摘要:

INCLUDING THE PROCEEDISGS OFTHE “SOCIETY OF PUBLIC ANALYSTS.”A Monthly Journal for the information of those interested in the purity of Foodand Drugs, and in general Analytical and Microscopical Research.[PRICE Gd, O r to Suhso+ibcrs 5s. 3 % ~ Bditetd G. 1%’. WIGNIIII,mmum. PostFrce. 3 and JUNE, 1870. [No* 39’1 by J. hiunI:.A. H. ALLEN, F.C.S.A. D U P R ~ , PH.D., P.R.S., F.C.S.C . HEISCH, F.C.S.CONTENTS.J. MUTER, YH.I)., MA., F.C.S.G. W. WIGNER, F.C.S.SOCIETY OF PUBLIC ANALYSTS’ MEETING ............ DRUGS ACT AWENDMENT BILL ..COEXESPONDERCE .................................. ..................................LAW RIVOETS NEN- NTTHOD F01i EXAXINATION OF BUTTER. By ...................................... By A. H. Allen, F.C.S.. ............. -. ............ NOTES ON ANALYTICAL EXAMINATION OF TINCTURES.C.A. CAMERON, M.D.OTTO HEHNER, F.C.S.Ur. Koettstorfer ................................ 106 NOTES OF THE NONTH .............................NEN NETHOD OF DISTINGUISHING BUTTER FROM I CHEllrICAL PATEXTS ................................OTHER FATS. Ey W. G. Crook.. ................ 111 1300~s RECZIVED ..................................J. FALCONER KING, F.C.S.C. H. PIESSE, F.C.S.....................INSTITUTE OF CHEMISTRY ......................... 112 I1115116117118119120120FiNEST BERLINPORCELAIN.-BOHEMIANGLASS.-GRADUATEDINS T RU M E N TS. -H OFMA N N’SAPPARATUS.ALSOELECTRICAL,GALVANIC,PN EUMA TICA PPA RA TUS,&c., &c.ScientificApparatus.IPureChemicals.COMPLETESETS OFQUALl TATIVE,QUA N T I TA TIVE,VOLUMETRIC,AND ASSAYAPPARATUS.-PLA T TN E R’SBLOWPIPE. -EGGERTZCARBON. -ANDTHOMPSON’SFUEL TESTil PPARATUS.Vv-i-fOLEShLE: ASD EXPOiIT.Makers of Apparatus to the Laboratories of the Inland- Revenue, Royal Arsenal, Royal MilitaryAcademy, Science Schools, India Office, South Kensington, Bcc.Catatogzces and Estimates sent o n application, enclosing Business C a d foy Terms, dcTHE ANALYST.WORKS BY DRm MUTER, M.A.9 FmGmSm,President of the Society of Public Analysts ; Public Analyst for Lambeth, Southwark,Bermondsey, Rotherhithe, Newington, and Wandsworth,Now ready, demy Svo, with copious Tables, price 7s. 6d.N INTRODUCTION TO ANALYTICAL CHEMISTRY. For Medical A and Pharmaceutical Students.Now ready, royal Svo, Second Edition, cloth, with Analytical Tables and copious Index, price 10s.6d.N INTRODUCTION TO PHARMACEUTICAL AND NEDICAL A CHEMISTY, Theoretical and Practical.processes published only a few months since being described in their proper places.”-Chemical News.been published.”-PubZic Health.( ( The book is m e of B very useful and original kind, and is brought up to the latest date, tests and6 6 Amongst the best chemiaal treatises of the day, and in many respects superior to any that have yetThird Edition, 600 pp., Svo. Price 12s. 6d.KEY TO ORGANIC MATERIA MEDICA, Analytical Chemists will A find this a concise and yet complete book of reference for the isolation and examination of theactive principles of drugs. Special appendix on the microscopic characters of the starches in food anddrugs. Copious index and qualitative courses or resins, &c.LONDON : BAILLIERE, TINDALL & Cox, 20, King William Street, Strand, and all Booksellers.NOW READY, crown Svo, cloth, 12s.6d.PRACTICAL CHEMISTRY (A Manual of).F.C.S., Public Analyst for the County of Devon.Butter, Cheese ; Tea, Coffee, Cocoa ; Alcoholic Liquids ; Condiments.-Organic or Inorganic. With Tables and Diagrams.of rare and valuable information.”-Chemist uizd Druggist.By A. WYNTER BLYTH, M.R.C.S.,PART I: ANALYSIS OF Foom-Flour, Bread, Milk,PART I1 : DETECTION OF POISOXS‘‘ A work of great value-contains a gast amountLONDON : CHARLES GRIFFIN & Co., Stationers’ Hall Court.THE ANALYST, Vols.I. & III.--(Vol. 11. out of Print,)INCLUDING the Proceedings of the Society of Public Analysts, and embracing alarge number of Original Papers on every branch of Chemical Analysis, with a comprehensiveIndex of Subjects and Names. Price, bound in cloth, 7s. ; in half-calf, 9s.Edited (under the direction of the Committee of Publication) by G. W. WIGNER, F.C.S., andJ. MUTER, Ph.D., F,C.S.Published by BAILLI~RE, TINDALL & Cox, King William Street, Strand, W.C.E. C E T T L & CO.,MANUFACTURERS O F BAROMXTERS, THERMOMETERS, CHEMICAL ANDPHILOSOPHICAL APPARATUS OF EVERY DESCRIPTION.Dr. Franklin’s Apparatus for Analysis of Water. Dr. McLeod’s Modification for Water and Gas.Professor Bischof’s Apparatus for Evaporation of Water.Dr. Sprengel’s Mercurial Air Pumps of everyDrs. Russell and West’s Apparatus for Estimating Urea in Urine. Dr. Blaokley’s Apparatug for Ditto,11 and 31, Brooke Street, Holborn, London, Wholesale and for Exportation, and Rose CottageGlass Works, Pratt Street, Lambeth.form. Water Pumps for quick filtration. Dr. Mill’s Colorimeter.REGISTERED ENAMEL BACK URINE SEDIMENT TEST TUBES.HARD OR SOFT WATER ?-THE PORTER-CLARK PROCESSiFor the Softening and Filtration of TVater in large quantities, within small space, at small cost.The removal of the carbonates of lime and magnesia and iron from hard waters is the removal of(a) The cause of enormous waste of fuel occasioned by incrustation of steam boilers and pipes ;( b ) The cause of imperfect cleansing and purification of and injury to linen and woollens in laundries - (c) The cause of the frightful waste of soap, soda, and other alkalies by which those injuries are’imparted and theimpurities retained.In County Asylums, Steam Laundries, and Manufactories * and for the Town Supply of Old and New Swindon and the RailwayWorks, the PorteraClark Process is trlating hundreds of thousands of gallons per day.The atration is exquisite, and everything arrested is removed daily,Patented by JOHN HENDERSON PORTER, C,E,, 1 & 2, Tudor St,, Blackfrim, London, E,C

ISSN:0003-2654    

DOI:10.1039/AN87904FP025

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

THE ANALYST.TURNMILL STREET,(Opposite Farringdon Street Station,)XANUFACTUBEE OFi CHEMICAL, ASSAY & BULLIONPURE ACIDS AND CHEMICALSFOR ANALYSIS.KNOWLES & PHILLIPS,47, MINORIES, E.C.PRICE LIST FORWARDED ON APPLICATION.N,B.-References as to quality and price kindly allowed by severalleading Analysts already supplied.5PL. OERTLING,BALANCES.Maker to the Bank of England, Assay Office Of the Royal Mint, &c., &c. By Appointment.-\\---.,--Z-L%VCOUNCIL UEDAL, 1851. FIRST CLASS MEDAL, 1854 and 1862.THE SANITARY FLUID.ANTISEPTIC DISINFECTANT for Preventing Epidemics and Destroying InfectiousDiseases, as supplied to the Royal Arsenal, Woolwich. This Fluid is a powerful Antiseptic, Disin-fectant and Deodoriser, and from its harmlessness may be applied in any direction without any ill-effects,and with the best possible results.THE " PRINCESS ALICE" CALAMITY.-The Sanitary Fluid was used at the Woolwich Dock-yard for Disinfecting over 600 bodies.The Clothing taken from. the Bodies and over 500 Sheets werealso Disinfected in large Cauldrons. Also the Building, Yards, &c., giving the greatest satisfaction to theDockyard and Parish Authorities. The work was carried out under the superintendence of Mr. HARXER.TESTINOBIAL.--" H.M. Dockyard, Woolwich, Beptember 23, 1878. SIR,-I beg to inform you thatI consider your Disinfectant, as applied in the Dockyard, both to buildings and clothing, after thcremoval of the dead from the premises, very efficaciow, and, from its cleanliness and absence of smell,very superior to the Disinfectants in the form of powder generally used.-Faithfully yours, J.T.BARRINGTON, Assistant Commissary General. Mr. Harmer, Stratford, E."For Asylums, Schools, Sanitary Authorities, Railway and Dock Companies, Workhouses, Shipping, &c.Price 1s. per bottle ; 3s. 6d. per gallon ; large quantities at a cheaper rate, of the Sole Rlanufncturer,W. J. HARMER, West Ham Lane, Stratford, E., or through Agents.The MAGIC FLUID for General Household Purposes, price 1s. 6d. per gallon. Write for Pamphletwith Teotimonials, &c, N ON- POIaONOU 8THE ANALYST.BORKS PUBLISHED by BAILLIERE, TINDALL 8r COX.Now ready, Sixth Edition, price 18s.ODEBN MEDICAL THERAPEUTICS. A CompeiicIinm of RecentFormdse a i d Specific Therapeutical Directions, from the Practice of Eminent ContemporaryPhysicians-English, American, and Foreign.By GEORGE H. NAPHEYS, A.M., M.D.Now ready, demy Svo, with copious Tables, price 9s.ATERIA MEDICA AND PHARMACY. For the use of Medical a dPharmaceutical Students preparing for Examination. By W. HANDSEL GRIFFITHS, Ph.D.,L.R.C.P., Edin., &c. Edited by GEORGE F. DUFFEY, M.D., F.C.S., Fellow and Censor, King andQueen’s College of Physicians, Examiner in Materia Medica in thc Queen’s University.Now ready, Fourth Edition, 1s. ; or monntecl on rollers, varnished, 3s. Gd.POSOLOGICAL TABLES : A Classified Chart of Doses; showiiig at a glancethe Dose of every Officinal Substance and Preparation. For the use of Practitioners and Students.By HANDSEL GRIFFITHS, Ph.D., L.R.C.P., &c., late Professor of Chemistry Ledmich School of Medicine.Now ready, with Plate and numerous Engravings, Second Edition, price 5s.THE URINE,Philadelphia.A Guide to its Practical Examination.By PROF. J. TYSON, M.D.,Professor of Morbid Anatomy in the University, and President of the Pathological Society ofLONDON : BAILLI~RE, TXNDALL & Cox, 20, King William Street, Strand ; and all booksellers.Price, ONE SHILLING.SEASIDE WATER. An Examination into the character of the Water Supply atthe Watering Places of England and Wales, being an abstract of a Series of Reports prepared forand published in the Sanitary Record during 1877-78, with Three Comprehensive Tables, giving Analysesof the Drinking Water at all the Sea-Coast Towns. By 0. W. WIGNER, F.C.S., one of the HonorarySecretaries of the Society of Public Analysts ; Public Analyst for Greemich, Plumstead, and WoolwiohDistricts.KENT & Co., Paternoster Row, London ; and at all Railway Bookstalls.Demy 8vo. Price 2s.O N THE ESTIMATION OF PHOSPHORIC ACID by Magnesia forChemical Purposes: with Remarks on the Differences to be met with in the Analyses of thePhosphates of Commerce. By E. I?. TESCHENACHER and J. DENHAM SXITH.LONDON : HARDWICKE & BOGUE, 192, Piccadilly, W.W- E- BUTT 8t GO.,UNION CHEMICAL WORKS, DEBNAMSRD., SOUTH BERMONDSEY, S. E.,MANUFAUSURERS OFPharmaceutic, Photographic, and Pure Chemicals for Analysis,dspecia1 18 rep ar at ion$ +HYDROGEN PEROXIDE. FRUIT ESSENCES,IODOFORM. ~ FERRUGINOUS SYRUPS.SCALE PREPARATIONS.Printed for the Proprietors b JOHN DAVIS Old Kent Road 8 E * and published by BAILLdRE, TXNDALL & Cox, KingWYilliam street, Btraad, WAY., to wiom commLic&tiotw s h o ~ l i G icibssed

ISSN:0003-2654    

DOI:10.1039/AN87904BP027

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

NOTES ON THE ANALYTICAL EXAMINATION OF TINCTURES. BY ALFRED H. ALLEN, F.C.S. Read before the Society of Public Analysts, 01% 30th &d, 1879. I HAVE had occasion lately to make some experiments on the L 6 Tinctures ” of the British Pharmrccopceia, and as Borne of my experiences are of a rather novel character they appear worth recording. spirits ” of pharmacy, are of two distinct alcoholic strengths.‘‘ Rectified Spirit, B.P.” ( ~ p . gr. 0838 = 84 per cent. by weight of absolute alcohol = 1554 per cent. of proof spirit), is directed to be employed iu the preparation of the tinctures and spirits of chloroform, ether, aconite, ferric chloride, ferric acetate, iodine, myrrh, nux vomica, camphor, ginger, &c. On the other hand, “Proof Spirit, B.P.” (sp. gr. *920 = 49 per cent.by weight of absolute alcohol), is directed to be used in making the tinctures of orange-peel, belladonna, cantharides, crttechu, digitalis, ergot, opium, rhubarb, squills, &c. In many instances, the alcohol is the chief element of cost in the preparation of tinctures, and there is consequently a Btroug inducement to economise it as much as possible. Hence, it is not unusual to find proof spirit substituted for rectified spirit, and a mixture of equal measures of rectified spirit and water for proof spirit.Of course, alcohol so deficient in strength is apt not to dissolve the sctivc oonstituenta of the drugs employed. I may premise that the so-called tinctures ” or102 THE ANALYST. On the other hand, some of the leading h e prepare their tinctures with alcohol of 60° O.P., and yet use it in the same proportion as if it were merely 5 5 O O.P., as required by the Phermacopaia.In many of the official tinctures, the determination of the alcohol presents no mculty. Mere distillation will’suffice to separate it in a state of approximate purity from the tinctures of aconite, arnica, belladonna, calumbs, capsicum, catechu, jalap, nux vomica, opium, quinia, &c.; and the same is true of the tinctures of iodine, ferric acetate, &c., if they be first rendered distinctly alkaline with caustic soda. On the other hand, the tinctures of benzoin, myrrh, ginger, camphor, rhubarb, &c., give a distillate contaminated with essentid oils or similar volatile matters in quantity sufficient to affect, more or less seriously, the determination of alcohol by the density.The same is true of the d 6 aromatic spirit of ammonia,’’ and tinctures prepared with it, With the additional objection that the distillate will contain ammonia, unless the rtlkacline reaction of the spirit be previously carefully neutralized by hydrochloric aoid. If any of the tinctures to which the distillation process is not directly applicable be diluted considerably with water, the essential oil is precipitated more or less completely, but usually in so fine a state of division that filtration is compIetely useless.I find, however, that this difficulty may be got over very simply by operating in the following manner :-50 C.C. of the sample are taken and diluted with water to about 350 C.C.This causes the precipitation of the greater part of the essential oil or resinous matter. A few drops of a strong solution of calcium chloride are next added, and this is followed by some solution of sodium phosphate, the liquid being vigorously stirred. The flocculent precipitate of calcium phosphate effectually entangles the finely divided essential oil and clarifies the liquid.The liquid is next diluted to a definite volume, 400 C.C. being sufficient if the tincture were prepared with proof spirit, but 500 is preferable if rectified spirit should have been originally employed. The solution is then thoroughly agitated and passed through a dry filter. A known measure is then carefully distilled at 8 low temperature, and the distillate made up exactly to the volume occupied by the liquid before distillation. The density of the distilled spirit is then taken, and the corresponding percentage of proof spirit learnt by reference to a table.Evidently the proportion of proof spirit in the original tincture will be either 8 or 10 times the amount found in the distillate, according to the extent of dilution practised.It is convenient to state the strength of the tincture in percentages of proof spirit, as any deficiency in strength is then at once apparent, and the extent of dilution is readily calculated. With a view of testing the accuracy of this mode of assaying tinctures, I have made various experiments, The following; data, indicate the extent to whioh the process may be relied on, A sample of thcture of myrrh ww prepared according to the directions of the Phamruoopcleia, ma on examination gave the following results :- 8p.Uravity = Proof spirit = Absolute Ahohol by volume. by weight. Spirit used for prepsring tincture.. . . . . . . -8378 166.7 841 Tincture.. . . . . . . . . . . , . . . . . . . . . . . . . . . . 146.0 77.3 16087 80.8 Bpirit in tinoture odoulated from results *8649 I 181.0 80.9 of distillationTHE ANALYST.103 It would appear from these results, that about 6 per cent. less of proof spirit was obtrtined than was present ~JI the dcohol used in prepaxing the tincture, and, therefore, that the method is in error to this extent. This conclusion is not justified, for in the above calculation it is tuisumed that no increase in the bulk of the spirit occurs on saturating it with myrrh; but the following data show that this assumption is not warranted :-5 grammes of myrrh previously dried at looo C.were added to 40 C.C. of rectified spirit of *a280 specific gravity. After standing 48 hours, the tincture waB filtered, the residue washed with a little spirit, dried, and weighed. Its weight was 3.142 grammes, so that 1.858 grammes had dissolved in the spirit.The density of the tincture was found to be -8432. The weight of alcohol used was 0828 x 40 = 33.120 grammes, which, added to the weight of the dissolved myrrh, gives 34-978 as the weight of the tincture. This, divided by the observed density, gives 41.4 c.c., as the measure of the tincture. Hence 100 C.C. would have increased to 103-5 C.C.In another experiment the volume was found to be 103 c.c., and in a third experiment, on double quantities, it came to 104*6. The mean of these estimations is 10387, Thus the percentage of alcoholfound in tincture of myrrh ought to be multiplied by 1.037 to get the true strength of that employed in its preparation. Applying this correction to the alcohol found by distillation of the tincture of myrrh, we obtain 156-3 and 156.6 per cent.of proof spir8, against 156.7 employed in preparing the tincture, a result which leaves nothing to be desired. A very striking example of expansion of the fluid occurs in the preparation of the ‘6 Spirit of Camphor, B.P.” In one experiment I pIaced 10 grammes of camphor in a graduated cylinder, and added 90 C.C.of rectified spirit of 0830 specific gravity, The tincture produced measured exactly 100 c.c., so that, as camphor has a density of 0996, 10 grammes would measure 9.96 c.c., and hence camphor dissolves in alcohol without sensible change of volume. The tincture was found by experiment to have a density of -8446, the theoretical density, assuming no change of volume, being 08466.Therefore the action of alcohol on camphor appears not to be strictly that of a solvent. It seems to act rather by causing liquefaction of the camphor, subsequently mixing with the resultant liquid without notable change of volume. Its action may be compared to that of chloral hydrate on camphor. In consequence of this peculiarity, the proportion by volume of proof spirit oontained in spirit of camphor will be ianths of that present in the alcohol used in its preparation, and there is no doubt that a similar correction ought to be applied in certain other cases.When the modified distillation process already described is applied to spirit of camphor, the determination of the alcohol can only be affected approximately. Even when the spirit is previously diluted with 9 times its volume of water, the distillate has a distinct smell and taste of camphor.This is doubtless a consequence of the solubility of camphor in water, for the distillate obtainelt from tincture of myrrh retains no trace of its. origin. It is very probable that Monell’s colorimetric method* might be advantageously utilized for the estimation of alcohol in spirit of camphor, but I have not been able to try the experiment.* Journ., Chem. Soc,, 1878, II., 246. .104 THE ANALYST. I have not made any attempt to determine the camphor in a spirit or tincture containing it, but may suggest that its action on polarized light would probably afford a fairly accurate means of estimating it. The specific rotatory power of common or dextro-camphor, in alcoholic r3olution, is + 47.4 for the transition tint.My attention has been recently called to the analysis of the offioial ‘‘ Compound Tincture of Camphor,” owing to the following circumstances. A medicd practitioner in Sheffield had reason to aupect some compound tincture of camphor supplied him by R well-known local pharmacist, and so submitted it to a wholesale firm in London, whose ohemist reported it to be deficient in alcohol anit some other constituents.The medical man thereupon, through the agency of n brother practitioner, called the attention of the inspector to the matter and supplied him with a signed written order (in Latin) for 8 oz. of the fiincture, In due course, the sample was procured and stlbmitted to me, and I certified that it contained only about 54 per cent.of absolute alcohol (=71*4 per. cent. of proof spirit), instead of being made with proof spirit, and was nearly destitute of benzoic acid itnd oil of anise. The proportion of opium was not found to be deficient, and I expressed 110 opinion on the proportion of camphor. In the sequel, the vendor was prosecuted and fined $5 and costs. From a consideration of the facts, it seems probable that the proportion of alcohol was cut down from motives of economy.The deficiency of alcohol oompels a considerable reduction in the proportion of the oil of anise, as the weaker spirit used will not dissolve the half-drachm to the pint prescribed by the Pharmacopceia. In devising a method for examining such a complex preparation as the compound tincture of camphor, it appeared desirable to analyse a number of samples of known purity. In this I have been assisted by Mr.L. Siebold, of Manchester, to whom I am indebted for the analytical results obtained by the examination of three samplw of the tinoture, and for a check-analysis of the adulterated sample. In the following description, A and B are specimens of the tincture purcharred br Mr. Siebold in Manchester, and probably prepared with spirit at 600 O.P.C ie a sample prepared by Mr. Siebold himself. C 1 S and C 1 A are the adulterated sample as examined by Mr. Siebold and myself respectively; and C 2, C 3, C 4, and C 5 we samples purchased from well-known Sheffield pharmacists ; C 5 being prepared specially for me. The following are the densities of the original samples, without distillation or my other manipulation :- A B C C 1 S C 1 A C 2 C S C 4 C6; -9147 *9150 *9206; *9608 09633 09231 *9321 *9212 09240 From these figures it is evident that the small proportions of solid constituents present in compound tincture of camphor do not very materially affect the density, and hence that the specific gravity dords a very good approximate indication of the strength of the alcohol with which it was prepared.However, the modified distillation process already described admits of the deter- mination of the alcohol with all desirable accuracy, provided that a slight exeess of alkali be added prior to distillation to prevent volatilization af Irenmic wid. By * The quantity of tincture at Mr. Siebold’s disposal ww very small, and the density wa8 determined by nowg the weight of 10 0.0.THE ANALYST.105 proceeding in this manner, the alcohol is obtained unmixed with anything except the 19 grains per ounce of camphor, an amount which I have proved experimentally has no appreciable influence on the density. The clarification of the liquid with chloride of aalcium and phosphate of sodium is really superfluous in the case of the compound tincture of camphor, for the small proportion of the oil of anise does not affect the densi€y of the distillate, though it renders it milky.A useful modification of the process is to employ chloride of calcium, but to precipitate it with carbonate of sodium instead of the phosphate, aid thus clarify the diluted tincture and render it dkaline at the same time.The experiments made on the samples of compound tincture of camphor already mentioned have shown that the true percentage of proof spirit, as determined by distillation, is never more than two degrees in excess of that deduced from the density of the original tincture. The alkaline liquid which remains in the retort after distilling off the spirit is of service for the determination of the benzoic acid. If concentrated to one-half of the volume of the original tincture employed, it should give an immediate and copious precipitate of benzoic acid on being strongly acidified by concentrated hydrochloric acid.If the acid liquid be then shaken with ether, and the upper layer of liquid removed with w pipette, the benzoic acid is readily obtained in a state of approximate purity.If the etherial layer be transferred to a small beaker, and the ether evaporated spontaneously by a current of dry air from an aspirator or bellows, the benzoic acid remains as a crystahe r e d u e , which may be further examined. If the shaking with ether be repeated the extraction of the benzoic acid is perfect, a very fair approximate determination of its quantity may be obtained, even on as small a quantity as 6 C.C.of the tincture. Chloroform may be substituted for the ether with some little advantage. In the adulterated sample, neither Mr. Siebold nor I could detect any traoe of benzoio acid; the etherial extract was but faintly acid, a re-action which proved to be due to the presence of a trace of meconic acid.A very fair idea of the proportion of opium present in compound tincture of camphor may be obtained by diluting the sample with proof spirit and adding ferric chloride. By comparing the depth of red colour produced with that given by a standard tinuture, in a manner similar to Eggertz’ colorimetric method of determining carbon in steel, a good approximation to the proportion of opium can be obtained.Of course the percentage of meconic acid contained in different samples of opium is somewhat variable, snd hence the determination is but approximate. A useful check is obtained by drying up a known measure of the tincture until the residue ceases to lose weight ; but such a process is quite invalid if the tincture has been artificially cohred by caramel or similar material, a practice which is extremely common, I have recently examined several ssmples of ‘( Paregoric Elixir ” which were found to be wholly destitute of opium.As the name “Paregoric Elixir” was formerly official, and has never been applied to any other preparation than that now represented by the compound tincture of camphor, this omission appears to be a distinct infringement of the Sale of Food and Drugs Act.* a Since this paper was read, two convictions have taken place at Dewsbury for selling k k Paregorio Elixir ” which W ~ S destitute of opium.106 THE ANALYST.The proportion of oil of anise present in a sample of compound tincture of camphor may be judged of by the readiness with which the liquid is precipitated on dilution with water. With a, proper proportion of oil, hardly any dilution can be dected without a milky precipitate being formed. In the case of the adulterated sample already described no precipitation occurred, no matter how much water WRS added. It was also proved by experiment that the proportion of oil of anise which could be dissolved in spirit of 30° 0.P. was but a mere fraction of that taken up by proof spirit. Mr. Siebold found that samples A, B and C were precipitated by water even when mixed with seven volumes of proof sph-it, and from this fact he estimated the proportion of oil of anise in C 1 S at less than one-eighth of the normal amount. In addition to assistance afforded me by Mr. 8iebold, I have to acknowledge my indebtedness to Mr. W, F. Cocker, mho has made most of the test experiments in trial of the processes described in this paper.

ISSN:0003-2654    

DOI:10.1039/AN879040101b

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

106 THE ANALYST. NEW METHOD FOR THE EXABIINATION O F BUTTER FOR FOREIGN FATS, BY DR. J. KOETTSTORFER. [We are indebted to Dr. Duprb, F.R.S., for the following important Translation from the Zeitschrift fiir dnalytische Chemie, von Dr. C. R. Fresenius, 1879, p. 199.1 THE analysis of butter, according to Angell and Hehner’s method, teaches us that this substance contains a far greater proportion of fatty acids with from ten atoms down- wards of carbon than had previously been assumed.Since most other fats contain only the higher fatty acids, and the lower ahids of the series have a smaller molecular weight than these, butter must contain more molecules of acid than an equal weight of mother fat, and from the above it mould appear that the difference in the number of molecules may be not inconsiderable.Therefore it seems feasible to estimate volumetrically the number of equivalents of acids contained in butter and other fats, from the amount of K H 0 necessary for complete saponification, and to distinguish butter from other fats by calculating the differences in potash used. In reality, this difference, as the experiments recorded below show, is such that it may be used for the detection of adulterated butter as readily as the difference between the insoluble fatty acids found in butter and in other fats. This new method for testing butter has the advantage over Angell and Hehner’s that it is much simpler and far more rapid of execution, since an analysis may be finished in half-an-hour, provided all necessary standard solutions are ready.The use of volumetric analysis in the examination of butter is not new. W. Heintz and Dupr6 * have already proposed, as modifications of Angell and Hehner’s method, estimating the soluble acids by titration. By my method, however, which is based on a dzerent principle, the whole of the acids contained in a fat are estimated by titration. The carrying out of the new metilod requires a standard hydrochloric acid and a standard alcoholic potash solution.I am in the habit of using half normal hydrochloric acid and a solution of K IT 0 in highly rectified spirit of about the same strength. As * DuprB’s method was published nearly two years before H&CZ’S.--EDITOBS AXALYBT.THE ANALYST. 107 indicator I use a dilute alcoholic solution of phenol-phtalein, as recommended by Dr.E. Luck, and always add the same quantity in each experiment. The examination of the fats is made as follows :-From 1 to 2 grammes of the fat, purified by melting and filtration, are weighed in a high beaker of about 70 C.C. capacity, 25 C.C. standard alcoholic potash are added, and the whole heated in a water-bath. When the dcohol is nearly boiling the mixture is stirred with a glass rod till all the fat is dissolved, which does not take more than a, minute.The glass rod is washed with a little alcohol and put into a safe place ; the beaker is covered with a, watch-glass and heated further for 15 minutes, in such a manner that the alcohol does not boil too violently. At the end of the quarter of an hour the watch-glass is washed with spirit and the alcoholic solution is stirred for one minute longer with the glass rod before used, so as to saponify any fat that might still adhere to it.The solution is now taken from the water-bath, 1 C.C. of alcoholic solution of phenol-phtalein is added, and it is titrated back with half normal hydrochloric acid. The point of neutrality is very sharply indicated, the liquid becoming pure yellow when changing to the acid re-ao tion.From the difference between the amounts of hydrochloric acid required by 25 C.C. standard alkali and the amount used in the above titration, the amount of E( H 0 combined with the acids of the fat is calculated. As regards the time of heating, I have convinced myself, by repeated experimenttr, that five minutes, as recommended by Aagell and Hehner, is not always sufficient- more particularly in the case of butter, but that a quarter of an hour is always enough to saponify fats completely and give uniform results. Since the titre of an alcoholic potash solution is always lowered slightly when if is heated with access of air in consequence of oxidation of the alcohol, it is advisable to standardise it by heating 25 C.C.for 15 minutes in a water-bath, as in the eaponi- fication of the fat, before testing with the standard acid. The difference between the heated and unheated potash solution amounts to from h t h to + C.C. normal hydrochloric acid. The titre of the potash solution diminishes by the same amount, in the course of five to six days, at ordinw temperature, owing to the oxidation of the alcohol, and it is therefore advisable to control the potash solution from time to time.Standard sulphuric acid cannot well be substituted for the hydrochloric acid, since this yields a precipitate of K,SO,, which masks the final re-action. The saturation capacity of the acids contained in a fat might be expressed in per cents. of KH 0 necessary for saponification.Since, however, 8s shown by the experiments given below, the errors of analyses of several samples of the same fat do not alter the figures in the first decimal, it may be better to convert them into full numbers, and calculate the amount of KHO used by 1000 parts of fat. In the following experiments, I therefore give the number of milligrammes of KH 0 which saponifv 1 gramme fat.SAMPLES OF BUTTER FROM TEIE NEIGHBOURHOOD OF FIUME. Substance 1.-1.224 grms. saponified K H 0 0.27868 p a . = on 1 grm. fat 227.7 rnillipu. H H 0. 9 , ,, 0'34584 ,, - 9 9 7, 227.5 97 9 , ,, ,, 0.32119 ,, - 9 , 9 , 227-1 f , ? ? 1.520 ,, 9 , ,, 0.28101 ,, - 7, 7, 227.4 1 , # I 1.317 ,, I , 9 , 0.29827 9, - 1 , , l 226.9 t 9 I t - - - 1.4145 ,, 1.236 ,, - Mean for 1 grm.fat 227.3 millignns, R H 0.108 THE ANALYST. Substance 2.-1,171 grms. saponified K H 0 0.26645 grms. = on 1 grm. fat 227.5 milligrms. K H 0. Mean for 1 grm. fat 227.2 milligrms. K H 0. Substance 3.-1,436 grms. saponified K H 0 0,32411 grms. = on 1 grm. fat 225.9 milligrms. K H 0. Mean fol' 1 grm. fat 225.7 milligrms. K H 0. Subrjtam 4.-1.403 grms. saponified K H 0 0.32556 gyms. = on 1 grm.fat 232.0 milligrms. K H 0. 99 9 , 9 , 226.8 9 , 1.395 ,, ,, 0,31712 ,, - - 1, - 1.481 ,, ? 9 ,, 0.33401 ,, =; :, 9 , 225.5 9, 9, 1.257 ,, 91 ,, 0.29266 ,, - $ 9 9 9 232.8 9 ) 9 , 1.237 ,, ,? ,, 0.28741 ,, L ! I I , 232.4 1, ,, - - Mean for 1 grm. fat 232.4 milligrms. K H 0. Substance 5.-1.451 grms. saponified K H 0 0-32847 grins. = on 1 grin.fat 226.4 milligrms, R H 0. 9 9 ,, 0.35293 ,, - 1, 9, 226.0 $ 9 9 9 1.470 ,, , l !, 0.33080 ,, - ,? ,, 225.8 1 , - - 1.562 ,, - Mean for 1 grm. fat 226.1 milligrms, K H 0. Substance 6 ~ 1 . 6 4 4 gmns. saponified K H 0 0.36546 grms. = on 1 grm. fat 222.3 milligrms. K H 0. Mean for 1 grm. fat 228.2 milligrms. K H 0. Substance 7.--1.885 grms. sapouitied 11 H 0 0,42632 grms. = 011 1 grm.fat 226.2 milligrms. K H 0. Mean for 1 grm. fat 226.5 milligrms. K H 0. Substance 8,--1.870 grms. saponified K H 0 0.41447 grms. = on 1 grm. fat 231.6 milligrms. K H 0. Mean for 1 grm. fat 221.8 milligrms. K H 0. Substance 9.--1.731 grms. sapollified K H 0 0.39691 grms. = on 1 grm. fat 229.3 milligrms. K H 0. Mean for 1 grm. fat 229.6 milligrms. K H 0. Subatance 10.-1-554 grms.saponified K H 0 0.36002 grms. = on 1 grm. fat 231.7 milligrms. K H 0. Mean for 1 grm. fat 231.3 milligrms. K H 0. 1.898 ,, ,? ,, 0.42137 ,, - 9 , 91 222.0 ,, 9 , - - 1,726 ,, ? 9 ,, 0.39137 ,? - 9, I , 226.8 9, 9, - - 10855 ,, $ 9 ,? 0.41176 ,, - 9, ,! 222.0 ,, 9, -... 1.759 ,, 9 1 ,, 0.40448 ,, - 9 , I > 229.9 ,, 9 , - 9, ,, 9 , 230.9 99 1.744 ,, ,, 0,40273 ,, - - 9 , Cladied butter from a reliable source from Upper Austria, by feeding with green clover, September- bbstance 11.--1.966 grms.saponified K H 0 0.43534 grms. = on 1 grm. fat 221.4 milligrms. K H 0. 1-524 ,, $ 9 ,, 0.33764 ,, - 9, 9 9 221.6 9, 9 , 0,662 ,, 9, ,, 0.14665 ,, - 7 , 9, 221.5 9 , 9, - - Mean for 1 grm. fat 221.5 milligrms. K H 0. Substance 12.--1.571 grms. saponified K H 0 0.35235 grms.= on 1 grm. fat 224.3 milligrms. K H 0. Mean for 1 grm. fat 224.4 milligrms. K H 0. Substance 13.-1*585 grms. saponified K H 0 0.35352 grms. = on 1 grm. fat 223.0 milligrms. K H 0. Mean for 1 grm. fat 223.3 milligrms. K H 0. If we take the clarified butter with the butters, the amount of K H 0 necessary for saponification varies in the thirteen estimations between 221.5 and 232.4 milligrammes for 1 gramme fat-a range of 10-9 milligrammes. Dr.U. Fleischmann has found 85-79 per cent. and 89.73 per cent. as the limits for the acids insoluble in water. If we compare these variations of butters with those found according to my method, they will be found nearly to agree ; since Clarified butter from same source, same feeding, October- 1.716 ,, 9 9 ,, 0,38526 ,, - 9, $ 9 224.5 3 , 9, - Clarified butter from same source, feeding with hay, November- 1.744 ,, I ! ,, 0.38992 ,, - 1, 1, 223.6 9 9 ? P - 221.5: 282.4 = 85-79 : 90.01.THE ANALYBT, 109 For comparison with butters, those fats used for the adulteration of melted butter, or for the manufacture of artificial butter, were examined. stearin, olein and palmitin. By calculation These generally contain 1 gramme steariu combines with 188.8 milligrammen K H 0.1 ,, olein ,, ,, 190.0 f 7 1 7 1 ,, palmitin ,, 9 , 208.0 9, $ 7 It was, therefore, to be expected that such fats would require less K H 0 for saponification than butter. This is found to be the case in the following analyses :- Beef dripping prepared in the laboratory :- Substance14.-lo269 grms.saponiiied K H 0 0.24985 grms. = on 1 grm. fat 196.9 milligrms. K H 0. ,, 0.28421 ,, - - 7 ) 9, 9, 196.1 7 9 9, ,, 0,29644 ,, - 9 , 7 , 196.7 I ? 1, 1.449 ,, 1.909 ,, 9, ,, 0.37448 ,, - 9 ) 9, 196.2 $ 9 1, 1.507 ,, 1 , - - Mean for 1 grm. fat 196.5 milligrms. K H 0. Substance 15.-1.820 grms. saponified K H 0 0.35788 grins. = on 1 grm. fat 196.6 milligrms. K H 0. Commercial tallow- 7 t ,, 0.27839 ,, - $9 ,, 196.9 7 , 9 ) 1.631 ,, 9 , ), 0.32119 ,, - $ 9 $ 9 196.9 3, 9, - I 1.414 ,, Mean for 1 grm.fat 196.8 rnilligrms. K H 0. Substance 16.--1.404 grms. saponified K H 0 0.27480 grms. = on I gym. fat 195.7 milligrms. K H 0. L a d , from kidneys, prepared in the laboratory- 9 , ), 0.26354 ,, - 9, ,, 196.1 9 , 9 7 1.658 ,, 3' ,, 0.32440 ,, - t , Y , 195.7 17 9, - - 1,344 Mean for 1 grm.fat 195.8 milligrms. K H 0. Substance 17.-1*544 grms. saponified K H 0 0.30256 grms. = on 1 grm. fat 196.0 milligrms. E H 0. Lard, from unsmoked bacon, prepared in the laboratory- 9 3 ,, 0.36031 ,, - 9 , $ 9 195.6 ?, 9 ) 1.751 7, ,, 0.34245 ,, - $ 9 ,? 195% 9 9 9 9 - * 1.791 ,, Mean for 1 grm. fat 195.7 milligrms. K H 0. Substmce 18.4.896 grms, saponified K H 0 0.36982 grms. = on 1 grm.fat 195.1 milligrms, E H 0. Commercial lard, professedly American- 1.991 7 , I? ,, 0.38963 ,, - 9, 9 8 195.7 9 9 19 - Mean for 1 gnu. fat 195.4 milligrms. K H 0. Substance 19.-1-608 grms. saponified I(. H 0 0.31653 grms. = on 1 grm. fat 196.9 milligrms, Tc H 0. Mutton dripping, prepared in the laboratory- 1.706 $, $ 9 ,) 093604 ,, - $ 9 $ 9 1974 9 , I? - Mean for 1 grm.fat 197.0 milligrms. K H 0. Substanoe 20.-1°647 grms. saponified K H 0 0.31653 grms. = on 1 grm. oil 192.2 milligrms. K H 0. Olive oil- $1 ,, 0.32644 ,, - $ 7 $ 9 191.7 ,, 1 ) 1-309 ,, 9 9 ,, 0.25068 ,, - 9 , ? y 191.5 $ 7 9 , - 1.703 Mean for 1 grm. fat 191.8 milligrms. I( H 0. Substanoe 21.--2.024 grms. saponified K H 0 0.36080 grms. = on 1 grm. oil 178.3 milligrms.K H 0. Colza oil- 9 , 9 , I , 179.0 1, 1.593 ,, ,, 0,28508 ,, -- - 9 , Mean for 1 grm. oil 178.7 milligrrns. K H 0. The maximum amount of K H 0 necessary for saponification is, according to the preceding analyses, for 1 gramme fat 197 milligrammes, and the difference from butter is lmge enough to be used for the approximate calculation of the percentage of other fats with whioh any given sample of butter may be adulterated.For exauple, in this110 THE ANALYST. plrtoe clarified butter is frequently mixed with lard. Two samples of clttrified butter bought in Fiume yielded the following results- Substance 22.-1.668 grms. saponified K H 0 0.37565 grms, = on 1 grm. fat 226.6 milligrms. I( H 0. 1.622 ,, ?, ,, 0,36779 ,, - 91 , I 226.8 $ 9 9 , - Mean for 1 g m .fat 226.7 milligrms, K H 0. Substame 23.--1.410 grms. saponified K H 0 0.30197 grms. = on 1 grm. fat 214.1 milligrms. K H 0. 9 , 91 Y , 214.5 9 9 1,390 ,) ,, 0.29819 ,, - - 9 , 9 , 9 , 213.6 3 , 1.625 ,, ,, 0,34711 ,, - - 1, $ 9 Mean for 1 grm. fat 214.1 milligrms. K H 0. This shows that the first of the two samples is unadulterated, the second dulterated clarified butter : for according to the previously given analyses of various kinds of butter the minimum amount of K H 0 necessary to saponify 1 gramme butter equals 221.5 milligrammes.Up to now I have, to my regret, been unable toprocure any so-calledoleo-margarin, from which, at present, most of the artificial butter is made. I have, however, received from Saxg some best Vienna Sparbutter (economical butter), made, according to the description which accompanied it, out of 50 kilos.oleo-Daxgarin and 26 litres milk. Since the proportion of butter which this amount of milk could add to the mixture is scarcely 1 per cent., the result of the examination of the fat will differ but slightly from that obtained from oleo-margarin. Oleo-margarin is obtained from beef tallow through separation of stearin.If we take into consideration the above given figures for stearin, olein and palmitin, one 8hodd expect that oleo-margarin, after the separation of stearin which combines with the smallest proportion of K H 0, would require more K H 0 for saponification than tallow. The examination of the economical butter yielded, however, the opposite result. Subattsnoe 24,-1.797 grms.saponified K H 0 0.35206 grms. = on 1 grm, fat 196-9 milligrams. K H 0. Best Vienna economical butter, from Sarg- 1-762 ,, 9 9 l , 0,34274 ,, - 9 , 9 1 195.6 $ 9 11 - Mean for 1 grm. fat 196.8 milligrams. K H 0. The addition of about 1 per cent. butter increases the amount of K H 0 necessary, by 0.2 to 0-3 milligramme; 1 gramme oleo-margarin, from which the sample of eaonomical butter was made, would therefore have required 195.5 milligrammes KH 0 for complete saponification.Beef tallow requires, according to the analyses given under NOS. 14 and 15, 187 7 milligrclmmes KH 0. It seems, therefore, that in the manufacture of oleo- margarin, somewhat more palmitin than stearin is separated: for, if Eltearin were chiefly removed, the oleo-margarin would require more & H 0 for saponification than tallow.As lmd, according to experiments 16, 17 and 18, requires nearly the same amount of KHO for saponification as oleo-margarin, and butter is moatly adulterated with these two substances, we may take the number 195.6 as the basis for calculating the amount of adulteration of a given sample of butter. According to the experiments given under Nos.1-18, the amount of K H 0 necessq to saponify 1 gramme butter or clarified butter, varies between 221-5 and 232.4 milligmmmes. We may, therefore, pass butter 118 pure, 1 gramme of whichTHE ANALYST, 211 requires 221.5 milligrammes or more of K H 0 for saponification, but as impure if it combines with less K H 0. For calculating the amount of admixed foreign fat, the mean of the two extreme values found for butter, namely 227, will probably be best.If we call X the percentage of admixed fat, and N the number of milligrammes of K H 0, which the sample of butter under examination requires for saponification, we obtain (227 - 195.5) : (227 -n) = 100 : x ; and x = (227 -n) x 3-17. In the calculation of the percentages of admixed foreign fats similar differences are found, owing to variations between various samples of butter, as in the method of Angell and Hehner.If, for example, in Calculating experiment No. 23, we take for butter the lowest figure, viz., 221.5 then X = 29 per cent. But if we take the highest, viz., 232.4, the result is 50 per cent., and by using the mean 227, the admixed foreign fat would come to 40 per cent.We might, therefore, if we calculate with the mean number of 227, make a mistake of 10 per cent. Under the most unfavourable condition, 29 per cent, foreign fat might escape detection ; namely, if butter which required 282.4 milligrammes KH 0 has been employed, and the adulterated butter =quires 221.5 milligrammes K H 0 for saponificdion. By using Angell and Hehner’s method, 40 per cent. might, under these conditions, escape detection. Irrespective of the ease with which butter may be examined by this new method, it will in some cases also furnish an insight into the constitution of fats. Besides this, this method may give a means of distinguishing between fats for which the proportions of K H 0 necessary for saponification differ sensibly. Thus, in the above experiments on olive oil and colza oil, the numbers 191.8 and 178.7 were obtthed, differing by 18.1. If once the extreme values have been fixed by a sufficient number of experiments for these two oils, we rnny use the difference between the numbers so fixed, not only for the detection of an adulteration of olive oil by colza oil, but also for calculating approximately the rmmount of adulteration. I reserve for a future time the continustion of the experiments on fats in thia direction, a d the publication of the results in due oourae. FIUME, Novenzber, 1878.

ISSN:0003-2654    

DOI:10.1039/AN8790400106

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

THE ANALYST, 211 A NEW METHOD OF DISTINGUISHING BUTTER FROM SOME OTHXR FATS. BY WILLIAM GUSTAVUS CROOK, Public Analyst for Noruich. EAVINC+ been lately specially engaged in examining several kinds of fat for the purpose of identification, I will, as briefly as I am able, describe a method arrived at, which will in a few minutes distinguish butter from the fat of beef, mutton, or pork, or mixtures of them.The sample to be examined (if in the form of butter) must be first melted and rendered pretty free from water and salt, by filtration if necessary ; ten grains axe then to be put into a test tube, and liquified by placing the tube in hot water at about lCOQ F. ; remove the tube when ready, and add thirty minims of carbolic acid (Calvert’s No. 2 acid, in crystals, one pound ; distilled water, two fluid ounces).Shake the mixture, aad again place it in the water-bath until it is transparent. If the sample thus treated be pure butter, a perfect aolution will be the result; if beef, mutton, or pork fat, the mixture d l Set the tube aside for a time.112 THE ANALYST. resolve itself into two solutions of different densities, with a clear line of demarcation : the denser of the two solutiom, if beef fat, will occupy about 49.7; lard, 49.6; mutton, 44.00 per cent.of the entire volume; when sufficiently cooled, more or less deposit will be observed in the uppermost solution. If olive oil be thus tested, the substratum will occupy about 50 per cent, ; with castor oil, there is no separation. With some solid fats (not likely to be used fraudulently) no separation whatever takes place ; the addition of a minute portion of alkanet root will render the reading of the scale extremely distinct by artificial light. The above method (although not intended to suiyass other processes) is capable of wide application, the saving of a large amount of time, and the reliability of its results will at once recommend it as a first step ” in butter analysis.

ISSN:0003-2654    

DOI:10.1039/AN8790400111

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

112 THE ANALYST. INSTITUTE OF CHEMISTRY. WE have received the reports of the discussions which took place on 27th February and 2nd April, on the subject of the Adulteration of Food. We believe this is the first work, partaking in any degree of a scientific character, which has been undertaken by the Institute since its formation ; and it would, therefore, be hardly just to criticise the matter as closely a6 the proceedings of an older society, and the more so because by reason of the mistaken preference which the Institute has shown for secret meetings, and the iigid exclusion of visitors, several chemists who could have given really useful information were unable to be present.We suppose that this rule will be relaxed in future, since it seems improbable that the Council will exclude visitors from he&g what they can afterwards read, unless indeed the accommodation should prove to be too limited for the members attending. This, liowever, seems unlikely.The discussion was opened by Dr. Voelcker, whose speech extends to some thirteen pages; we can, therefore, only briefly notioe some of its salient points. Dr. Voelcker said there was no difficulty in determining ig whether milk had been adulteratedwith a considerable quantity-say 20 per cent.-of water, or whether skimmed milk had been sold as fresh.” h cases of that kind, the chemical or microscopical examination of the articles in question decides, with certainty, whether they are genuine or adulterated.” This, however, hardly accords with a statement a few lines lower.I need hardly aay that it is now admitted by all personn who possess some knowledge of dairy matters that the composition of equally genuine samples of milk varies greatly.” The speaker then went on to refer to his old milk experiments at Cirenoester, in 1863, and again quoted his analyses of the milk from the half-starved cows, bringing the produce of these wretched animals forward to show how variable milk is.He then referred to the limits laid down some years ago by the Society of Public Analysts, oalling them, however, by the erroneous name of standards.” After acknowledging that some analysts, ‘‘ no doubt very young and inexperienced,” had challenged the accuracy of his analyses, he said that the L L best informed ” of his opponents had altered their views on the milk question, and come round to his own.After a well-deserved passing sneer at half-crown milk analysts, Dr. Voelcker stated that he objected in toto to all milk standards, and characterised the present one as iLsomewhat low,” Four pages of the report are then occupied with a reprint of part of an oldTHE ANALYST. 118 paper on the importance of the hydrometer for determining the adulteration of milk, and mother page with an old paper on cream.Dr. Voelcker, carefully avoiding making any remarks which were capable of criticism in reference to butter, bread, tea, coffee, cocoa, or arrowroot, referred to the well-known selenite water used in making the Worcester vinegar ; and then passing rapidly over colouring matters, metallic poisons, salicylic acid, and spirits, concluded by pointing out what in his view was the absurdity of fining R man for 80 grains of salt per gallon in beer, The President (Dr.Frankland) followed with a few remarks, of which the most novel was the statement that, in taking the specific gravity of milk, the quantity of h t present would exercise no influence on the indications of the lactometer.” Dr.Dupr6 pointed out the error into which Dr. Voelcker had fallen, in calling the limits fixed by the Society of Public Analysts (‘ standards,” and remarked on the special attention which had been paid to these limits in Germany as compared with the consideration they had received in England. Referring to the milk question, he remarked that milk from under-fed cows was certainly not of the nature, quality, and substance demanded, He considered that Dr.Voelcker’s analyses of the milk of such cows had done much harm. In reference to alumina in bread he considered it impossible to lay down a proper limit, except by the comparison of the silica with the alumina present. He pointed out that in the case of flour it was easy to determine the alum by means of his process, already published in THE ANALYST.Referring to butter, Dr. Dupr6 again pointed out the fallacious inferences which may be dram from the sp. gr. only, when mutton fat has been used as an adulterant, and urged the necessity of the determination of both insoluble and soluble acids. With reference to the fines inflicted by some magistrates lie remarked that, by the addition of only 10 per cent.of water to the milk consumed in London, the sum of &150,000 a year would be paid for water. He concluded with a few observations as to the changes which may take place in drugs by long keeping. Dr, Stevenson regretted that Dr. Voelcker’s paper referred to so few subjects, and introduced so little new matter ; he believed that Public Analysts as a body were as trustworthy as the members of any other profession.He thought it would have been well had Dr. Voelcker’s analyses been made by modern methods instead of by methods now soarcely ever adopted by analysts, and considered that the milk of f&irly-fed cows did not present that wide difference which they had heard of that evening. Dr. Redwood thoughatthat spirits should be kept within certain limits, in order to justify the application to them of their popular names.He appeared to think that SO U.P. was a fair and proper strength-for gin, and that lower than that should not be allotred. He justified the addition of annatto to butter and cheese for the purpose of colouring them, but condemned the colouring of pickles with copper. Dr. Tidy objected to a standard in which the analysis of any article as a whole was not taken account of.He stated that, on referring to Dr. Letheby’s old note books, he found that he (Dr. Letheby) examined the milk yielded by two cows for 115 consecutive days. The solids not fat in the milk of one cow never fell below 9 per cent., but in the milk from the other cow, on foyr different occasions, the amount of solids not fat was less than 7.5 per cent.He thought, however, there were ninety-nine chances in a hundred that milk which gave such a figure as thia was adulterated, He gave some114 THE ANA&YST. interesting statistics as to the average total solids found in human milk in health and disease, which led him to the opinion that in some cases the children of diseased women appeared to thrive on milk which contained far less total solids than in other cases where the proportion was abnormally high.Mr. Bell stated that at Somerset House they did not subscribe to the limits laid down by the Society of Public Analysts, because having taken great trouble to investigate the subject of milk, they had found considerable variations in its com- position, and that no one constituent forms a, constant quantity in genuine milk.In judging whether a milk had been watered or not they took the whole of the constituents into account, and formed from these an opinion as to the genuineness or otherwise of the sampl6." Mr. Bell then gave some statistics of the examination which they had made of the character of various samples of milk, which are no doubt of interest, but would have been more so had they been given in a rather more intelligible form.The net result appears to be, that in the case of individual cows 4 per cent. yielded less than 11 per cent. of total solids, and 18 per cent. less than 8.6 per oent, of solids not fat ; while iu the case of dairy mixture 20 per cent. showed less than 12 per cent.of total solids, and 12 per cent. contained less than 8.6 per cent. of solids not fat. In the case of individual cows only 6 per cent. yielded less than 2-45 per cent, of fat, and in the case of dairy mixtures only 4 per cent. were found to contain under 3 per cent. of fat. Mr. Bell evidently considered the Society's limit of 2.5 per cent, fat in milk too low. It appears to us a singularly unfortunate thing, that when Mr. Bell was asked to meet the Society of Public Analysts, in order to give them the very information contained in this speech, and to discuss the matter with those who are presumably most capable of dealing with the subject, he should have sheltered himself behid letter from the Inland Revenue Commissioners stating that they did not '( think it expedient ') he should meet the Society, and then that Mr.Bell should have brought these atatistics forward on an occasion when they could scarcely be discussed with equal knowledge or authority. After a few remarks with reference to the question of salt in beer the discusaion was adjourned. In resuming the discussion on April 214 Professor Attfield said he thought a good deal more should be done towards settling the limits or standards. After healing the remarks of Dr.Voelcker and Mr. Bell, he thought they ought to be revised. He could not subscribe to the statements of the Society. Professor Attfield then criticised at some length the '( limits " of the Society, asking whether even salt must be sold free from arsenic. A communication was then read from Mr.Angel1 on the subject of milk, supporting the Society's standard of 9.0 solids not fat. M i . Hehner somewhat severely criticised Dr. Voelcker's and Mr. Bell's figures, and pointed out that it was incredible that Public Analysts all over the country should have made such an erroneous estimate as 9.0 of solids not fat in milk, as waB * We fancy this remark of Mr.Bell's must be misreported, for a copy of a certificate relating to a milk sample is now lying before us signed by Mr. Bell and his coadjutors, and bearing a date in last month,in which certificate no determination of ash is given, and no estimation of the constituents contained in that ash, and this notwithstanding that the milk had been condemned by a Public Analyst, partly beo&use sdt or other preservative material had been added to it.-EDITORS.hbTbLPsT.THE ANALYST.116 implied by M i . Bell’s statements. He also denounced the sp. gr. of fat process as unreliable for butters, and traced the high percentsge of fatty acids sometimes found at Somerset House to imperfect washing. He concluded by protesting against “ secret ” methods of analysis.Dr. Duprd pointed out that in every case in which he had received a milk containing less than 8.6 per cent, solids not fat, he had given a certificate of adulteration ; and in all those cases a prosecution had ensued, and a fine had been inflicted and paid ; a pretty conclusive proof that the vendors did not dare to appeal. He then brought forward some experiments which entirely controverted the remarks of the President as to the effect of cream on the hydrometer.Dr. Alder Wright made a few remarks in reference to the hydrometer to the same effect. Mr, Neison put the hydrometer question in a still more intelligible form, and pointed out that it was simply a measure of the weight of the column of liquid above it. Mr. Bannister referred to certain articles in THE ANALYST, to show that the term standards was sometimes used instead of limits even in this journal ; but his quotation seems to us to apply really to Mr.Wanklyn’s C‘ standard,” not to the Society’s ((limit.” He then referred to two well-known old cases in which analysts had unquestionably made mistakes, both of which cases were immediately and promptly dealt with by the Society of Public Analysts.Of this latter fact Mr. Bannister made no mention. After a few remarks from Dr. Dupr6, expressing surprise at some remarks of Mr. Bannister’s, Mr. Helm did little more than reiterate Mr. Bell and Mr. Bannister’s statements in reference to milk. He complained however of the low fines when samples were proved to be adulterated, and introduced a personal element into the matter, by pointing out that his own milkman had just been fined.After Mr. Bell had again defended the sp. gr. test for butter, Dr. Alder Wright said he thought the amount of added water should be calculated from the limit used in the case of milk, and not from the average results of general samples ; but, from his remmks, it would appear that he did not understad that this was the course almost invariably taken by Public Analysts.He then referred again to the hydrometer, and clearly showed that the statements first made about it were incorrect. The President, in his concluding remarks, appeared to think that the troublous times of the Public Analysts were coming to a conclusion, and that chemists were rapidly converging to fairly unanimous opinions as to the processes and limits or standards. He thought there should be a difference between the fine inflicted upon the man who intentionally adds water to his milk rtnd the man who sells milk from a poor cow ; and therefore he thought there should be two standards, one of average quality and one of minimum, and that any milk falling between the two should be regarded not as adulterated but as not of the qudity demanded. The President then made some rather strong remarks in reference to low fees paid for analytical determinations, suoh for instance as 2s. Gd. or 5s., and the discussion mas concluded with a vote of thanks to Dr. Voelcker, and its acknowledgment by him.

ISSN:0003-2654    

DOI:10.1039/AN8790400112

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

THE ANALYST. 116 SALE OF FOOD AND DRUGS ACT (1875) AMENDMENT BILL, Mr. Anderson as stmended by the Select Committee. WHEREAS conflicting decisions have been given in England and in Scotland in regard to the meaning and effect of section six of the Sale of Food and Drugs Act, 1875, in this Act referred to 8s the principal Act, and it is expedient, in this respeot and otherwise, to amend the said Act : Be it enacted by the The following is a Copy of the Bill introduced into the House of Commons by116 THE ANALYST.Queen's most Excellent Majesty, by and with the advice and consent of the Lords Spirikal and Temporal, and Commons, in this present Parliament assembled, and by the authority of the same, as follows : 1. This Act may be cited for all purposes as the Sale of Food and Drugs Act Shorttitle.Amendment Act, 1879. 2. In any prosecution under the provisions of the principal Act for selling to the In sale of prejudice of the purchaser any article of food or any drug which is not of the nature, ",,"'t$E subshnc8, and quality of the article demanded by such purchaser, it shall be no defence z:g:&hh.se to any such proseoution to allege that the purchaser, having bought only for analysifi, was for snaIyuie.not prejudiced by such sale. Neither shall it be a good defence to prove that the article of food or drug in question, though defective in nature or in substance or in quality, wag not defective in all three respects. of section seventeen of the principal Act. 3. Any street or open place of public resort shall be held to come within the meaning Exteneion of Act as to Bale in streete, Lo.4. In determining whether an offence has been committed under section six of the Reduction at said Act by selling, to the prejudice of the purchaser, spirits not adulterated otherwise than :fEe$zz by the admixture of water, it shall be a good defence to prove that such admixture has not 25~ercent- under proof.reduced the spirit more than twenty-five degrees under proof for brandy, whisky, or rum, or thirty-five degrees under proof for gin. 6. Every liberty having a separate court of quarter sessions, except a liberty of a z z O & O f 6. The town council of any borough having a separate court of quarter sessions shall be exempt from contributing towards the expenses incurred in the execution of the bomwbnot principal Act in respect of the county within which such borough is situate, and the Ez:ph treasurer of the county shall exclude the expenses so incurred from the account required by analyst.section one hundred and seventeen of the Municipal Corporation Act, 1835, to be sent by him to such town council. borougha w i t h Parliament, or otherwise, a separate police establishment, and being liable to be assessed to sepsrab pouoe, the countyrate of the county within which the borough is situate, shall be paid by the justices of such county the proportionate amount contributed towards the expenses inourred by the county in the execution of the principal Act by the several parishes and parts of psrishes within such borough in respect of the rateable value of the property assessable therein, as ascertained by the valuation lists for the time being in force.8. In all prosecutions under the principal Act, and notwithstanding the provisions of speoial P section twenty of the said Act, the summons to appear before the magistrates shall be timefor pro- servedupon the personcharged with violating the provisions of the said Act within a '-* reasonable time, and in no case exceeding twenty-eight days from the time of the purchase from such person for test purposes of the food or drug, for the sale of which in contravention to the terms of the principal Act the seller is rendered liable to prosecution, and particulars of the offence or offenoes against the said Act of which the seller is aocused, and also the name of the prosecutor, shall be stated on the summons, and the summom shall not be made returnable in a less time than seven days from the day it is served upon the person summoned.cinque port, shall be deemed to be a aounty within the meaning of the said Act. " county." 7. The town council of any borough having under any general or local Act of Proviaionfor vision u to

ISSN:0003-2654    

DOI:10.1039/AN8790400115

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

116 THE ANALYST. CORRESPONDENCE. [The Editors are not responsible for the opinions of their Correspondente.] To THE EDITOR OF L‘ THE ANALYST.” SIR,-M~ ahort ‘‘ Note on Violet Powder ” evidently contains some wholesome truths which have proved very unpalatable to various of your readers, since their anger has made them forget logic, fairness, and even ordinary propriety. With such I can of cour~e not enter into any discussion, but I would ask for space to assure your correspondents, ‘‘ The Manufacturers of the Steamer Over a Globe Violet Powder,” that I am not above learning even from manufacturers of scented selenite powder.If they will, therefore, kindly point out the fallacies and erroneous conclusions contained in my Note, I will carefully consider their statements, and should I find them correct will alter my own accordingly.I must, however, at once protest against the assertion that I have included arsenic au among the oonetiktePts of various violet powderer. I remain, yours, &o., A. DUPR6.THE ANALYST. 117 To TEE EDITOR OF “ THE ANALYST.” SIR,-AS you have called upon me to produce whatever evidence I may have relating to the nature of the 88cch81111 ’ e substances contained in malt wort, and to the detection of oane sugar in wort, will you give me space to wy that I have for a long time pa& been actively engaged in investigating the matter, and have notes of a very large number of experiments, showing, analytically, that the sugar of wort is naidtOSt?, not glucose.But, since my experiments oannot be ~ o m p ~ ~ s e d into the namw eompass of a letter, I trust to be allowed to give them at length at an early meeting of the Swiety of Public Analysts.As far as I could ascertain, the method adopted by the Somerset House chemists to determine the quantity of cane sugar in wort consists in boiling the wort for a few minuteB with a little dilute sulphuric acid, by which treatment dextrin is said not to be affected, cane sugar being converted into glucose, the increase in the amount of saccharine matter capable of reducing Fehling’s solution being calculated as cane sugar. How faulty and untrustworthy this method is, especially when only comparatively small quantities of cane sugar are in question, I tam ready to show. I remain, yours obediently, OTTO HEHNER.

ISSN:0003-2654    

DOI:10.1039/AN8790400116

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

THE ANALYST. 117 THE BATH MILK PROSECUTION, WITH reference to this case, reported on mother page, our readers will probably be interested in the results of Mr. Gatehouse’s experiments, as detailed in the following report :- I, the undersigned Public Analyst for the city and borough of Bath, hereby certify that on Thursday, May lst, 1879, Mr. Francis, of Compton Dando and the Bath Market, brought to my laboratory a tall can (about four feet high) full of milk for experimental investigation.This milk at 9.15 a.m. he proceeded to transfer in my presence into another vessel by means of an ordinary tin milk onp, dipping at intends of a few minutes so that in the course of two and a half hours he had transferred in this manner 25 quarts, being about one-half the quantity originally in the tall tin, He also at the =me time delivered to me a bottle of milk taken from the same tin at the time it ma put therein at his farm.Having analysed the milk in the bottle and also samples of that taken from the tin when first opened and when the dipping was completed, I found the following results :- The City Analytical Laboratory, 36, Broad Street, Bath, May 9th, 1879. Milk from the bottle as origindy plaaea in the tin.Milk from the t ~ p of the tin aa received at 9.15 a.m. Water.. ........ 8692 Water. ......... 74.20 Water.. ........ 8940 Fat.. .......... 3.2 Fat ............ 16-03 Fat 078 Solids not fat .. 9.88 Solids not fat .. 9.77 Solids not fat .. 9.72 Cream ........ 15 per oent. Cream ........ 95 per cent. Crearn ........ 4 per cent.On Monday, May 5th, Mr. Francis at my request supplied me with eight quarts of milk in a milk can of ordinary construction, as used for selling milk in the streets. Five quarts of this milk I transferred during a space of three hours by dipping at intervals of a few minutes from the top of the %ilk, so a8 to disturb the aream as little aB possible, and made the three following analyses of diilerent portions thereof :- Milk taken from the tin at 1045.Water 07.4 Water 07.3 Water .......... 8755 Fat 13.1 Fat 3.4 Fat ............ 2.8 Solids not fat.. 9.4 Solids not fat.. .. 9.3 Solids not fat.. .. 12.45 Cream ........ 13 per cent. Cream .......... 15 per cent. Cream .......... 9 per oent. From these facts I conclude :-1. That the milk originally placed in the tall tin, received by me on May lst, was of excellent quality.2. That this milk had been standing in the tin for a considerable time before it was received, and that its removal from place to place was not suflicient to prevent the cream rising to the surface and remaining there. 3. That by selling milk from such a tin without taking care to mix the contents occasionally, the milk is ultimately reduced to the state of “ skim milk,” losing the greater part of its fat by the cream rising. 4.That by selling milk from theo- open tin in the usual manner, no appreciable difference occurs in the quality of the milk. (Signed) J. W. UATEEOUBS. Milk remaining at 21.50. in the tin ............ 8-11. Milk aa originally in the tin. Milk rmdnhg in the tin at 19.15. ........ .......... .......... ............ Mr. J. Napier has been appointed Public Analyst for Bury St. Edmunds. Mr. W. W. Stoddart harr been appointed Public Analyst for the Borough of Chard. Dr. W. Morgan has been appointed Public Analyst far the Ebrough of Neath,

ISSN:0003-2654    

DOI:10.1039/AN8790400117

出版商:RSC    

年代:1879

数据来源: RSC

摘要:

118 THE ANALYST. LAW REPORTS. SPIRITS OF NITRE AND CREAM OF TARTAR.-John Pennock, grocer, of Norton, was charged at the County Petty Sessions, at Stockton, with selling adulterated spirits of nitre and cream of tartar. Mr. C. H. Archer, of Stockton, defended. Supt. Bell, inspector under the Act, stated that on the 4th February he purchased six ounces of spirits of sweet nitre at the defendant’s shop.He told the defendant it was for purposes of analysis. He divided it into three portions, one of which he gave to the defendant, the second he retained, and the third he sent to Mr. Edger, of Newcastle, the County Analyst, who certified it to contain 25 per cent. more water than genuine iiitre contained. There was a fair proportion of nitrous ether. On the same day he purchased four ounces of cream of tartar, and the same process as mentioned in the first case was gone through.Mr. Edger certified the article to contain an excess of tartrate of lime-tartrate of lime, 8.5 per cent. ; sand, 1.2 per cent. ; sulphate of baryta, 17 per cent. He produced the analyst’s certificate in each case. Mr. Archer said that in the first case his defence was that although the nitre was of inferior quality it was a commercial article, and of the quality usually sold.The first quality of nitre was seldom produced, the second was usually sold in town, and the third was generally sold in the country for cattle. Mr. Bell paid for an inferior article, and he was entitled to no better quality than he got. Mere inferiority was no ground on which to convict a man under the Act, and he therefore asked the bench to dismiss his client.As to the cream of tartar, the tartrate of lime was left in through the mode of production ; and the article, like the nitre, was sold precisely as it was got in the first instance. Mr. Dodgson, of the firm of Mandale, Dodgson and Co., bore out Mr. Archer’s remarks as to the nitre, and added that people objected so much to paying for a superior quality that it was seldom offered ; cream of tartar, he explained, was produced from the crust of wine.The crust of red wine was cleared by means of white clay, and there usually remained a oertain amount of tartrate of lime, and not unfrequently a small quantity of the clay. He supplied the defendant with the nitre, and the cream of tartar.Supt. Bell : And of course you are consequently anxious that there should be no conviction. The bench said they were satisfied that there had been an infringement of the Act, but it mas not a serious one. They fined the defendant 1s. and costs in each case. F3upt. Bell stated that in this case the analyst had certified the sample to contain 24 per cent. mom water than waB contained in genuine nitre.Cream of tartar purchased at the defendant’s was found to be much better than that sold by Mr. Pennock ; it was nearly pure, and a summons had, therefore, not been taken out. -The Defendant said he sold the nitre exaetly as he got it from the wholesale grocers. The Bench : We fine youls. and costs. You must not sell any more of this unless you tell people what it is.h n u IN BREAD.-George Allen, baker, of walsall, was summoned at the instance of &. C. W. Stephens, sanitary inspector, for selling an article of food not compounded of the ingredients demanded, and also for selling bread containing alum, so RS to be injurious to health. The inspector stated that he purchased a two-pound loaf at the shop of defendafit, and forwarded it to Mr.E. W. T. Jones, the Borough Analyst, whose certificate of analysis he produced. The certificate showed that the loaf was adulterated with alum in the proportion of 36 grains to the four-pound loaf, and that such adulteration would tend to render the bread indigestible. Dr. J. Maclachlar, medical officer of health, gave it a8 his opinion that the quantity of alum stated would be likely to make bread injurious to health. Addressing the Bench for the defence, Mr.Nanson said he did not dispute that there was alum in the loaf, but he urged that none was put in by the defendant or at his establishment, and that the flour was used just as it came from the miller. The Bench, after hearing the defendant, considered the case proved, and imposed a fine of $3 and costs (including professional charges), on the first mmmons, the other being withdrawn.The fine and costs amounted to S7 14s. ADULTERATING MILK.-William Berridge, farmer, of Duntox Bassett, near Lutterworth, Leicester, was summoned for selling milk adulterated with water, Mr. Ricketts, solicitor, prosecuted on behalf of the Netropolitan Dairymen’s Society; Mr.Louis Lewis appeared for the defence. Mr. Rickettssaid that the prosecutor in this case-Mr. Thomas Gibson, of Walbrook Dairy, East Road, City Road-was a member of the Dairymen’s Society, and had contracted with the defendant to supply him with milk every day, which was delivered at the Midland Railway terminus. In consequence of some suspicion which he entertained as to the quality of the milk he communicated with the society’s officer.Xr. Parish, who took a sample of some of the milk in a bottle on its arriving at the St. Pancras Station, when it had become the property of Mr. Gibson. The sample was taken to Dr. Stevenson, Public Analyst, who, upon examining it, found it to be adulterated with 14 per cent. of added water. Witnesses having been called to bear out Mr.Ricketts’s statement, Mr. Barstowe said this was the kind of offence he wiahed to get hold of. Aa there appeared to have been no complaints made in the neighbowhood where J. Clay, general dealer, of Norton, was also charged with selling adulterated nitre.THE ANALYST. 119 the defendant carried on his business, he would inflict a somewhat mitigated penalty. He had power to impose a fine of $20.The costs had been heavy in this case, and amounted to $10 10s. and this, with li fine of 25, was the penalty he would inflict. The fine was at once paid. SXIXMING MILK.-& the Bath Police-court, before the Mayor apd other magistrates, Henry Francis, dairyman, of the Market, was summoned for selling milk, which was not of the nature, substance, and quality demanded. Mr.F. H. Moger and Mr. F. S. Clark defended. Mr. Moger stated that Inspector Montrtgu, on the 8th May, bought at a stall, which defendant Kept in the market, some milk, Mr. Montagu informed the person in charge of the stall that it mas purchased for the purpose of being analysed, and divided the sample into three parts. The inspector took a portion to the Public Andyst, Mr.Gatehouse. The certificate of Mr. Gatehouse certified that ‘‘ I received, on the 8th day of April, 1879, of Mr. H. 0. Montagu, a sample of milk in a sealed bottle, labelled No. 5 , signed H. G. M., for analysis, which then weighed seven ounces, and have analysed the same, and declare the result of my analysis to be as follows :-Water, 89-79 ; fat, 1.13; casein, sugar, &c., 8.40; ash, -68; cream, 4 per cent.by volume. I am of opinion that the same is a sample of milk which is deficient in fat to the extent of 66 per cent.” Mr. Gatehouse was examined in support of his certificate ; and the defendant was then called, and aocounted for the absence of fatty matter by constant dipping in the can which contained the milk, and from which milk had been sold four and a-half hours before the sample in question was taken from it, and undertook to supply Mr. Gatehouse with a can of milk to experiment upon, Mr. Gatehouse considering that the constant dipping would, to a certain extent, mix the cream with the milk. After consulting privately together, the Mayor announced that the Bench could not agree on a decision, and therefore the case would be dismissed.

ISSN:0003-2654    

DOI:10.1039/AN8790400118

出版商:RSC    

年代:1879

数据来源: RSC