234 ABSTRACTS OF CHEMICAL PAPERS ABSTRACTS OF PAPERS PUBLISHED IN OTHER JOURNALS. FOOD AND DRUGS ANALYSIS. Faced Pearl Barley. J. F. Liverseege and H. Hawley. ( J . SOC. Chem. Ind., 1915, 34, 203.)-Of 73 samples of pearl barley examined, 50 contained less than 0.05 per cent. of ash insoluble in dilute hydrochloric acid ; 6 of the samples yielded more than 0.1 per cent. of ash, the amounts ranging from 0.22 to 0.82 per cent.Other samples were found to be faced with rice, and 2 samples were faced with a mixture of rice and talc. w. P. s. Beans from British West Africa. (Bull. Imp- Iqzst., 1914, 12, 547-552.)- Beans. origin. I Mois- 1 ture. I _~ ____ I I 1 Per 1 Cent. Yigna C'atjang (" Kroo $ierra Leone1 11 *3 beans ") PhaseoZm Zunatzu (" Towe ltJierra Leone 11-3 1 13.4 beans 'I) Ditto ...Sword beans (G&aca~~~ j Gold'boast 1 8.2 e?zsiformis) I Ditto . . . . . . . . . I Honduras ' 14'4 Cm~avnlic6 obtus@lia ... Gold Coast . 10-9 Ditto . . . . . . . . . Nigeria 8.7 Ditto . . . . . ... 1 Hong-Kongl 11.7 I Crude Pro- teins. Per Cent. 24-3 22.0 22.9 23-4 27-4 25.0 22.0 22.5 True Pro- teins. Per Cent. 22'3 20.4 21.0 21 -0 17.5 14.8 21 -0 - Fat.Per Cent. 1'1 1'2 0.8 0.8 1.3 2 *7 1.9 0 -7 Starch etc. Per Cent. 55 -2 58-0 55 *7 55 -8 45.7 48-4 54'5 61.6 Fibre. Per Cent. 4 *9 3.8 4 -8 3 '8 14.7 6 -8 8 -1 2.9 Ash. Per Cent. 3.2 3.2 2.7 2 'a .a*7 2.7 2 -6 3-6 Nutri- ent Ratio. 1 : 2.4 1 : 2.7 1 : 2.5 1 : 2.5 1 : 1.8 1 : 2.2 1 : 2.6 1 : 2.8 Food Units. 118.7 116.2 115.0 116.0 117.4 117.0 114.0 120.0 The two samples of Tow6 beans yielded, on hydrolysis, 0-025 and 0.03 per cent.of hydrocyanic acid respectively. The other species of beans were free from cyano- genetic glucosides or alkaloids. C. A. M. Estimation of Bolted Flour in Bread. C. J. Koning and W. C. Mooij. (Chem. Weekblad, 1914,11,1064-1066.)--Estimation of the pentosans in bread affords a means of calculating the amount of bolted flour in bread.This is illustrated by the following results, in which the pentosans were estimated by distillation with dilute hydrochloric acid and precipitation with phloroglucinol : I Pentosans calcnlated ' on the Dry Material. Per Cent. Water* I I - -- ~ ~ ~- Unbolted flour ... ... ... I 14.2 Bread containing 25 per cent. bolted Bread containing 35 per cent. bolted I Bolted flour ...... ... ~ 12.1 Bread baked from unbolted'flour ... I 50.22 flour ... ... ... ... ! 49.42 flour ... ... ... ... I 49.33 I. 6.12 2.41 6.23 5.36 4-93 11. 6.39 2.55 6 -23 5.50 5.13 Pentosans calculated. Per Cent. - j - - i - 4.82 i 5.05 C. A. M.FOOD AND DRUGS ANALYSIS 235 Microseopieal Detection of Potato Starch in Bread. G. Schutz and L. Wein. (Chem. Zeit., 1915, 39, 143.)-The large gelatinised granules of wheat and rye, though somewhat irregular, preserve their spherical type, while those of gelatinised potato starch are irregularly oval, with brain-like convolutions and one or more forks; they are also larger and more highly refractive.The potato-starch granules, even when gelatinised, possess a greater affinity towards certain dyestuffs than the granules of the cereal starches, and are easily detected by the use of micro- chemical stains.A few crumbs of bread are steeped in water in a watch-glass, well kneaded, and a portion is placed between two cover-slips, which are then forced apart. The preparation is dried in the air, fixed by passing three times quickly through a flame, and then treated with a drop of the stain. Suitable stains are neutral red used fairly strong, and methylene blue well diluted.The best differen- tiation, however, is obtained with concentrated thionine solution, diluted with twice its volume of water. The stain is allowed to act for two and a half to three minutes, and the excess removed by washing. In the case of thionine the cereal starches remain unstained, while the potato-starch granules are stained a lilac colour.The cellular tissue of the potato is coloured deep reddish-violet, also the endosperm tissue of the cereals. The tissues of the fruit and seed husks of the cereals, the cortical tissue, reticulated vessels, and sclerenchyma cells, of the potato rind, are all stained blue; but since the potato rinds are mostly removed, it may be assumed for practical purposes that all blue-stained elements are derived from the cereals.By comparison with typical mixtures of known composition approximate quantitative results may be obtained, and, owing to the strong contrast of the tigsue colorations, the degree of grinding of the flour may be estimated. When boiled or steamed potatoes have been used in making the bread, some of the highly gelatinised starch granules might be destroyed by the above method of mounting.In such cases a well-mixed sample of the crumbs is moistened on a, glass slide, and broken down by simple pressure with a scalpel without any rubbing action. The preparation is drained with blotting-paper, and stained and washed on the slide in the same manner by irrigation, the cover-slip being then pressed very gently on.The gelatinised paste-granules of the potato, very large and mostly well preserved, are distinguished by a red stain. J. F. B. Estimation of Total Fatty Acids and Other Ether-Soiuble Consti- tuents of Feeding Stuffs. (J. Ind. and Elzg. Chem., 1915, 7, 218-220.)-1t is shown that extraction with ether, no matter how prolonged, fails to extract the whole of the fat from many materials.From hay and from the excrement of herbivorous animals, less than one-third can be extracted. On the other hand, ether extracts are not necessarily all fat or fatty acids, the ether extracts of the above-mentioned materials containing on a average nearly 70 per cent. of material which is either unsaponifiable, or saponifiable but still not common fat or fatty acid, since the acids set free by acidifying a solution of the soap are largely insoluble in petroleum ether.If anything more than approximation of the fat content of such material is desired, some such method as the author’s Precipitation Method (Texas Exp. Sta. BUZZ. 169) or the method now described must be employed. J. B. Rather.236 ABSTRACTS OF CHEMICAL PAPERS The Precipitation Method consists in extracting the material with ether and frac- tionating it as described below.In the new method, instead of being extracted with ether, the material (10 grms.) is saponified with 50 C.C. of 8 per cent. alcoholic soda for an hour under a reflux condenser. The extract is filtered through asbestos in a carbon funnel, and the residue washed with hot alcohol.The filtrate and washings are evaporated to about 10 c.c., washed into a separator with warm water, acidified with 10 C.C. acetic acid, and the warm solution extracted five times with 50 C.C. of ether. The ethereal liquid is washed once with water in a pear-shaped separator, which makes it easier to run off suspended solids with the water. About 10 C.C. of warm aqueous sodium hydroxide solution(1: 2)is shaken gently with the ethereal solution.About 25c.c. warm water is added, a rotatory motion given to the separator, and the aqueous layer drawn off, leaving any emulsion in the separator. This treatment is repeated, and followed by five washings with cold water, after which the ethereal solution is evaporated and the residue weighed. The extreme error involved by assuming this to be wholly unsaponifiable matter appears to be about 0.2 per cent.on the sample. The error ,may be eliminated by shaking the ethereal extract with about 20 C.C. of hydro- chloric acid before evaporation, running off the aqueous layer, evaporating the ethereal layer, and weighing the residue, and then proceeding as follows : The residue is dissolved in 20 C.C.of hot alcohol, the solution titrated with TG sodium hydroxide, and the consumption of the latter in C.C. multiplied by 0.28 is subtracted from the apparent percentage of unsaponifiable matter as previously determined, and added to the percentage of fatty acids found in the next operation. The soap solution is deprived of ether, cooled nearly to room temperature, acidified with 8 C.C.acetic acid, and extracted with 40 C.C. of petroleum ether, shaking violently. The aqueous layer and any suspended solids are drawn off and washed three times in a similar manner. The combined ethereal extracts are washed twice with 50 C.C. of water, allowing any emulsion to run out with the aqueous layer. This is washed once more with petroleum ether, which is washed twice with water and added to the main extract, which is then evaporated and the fatty acids weighed.The aqueous residue, after exhaustion with petroleum ether, is made more acid by adding hydrochloric acid, and is extracted warm with five portions of ether, each of about 40 C.C. The ether extract is washed twice with water, evaporated, and the (' saponified residue " weighed.The term '' saponified residue " is used to cover ether-soluble, saponifiable material difficultly soluble in petroleum ether, Practically all the chlorophyll, when present, is found in this fraction. The other constituents are acids of approximately the 8ame mean molecular weight as the acids derived from the commoner fats. G. C. J. Estimation of Crude Fibre. R. Fanto and W.Nikolitsch. (Zeitsch. anal. Chem., 1915, 54, 73-76.)-The following procedure is recommended for accelerating the rate of filtration of the acid and alkaline digestion liquids in the estimation of crude fibre : The substance is boiled for thirty minutes with 100 C.C. of 1-25 per cent. sulphuric acid, and the mixture is then poured into an ordinary extraction thimbleFOOD AND DRUGS ANALYSIS 237 of such capacity that it will hold the whole of the liquid and residue : when the liquid portion has filtered through, the thimble is suspended in a beaker of water so that the level of the water is just below the edge of the thimble.The water passes rapidly inwards, and when the thimble is full it is raised and allowed to empty. These operations are repeated until the residue is washed ; the residue remaining after the alkali treatment is washed in the same way, and is then rinsed into a platinum basin, dried, and weighed. This method of filtration and washing prevents the pores of the filter being clogged by the finely divided substance.w. P. s. Estimation of Formaldehyde and Methyl Alcohol in Aqueous Solution (Analysis of Formalin).G. Lockemann and F. Croner. (Zeitsch. anal. Chem., 1915,54, ll-26.)-1n an aqueous solution containing both formaldehyde and methyl alcohol, the former may be estimated by adding hydroxylamine hydrochloride and titrating the liberated hydrochloric acid, or by adding sodium sulphite and titrating the free alkali formed; the methyl alcohol is estimated by oxidising the solution with permanganate and calculating the quantity of alcohol present from the amount of permanganate reduced, allowance being made for the permanganate reduced by the formaldehyde.In the hydroxylamine method the reaction proceeds according to the equation and methyl-orange is used as the indicator in titrating the acid produced. The reaction with sodium sulphite is shown by the equation CH20 + NH20H.HCl = CH2NOH + H20 + HCI, CH,O + Na2S03 + H20 = CH,(OH)SO,Na + NaOH ; rosolic acid is used as the indicator in the titration, since it gives a sharper end- reaction than does phenolphthalein (cf.ANALYBT, 1903, 28, 363). For the oxidation with permanganate, the formalin (40 per cent. formaldehyde solution) is diluted with 100 times its volume of water, and 5 C.C.of this solution are mixed in a flask with 75 C.C. of water and 25 C.C. of alkaline permanganate solution (15-82 grms. of potassium permanganate and 40 grms. of sodium hydroxide per litre) ; the mixture heated for twenty minutes on a water-bath, then treated with an excess of oxalic acid solution (31.51 grms. of crystallised oxalic acid and 75 C.C. of concentrated sulphuric acid per litre), and the excess of oxalic acid is titrated with acid per- manganate solution (containing 40 grms.of crystallised phosphoric acid per litre). One C.C. of permanganate solution is equivalent to 0,00375 grm. of formaldehyde or 0.00267 grm. of methyl alcohol. The authors found that it was impossible to separate the aldehyde from the alcohol by distillation even after the addition of substances such as ammonia, alkali bisulphite, the sodium salt of sulphanilic acid, etc.; traces of formaldehyde were always found in the distillate.Attempts were also made to bring about the separa- tion by converting the formaldehyde into an insoluble compound by treatment with aniline or p-nitrophenylhydrazine and subsequent filtration, but it was not possible, by distillation, to separate the methyl alcohol from the excess of precipitant in the filtrate.w. P. s.238 ABSTRACTS OF CHEMICAL PAPERS Detection and Estimation of Free or Combined Glycerol. Analysis of Glycerophosphates. M. Franeois and E. Boismenu. ( A m . FaZs$., 1915,8,3-16.) -Free glycerol, after having been heated to expel aldehydes, alcohol, and other volatile substances which may be present, can be identified by heating it with potassium hydrogen sulphate ; acraldehyde (acrolein) is formed, and if the vapours containing this substance are conducted into magenta-sulphurous acid reagent, a red coloration is produced which changes to blue when the mixture is heated.The glycerol in glycerophosphates may be identified by this test. For the estimation of glycerol in glycerophosphates the bichromate method is recommended ; the authors find that the oxidation is complete only when a large excess of bichromate is employed, and the mixture boiled for two hours under a reflux apparatus. The phosphorus in glycerophosphates may be estimated by boiling the substance for two hours under a reflux apparatus with a mixture of 10 grms.of water, 10 grms.of concentrated sulphuric acid, and 4 grms. of potassium bichromate. The mixture, while still hot, is diluted with 30 C.C. of water, 10 grms. of sodium sulphite are added, followed by 20 grms. of sodium acetate; after the solution has been heated for fifteen minutes on a water-bath, the phosphoric acid is precipitated by the addition of molybdic acid reagent, the precipitate is converted into ammonium magnesium phosphate, and weighed as magnesium pyrophosphate (cj.ANALYST, 1915, 152). w. P. s. Colouring Matter of Raw and Cooked Salted Meats. R. Hoagland. (J. Agric. Research, 1914, 3, 211-225.)-1n uncooked salted meats the colour was soluble as a rule in alcohol, and in some cases in water. All samples gave extracts showing an absorption band just at the right of the D line.In general, treatment with hydrazine hydrate or sodium nitrite did not affect the colour or spectrum of the extract. Potassium ferricyanide and hydrazine chloride generally destroyed the red colour of the extract, and caused the absorption band to disappear. The NO-hemo- globin (nitric oxide), to which the red colour is due, is readily soluble in water, but insoluble in alcohol and ether.There is ample evidence to show that the action of potassium nitrate in the curing of meats is primarily to cause the formation of NO-haemoglobin, but it is probable that under some conditions of manufacture this oompound may undergo changes, and in such cases may yield a colouring matter soluble in alcohol but not in water. Haldane (J.Hygiene, 1901, 1, 115-122) has shown that the red colour of cooked salted meats is due to the presence of NO-haemo- chromogen, a, reduction product of NO-hmmoglobin. NO-haemochromogen is soluble in alcohol, and is characterised by its resistance to the action of reducing agents and by a spectrum showing a distinct band just to the right of the D line and a faint band a trifle to the left of the E line.I t is concluded that the colour of uncooked salted meats cured with potassium nitrate is generally due in large part at least to the presence of NO-haemoglobin, although in some cases part of the colour may be due to NO-haemochromogen. The NO-hemoglobin is produced by the action of the nitric oxide resulting from the reduction of the potassium nitrate used in salting upon the haemoglobin of the meat. The colour of cooked salted meats cured withFOOD AND DRUGS ANALYSIS 239 2.9 13*5 3.9 1 16.4 4.2 1 15.9 saltpetre is due to the presence of NO-haemochromogen resulting from the reduction of the colour of the raw salted meat on cooking. H.F. E. H. 12.9 15.5 15.3 Studies in the Expansion of Milk and Cream. H. W. Bearce. (J. Agric.Research, 1914, 3, 251-268.)-Certain variations exist in the coefficient of expansion of different samples of market milk, single cream, and double cream. The principal object of the author was to determine the change in volume which occurs when the temperature of a given volume of milk or cream is changed, and thus to construct a table of relative volumes of milk and cream at various temperatures.Thus, when milk is pasteurised and put into vessels at a high temperature, it is often desirable to know what volume of milk must be measured out at that temperature so that it may occupy the required volume a t some other temperature. It was found that by the method adopted the density determinations of individual samples may be depended upon to about 1 unit in the fourth decimal place.The rate of expansion of any given sample appears to depend upon something more than the density or the percentage of fat present, and is undoubtedly dependent upon the physical and chemical condition of the sample at the time the observations are made. This condition is probably much affected by the time that has elapsed since the preparation of the sample and upon the temperature at which it has been kept.The density deter- minations were made by the method of hydrostatic weighing, a sinker of known mass and volume being suspended in tbe liquid and weighed, Elaborate precautions were taken to correct for all probable sources of error, and a very large number of results are appended in the form of tables and graphs, for which the original paper should be consulted.H. F. E. H. 72.3 70.5 64.6 Seeds of Carnardurn Species. (Bull. Imp. Inst., 1914, 12, 545-547.)-The kernels of Canarium commune and C . rufum from the Straits Settlements, and of C. Colophania from Mauritius, gave the following results on analysis. I n the case of the two first, the seed-coats were removed before the analysis. 7.4 trace 3.9 1 : 12.5 j221-9 4.2 trace 5.0 1 : 10-1 i231-4 9.0 2.1 4.2 1 : 10.0 210.5 ! I Species.C. commune C, rufum C. Colop han"& I I --I I- I -I /-I-- I I .. The seeds of C. Zuzonicum, from the Philippine Islands, are used in United States for dessert under the name of (( pili nuts." C. A. M. * The ratio between the percenta.ge of crude proteius and the sum of the percentages of starch and t The total obtained by adding the percentage of starch to 2.5 times the sum of the percentages of fat, the latter being first converted into its starch equivalent.fat and crude proteins.240 ABSTRACTS OF CHEMICAL PAPERS Organic Phosphoric Acid of Rice. A, R. Thompson. (J. Agric. Research, 1915, 3, 425-429.)-Phosphoric aoid occurs in organic combinations with inosite as phytin or phytic acid in the seeds of many plants.Phytin is probably a hem- phosphoric acid ester of inosite, and is completely hydrolysed into phosphoric acid and inosite with difficulty, even when boiled for several hours with concentrated nitric acid. The total phosphorus in rice bran is 2.29 per cent., in unpolished rice 0.32 per cent., and in polished rice 0.14 per cent. Phytin was determined in the bran by extracting with 0.2 per cent.hydrochloric acid and precipitating with alcohol, after which it is washed with 50 per cent. alcohol, then with ether, and dried. Phytin so prepared formed 8.2 per cent. of the bran, and as phytin contains a considerable amount of organio phosphorus, it is evident that rice bran contains much of its phosphorus in the organic form.Phytin could not be obtained from polished rice ; that obtained from unpolished rice was doubtless contained in the outer layer removed by polishing. Preparations of barium phytate were made, having the following composition, calculated on the anhydrous substance : Unpolished rice, 1 ... 6-63 1.75 16.43 36.93 Rice bran, 1 ... ... 6-62 1.82 16-06 37.79 9 , 9 9 2 a * * ... 6.51 1-87 16.05 37.84 C. H. P. Ba. , 9 ,, 2 ... 6.97 1-84 16.38 36.84 (Cj. also ANALYST, 1913, 38, 279.) H. F. E. H. Tea from New Sources. (BUZZ. Imp. Inst., 1914, 12, 540-545.)-Samples of tea from Uganda, East African Protectorate, and Fiji gave the following analytical results : Moisture , per Cent. Uganda, 1913 ... ... 8-05 Uganda, 1914, " Golden Tip " 8-8 Y7 ,, '' Broken Leaf '' 8.8 East African Protectorate .. . 8.6 Fiji, 1909 ... ... ... 10.6 Caffeine, Tannin, Ash, Extract, per Cent. per Cent. per Cent. per Cent. 3.67 9.5 4.76 36.0 4-90 12.6 4.2 35.2 3-85 15.5 4.8 35.0 5.0 9.6 4.8 33.9 2 *8 7.9 4.6 26-2 C. A. M. Reactions of Vanillin. E. P. Haussler. (Zeitsch. anal. Chem., 1914, 53, 691-695, 1915,54,104.)-Albumin, casein, peptone, and fibrin yield violet colorations when evaporated with an alcoholic solution of vanillin and the residue warmed after the addition of a drop of dilute hydrochloric acid (see ANALYST, 1914, 39,315).Urea, under these conditions, yields a yellow coloration, whilst gelatin gives a red colour which changes to brown and then black. A sample of pepsin when tested in this way yielded a brown-violet coloration which changed to brown-red. By using con- centrated hydrochloric acid in place of the dilute acid, a violet coloration was produced. In the absence of vanillin, the pepsin gave a brown coloration with con- centrated hydrochloric acid, but no trace of violet. The pepsin gave a, slight biuret reaction, but it was not ascertained whether the violet coloration obtained in the treatment with vanillin and hydrochloric acid was due to the pepsin itself or to the presence of traces of proteins in the same. w. P. s.BACTERIOLOGICAL, PHYSIOLOGICAL, ETC. 241 Composition of Date Wine. D. Bachilli. (Annali Chim. AppZic., 1915, 3, 101-110.)--The fruits of different varieties of Phmix dactylifera are used by the Arabs in the preparation of a light wine called Zdghtbi. Three samQles of the musts and of the wines made from them in Tripoli had the following corn osition in parts per litre : 1-0542 ' 1'0153 1-0679 19285 1.0718 1'0220 1. Must .. Wine .. 2. Must .. Wine .. 3. Muet .. Wine .. -- -- 143'89 57'16 1S6'19 97'24 182'43 80.15 I l'S1 1-55 1-51 2-04 2-17 2-57 0'31 4.4 2 0.36 5'89 0'06 6.20 0'35 0'33 0-45 -- 12.82 l(i'12 8'3% - - - - - - lOO%'i 113'06 116'70 - - - 11'86 37'6G - 30.07 - i 3 13 d - 10'40 12-36 10'96 - - C. A. M.