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1. |
Contents pages |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 041-042
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摘要:
IKCLUDING THE PROCEEDINGS OFTHE “SOCIETY OF PUBLIC ANALYSTS.”I;(/itc;/ , (;. VJ. \\~lGST.K,A Monthly Journal for the information of those interested i n the purity of Foodand Drugs, and in general Analytical and Microscopical Research.[PRICE Gil, 01’ I P S i c b s r r i b r ~ ~ ji. p t , OCTOBER, 1879. r I l l l l l ‘ l I I . P O J t f i r c t . 1 nnil [”’ 43*! hy 1. >lC.rJ<R.lomc ACID TEST Fon h I o r t ~ ~ r . 4 . . By J. C. fjell, F.C.S. 181ON THE RELATION BETWEEN Dr. KOETTSTORFER’SI’ROCEES OF UUTTEII ASSAY. ASD THE OLD PRO-CESSES. Gy 0. W. Vigncr, F.C.S. .............. 182ON THE: IthTIO olr ExPAssrOS BY IiEAT OF BUTTER FAT,&c. By 0. W. Wigiicr, P.C.S.. ................... 183EOTES 0s PETnOLEUN SI’IKIT 011 “ XZXZOLINE.” Ej’ 8.H. Allen, F.C.S................................. 135KOTR ON THE SPECIFIC GILiVl’rY OF LIQUIDS. By L.Siebold, F.C.S. ................................ 189THE APPI.ICATION OF CII~OXOFCIXI is TIIE TLCTISGOF DRUGS. By L. Siebold, F.C.S.. ............... I90ON THE VALUATION OF C1TnA-m OF IROX AND Qumiiis.ASALYST’S REPORT ................................ 193LAW EEPORTS ...................................... 194NOTES OF TRE MONTH ............................. ptjCHEMICAL PATENTS ................................ -00UOOLS RECEIVED .................................. BOOBy P. W. Flctchcr, F.C.S. ........................ 191Pure COMPLETEChemicals. SETS OFQUALITATIVE,QUA N T I TA T l V E ,VO LUiM E TRI C,AND ASSAYA PPA RA TUS._.F I N EST BE I! L I N ScientificPORC ELA i N .Apparatus.-EO ti EM I A NGLASS.-PLA TTN E R’SBLOWPIPE.--EGCERIZCA RJO.’J.--A N DTHOM PS2M‘SFUEL TLSTA PPX RA TUS.16 GRADUATEDINSTRUMENTS.-tIOFMA N N’SX PPARATUS.-ALSOELECTRICAL,G.4 L ‘JA h’lC,P !i E L‘M A TICk PPARk TUS,ec., Rc.A. H. ALLEN, F.C.S.A. D U P R ~ , PH.D., F.R.S., F.C.S.C. HEISCH, F.C.S.TYHQL’.: X‘i 1,:s: hN D EX1’0 L:T.Makers of Apparetus to the Laboratories of tl:e Inland Revenue, Royal Arsenal, Royal MilitaryAcademy, Science Schools, India Offlce, South Kensington, Bco.Catalogues and Estimates sent on application, cizclosing L’iirincss Card foi. Terms, &e.J. IfuTan, PILD., M.A., F.C.S.G. W. WIGNER, F.C.S.A. WYNTER BLYTH, M.R.C.S.C. A. CAMERON, M.D.OTTO HEHNER, F.C.S.E.’CV. T. JOHES, F.C.S.J. FALCONER KING, F.C.S.C. H. PIESSE, Y.C.STHE ANALYST.WORKS BY DR. MUTER, M.A., F.C.S.,President of the Society of Public Analysts ; Public Analyst for Lambeth, Southwark,Bermondsey, Rotherhithe, NBwington, and Wandsworth.Now ready, demy 8v0, with copious Tables, price 7s. 6d.A N INTRODUCTION TO ANALYTICAL CHEMISTRY. For Medicaland Pharmaceutical Students.Now ready, royal avo, Second Edition, cloth, with Analytical Tables and copious Index, price 10s. 6d.A N INTRODUCTION TO PHARMACEUTICAL AND MEDICALCHEMISTY, Theoreti03 and Practical.The book is one of a very useful and original kind, and is brought up, to the latest date, tests and‘‘ Amongst the best chemical treatises of the day, and in many respects superior to any that have yetprooesses published only a few months since being described in their proper places.”-Chemical News.been published.”-Pztbl ic Hca I t h.Third Edition, 600 pp., 8vo. Price 12s. Gd. A KEY TO ORGANIC MATERIA MEDICA.nctive principles of drugs.drugs. Copious index and qualitative courses or resins, &c.Analytical Chemists willfind this a concise and yet complete book of reference for the isolation and examination of theSpecial appendix on the microscopic charactcrs of the starches in food andLONDON : BAILLI~RE, TINDALL & Cox, 20, King William Street, Strand, and nil Booksellers.By A, WYNTER BLYTH, M.R.C.S., F,C,S,, Public Analyst for the County of Devon.NOW READY, crown 8v0, cloth, 12s.6d.PRACTICAL CHEMISTRY (A Manna1 of).DETECTIOW OF PoIsoNs-Organic or Inorganic. With Tables and Diagmms.Analyst.”-Lancet.PART I : ANALYSIS OF FOODS-Flour, Bread, Milk, Butter, Cheese; Tea, Coffee, Cocoa; Alcoholic Liquids; Condiments. P&T II :I‘ Will be used by every‘‘ Stands unrivalled for completeness of information.”-Sanitary Record.LONDON : CHARLES GRIFFIX & Co., Stationers’ Hall Court.By G, W, WIGNER, F.U.S,, one of the Honorary Beoretaries of the Society of Public Analysts;Public Analyst for Greenwich, Plumatead, and Woolwioh DiBtriota,Price, ONE SHILLINQ.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 nt all the Sea-Coast Towns.KENT & Co., Paternoster Row, London ; and at all Railway Bookstalls.E.C E T T X aZ; CO.-aMANUFACTURERS OF BAROMETERS, THERMOMXTERS, 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. Blackley’s Apparatus 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.THE ANALYST, Vols. I. & III,-(Vol. 11. out of Print.)INCLUDING tlie Proceedings of tlie Society of Public Analysts, and embracing a,large number of Original Papers on every branch of Chemical Analysis, with a comprehensiveIndex of Subjects and Names.Edited (under the direction of the Committee of Publication) by G. W. WIONER, F.C.S., andJ. MUTER, Ph.D., F.C.S.Published by BAILLI~RE, TINDALL & Cox, King William Street, Strmd, W.C.Price, bound in cloth, 7s. ; in half-calf, 9s
ISSN:0003-2654
DOI:10.1039/AN87904FP041
出版商:RSC
年代:1879
数据来源: RSC
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2. |
Back matter |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 043-044
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摘要:
THE ANALYST.PURE 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.Now ready, Sixth Edition, price 18s.MODERN MEDICAL THERAPEUTICS.Physicians-English, American, and Foreign.A Compendium of RecentFormuls and Specific Therapentical Directions, from the Practice of Eminent ContemporaryBy GEORGE H. NAPHEYB, A.M., M.D.Now ready, demy 8v0, with copious Tables, price 9s.MATERIA MEDICA AND PHARMACY. or the use of Medical andPliarmacenticaI Students preparing for Examination. By W. HAKDSEL GRIFFITHS, Ph.D.,L.R.C.P., Edin,, &c. Edited by GEORGE F. DUFFEY, M.D., F.C.S., Fcllow and Censor, King andQueen's College of Physicians, Examiner in Materia Medica in the Queen's Uninxsity.Now ready, Fourth Edition, 1s.; or mounted on rollers, Tarnished, 3s. 6d.POSOLOGICAL TABLES : A Classified Chart of Doses ; showing at a glaiiccthe 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 Leclmich School of Medicine.A SMALL LABORATORY to be DISPOSED OF, situate in the EUSTONROAD (near Gomer Street Station), suitable for either Educational or Analytical Purposes. It isfitted up with Operation Table ; Gas and Water laid on ; a Fume Chamber, and a large quantity ofChemicals and Apparatus.-For particulars apply by letter to F. C . S., cwc of 31.PITTMAN, Stationer,2 and 2, Silver Street, Campden Hill, Kensington, W.WANTED, ail engagement as Junior Assistant in a Laboratory.-J. GORDELIEIE,Sit tingbourne THE ANALYST.THE ANGLO-ANERICAN TIN STAMPING COMPANY, LIMITEDSTOUHPORT, WORCESTEX3SI-3CIEE.S E A M L E S S , PLAIN, RETINNED, AND JAPANNED WARE.MAX'FACTTIWRS 01' II,IPBOVED, which in tlictiire : i l l the n b s- nric1i.r ally ac:ioil of ll.:~lt, n i l , 0:' wtXuhx, ill cnlirlary oporntiorls,:: certificate will testify :-Zlc'tcrs t o tho Bnrik of E:iziaiicl, Her ?,Tajestp'G iCIiiit, &(;.Asmy 0.niccs and Ore Flo~:s, HnttoLi Gardell. London, E.C.C%RTITiICITl: 01' ASSAY. Fe11x.m~- 8th, 1879.We esarniiied the sampk ENAIIELLZD P.WS FOX EXA3lIN-~TIOX AND AShLYSIS, r~zrlicd as uxler, am1 fiad thefollowing to b? the wsnlt :Tho pieces of ennmel consist of a silicab ol Soil.:, Aliiminn., and Lime ; entirely froo fr3i-n Anti;?ioq/ and Lea,?.Theenamel, as set npon the pans, coilfirms oiir experinients vith the snmplo of cnamsl itsclf received separately. The pails havebeen subjected to the action both of nwtic acid anil dihite mhieral acids, wliich they resist perfectly. We coiisider, therefore,that as eiirtmelled vare i t is thoroughly adapted for cnlinnrg and domei;tic purposes.For the Ar@c-Anierioan Titi Stamping Compnny. T,hiit~(i.JOHNSON, NATTHEY SG CO.Tlie Anglo-American Till Stainping Go. will be glad to correspond with buyer.-; rc:::irdhig spocinl sizes or patterns of gooctsfcr their innrkets.I~kta':r*n!ed C a t d ~ g ~ , $';.ices, an:l T m m f [ ~ ~ ~ : ~ i ~ h c Z ox rc:).97ic4t;on, or thro:i.?!b m y Mercknnt or Facfor.ExDort Liverpml A:anta, ITENWRY PT,QSH tc Co., 12 a28 12, Tswar 3al!Aitings No-rtii, !Vattar Stre&.Export Lolidon Agents, BROOKER, DORE 8 Go., 2, Rood Lane, Peschurch Strset.WK P PPrinted for the Proprietors by JOHN DAVIS, Olcl Xeiil Coad, 5 E. ; slid pub1ishe:I by BAILLII~E, TIXDALL 6; Cox, IiiilgWilliam Strcet, Strand, V . C . , t o nhoiu nll coiniminicatims chnnld be n d d r e ~ ~ ~ l
ISSN:0003-2654
DOI:10.1039/AN87904BP043
出版商:RSC
年代:1879
数据来源: RSC
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Iodic acid test for morphia |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 181-181
J. Carter Bell,
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摘要:
181 T H E ANALYST. OCTOBER, 1870. SOCIETY O F ’PUBLIC: ANALYSTS. The next Meeting of this Society will be lielcl 011 Weclncsdny, tlie 19th November, at Burlington House. IODIC ACID TEST 3’0% MORPHIA. BY J. CARTER BELL, F.C.S. IN this note I wish to call tlie attention of chemists to this most unsatisfactory test. I n the chief aiialytical works iodic acid is quoted as an important test for morphia.A solution of iodic acid should be mixed with its volume of sulphide of carbon, there should be no cliange of colour; on adding a small quantity of these mixed liquids to morphia, or its salts, either solid or in solution, the iodine is separated from the iodic acid and dissolved by tlie sulphide, ml~icli sinhs to the bottom, acquiiing tl pink or red colour, varying in its intensity according to the quantity of morphia present.This reaction clis tiiignislies morphia froin the other alkaloids which do not decompose iodic acid.” Professor Taylor seems to lay stress upoii tliis test, because a t tliz c i d of his chapter on morphia, lie meutions it again. I n TVutts’ Dic~iona~y the test is also mentioned. Blyth in his Jlmzcal says :-(( One of the best confirmatory tests is the actioii of iodic acid.’’ He even goes farther, and gives a special note upon this test, but no prec autions.Iu Frcsmiiis’ Qitu7iratice, eiglitli eclition, tlic test is mentioned, but with precautions as to its use, thus :-“ As other iiitrogcnous bodies (albumen, caseine, fibrine) likewise reduce iodic acid, this reaction lins oiily a relative value ; l~oiccccr, if aniuioitin is added after tlie iodic acid, tlie fluid becomes colourless, if the separation of iodide has beer1 caused by other substances, whilst tlie coloratioii becomes mnch more inteiise if it is owing to the presence of morphia.” The foregoing statements do not accord with niy experience : for I find that otller substances, such as ipecacuanlia, guaiacum, will produce the pink colour ; a d , also, that airinionia is n o t able to distinguish between tlic piiili colour of morphia and that produced by other substances.This statement may bc! casily verified by putting into n test tube 2 C.C. of a solution of iodic acid (one part of the acid t o 15 of water), and 2 C.C. of bisulpliide of carbon ; to this mixture is added a izlilligramme of hydroclilorate of morpliiiic, slid, on shaking, tlie beautiful pink colour is communicated to the bisulpliide of carbon ; on adding 5 drops of ammonia, the colour disappears. A few drops of ipecacuanlia wine, in the place of the morphia, will produce tlie same result. Such a doubtful test ought to be banished from all toxicological works ; or, if mentioned, should be qualified by tliis stmate- meiit-that if no pinlr colonr is produced, tlie absence of morpliin may be presumed. Professor Taylor, in his Jfeeclical Jiirispricdence, says
ISSN:0003-2654
DOI:10.1039/AN8790400181
出版商:RSC
年代:1879
数据来源: RSC
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On the relation between Dr. Koettstorfer's process of butter assay, and the old processes |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 182-183
G. W. Wigner,
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摘要:
188 THE ANALYST. ON THE RELATION BETWEEN DR. KOETTSTORFER’S PROCESS OF BUTTER ASSAY, AND THE OLD PROCESSES. BY G. W. WIGNER, F.C.S. Rend before the Society of Public Analysts, at 8 l ~ J i i e l d , on 22nd Ampist, 1879. DR. KOETTSTORFER’S process appeared to me likely to prove very valuable in the ordinary analyses of butter, by at least disposing without further labour of most of the genuine samples; but it was obviously impossible to adopt a new process as a basis of an adverse report, uutil it had been thorouglily tested.I t appeared to me, that the most practical mode of testing it mas to submit to this process (in addition to the tests which would otlierwisz have been made) every sample of butter or other fat which was received. I thcre€ore adopted it as an auxiliary process, and have examined nearly 100 samples by it.As a general opinion, I may state that I am well pleased with the process for the piwpose above mentioned. It is not, however, free from its veak points, Carbonic acid acts very much on the colour of phenol-phthalein, and, in order to cnsure fair accuracy, it is essential that the fat slionld be saponified with the alcoholic potash solution in a flask, wliicli certainly ought to be corked with a cork having a notch in the sidc.While tlie alcohol itself is boiling pretty freely there is, of course, no risk of carbonation, but, as soon as the water is adcied to clilnte the soap for titration, tlie risk increases greatly. My experience also indicates the necessity for the use of n very large excess of potash solution, an excess very much larger than mould be ordinarily employed when the fatty acids were to be weighed.It appears desirable to use at least twice as much potash as would be actually required to combine with tlie soap present. Again, in reference to the potash solution itself. I find that a very small amount of colour seriously masks the end of the titration, and it becomes essential to use pure potash, and to keep the solution in hard glass bottles, so as to prevent the additional colour which is often imparted by the decomposition of the glass of comruoii Winchesters, Taking all tliese precautions, however, I find the process a useful one.But I must call special attention to tlie following exceptions :-It is comparatively useless when applied to old samples of butter, which have been alternately heated, and cooled; and, even in the cases of lard and butterine, repeated heating exercises a inom uncertain effect than it does 011 tlie fatty ncid determinntioiz ; but, although useful, it can never come iiito general use as a substitute for the determinations of fattr acids and solablc acids, because any alkalies added to the fat, mhether frandnlentl~, or for supposeJ preservative purposes, entirely upset tlie estimation.Therefore, while it inay bc-and in my opinion is, when properly carried out--a safe process 011 which to pass a buticr RS genuine, it is quite unreliable as a proof that the butter is adulterated. The admixture of three per cent. of carbonate of soda with the salt added to the butter, will, by this process, change the results so much, that a genuine buttel.moul~ be coiidemneil ; 2nd such a perceutage of admixture is one that has been used, while smaller percentages are corninon,THE ANALYST. 183 By the fatty acids’ process, sncli an acliuiskure would liave scarcely any sensible effect, but it ~vould exercise a very important effect on the actual density of the fat, and, indeed, in certain cases, might render the determination of actual density quite fallacious.Unfortunately merely testing the water present in the sample of butter for alkalinity is not sufficient to prove Ivvhetlier alkaline carbonates have been added, and no test seems readily available. I have, therefore, come to the conclusion that it is unsafe and unjust to condemn any sample of butter as adulterated on either the titration or specific gravity processes.I€ the sample passes these tests well it may be relied on as genuine, but it may fail to answer both tests, and yet have no foreign fat mixed with it. In such a case, a full determhiation of loth soluble and insoluble fatty acids, is the only safe course to adopt. Of course, therefore, I view the relation between the actual density, fatty acids and titration results as a matter of no great importance in adulterated samples, but in genuine samples it is otlierwise.Dr, Koettstorfer found tlizlt tlie amount of KHO required by genuine butters ranged from 23.24 to 22-15 per cent. I t is, of course, with the lowest limits only that we have to concern ourselves, and iny oyhion is, that tliis limit is not low enough eveu in the case of fresh saiuples, and that it is very seriously deficient in the case of samples wliicli liavc been kept and s-abjected to even moderate variations of temperature.I have had seveml samples of butter apparently recently made, a d , certainly, h good condition, wliicli have required 2,s little as 21.34, 21.36, 21.50 per cent.of KHO to saponify them, and which have yet given less than 89 per cent. of fatty acids by the flask washing process, and which, independently of the otlier conditions, I certainly would not condemn as adulterated. In my opinion, therefore, the titration process can only be relied on mlien it shows figures liigher than Koettstorfer has put as the limits. As, however, three samples out of every four received are probably genuine, tlio process may be advantageously used for passing these pure samples, provided proper care is taken to carry tlio analysis further if these results are adverse, and it is for this purpose only that tlie process can come into general use. I think that any sample of butter fat, which requires more than 22.60 per cent. KHO for saponification, as determined by the titration process, may safely be passed as genuine ; but that any lower result should be checked by tt full analysis.
ISSN:0003-2654
DOI:10.1039/AN8790400182
出版商:RSC
年代:1879
数据来源: RSC
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5. |
On the ratio of expansion by heat of butter fat, lard fat, and butter substitutes |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 183-185
G. W. Wigner,
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摘要:
THE ANALYST. 183 ON THE RATIO OF EXPANSION BY HEAT OF BUTTER FAT, LARD FAT, AND BUTTER SUBSTITUTES. BY G. W. WIGXER, F.C.S. I HAVE made some accurate deterrniiintioiis of the ratio of expansion of fats, especially butter fat and the fats used for adulterating butter. These determinatioiis will be of service, since, by tlieir use, the specific gravity of melted fats may be taken at temperatures varying within reasonable limits from tlic looo F.usually adopted, and the results so obtained may be directly compared with the specific gravity at looo. They will, also, have the advantage of rendering tlie use of tlie specific gravity bubbles, which I proposed some years ago::: for this purpose, more convehieut. #t See ANALYST, vole i., 1). 146.184 THE ANALYST. I have tested the ratio of expansion of butter fat for every 50 betmeen looo Falir.and Tlie determinations have been made independently by three different processes. 1st. By direct weighing of the melted fat in a specific gravity bottle, wit11 thermometer stopper. At tlie higher temperatures this method is certainly open to greater errors than are desirable, on account of the low conductivity of the melted fat for heat, which reiiders it a long task to secure an absolute temperature throughout the bottle.Tliis process would, lxoba>bly, give the most accurate results, if it were not for tlie tendelicy of the different €ah to crystallize, and, apparently, to Borne extent to separate when enclosed in the bulb, without the possibility of agitating them. This latter process gives results slightly inferior in accuracy to the other processes, when they are carried out in the most careful way ; but it is yet so simple and certain in its results, that it is impossible, with ordinary care, to incur any error which is of importance, when tlie process is used for analytical purposes, I have not corrected thc figures for tlie cubical expansion of glass, because ',he results are primarily intencled for the use of analysts who will mcigli tlie fats, or measure them in glass vessels, as I have done.1 s t . E.rpnnsion 01 Pure Butter Fat.-100 volumes of pure butter fat, at looo F., expaiid to 1047.2 volumes, at 2120 F. This result is the average of seven closely agreeing determinations, on four different samples of butter.This gives an average expansion of 00434 per degree F., or e0780 per degree Centigrade. The ratio of expaiisioii is not absolutely uniform throughout, but differs between 150° and 100° I!. From 100° I?. to 150° F. it is smsibly in accordance with the average ; from 150" F. to 190° F. it incrcascs sliglitly ; and from 190@ F. to 210° F, it appears to expand at its former rate of *0434".This change in the ratio of expansion is morc clearly shown by tlie lithographed diagraiu wliicli accompanies this paper. At first I was inclined t o attribute tliis cliangc to a partial decomposition of some of tlie constituents of the fat, but, on examining a sample of lard in the same way, I fouiicl that an almost identical change took place, and at nearly the same temperatures.Since lard has already been melted at much higher temperatures, and is practically free from tlie soluble and volatile fatty acids, tliis explanation seems donbtful. An artificial butter-" butterine," also showed a similar abnormal rate of expansion, but I cannot speak so exactly as to the temperatures at which the ratio changed. 2nd. Exyamion of Lard and Bzctteo.ine.-Tlie average expansion of lard and butterine (animal) are almost identical.The average ratio for lard, as deduced from tlie experiments, is *0420 per degree F. Tlie difference from the butter ratio is so small that it is of no importance for analytical purposes, except for wide ranges of temperature. It will bc more coiivenieiit for the use of these figures in the detection of nclulteratioii, to reduce these results to the ordinary figures of actual density, as compared with water at 100 O , Actual density, strictly speaking, is weight, as compared with the weight of the same bulk of water at the same temperature, and it was in this sense tliat lluter first used the term in butter analysis, but it is not convenient to 212O.2nd. By means of thermometer tubes with large bulbs.3rd. By means of specific gravity bubbles of various weights.RATIO OF EXPANSION OF FATS (3. W. WIGNER, ‘‘ The Analy6t,” OCTOBER, 1879. I [ I 1 ______l___-l_ .___- ----------- ----I---- -_ I ~~ i i I I 1 , I , I I 1 I I I I 1 1 I i I I I I I . I 1 1 I l l 1 I 1 I I I I t ’ . I I . . . . . < . . . I . , , , I . , . , . . : . . . ! , . . , ! , , , , , , ., , , ! ! ! , ! ,.!!H,!! . . . _ _ ! . . I . A Aotud Density of Lard at3 oombined with water at looo. B P P ,, Butter of 911O Actud Deneity. c *P ,, Mixed Butters of 912.6 Actud Density. D Curve of Expansion of Mhter. (The figures of weight do not apply to this curve.) At??&&i?lW* 860 a70 1890 ,800 ‘910 920 0’THE ANALYST. 185 follow this rule at temperatures above 100 O, because whereas water expands more rapidly with increase of temperature, fats do not do so.I therefore compare all the figures obtained with water at looo as the standard. Assuming the limit of 911 as the lowest average actual density of a genuine butter at 1000 F., we obtain the following rule : If the temperature exceed looo F., add to the actual density found by weighing *377 per lo F.of excess temperature over the loo0. It is obvious that the correction to be applied to fats, of slightly lower specific gravity, will scarcely differ from this. In practice it will generally be found that more accurate results can be obtained, by allowing for the error of temperature by this calculation, than by endeavouring to secure an absolute temperature of 1000 F.The diagram of the expansion of the fat will, however, be of assistance in enabling the specific gravity bubbles to be used for the purpose of taking the actual densities of fats. These bubbles expand under the influence of heat, very nearly in the same ratio as the ordinary specific gravity bottles ; in other words, notwithstanding the different conditions under which specific gravity bottles and bubbles are made, the cubical expansion corresponds very closely, and, consequently, in this respect no sensible error is incurred by the use of the bubbles, since the results obtained are practically identical with those which would be obtained by weighing in glass bottles.An accurate determination of the specific gravity of a bubble, at a temperature of 60°, d l be all that is necessary; or, if preferred, the actual specific gravity of the bubble may be f o l d by testing it on melted fat, the actual density of which has been accurately determined at looo, and calculating the result obtained from the expansion of the fat.I need hardly point out that it is useless to rely on any approach to accuracy in the bubbles as sold. I believe this inaccuracy is mainly due to the bubbles being marked before the glass has assumed its permanent form.If the sample of fat to be tested is gently and slowly heated, until the bubble of known specific gravity begins to fall, and the temperature of the fat noted, a glance at the diagram will shom’at once the agtual density of the fat at looo F. Every degree F. difference of temperature corresponds to -377 of actual density, and, as it is perfectly easy to determine the sinking point to *5 F., the actual density can in this way be ascertained to within *20, which is as near an approach to accuracy as is-requisite in most cases, or even practicable, from a single experimental weighing. Should the specific gravity determinations not coincide with those of a genuine fat, a further anrtlysis is in any case essential.
ISSN:0003-2654
DOI:10.1039/AN8790400183
出版商:RSC
年代:1879
数据来源: RSC
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6. |
British Pharmaceutical Conference. Notes on petroleum spirit or “benzoline.” |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 185-189
Alfred H. Allen,
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摘要:
THE ANALYST. 185 BRITISH PHARMACEUTICAL CONFERENCE. The following are abstracts oj‘ sonte of the Papers q*ead at the Meeting at Shefield in August last :- NOTES ON PETROLEUM SPIRIT OR “BENZOLINE,’’ BY ALFRED H. ALLEN, F.C.S, ALTHOUGH it is well known to professional chemists that petroleum spirit is composed of hydrocarbons quite distinct from those coiistitutiiig coal-tar usphtha, among the general public, and to il certain extent among people possessed of some knowledge of186 THE ANALYST.chemistry, great coihsioii has arisen as to tlie nature of tlie liquids hiowii iii commerce its (‘ benzine,” ‘‘ benzene,” beiizol,” niid 6 L beiizoline.” Of these, tho liyclrocarboii h i d or ~ C I L : P I ~ C , C,H,, is tlic cliief niid clinractcristic coiistituent of coal-tar naplitliit, vhile it is present in very iiisigiiificaiit amouiit in petrolcum spirit or mineral naplitlin.‘The terms bewine ancl b e x o l i n e liave no scientific application, ancl are merely commercial names for petroleum spirit. It is owing, in a great measure, to tlie similarity of these names to those of tlie cliief constituent of coal-tar naphtha that coiifmion lias occurrccl, h i t it has been made far worse by tlie acciclental or intentional substitution of one liquid for the other, until it is clifficalt to obtain the coal-ttir prodnct retail, even when it is asked for by its proper name.This would be-of but little consequence if the two liquids were of exactly similar naturc, but ili certain cases they present decided differences of beliavionr, although in general characters tliere are very close resemblances.The following tabular s t 5 t em en t of tlie character is t ic cliff ereii c c s bet me cii petroleum spirit and coal-tar naplitha has been compiled froin various sourcos ,znd iiicludes a few original tests. All the characters given have been carefully verified by acturtl experiment on representative samples of commercial petroleum spirit and coal-tar benzol.Petroletm Spirit, ‘‘ bcnzoliire,” or ’‘ beniiiic.” 1. Consists of hptnne, C7111 $, aiiJ its honio- 2. Heptane ccntains 84.0 per cent. of carbon. 8. Burns with a somewhat smoky flame. 4. Commences to boil a t 619 to GOD C. 6. Specific grnvity about a 6 9 to *72. G . Smells of petroleum. 7. Dissolvcs iodine, forming a solutioii of a lognes.rsqberry rcd colour. 8. Does not sensibly dissolve pitch, auci is s-arcely coloui.ed by it, even on proloiigecl contact. 9. Wlien slii&en in the cold with oce-third of its volume of fused crystals of absolutc carbolic i-xid, tlie latter reniniiis undissolved. 10. Requires two volumes of absolute alcohol, or four or five volumes o€ inetliylated spirit of -838 specific gl’avity for coinplete solution a t the ordinary temperature.Cod- Tll)’ NclphtlLn, 0)’ ‘( lMl1201.” I. Consists of benzene, C,H,, and its honio- 3. Benzene contains 02.3 per cent. of carbon. 3. Curils with a very smoky flame. 4. Commences to boil at, about 80° C. 5. Specific grnvity about ~88. 6. Smells of coal-tar. 7. Dissoires iodine, forming a liquid having the colour of a solution of potassium perinan- ganate.8. licaclily dissolves pitch, forming a deep browi soln tioii. logucs. 9. Miscible with nbsolnte carbolic acid in all yroprtions. 10. Miscible with absolute alcohol in all pro- portions. Forins tl homogeneous liquid with an equal measure of methylated spirit of -825 specific gravity. Althongli the foregoing tests are abundantly sufficient for the distiuzti0:l of petroleum spirit aiici bmzol, wlien applied to mixtures of the two products they aye of but little value even as qualitative indications, and in that case the density is the only one of thc above characters which is capable of giving even an approximatiou to the quantities in whicli the coiistitueiit liquids are mixed.Tlic actioii of nitric acid 011 coal-tar naplitlin is well known to result h the formatioil of iiitrobenzerie niid its liomologues, and litts been employed by Schorlemmer for detecting traces of benzenc, kc., in petroleum.On the other hand, tlie action of nitric acid on the liydrocsrbons of tlie paraffin series, which constitute practically the whole of petroleum spirit, is almost nil in tlic cold, even if fiming acid be used, aiid is veryTHE ANALYST.187 limited iii csteiit if liot acid be employed, p:.oviC!ccl that tlie very strongest be avoitled. I found by experiment tlist the action of nitric acid on petroleum spirit was, uiider certain conditions, even more limited than I had stpposed, and eventually I found that by employing the acid in a particular manner, it was not only possible but easy to effect a tolerably perfect quantitative separation of coal-tar naphtha aiid yetrolenm spirit.The following was the moiIe of treatment eventually employed-, and, by adliering to it, it is possible to detect and approximately estimate the proportion of petrolemu spirit existing in a mixture of it with benzol, in ten or fifteen minutes : A known measure of the sample (from 4 to G c.c.) vas treated with four times its measure of yellow nitric acid of 1.45 specific gmvitj-.Tlic mixture i ~ n s mads in n flask, to which a coiideiising arrangement was attached. Slight licat was npplid externally by ixeans of a flame if the spontaneous action mas not sufficiently vigorous. After about five miniites tlic contents of the flasli were cooled, and then poured into a iiarrow graduated tube.Any oily layer was measured and removed with a pipette, and the remaining liquid poured into a large excess of water. When ordinary petroleurn spirit is thus treated the nitric acid becomes coloured more or less brown. Very little heat is evolved, but on applying moderate liest externally tlie production of red fumes proves the occurrence of a certain amount of action.The effect, however, is not so violent as I had anticipated from a perusal of Schorlemmer’s description of the reaction, and, if the experiment be carefully made, the petroleum spirit employed forms a layer on tlie nitric acid, and 011 transferring tho liquid to a graduated tube is found to occupy the original volume of tlic sample usr~l. This is true whether petroleum spirit alone be operated on or wlietlier it be previously mixed with various proportions of coal-tar naphtha.If the proportion of the latter be large, the quantity of nitrobenzene forrne.1 is larger than can be retained in permaiieiit solution in the nitric acid. This fact causes no iiiconveiiience, for the nitrobenzene forms a separate layer bclow the petroleum spirit, and in preseiice of nitric acid is not miscible with it.Nitrobenzene and petroleum spirit are perfectly miscible alone, but on shaking the mixture with strong nitric acid tlie nitrobenzene is dissolved out. It will be seen, therefore, tliat the react’ion with nitric acid may be conveiiiently employed for the determinatioii of petroleum spirit in admixture with benzene, Very fair approximate results are obtainable. If t h e layer of petroleurn spirit be removed mitli a pipette and shaken with water to remove dissolved nitrous fumes, it is obttiined in a suitable condition for further exaixination.If, after removing the layer of unacteci-on petroleum spirit, the nitric acid solution be poured into water, a very sensible turbidity is usually produced, even with petroleum spirit free from coal-tnr prodncts, aiid on filtc~iiig of7 the precipitate, or allowing it to settle, and decanting the liquid, distinct evidence of tlie formation of nitrobenzene is obtainable by the aniline test.When the more volatile portion of petroleum spirit is thus treated, tlie nitric acid is scarcely coloured at all, and hardly a trace of milkiness is produced when tlie acid is poured into wfxr.Tlie brown colour and turbidity 011 dilution increase with the boiling point of the sample of naphtha, and are strongest with kerosine oil ; but in a11 cases in which petroleurn prodncts arc treated with nitric acid, the quantity of precipitate 011 ililution is very insignificnnt. A1 ttli~i,o1i nitrobenzene is188 T€IE ANALYST. recognizable among the products of the sctioii of nitric acid on petroleum spirit, as was shown long since by Schorlemmer, I do not think tlie turbidity prodncecl on dilution is clue solely to its formatioil.It' is probably rather due to tlie production of various nitro-substitutioii products, as it is wll known tliat the higher numbers of the paraffin series are far inore readily acted on by nitric acid tlian their lower liomologues.I lime attempted to determine tlie proportion of benzene in a mixtiwe with petroleum spirit, by measuring the nitrobenzene produced, but the results have not been satisfactory, partly in consequence of tlie solubility of nitrobenzene in water and acid liquids. By employing 250 C.C. of water for dilution, allowing the nitrobenzene to settle completely, decantiiig tlie greater part of tlie water, and pouring the '' bottoms '' into a graduated tube, the nitrobenzene may be readily measured.If an allonranee of 1.5 C.C. be madc for solubility in the one-quarter litre of acid liquid, the measure of benzene present in the sample taken may be rouglily ascertained by multiplying the number of C.C. of nitrobenzene obtained by tlie factor 0.85.Thus if V be the volumc in C.C. of nitrobenzene, then the benzene in tlie amouiit of szuple taken mas (V+ 1.5) x ~ 8 5 . The method is not capable of giving actual results, but may be useful in some cases as a check 011 tlie deterininatioii of petroleum spirit by m2asurement of the layer insoluble iii nitric acid. With a view of learning something respecting tlie proportion of lieptane present in ordinary petroleum spirit, I madc a mixtiire in equal measures of fonr samples of commercial '' benzoline," such as is ascd for sponge lamps.This mixed specimen had a density of -7001 a t 15.5O C., and commenced to boil at abont 5 4 O C. It was distilled in the manner first described by Warren, in a flask furnished with an inverted condenser, filled ivit1-L water, inaiiitained at a temperatnre of 70° C., a second condenser being kept well cooled by a current of cold water.The distillation ceased when tlie temperature in tlie flask was 840 C., that is, 14" C. above that of ihe first condensei-. Tlie water in the first condenser was tlien raised to the boiling point, and the distillatioii continned till scarcely any more came over, by vhich time the contents of the flask wore at 114O C.The result of tlie distillation was as follows-for 100 measures of petroleum spirit t a ,1 {en :- Condensed Condensed Condensed between above $$; 700 and IOOQC. loop C. (reRidne). Percentage by measure . . . . . . . . . . . . . . . . 16 58 26 Deiisity at 15.5Q C., compared wit11 watcr at mine temperature .. . . *G67 ,707 .r ('4, 0 Tlie loss ~ v a s abont 2 per cent. of tlic original incns~irc. Another sl~cciirieii of petrolenm spirit gave 224 measures of distillate with the receiver a t 70° C., 42 per cent, betjveen 700 and 1000 C., and 32 per cent. of residue ; thc loss being 3+ per cent. Tile densities of the tllree prodncts jyere a h o s t identical with those previously obtained. Tl1e observed specific gravities of tlie first and second distillates correspond approximately with tlie recordcd deiisities of liesaiie niicl heptsne, and from this and tlie knowii boiling points of these liqiiids it is evident that tlie portion of petrolcim spirit not coiiileiised a t 70" C. will consist chiefly of hexane and lover hornolognes, nTllile the part condensed at 700 C., but distilling at 100" C., will be chiefly heptancTHE ANALYST. 189 and isoheptane. As, in tlle experiments described, this fraction measured from 42 to 56 per cent. of the entire spirit, it is evident that the proportion of heptane present equals if it does not exceed that of dl the other constituents.':
ISSN:0003-2654
DOI:10.1039/AN8790400185
出版商:RSC
年代:1879
数据来源: RSC
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7. |
Note on the specific gravity of liquids |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 189-190
L. Siebold,
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摘要:
THE ANALYST. 189 NOTE ON THE SPECIFIC GRAVITY OF LIQUIDS. BY L. SIEBOLD, F.C.S. While tlie great usefulness of the liydrometer for the rapid determination of tlie specific gravity of all lrinds of clear liqnids is universally recognized, there appears to be aiiytliing but unanimity of opinion as to the value of this instrument as an indicator of the specific gravity of mixtures owing part of their weiglit to tlie presence of uii- dissolved or suspended matter.I have therefore made a number of experiments wit11 tlie object of deciding whetlier or not the indications of the hydrometer may be depended upon in tlie case of mixtures containing insoluble powders, oils, resins, kc., uiiiformly suspended. The results were as follows :- Xixturcs of Przcipitated Chalk, Mucilnge of Acacia, Syrup altd Watey- Specific gravity Specific gravity by hydrometer. by balance.No. 1. . . . . . . . . 1.106 .. 1.1066 .. 2. . . . . . . . . 1.070 .. 1.0710 Uixcfures of X q n e s i a , N u c i l a g e aiid Jb-uter- Specific grauity Specific gravity by hydrometer. by balance, No. 1. . . . . . . . . 1.039 .. 1.0598 ,, 2. . . . . . . . . 1.036 .. 1.0359 DIixture of Precipitated Chalk and W’ater only- Specific gravity Speciflc gravity by hydrometer.by balance. 1.037 .. 1.0396 Tlie difference in this case arose from the fact that it was impossible to read off tlie specific gravity quickly enough, for in the absence of the mucilage or any other binding substance, the chalk began to subside immediately after shaking, thus causing a continual decrease in the specific gravity, Mixtures containing subnitrate of bismuth, heavy spar and other mineral powders, each suspended by mucilage, were tested in the same manner and likewise gave con- cqrdant results.Emulsions of Oil of Almonds, Giiin Acncia, and V a t u - Specific gravity Specific gravity by hydrometer. by balance. No. 1. . . . . . . . . 1.010 .. 1.0110 .. 2. . . . .. . . . 1.007 .. 1.0070 Emulsion of Coliaiba, Xucilnge and Water- Specific gravity Specific gravity by hydrometer. by balance. 1.014 a . 1.0144 * The physical properties of the benzoliiie examined by me are very different from those attributed to the liquid by Wiederhold, who on fractionally distilling benzoline of *716 sp. gr., which commenced to boil at GOo, obtained- 48.6 per cent.of -70 sp. gr., boiling at loo0. 45.7 ,, -73 ) ) ,, 200”. 6.7 ,, ‘80 .. I . above 2003.190 THE ANALYST. VCZ r i m s sn Iitples n f illill; - Spscilic gravity Specific gravity by hydrometer. by babncc. So. 1. . . . . . . . . 1.030 .. 1-0305 .. 2. . . . . . . . . 1.028 .. 1.0278 , , 3 . . . . . . . . . 1.032 .. 1.0316 ,, 4. . . . . . . . . 1.029 * . 1.0300 Spxific grarity by belance.1.1670 Tlie last determination was made in order to see wlietlier tlic gred viscosity of thc liquid would have aiiy notable effect on tha iiidications of tlie hydrometer. All the determinations were made at 62Q F. The set of liydrometers used consisted of instruments specially made for very short ranges of specific gravities, the correctness of which I had frequently checked in previous detcminations. The foregoing experiments prove that carefully made hydrometers aflord reliable iiidications of tlie specific gravities of liquids, no matter whether their gravity is due t o dissolved or suspended substances.
ISSN:0003-2654
DOI:10.1039/AN8790400189
出版商:RSC
年代:1879
数据来源: RSC
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8. |
The application of Chloroform in the testing of drugs |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 190-191
L. Siebold,
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摘要:
190 THE ANALYST. THE APPLICATION O F CHLOROFORM I N THE TESTING OF DRUGS. BY L. SIEBOLD, F.C.S. In the ‘ Year-Book of Pliarmacy ’ for 1877 there occurs an abstract of an article by Dr. C. Himly on tlie Detection of lfineral Adnltsrants 111 Yloiir by means of Chloroform. Having frequently tried this test and finding it extremely useful both as n qualitative and as a qmntitativc process, it appeared to ine desirable to ascertaiu to what extent it might be advantageously employed in the testing of powdcred vegetable drugs.As many of the latter are liglitcr tlinii cliloroform, aid the usual mineral adulterants sink in that liqiiicl, it m s but reasonable to infer that this mode of seyaratioii might prove of ndue to the pharmacist. I will not trouble tlic meeting with the details of my experiments, but confine myself to a, brief summary of the results, In each experiment (?I small quantity of the dry powder mas well shalreii witli about half a test-tubeful of chloroform, and the mixture allowed to stand at rest for twelve hours.The following drugs were found to rise so completely to the surface of the chloroform, that the observation and estimation of any mineral adulterant became a very simple and easy task :-Acacia, tragacanth, starches, myrrh, Barbadoes aloes, jalap, saffron, cinchonas, nux vomica, mustard, white pepper, capsicum, aiid guarana.Known quail tities of selenite and of chalk were added to these drugs, and subsequently determined by running tlie lower stratam of the chloroform with the sediment into a small dish, carefully pouring off the chloroform, drying the sediment at a gentle heat and weighing it.The result in each case was very satisfactory. No such accuracy could be attained by incineration, as in the presence of clialk there was always n loss of carbonic acid, anctin that of selenite a loss of water and of oxygen, the sulphate being partly reduced to sulphide. An estimation of these adulterants by the usual analytical processes would, of course, give exact results, but prove much more tedious.Both for qualitative and for quantitative purposes, the chloroform test thereforeTHE ANALYST. 191 answers extremely well with tlie drugs named. In the case of the following substaiices no complete rise to the surface of the chloroform took place, but a portion was found to float and another portion to sink, though the absence of mineral adulterants was proved by analysis :-Gamboge, scammony, opium, Socotrine aloes, liquorice root, ginger, colocyn th, C O U S S ~ , ipecacuaiiha, cinnamon and cardamoms.Of the last two by far the greater portion was found to sink in chloroform. But even in these cases the test is not altogether without value, for a careful inspection of the sediment will show whether or not it is a mixture of various substances, differing in appearance, weight, kc.The mineral adulterant will generally, in such a case, form the lowest stratum of the sediment. A comparison witli a genuine sample helps to arrive at a correct conclusion. Moreover the chemical examination of the sediment gives results which cannot always be obtained by testing the ash.Take the case of cinnamon, for instance, wliich contains organic calcium salts. These upon incineration leave calcium carbonate, a i d a qualitative analysis of the ssh would therefore fail to show whether this calcium carbonate was solely the result of ignition, or whether n part of it pre-existed in the cinnamon powder as an adulterant ; while the addition of hydrochloric acid to the lowest stratum of the chloroform sediment would settle this point at once. It is, however, in the case of the drugs first iiamed that I wish specially to recommend this mode of testing to pharmacists,
ISSN:0003-2654
DOI:10.1039/AN8790400190
出版商:RSC
年代:1879
数据来源: RSC
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9. |
On the valuation of citrate of iron and quinine |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 191-194
Frederick W. Fletcher,
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THE ANALYST. 191 ON THE VALUATION OF CITRATZ OF IRON AND QUININE. BY FREDEXICK W. FLETCHER, F.C.S. THE author said that observations have hitherto been confined, with scarcely an exception, to the determination of tlie total alkaloid present in the citrate, without regard to its purity as quinine. He had adapted to this salt the process described by Dr. Paul for testing quinine, in the valuable paper which he communicated to tlie Pharmaceutical Society at an evening meeting in February, 1877.Dr. Paul had stated that a sample of sulphate of quinine, containing an admixture o€ no less than 30 per cent. of cinchonidine, might, if examined by the Pharumcopceia test, be passed as pure quinine. The author had found 10, 15, and even 25 per cent. of sulphate of cinchoni- dine in foreign quinines, which would, however, pass the Pharmacopoeia test.Nor will the PharmacopoPlia test detect cinchonidine in citrate of iron and quinine. The alkaloid obtained from the citrGte in tlie manner directed in the Phar.macopceia will dissolve in pure ether, even though 25 per cent. of its weight is cinchonidine. The adaptation of Dr. Paul's plan of fractional crystallisation, which the author had devised, is easy of application, a d althou$h a considerable quantity of the citrate has to be operated upon, there is little or no loss of quinine, most of the alkaloid being recovered as sulphate.It has, moreover, the advantage of combining three operations in one, as the results in- dicate :-(I) The exact amount of anhydrous alkaloid ; (2) the'proportion of the latter which can be converted into crystallisable sulphttte of quinine, and (3) the percentage of alkaloids other than quinine.The operations involved are briefly as follows :-Place 20 grammes of the citrste in 100 C.C. flask, dissolve in 50 C.C. of distilled water, and add gradually an excess of ammonia (*960), shaking well after each addition, This is important, in order that the192 THE ANALYST.quinine may separate in a state of fine division, as otlierwise it is apt to be thrown out in tough lumps, difficult of subsequent solution. Pour in 25 C.C. of washed ether, and agitate with a rotatory motion till the alkaloid has completely dissolved. Transfer the mixture to a small glass separatory funnel, and having run the lower stratum of liquid back into the flask, pour tlie ethereal solution into 100 c,c.platinum capsule. Treat tlie liquid in the flask with 20 C.C. more ether, and proceed as before. Repeat this operation a third time. The capsule containing the mixed ethereal solutions is then placed in a saucer of water, and the ether blown off by a current of air from a Fletcher's bellows. This immersion of the capsule in water obviates the tendency of the ether to creep up the sides.The platinum ciisli, which will now contain a pasty residue, is next placed in the air-bath, previously heated to- 120°, and in 15 minutes desiccation is complete. After cooling in an exsiccator, the capsule is covered and removed to t,lie balance. The weight, minus that of the capsule and cover, multiplied by five, is the percentage of total alkaloid.The author liad made many huiidreds of analyses by this process, and in cases where a determination had been repeated had never found the results vary more than 0.1 per cent. When an estimation of total alkaloid only is required, 2 grammes of citrate is a sufficient quantity to operate upon. The snliydrous alkaloid is now to be converted into basic sulphate.According to calculation the weight of anhydrous alkaloid in grammes is multiplied by 30.86, and the number of C.C. of decinormal sulpliuric acid thus indicated are run into the pl n t' inum capsule from a burette, and the former being placed on wire gauze over the flame of tt rose burner, the contents are briskly stirred until tlie alkaloid is all taken up, and a clear solution obtained.This is then transferred to a flask and allowed to cool spontaneously. The crystalline mass which will have formed is thrown on a small calico filter, about 3 inches square, stretched over a beaker, and, when drained, tightly squeezed to remove the last few drops of liqnid. The latter is then filtered into a stoppered graduated tube of about 150 C.C.capacity, a d its volume noted. Twenty C.C. washed ether and ail excess of ammonia are then introduced, and the whole, after being well agitated, set aside for six hours. In the meantime the squeezed residue is detached from the calico filter, and dried in the air-bath at a temperature of looo C. The weight multiplied by 1-18 represents its value as crystallised sulpliate of quinine.To this is added the amount of the latter contained in the mother liquor which has been separated (and which may be estimated to contain 1 part in 750), and the total will then represent the proportion of anhydrolls alkaloid which can be comer ted into sdphate. At the expiration of the time mentioned, the tube which lias been set aside is examined, when the cinchonidiiie and quinidine present will be found to have crystal- lised out, at the junction of the two liquids.The stratum of ether is removed by a small Nessler pipette ; tlie crystals washed with two successive portions of 10 C.C. of ether, the last few drops of mliicli can be absorbed by a little roll of filter paper. The crystals are then thrown upon a double-tared filter, made, of two papers weighed one against the other, by cutting down the heavier, dried at 120°, a d placed on the balance, the outside paper acting ns a counterpoise.In practice the author finds that the weight of this first crop of crystals represents on ail average two-thirds of the total cinchonidineTHE ANALYST. 193 or quinidine present, If, therefore, tlie amount does not exceed a 1 gramme, tlie per- centage of these alkaloids may be estimated to be below 5 per cent.Should the first weighing exceed this limit, tlie sulpliate obtained from the first crystallisation must be dissolved in 100 C.C. boiling water, and treated as beforc, iilie wiglit of allsaloid sepnrated by ether being of course added to the amouiit first obtained. As thus desci-ibed, tlie process may seem tedious, but in reality it is not so.Xot counting tlie time which must be a!lowed for crystallisiiig, the entire estimation may be completed in soivetliiiig under two iionrs. Tlic method, of course, does not distinguish between quinicline aiiil cinclionidiiie, tlie usual tests for mliich must be applied to tlic solution of tlie mixed sulphates. Two examples mill be sufficieiit to illustrat,e the worlciiig of tlie process.Descriptions of experiments were then given, and tlie author nddccl in coiiclusioii :- Whether the presence of 5 , 10, or 20 per cent. of ciiichoiiidiiic would bring a, sample of citrato of iron niid quininc, which iievcrtlieless nnswcreci the B.P. test, witliin tlic rcacli of the Adulteration Act is a point upon wliicli I offer no opiiiixi.An eminent analyst with mhom I was lately discussiiig tlie point took tlie negative view. If such is really tlie case, a revision of tlie Pliarinacopceitt will come none too soon, The plausible excuse mliich is sometimes set up that manufacturers cannot perfectly separate tlie ciiichonidino from the quinine except at a greatly eiihancecl cost is utterly without foundation.The wliite sulphate manufactured both by Messrs. Howard niid Mr. Whiffen I have never found to give the slightest reaction with Paul's test, and, vliat is il, still more striking fact, the so-callecl u l l b l c d d quinine of the latter ivalrer is frequently quits free from cinchonidine. Certain of the foreign makers are also, as a rule, niiimyeacliable in this respect, whilst, on the other hand, some others are systematically adulterated.It ma'y be worth noting, as a matter of practical interest, tliat the substitution of 1 per cent. of cinchonidine for quinine in the manufacture of citrate of iron and quiniiie reduces tlie value +d. per 02. for each such addition ; and wlieii if is remembered tliat the Pliarmacopoeia test will easily pass 20 per cent.of cinchonidiiie, and that tlie coiisumptioii of tlie citrate is considerably over 100,000 02. per aniium, tlie valuation of this preparation beconies n question of commercial as well as of chemical interest. This, however, is a point of ininor importance. ANALYST’S REPORT. THJ: ADULTRRATION O F RIILK.-lh. c. hfeyniott Tidy, the medical ofticcr of health for Islington, in his annual report which he has just issued, states that during the year encliiig Lady-day, 1979, lie examined 172 samples of food, and, except in the milk, he found no such evidence of adultcration as warranted him in advising a prosecution.In 12 of the milk cases he gave certificates of adulteration. They were all cases of added water, the adulteration varying on the lowest possible calculation from 10 to 30 per cent.Dr. Tidy adds:--“ The milk-sellers have raised the price of their milk, but I can scarcely say that the quality has been improved, the price being, in fact, no guarantee of genuineness. The extent to which milk is adnlterated is serious. For me must remember that to many (and thosc for the most part the rery old and the very young) milk constitutes the sole article of diet.The doctor call easily be thwarted in his tre;ltment of a patient by the dairyman. The public are in this way cheated of their money ; and if that vcre all it would be bad enough, but they are cheated of their health too. Aad yet during this year only a single sample of food was submitted to me by the public for examination, and that one articlc was not milk, but whisky.” In concluding his report Dr, Tidy says :-Would it not194 THE ANALYST. bc worth while, remembering that there are yet 60 many things to be attended to, aid so many reforms needed, in respect chiefly to the drinking habits of the people and their method of life, for sanitarians to turn their attention for a few years to these sadly-neglected topics, instead of confining their thoughts almost exclusively, as thcyliave been doing of late years, to the water as th9 source of all ills and miseries? It is not simply the time wasted on the subject that is to be deplored, but it is the un- necessary alarm the discussion of such subjects excites in the public mind.”
ISSN:0003-2654
DOI:10.1039/AN8790400191
出版商:RSC
年代:1879
数据来源: RSC
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10. |
Law reports |
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Analyst,
Volume 4,
Issue 43,
1879,
Page 194-196
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摘要:
194 THE ANALYST. LAW REPORTS. CAMBERWELL BUTTER CASE.-^^^ the Lambeth Police Court, a charge of selling adulterated butter was investigated. The case had previously been remanded on the application of the defendant, Mr. A. Bullard, cheesemonger, New Chnrch Roxl, that the sample might be sent to Somerset House for analpis. On the cme being proceeclecl with on the 13th September, the msgistr& read the following certificate, which had been received from the Somerset House authorities, sigiled by bIessrs.R. Bannister, G. Lenin, and J. Cameron :-‘‘ We hereby certify that we have analysed thc butter, and declare the results of our analysis to be as folloiys :--Water 12.05, curd 1.95, salt 0.96, fat 85 04 in the 100 parts. From ;z consideration of thc results of a full analjsis of the fat we are of opinion that the butter is genuine.” The magistrate, RIr.Saunders, remarkcd that there liar1 evidently been a lamentable miscarriage on the part of some of the Cnmberwell authorities, for a case of this ltinil was calculated to do much harm to a trader, inasmuch as tlic fact of his being prosecuted for selling an adulterated article became widely known, and thongli thz fact of its being adulterated was afterwards publicly disclaimed, yet this dis- claimer would not reach a tithe of the number who had heard of the charge against tlic trader.The defendant’s solicitor, Mr. Chipperfield, assented to the magistrate’s remarlrs, and stated Clint samples had on several previous occasions been taken from his client, which had almaJ-s proved pure, whilst, in addition, a sample of lard, taken at the same time as the butter which was the subject of this rase, had been found unadulterated.He should therefore ask that full costs be given. He further remarked that he had sent a sample of this same butter to Mr. Hehner, who had had considerable experience, and Mr. Hehner was then present, and would say that the butter was entirely pure. The Prosecuting Solicitor, Mr.Ilsrsden : I shall ask for an :tdjournnient that I may get the Government analyst liere, because the certificate I have is equally strong. Mr. Snunders : This has been referred to Somerset House, the chief authority on the sdiject, slid I can do nothing if you have these analysts here. Mr. hIarsden : May Inot be allomcd to cross-examine t h o chemist ~ l i c , made this analysis ? Mr.Saunders : No, I think not. Mr. Chipperfield : Mr. Hehner would show yon, froin tlie Public Analyst’s own report alone, that the butter is pure. Mr. Saunders (to prosecuting solicitor) : If you cross-examine them I could not do anything. I must take this certificate as conclusive, and that being so, it would be mnnifestly iccon.venieiit in conducting public busiiiess to send a eample to Somerset House for niialysia RIIC~ theii bring the analysts here to be cross-examined. You may be quite sure that the Somerset Eonse authorities arc the most efficient people, for they have to decide for tlie whole kingdom, and in most important cases. Mr. Chipperfield : Mr. Hehncr reports :-“ I have analysed the sample, and find it to coiitsin 87.75 per cent. insoluble fatty acids.From this result it is obvious that the sample was free from foreign fat.” And yet Dr. Bernays says that it contains 25 per cent. of foreign fat. Mr. Saunders : I think I ought to allow all reasonable costs, as great inconvenience has been caused to this man. I will say six guineas, I think. When traders act dishonestly I am always willing to punish them, but they onght fairly to be recouped their expenses when it is found that they have acted properly and fairly by the public.Six guineas fop costs, nnd one guinea for the analyst you have brought here, will therefor2 be allowed. HEAVY FINES FOR MILK ADuLTEn-mori.-Robert Piko, a dairynian, of James Street, Exeter, was suminoned for having sold adulterated milk.Mr. C;. H. Shorto appeared on behalf of the Town Council. The proceedings were taken under the Milk and Drags Act of 18?5. Mr. Shorto said a nominal penalty would not be considered adequate to meet the denialids of justice. Mr. Lendon, Sanitary Inspector, said that on Thursday, tlie 7th September, he purchased three half pints of inilk of the defendant’s wife.On being tendered the iiiilk witness inforiiied lier that he intended to have it analysed, where- upon she said she could not spare it. Witness, however, remarked that “ he had got it,” and left. Mr. P. P. Perliins, Public -4nalyst, said he had made an analysis. He found the milk to be diluted wit11 Over 25 per cent. of wvatcr. Defendant said he kept no cows himself, but bought his milk of Mr.Brick- ncll, a dairyman. Defendant called liis wife, who bore out this statement. The Bench retired for a &ort time, and, on rclurniug, the Chairman said the case had been carefully considered by theTHE ANALYST. 196 magistrates, who regarded it as a very >;crions case. Milk was a necessary elemeiit in the food of invalids and children, who must be protected froin such imposition.Defendant would therefore be fined in the lomest amount in such cases, viz., 325 and expenses ($1 2s. 9d.)-Samuel Bricknell, dairyman, of €Iolloway Street, was summoned for a similar offence. The evidence of Mr. 3’. Perkins showed that the milh supplied by the defendant was adulterated with water to the extent of 20 per cent., and a portion of the cream to the extent of 9 per cent.had also been removed. Mr. Fryer appeared for the defendant, and it appeared, in cross-examination, that the defendant mas not present when the sample was taken, and that on the morning on which the milk was seized rain had fallen in torrents. Mr. Fryer contended that the case had not been made out, illasmuch as the Act of Parliament had not been complied with. The Act stated that the prosecutors should prove to the satisfaction or” the justices that the defendant had had notice of the iatendecl analysis and should accompany him to the analyst.He contended that inasmuch as the complainant gavc the defendant no opportunity of acconipanying him to the analyst, the Act had not been complied with. He also suggested that the water in the milk might be accounted for by the heavy rains which fell during the time of milking.Mr. Shorto, replying to Mr. Fryer’s objection, said the Act to which Mr. Fryer alluded had been repealed in 1875. Mr. George Henry Mugford, boot- maker, of Magdalen Street, and Mr. Mawrice Sewell, grocer, South Street, said they had dealt with the defendant for a number of years, and had never had caus:: for complaint. The Bench, after a brief consultation, fined the defendant 25 and ths expenses.The Chairinan said he hoped the present proceediiigs mould be a warning to parties who were veiidors of milk not to come before the magistrates. THE TINE LIXIT FOR SERVING Sum~oNsEs.-At Clerkenwell Police Court, William Gunning, niilk-vendor, of Xorih Street, Pentonville, was sumnzoned at the instance of the Vestry of Clerkenwell, to answer a cornplaint of haviiig sold milk adulterated with water.Mr, Ricketts, solicitor, attciided for the defence. From the eyideizce of Thaiq om of the sanitsry inspectors of Clerkenwell, it appeared that on the 30th June he purchased at the defendant’s shop a pint of milk, for which hc paid twopence. He told the pemm from mh3m he purchased ths milk that he should take a third portion of it to Dr.Iiedwood to have it analysed. He did so, and the certified result of the analysis was that there was 30 per cent. of water added to the milk. He understood that defendant kept no cows, but got his milk fro= wholesale dealers. Mr. Ricketts, for the defence, said, had he gone on with the case, he should havo, bceii able to show that the defendant was not much to blame in tho matter, but he hzd an objection to take to the summons mliicli he thought mould prove fatal to the proceeding, and would enable the mrtgistrate to dismiss it.The milk mas purchased on the 30th June, and these prc- ceedings were not commencsd in this Coljrt until the 12th of August ; coasequcntly, under the Act to Amend the Sale of Food m d Drugs Act, 1S73, which rcceived the Royal Assent and c ~ m e into operation on the 21st of July of the pxssnt year, the whole proceeding must be quashed unless the hearing* took place within 28 days of the day of purchttse.Milk WAS a perishable article, and this m,s specially provided for in the amended Act. Mr. Hosack (the magistrate) p3lnted out that the milk in this case was purchased before the passing of the Amendment Act.Mr. Ricketts said that did not matter. The words of the 10th section of the amended Act vero very plain, and vere as follows :-‘‘ In a11 prosccu- tions under the principal Act, and notwithstanding th3 provisions of section 20 of the same Act, the summons to appear before the magistrate shall be sexed upon the person charged with iiolating the provisions of the said Act within a rcnsonablc time, and, in case of a perishable article, not exceeding 28 days from the time of the purchsse froin such person for test purposes of the food or drug, for the sale of which iii contravention to the terms of the principal Act the seller is rendered liable to prosecu- tion, and the particulars of thc offence or offences against the ssicl Act, of which the seller is accused, and also the name of the prcsecutor, shall be stated on the summons, and the summons shall not be made returnable in a less time than seven days from the day it is served upon the person summoned.” That section made it clear that the magistrate could not convict, and therefore he had to ask for the dismissal of the sunimcns.Mr. Hosnck, having considered the section, at once dismissed the com- plaint.-Daiiid Edwards, of 230, St. John’s Street, Clerkenwell, was likewise summoned for the committal of a like offence. Inspector Cheshire said in this case the milk was adulterated with 27 per cent. of water, but as he purchased the inilk prior to the purckase of the milk in the other case, he would, with the permission of the magistrate, withdraw the summoiis. Mr.Hosack allowed that course to be adopted.- John Campion Kent, of 52, White Lion Street, Pentonville, was summoned for selling milk that was adulterated with 14 per cent. of water, but thrrt summons was also withdrawn. * This is an error. As mill ba See11 by tho sectioil qnoted, the SL(ntJJl.011.8 n w t be served within 28 days, not t,l:e lienring take place withiu that time.- [EDs. ANALSST.1196 THE ANALYST.ADULTERATED BUTTER CASE.-At Clerkenmell Police Court, Thomas Jones, butterman, of 97, Lever Street, St. Luke’s, was summoned by Mr. Edes, sanitary inspector, for having sold butter which wa8 adulterated. Mrs. Robins, of Hull’s Terrace, York Road, said that in accordance with instructions she had received from Mr.Edes, she went to: the defendant’s shop and purchased half-a-pound of butter, at 1s. 2d. per lb. After she had purchased it the sanitary inspector entered the shop and told the defendant he should have the butter analysed by the Public Analyst. The butter was not exposed in the window, and was brought by the defendant from a room behind the shop.The defendant said he had bought the butter from another person, and he did not know it was adulterated. Mr. Edes said the result of the analysis showed that the butter had been adulterated to the extent of 80 per cent. of fatty matter other than butter. HEAVY FIm.-At the Police Court, Bath, John Croswell, of 5 , Bridge Place, Holloway, was Bum- moned for having Rold during last month a pint of new milk which was not of the quality and substance demanded.On the 25th ult. Inspector Montague visited defendant’s house and asked for a pint of new milk for the purpose of having it analysed. He was supplied by the defendant with a pint of milk, for which the inspcctor gave him three half-pence. Mr. Gatehouse, Public Analyst, on analysing it, found that it contained 15 per cent. of water.In his defence defendant admitted selling the milk to the inspector, but stated that it was the last that remained of six quarts which he had purchased for another person. The magistrate fined defendant ;El0 and costs, or 14 day’s imprisonment with hard labour. Defendant replied that he could not pay the amount as he had a wife and five children. AT the Marylebone Police Court, Joseph Mason, of 55, Weedington Road, Kentish Town, wns sum- moned for selling a pint of milk, found on analysis to be adulterated with water. Mr. Ricketts prosecuted for the St. Pancras Vestry. I t was stated that the defendant was in a small way of business, and that the sample, when analysed by Dr. Thomas Stevenson, the Public Analyst of St. Pancras, was found to be adulterated with added water to the extent of 17 per cent. The magistrate fined the defendant 10s. and 2s. costs. AT Stockton-on-Tees Borough Police Court, Anthony Watson mas fined S5 and costs for selling adulterated milk, this being his fourth offence. The magistrate ordered the defendant to pay a fine of S3.
ISSN:0003-2654
DOI:10.1039/AN8790400194
出版商:RSC
年代:1879
数据来源: RSC
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