violet vivid violet INOs+H280 Teat, Before Stirring. __ orange pink brownish pink bright violet pale brown brown light brown )range brown pale brown pale orange light brown pink light brown brown HNO3+ &SO4 Test, After Stirring. -- vivid salmon pink vivid salmon pink, but not so vivid greenish brown very pale pink brown orange pale pink pale orange very pale brown pale brown light brownish pink pale orange pink pinkish orange As regards the figures, it will be seen how generally uniform they are, there being no sharply-defined property by which pure cod-liver oil can be identified.Haddock oil has a high iodine number, and possesses marked drying properties. The nitric and sulphuric acid test gave the most promising colour reaction. The author has not met with an oil other than genuine cod-liver oil which gives the charac teris tic coloration. w. P. s. Essential Oil of Boldo. E. Tardy. (Journ. Pharrn. Chim., 1904, xix., 132-136.) The leaves of the boldo (Boldoa fragrans, Pneumus boklus) have been used since 1872 in France as a, therapeutic agent in diseases of the liver. They contain aTHE ANALYST. slight amount (0.5 gramme in 20,000) of an dkaloidal substance, boldine, together with citric acid, glucose, tannin, and about 2 per cent.of an essential oil. The author has studied the composition of a specimen of this oil extracted by himself from 12 kilo- grammes of the dried leaves. It was a very mobile liquid, with a slight yellowish-green colour and a fragrant odour. Its specific gravity was 0.876 at 15" C., and its optical rotation in a 100 millirnetre tube, uD = - 6" 30'. When submitted to fractional dis- tillation it yielded three main fractions, boiling respectively at 155" to 160" c., 175" to 177" C., and 215" to 220" C. I t consisted, in the main, of a divalent dextro- rotatory hydrocarbon of the pinene series, and of a tetravalent laevo-rotatory terpene, with smaller amounts of cuminic aldehyde, terpilenol, end probably a little eugenol. Acetic acid and a sesquiterpene were also recognised.C. A. M. The Adulteration of Saffron. A. Nestler. (Zeit. fiir Urttersuch. der Nahr. und GenussmitteE, 1903, vi., 1034-1035.)-Safflower and marigold petals appear to be the most common adulterant8 of saffron, but the authors have also met with samples containing iron oxide, barium sulphate (12-93 per cent.), potassium nitrate (27.05 per cent.), and borax. Some samples of saffron had peculiar crystals on the stigma. These crystals were yellow or colourless in appearance, and when examined under the microscope were seen to be either flat plates, rhomboidal prisms, or pyramids in shape. They were soluble in water, but insoluble in alcohol and in ether. The author considers them to be a natural constituent of saffron. w. P. s. The Ash of Certain Drugs. J. C. Umney.(Pharm. Journ., 1903, lxxi., 879, 88O).-The paper by Chattaway and Moor (ANALYST, 1903, xxviii., 202-212) shows that workers are agreed as to the average ash of drugs with but very few exceptions. The most acceptable percentage for some drugs, however, still appears to be doubtful, and the author gives a few observations on the differences which occur in these latter, and the probable reason for their existence. Cimicificga Rhizome.-Well-brushed samples of the root gave an average of 95 per cent. of ash. Some specimens, having a large proportion of rootlets, yielded as much as 1305 per cent., and one sample even as high as 17.4 per cent. This shows the necessity of cleaning this and other roots before utilization in pharmacy. Eight per cent. of ash as a maximum is considered a reasonable limit.CoZocylzth PuZp.-No great reliance should be placed on the amount of ash yielded by this substance, as it may vary from 7.2 to 13.5 per cent., according to its source. A microscopical examination, and ascertaining that the sample is free from fixed oil, are the best means for detecting adulteration. Conium Leaves.-Widely varying percentages have been recorded, but the difference appears to be due to the proportion of leaves and stalks in the drug. The leaves have from 13 to 14.5, and the stalks from 16 to 18 per cent. of ash. Sixteen per cent. is suggested as a maximum limit. Cubebs.-Here, again, the stalks have a higher ash than the fruit, the amount for the former being from 10 to 11 per cent., and for the latter from 5.5 to 6.5 perTHE ANALYST.95 cent. A maximum limit of 7 per cent. is considered fair. Elaterium-A previously suggested limit of 14 per cent. may reasonably be reduced to 10 per cent. or slightly lower, the average being about 6 per cent. Provided the cucumbers be properly cleanged and prepared, the ash need not exceed 5 per cent. Loss of volatile oil in drying also increases the ash. Jaborandi Leaves.-The ash should not be more than 7 per cent. LobeZia.-The leaves contain from 10 to 12 per cent. ol ash and the stalks about 3.5 per cent. As, however, the leaves yield a much higher proportion of extractive and alkaloid than the stems, as high a ratio as possible of leaves to stems is to be recommended. From 9 to 10 per cent. of aih is a fair maximum, although samples giving as much as 12 per cent. cannot be objected ‘to. Rhubarb.-The ash varies enormously, and the author thinks it is not a matter of great importance to fix an ash standard for this drug. Reliance should be placed on more definite chemical characters for valuation purposes. Stramonium Leaves.-The amount of ash is considerably influenced by the time of collection of the leaves, and also by the soil on which the plants are grown and the method of manuring. Quantities from 13.6 to 20.3 per cent. have been obtained, and probably the latter figure ought to be taken as a limit, unless it can be shown that a drug with a high ash is deficient in alkaloidal strength. W. P. s. Distinction between Distilled and Ordinary Water in Artificial Mineral Waters. W. Lohmann. (Zeit. fiir 3fle.ntl. Chem., 1903, ix., 458, 459.)-The method devised by J. M. Silber (Farmceft, 1903, xi., 691), based upon the determination of silica in the mineral water, is considered to be untrustworthy. The distilled water employed in the manufacture of artificial mineral water is frequently aerated before use by passing it through sand filters, from which it dissolves traces of silica. The chemicals (sodium carbonate, sodium chloride, etc.) used are rarely free from traces of silica, and earthenware or glass vessels are employed for making up the solutions. In this way a mineral water actually made with distilled water may contain appreci- able quantities of silica. Furthermore, sodium silicate, as one of the constituents of natural mineral water, is added to the artificial water. w. P. s.