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Las diagrammes suivants illustrant la mAthode. 1 2 3 1 2 3 4 5 6 r^c 326 HOWb SJ -on ctPT, oft;^ MAY'-') ]9?C w'Vy VANCOl'VtJi. it C. <;^\ V'-' J., , , .L ■''■. V .y^ LABORATORY OF THE INLAND REVENUE DEPARTMENT OTTAWA, CANADA BULLETIN No. 401 LIQUOR ARSENICALIS 41267—1 "1 NOTES AND COMMEN'' ^ Under this headingr, as occasion arisefl, the Bulletins issued by this Department will contain, as an appendix, such comment as may seem necessary or advisable upon matters relat ^ to the work of the Department in connet'tion with the administration of the Adulteration Act, the Fertilizers Act, the Feeding Stuffs Act or the Proprietary Medicines Act. It frequently happens that correspondents ask information regarding the above Acta, of sufh a nature that the matter in question possesses general interest, and comment upon it would prove acceptable and useful to others than the immediate questioner. In such cases the reply may find a place in these columns. For con- venience of reference these notes will be numbered in scries. A. McGILt, Chief Analyst. 0Uii4 7? J LABORATORY or THI INLAND REVENUE DEPARTMENT OTTAWA, CANADA BULLETIN No. 401 LIQUOR ARSENICALIS J. U. Vincent, Esq.. K.C., B.A., L.Ph., Deputy Minister of Inland Revenue. Ottawa, May 4, 1918. Sib,— b.isr herewith to hand you a report upon ninety-one samples purchased by our insi)ectors throughout Canada as Liquor ArsenicalU. or Fouler $ Solution, in October. Nc < mbe-. and December of last year. The ;.-. . inspection of this drujr. under the Adulteration Act. was made ill 1909, - ted in Bulletin No. 175 of thU series. It dealt with seventy-five >ainple.s w.. .e' judffed by the standards for this article as defined by the British I'lmrmac. p«>in, edition of 1898. The arsenic solution of the 1914 edition is essentially identical with that of 1898, and is of 1 per cent streiiffth. No rocopiized variation from theoretical values was indicated in 1898, except in so far as tiis might be inferred from the fact that 25 cubic centimetres (mils) should discharge the colour of .50-8 to 509 cubic centimetres of deci- normal iodine. Theory requires 50.5.3 mik of the iodine solution, so that the instruc- tions of this edition permitted the liquor arsenicalis to be slightly stronger (1-007 ■ n.toad of 1000) than 1 jK-r cent. The edition of 1914 requires that only 50-4 mils of deei-normal iodine should be decolourized by 25 mils of the liquor, thus permitting a trace less than 1 per cent of arsenious acid. The error, if any, is on the side of safety. 1 made a suggestion to the effect that a variation in arsenical strength not to exceed 0-020 per cent should be allowed in the drug. The United States Pharmacopoeia (revision of 1916) permits a variation of 0-025 per cent in either direction, thus requir- ing the arsenic content to vary from 0975 per cent to 1-025 per cent 41207— 1 J i it il it It is upon this basis, which in my opinion is very reasonable, that 1 have judged the ninety-one samples now rettorted. The results are very disappointing. 1 find thut only twclvj samples meet legal r< liroments, the British Pharmaoopctal requirements being even more stringent than those of the United States Pharmacopffla. Many of the oanipies are so far from accurate as to compel the conclusion thut great and culpable carele»stie»8 is shown in their preparation. While the perfectly definite limits of varia'ioii permitted by the pharmacopoeias compel me to dcclan- adultered all samples showing excess of arsenic amounting to 0025, or deficiency to the same amount, it is proiK-r to point out that while many samples depart quite widely from these limits, a considerable number are but ulightly over or under strength in mraenio. The following synopsis shows the variation : — Deficiency tn ArienU;. From 0.0:S to O.OfrO. Above o.oso 0.075 0.100 0.200 0.300 0.400 0.600 . Total. 0.075. 0.100. 0.200. 0.300. 0.400. 0.500. Samples. 13 11 10 25 7 4 t 1 76 Exceat of Arienic. From 0.026 to 0.060. " 0.050 0.076. Above 0.100 Total . The work of analysis of this collection was placed in the hands of Mr. Westman. assisted by the aiialyste in charge at Halifax (Mr. Forward) and Winnipeg (Mr. Forster), and I have pleasure in submitting his carefully prepared report, as follows:— giB, — I beg to submit to you the following report dealing with the examination of ninty-one samples of Liquor Arsenioalis, commonly known as Fowler's Solution. These samples were collected in October and Norember of last year, and are reported from the laboratories as follows : — Halifax i 10 samples Winnipeg ^^ Ottawa *8 Total 91 " Liquor Arsenicalis is essentially a 1 per cent (1%) solution of arsenioua acid (AsiO.) and should contain 3 per cent by volume of compound tincture of lavender, B.P. 1914, p. 213. The powdered arsenious acid is completely dissolved in potassium carbonate, equal proportions by weight being specifio'l in the official preparation. The limitations of the official solution may be derived fr ;n the following characters and tMti quoted from B.P. 19t4; "A reildi»li liquid, iilkalino to litmug, und having the odour of lavender, 'Jj inilli..tre«, neutralized with hydrochloric acid, dischurife the colour of 60-4 millitres of N/10 solution of iodina, the presence of a slight czceM of sodium bicarhoniito being maintained throughout the operation." The United State* Phaminc'ipn-ia IX, p. 251, describes Fowler's Solution as an aqucouit solution containing potaMHtiini arsenite, corretuponding in amount to not less than 0-975 per cent, nor more than lO'iS per cent of A^jO. (1»7-92). The solution is to be free from arsenate compounds and is made up originally with potasaiura bicarbonate and titrated with standard iodine solution in the usual manner. Examinaiion of Samples of Arsenioun Acid, Samples of Liquor Arsenicalis maj reach the public in unofficial strength for ai li'ast four reasons ; — (1) A prop.>rl'- made up and standardized solution may deteriorate or change slightly in strength on loiif standing if not kept in a proper container under constaiit seal. (2) The rotailer may sell a solution of his own manufacture carelessly prepared and unstandardized. (3) A wholesale firm may furnish the retailer with a carelessly prepared and unstandardized solution. (4) If accurate weighing of the arscnioua acid be taken as the only method of standardization, slight impurities in the acid along with incomplete solubility would account for solutions being slightly below standard. The last of these possibilities will be considered first. From the nature of its manufacture it was considered improbable that any great variation would be shown in the quality of different samples of arscnious acid found on the market. With this in view, samples were taken from various retail stores and from wholesale houses. Ono per cent solutions of these samples were made by weighing 1^'. of a powdered arsenic, without previous drying, and making the volume up to 100 mils in the manner dejcrihod in the official method. No e-xtraordinaiy care was taken with this work and tlie volumetric glassware was such as is found on the present market. By carrying out the work in this manner it was hoped to duplicate the conditions obtainable in any ordinary laboratory or drug store. Ten mils of the solution thus made up was acidified with concentrated hydrochloric acid, and on further dilution with water to about 50 mils, was neutralized by the addition of considerable excess of sodium bicar- bonate. This solution was then titrated with standard iodine solution, using fresh soluble starch solution as indicator. All solutions used were carefully prepared, heiag standardized with repurified potassium bichromate and iodic acid. Samples of arsenious acid examined in this manner were found to give fairly close approximations to standard 1 per cent solutions. Twenty-three samples in all were collected from leading wholesalers and from some retail stores. The detailed analysis of solutions made aa above from these sami>Ies is given below. In some cases these were given a regulation sample number; in other cases they were simply procured in a semi-official manner by our inspectors. ;( l>niii(iiiitit Kivrii . |\»t. l»riif V«yiii»na Ltd. ... - . . jNdt Miv«ii !Nat. UniR lUmiiida DriiK Co. Ltd, |N«t. l)n.gCo Msruki. II. .1 HtalkiT. let Ki'Wmi Ht. J. .HkiiimrftS..ti. :W\V.llinuton Ht. Hull .Mi'diiul IIhII IliirriMin'M I'hMriiiacy Allrii & Oichrano X»t. Dnm ArtH*nic. 7»aw> 812311 79728 1 Anumic Triuxiilr VM.P. IX. :M«rck. AraeniuuM Acid C. P. I iNat. DniK jRwl Cni«» rhannacy. !|)r. .MtirinftCo ' Nn A Wait, Ltd. . ( 'lia|>iiiaii. i>art A Oi., CraiK >4t. W Nat. l>niK I 'unada I Iriiit Cu K. Whitiiinrp, .Smith Kiid I'hariu N.it linig Kiii'n.w rhuniiicy Dr. .M Tin ft Cii W. K. SiimidHm I'ark, llavm A Co Nat. I>rin( I'lacv «>lfl at. IHUwa Hull . . le arising from this cause does not exceed 4 per cent. The pluirmacopraMas allow a variation, taken on the same basis as above, of :.' ."> |«t cent. Orjtiiuic matter and dust seem to constitute the major portion of the impurities found in those samples which ran from 3 to 4 per cent lujow strength. It is evident that the maximum error should not exceed 4 per cent or the percontaffe of arsenious acid in Fowler's Solution should never be lees than 0.960, when reasonable care h.is lieen taken in preimrinfj the solution from such materials as are obtainable .m the niarki^t. In any case, even after the nmst care- ful weighinK the final solution should be tested by titration. In this way no matter how impure tho original arsenious acid may be, by reason of non-oxidizable materials, tho error '■• reduced to the very small error of titration. The responsibility for this further standardization must be plac(> of FowWi Solution. It rery often hapiwiM that munh «»i>nfu»i(m nt\»<» w)i< thiftinif "^ rwpmiiibility ii atti-mptcd by retail flrnw by dwIariuK that they Imve Ih«.ii RUppiied with iniprop«rly made tolutiuuN and undercrradn products. On the other hand tli, maiiufuptiircr nmy bi- kMw\ u\wn t.» d«tfi-nd bimitMlf from the rutttiler who ban in BDmo niuaner Iow.t.mI thy l«M of liquor nrwnicalis at the name time that an official "ollection wa* Xmng madK. Tliln iixcial ••■•ll««ctii(n connUti-d of aam- plo» taken directly frim the manufaotuririK plant* of whoi,-,8le firnw or other of the larjfer firms. In this way it wnn h"iN>d to truce out any discrepancies and find what the bi>gt practice in thi* connection wan placing on the market. It was thought that the larger firms, of national reputation, might obtain a higher degriw of accuracy in their producti working under more uniform and standnrd methods. With certain eacei)tion», however, little difference was observed l»ecial collec- tion some samples iiide«« 09i» 0H6 070 016 096 159 7H721 (*122» «7:ig in particular with the possible presence of antimonousi oxide rpference is made to an article by R. M, Chapin (J. Ind. and Eng. Chemistry vol. 10. No. 7, p. 522, 1918) on " The Preparation •nd Testing of Pure Arsenious Oxide." The avcriiRe accuracy of this preparation as found on tlio market at the present time shows a striking decrease when compared with conditions as they wore found in 1909. The tiililc which folhpws gives a conii)arntive synopsis of tliese conditions. Although the condition of this drug was extremely bad when first collected in 1900, it is obviously worse at the present time. The table contains the results of analysis of samples eolleeted in tiie general collection as well as those forming the special col- lection which was examined entirely at Ottawa. Liquor .ArM^nioali.'^ Witliin O.OIO of alt^olute accuracy From (1.010 to O.OV) abxulute accuracy ., 0.0)0 to 0.100 ■' 100 to 200 Al«)ve 0.200 absolute accracy Total .Samples lilOU. Sa.nplcB 1918. 15 . 1 21 22 21 3A lu 34 M 22 118 Samples meetiiif; B.P. and I'.S.P. requirements of not more than O-OSf)- variation from standard 1-CMJ per cent solution of arsenious acid given in iH'rcentages of total samples exam i mil: — ' Year. I'ercentaffe of Samples Meeting Re^juirenitints. 1909 1918 21 3 li M Summary. 1. Solutions of Liquor Arsicnicalis as sold in Canada at the present time are on the average much below their proper strength and 93-2 per cent of samples examined failed to meet pharmaeopoeal requirements. 2. The accuracy with which solutions of this drug are being prepared is notably on the decrease. 3. Both the larger wholesale firma and retail druggists are guilty and responsible for this condition. 4. The purity of the chemicals used is such that only carelessness in preparation may hope to account for this situation. 5. If this may be taken as significant of general practice in many instances it is indeed time that certain leforms were introduced and radical changes made in the test- ing laboratories of many firms. I have the honour to be. Sir, Your obedient servant, L. E. WESTMAN, Public Analyst. 41267—2 10 I present this report to yoii, bcoauso I find that ^Fr. Westnian'a conclusions are based upon fact. Section 7 of the Act makes the pharmncoponias the standard for drugs, and I am compelled, for this renson, to declare more than 90 per cent of these samples adulterated under the Act. There aro, however, conaidorable differences in the amount of deviation frrm standard requircmont-s; ;.nd it is jKisaible that a deficiency or excess of arsenic in liquor arsenic;ili..i, within limits, miiy be considered ns involving no danger to the iiealth of the consumer. If this be the oaso, the lino of safety mtist bo drawn by the medical profession; and for this reason I am siibmittinif copies of this report tc the official medical advisers of this depr.rtment, Prof. Blaokador of J[eGill College, Montreal and Prof. Kudolf of the University of Toronto. Their opinions will bo furnished to you when received; but delay must be expected, sinoo Professor Rudolf is " somewhere at the front " on mili- tary duty. Seition 32 of the Act distinguishes between adulteration of a kind injurious to health, and that which is not injurious to health; and for this reason, the point sub- mitted for a medical opinion is of importance. 1 leg to recommend publication of this report as Bulletin No. 401. I have the honour to bo, Sir, Your obedient servant, A. McGILL, Chief Ancdyst. 11 it: Vi < 1^ o 6 5? « '»|J '^1 -^ •D'ti .iiuotuy I Jii.i[v.\iiil);4 I .«- , s_ il: i i. - * a- • =5 ■* 5 i-' I S £ I i ■a t '- •"»u»0 •Xjiju«nf> •<-o 1 ^ •rflJra»)^ JO -ojj !5 ^ •uoirwiioa JO a(»(j S § S g 2 r-. 3t c. t* o a'^. i fe i . -'-5 -o -a ■§ UOE g g g 5^ > > U > s s s § e ■5 a. I 5 .£ a! 3 _ -Q -a . M Z O 1 i i S 1- *' t^ I s a s ^ o J o o 1 1 ^ b ? s e b S S '£ X o « b C C S 9. 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