shaken with 10 c.c. acidified water. The mixed acid fluid, after being once more shaken with a little ether to remove any colouring matter, was rendered alkaline with sodium carbonate, and the isolated alkaloid shaken out with ether. The author obtained ·49 per cent. of alkaloid, but objects to the process on the following grounds: 1. The quantity of alcohol ordered is too small, and should be doubled. 2. As a rule, the ethor, when shaken with acid water, forms a troublesome emulsion. 3. Twice shaking with ether is insufficient. 4. The residue left on evaporation is not pure cocain, as it did not dissolve completely in hydrochloric acid, and left about 50 per cent. of insoluble residue. It is also dangerous to distil a strongly acid alcoholic solution of cocain, as it so readily decomposes. The author next tried the process of Castaing. Fifty grammes of coca leaves were treated with 400 c.c. of boiling water, and after standing for half an hour percolated. The residue was then percolated with alcohol of 85 per cent., and the mixed filtrates thrown down with lead acetate, After the excess of lead had been removed with sodium sulphate, the liquid was concentrated, filtered, rendered alkaline with sodium carbonate, and shaken out with ether. The amount of cocain was 38 per cent., but it was only partly soluble in dilute hydrochloric acid, and much coloured. The next process tried was that of Albertoni and Guareschi. Fifty grammes of the leaves were exhausted with ether, the ether was distilled off, the residue treated with boiling water, and the solution evaporated to dryness with a little magnesia. On extraction with amylic alcohol, 14 per cent. of alkaloid was obtained. As a last resource, Bignon's process was tried. Fifty grammes of the powdered leaves were macerated for fortyeight hours with a 20 per cent. solution of sodium carbonate, then dried on the waterbath and exhausted with petroleum spirit to dissolve the cocain. The solution was shaken with dilute hydrochloric acid, which takes up the cocain. The acid fluid was then rendered alkaline and shaken with ́ether, which extracted the cocain. The percentage of cocain got by this process amounted to '06, a proof that most of the alkaloid had been decomposed by the strong alkali. The author then tried the following idea: 25 grammes of the powder were mixed with 10 grammes of magnesia and a little water, and dried on the water-bath. After percolating with ether (so as not to dissolve any hygrin), the ether was distilled off and the residue treated with acid water and filtered. After rendering alkaline, the alkaloid was extracted with chloroform. Obtained 2 per

cent. alkaloid. A similar experiment was made with 50 grammes of the leaves, and 19 per cent. of alkaloid was obtained. Ether may, however, be advantageously substituted for chloroform. The author finally recommends the following process: 50 grammes of the powdered leaves are mixed with 20 grammes of magnesia, and dried at 60° C., then extracted with ether. After distilling off the ether the residue is taken up with 30 c.c. of 2 per cent. hydrochloric acid. The acid is filtered and repeatedly agitated with ether, to remove colouring matters. Ammonia is then added, and the mixture shaken out three times with 25 c.c. of ether. After standing for a little while over a few pieces of calcium chloride, the ether is evaporated and the alkaloid weighed.

L. DE K.

Nederl.

ESTIMATION OF DEXTRIN IN NARCOTIC EXTRACTS. PROF. VAN DER MARCK. Tydschr v. Pharmacie, etc., April, 1889.-The author tried Pannetier's process, which

apparently leaves nothing to be desired, and is performed as follows: Two grammes of the extract are dissolved in 50 c.c. of water and precipitated with 5 c.c. of liquor plumbi. The filtrate is freed from lead by sulphureted hydrogen, and concentrated to one-fifth of its bulk. An equal volume of spirits of wine is next added, which precipitates dextrin, and some alkaline salts. The precipitate is washed with alcohol, dried and weighed. To make sure, the dextrin may be inverted and estimated by Fehling's solution. Feeling no confidence in the method, the author tried the following experiments: Two grammes of extract of belladonna were dissolved in 50 c.c. of water, precipitated with liquor plumbi and filtered. After freeing the filtrate of lead and concentrating, alcohol was added and the fluid remained clear. Two mixtures were then made up containing respectively 5 and 10 per cent. of dextrin, but alcohol failed to produce a turbidity. With a mixture containing 15 per cent. of dextrin, a faint cloud was obtained, and, when 20 per cent. had been added, about one-third of the dextrin was recovered. On repeating the last experiment, but with addition of much more alcohol, 67 per cent. of the dextrin was recovered. The author, therefore, concluded that the method is perfectly useless, and endeavoured to find a better way. It is, of course, perfectly well known that dextrin, when heated with a 2 per cent. strong hydrochloric acid is gradually converted into glucose. Before applying the inversion process, it was necessary to prove: 1. Whether the extracts themselves contain copper reducing bodies; 2. Whether the inversion can be quantitatively depended on. Two grammes of belladonna extract were dissolved in 10 c.c. of water, and made up with alcohol to 75 c.c. The precipitate was filtered off and washed with alcohol of 75 per cent. The alcohol was evaporated, and the residue treated with Fehling, which was partly reduced. Fehling's solution was also reduced by the watery solution of the precipitate. Two grammes of the same extract were precipitated with liquor plumbi, the filtrate freed from lead by passing hydrogen sulphide, and after boiling neutralised. The liquid strongly reduced the Fehling. As these experiments proved that the extract contained reducing bodies, it became important to know the reducing power of different extracts from various origins. The author, therefore, took samples of extract of belladonna (Nos. 1, 3, 5, 7) and extract of hyoscyamus (Nos. 2, 4, 6, 8). Two grammes were dissolved in 50 c.c. of water and precipitated with 8 c.c. of liquor plumbi. After removing the lead, the liquid was evaporated down to 20 c.c. and titrated with Fehling's copper solution. It was now found that 10 c.c. of the filtrate (=1 grm. extract) required of Fehling:

corresponding with an average percentage of 8 per cent of glucose, which may be disregarded. The next step was to ascertain whether dextrin may be completely converted into glucose. Ten grammes of the best commercial dextrin were dissolved in 100 c.c. of water. Ten c.c. of this solution took an average of 9.6 c.c. of Fehling, corresponding with 5 per cent. of glucose. The sample lost in drying 11.6 per cent. of water; 2 grms. of the sample was dissolved in 100 c.c. of 2 per cent. hydrochloric acid, and heated for two hours in water of 90° C. After cooling, the liquid was made up to the mark and then titrated. 10 cc. of Fehling required 23 c.c. of the liquid, which proved a loss of 8.8

per cent. dextrin. In a second experiment, when the heating was continued for three hours, the loss amounted to 18.9 per cent.* These results are, however, more satisfactory than those obtained by Wertha and Payer, who respectively got a loss of 58 and 38 per cent. The author thinks, however, that this process may be still found useful in cases of serious frauds. L. DE K.

COPPER IN GHERKINS. WESENER. Zeitschr. f. Angew. Chemie, No. 5.—One sample possessing an unnatural green colour gave on analysis 0036 per cent. of copper oxide, or 058 per cent. on the dried substance. A second sample of a yellowish-green colour only showed traces of copper, whilst a third sample seemed to be quite free from that metal. The copper in the first sample was no doubt the cause of the serious illness of a child. It will be interesting to analysts to read that not a trace of copper could be detected in the preserving vinegar. L. DE K.

Nederl. Tydschr. v.

ESTIMATION OF ALKALOIDS IN EXTRACTS. L. VAN ITALLIE. Pharmacie, etc., January, 1889.-Five grms. of the extract are dissolved in water with the aid of 10 drops of dilute sulphuric acid (1-20), and then made up to 50 c.c. After standing for an hour or two with occasional shaking, 25 c.c. of solution of lead acetate (1—10) are added. After settling, the fluid is filtered through a dry filter. 50 c.c. of the filtrate are now mixed with 10 c.c. of the dilute sulphuric acid, and again filtered. From this second filtrate 50 c.c. are put into a separating funnel, and after rendering alkaline with ammonia, shaken out three times with 50 c.c. of chloroform. The chloroform is distilled off, and the residue, after dissolving in 5 c.c. of spirits of wine, titrated with hydrochloric acid, 1 c.c. of which represents 00289 grm. atropine or hyoscyamine, 0053 aconitine, or 00127 coneine, lackmoid being used as indicator.

n

100

L. DE K.

ANALYSIS OF SULPHATE OF SODA. ISBERT AND VENATOR. Zeitschr f. angew Chemie, No. 3, 89.-The anlaysis of commercial sulphate of soda is very troublesome, and con. sequently highly charged for by analysts, which causes the manufacturers to send but very few samples. The authors have found a very accurate and simple process, which suits the manufacturers. It is as follows: About 2 grammes of the samples are dissolved in the smallest quantity of hot water and mixed with a little ammonia and ammonium carbonate as long as a precipitate forms. The precipitate must be freed from soda by re-dissolving in hydrochloric acid and reprecipitating with ammonium carbonate. The mixed filtrate and washings now contain sodium sulphate, ditto chloride, and also the excess of sulphuric acid the sample might have contained. The liquid, which will measure about 100c.c., is evaporated in a platinum dish, to dryness. The residue is gently ignited to expel ammoniacal salts, and then weighed as pure sodium sulphate, any sodium chloride having been decomposed by the ammonium sulphate. If the sample should be rich in chlorine, a little extra ammonium sulphate should be first added to the filtrate. From the weight of the sodium sulphate is deducted the weight of sodium sulphate corresponding with the sodium chloride the sample contained, and which is estimated with deci-normal silver. The test analyses are very satisfactory. L. DE. K.

* See also ANALYST, 1887, p. 138. L. de K.

LAW NOTES.

BOROUGH ANALYST V. THE BEDFORD CORPORATION.

This was an action in which Dr. Voelcker, of London, the Borough Analyst, claimed £21 from the Bedford Corporation for fees for making analyses. Mr. F. Low (Solicitor to the Society of Public Analysts), appeared for the plaintiff, and Mr. Bonsey (instructed by the Town Clerk) for the defendants.

Dr.

Mr. Low, in opening the case, said no doubt his Honour was surprised that a public official of the Borough of Bedford should have to come to that Court to recover work done as public analyst, but public analysts generally, and particularly the Bedford analyst, were not popular officials, and Dr. Stevenson, the former borough analyst, terminated his engagement under circumstances which probably his Honour was aware of. [The Judge said this matter was perfectly immaterial to the action]. This was a material observation so far as his client was concerned, because he would not have taken the appointment had it not been for the persuasion of the late Ald. Howard, who was a friend of his. Voelcker was appointed as public analyst to the Bedford Corporation in May, 1887, on the condition that he was to receive one guinea for every sample submitted for analysis. In the following November various articles were sent to him from Bedford for analysis, and among them were two samples of coffee. Of the fourteen samples, thirteen were reported genuine, and no question could be raised on these, as no prosecution could follow. One sample of coffee was found to contain 80 per cent. of chicory, and in reporting this case Dr. Voelcker did not use the form of certificate as prescribed by the Act, and failed to insert the weight of the sample quite by accident, and in consequence of that the Corporation said it was useless to them as they could not take proceedings on it against the owner of the sample. But while refusing to pay for this one sample, the Corporation also refused to pay for the whole fourteen samples. With respect to the blank left for the weight, a foot-note on the certificate said that when the sample could not be conveniently weighed the weight need not be inserted, and he contended that it was perfectly immaterial, but it would not be so with some substances. The omission of the weight in this instance did not render the certificate useless, and he submitted that it was a good and sufficient statutory certificate under the Act. In the case of a prosecution, in case the Court did not accept the certificate, the presence of the Analyst would be all that was necessary, and he informed the Corporation he would be ready to attend if wanted. He also offered to amend the certificate, but the Corporation said that after the certificate had once left his hands he could not alter it. Six guineas had been offered by the defendants, but plaintiff would not accept it because he was entitled to twenty guineas, six other samples having later on been analysed. The Judge said the point was as to whether the insertion of the weight was material in this instance.

Dr. Voelcker stated that he weighed the sample of coffee, and it weighed 5oz. In all cases of analysis of coffee, the weight was perfectly immaterial to the analysis, however small the sample might be. In some substances, such as drugs, weight was material.

Cross-examined: Had the sample been smaller, he should have retained it and asked for another sample, not for chemical reasons, but because it was always advisable to have a fair representative sample, but a very small sample from a large bulk might give a fallacious result. He examined every sample, and truly stated the result in the certificates.

The Judge expressed his opinion that it was the intention for the weight to be inserted in all cases, except where it could not be done.

Mr. Bonsey pointed out that one of the certificates was not signed, and was therefore useless. It was provided that in cases of articles liable to decomposition or change in constitution, mention must be made of it in the certificate, but in some of the certificates that came under this head this had not been done.

Mr. Low said it was unnecessary because all those samples were genuine.

Mr. Bonsey said that the object of the Act, was that the form of certificate should be strictly complied with, and no proceedings could be taken before the production of the certificate properly filled up and signed.

The Judge was satisfied that the certificate must be made out according to the Statute, and after it had once left the analyst's hands he could not alter it.

Mr. Bonsey asked how they were to know that a proper sample had been sent if the weight was not stated. The plaintiff had left out the material part by not inserting the weight, and the analysis was not complete until a proper certificate had been given.

His Honour thought some of the certificates informal, but reserved judgment, and Mr. Low pressed his Honour to carefully consider the question of power to amend the certificate.

AN OLD QUESTION REVIVED.--A case of importance was heard at the Worship Street Police Court on the 9th ult., before Mr. Bushby, the presiding magistrate, against a tradesman who had been summoned at the instance of the Vestry of Bethnal Green for selling an article, to wit, coffee, adulterated with 60 per cent. of chicory, contrary to the statute, and was, therefore, not of the nature, substance, and quality demanded by the purchaser. Mr. Ogle appeared for the defence, and contended that his client was protected by the notice printed on the wrapper, that the article sold was a mixture. Mr Lapworth, of the Sanitary Department, who appeared in support of the summons, addressing the magistrate, said this was the first case of the kind that had come under the notice of the Vestry, who

were desirous that it should be considered as a test case, and to have the decision of the Court upon it. The points to be considered were whether the sample was sold to the prejudice of the purchaser, as set forth in section 6 of the Act, and how far the vendor was protected by giving a label stating that the article was a mixture. It had been generally thought that if a customer asked for coffee the vendor might supply a sample containing any quantity of chicory, providing it is placed in a wrapper labelled, "A mixture of chicory and coffee." The wrapper produced by Mr. Ogle was itself an ingenious device; it was somewhat misleading, and was printed as follows: "The finest fresh-roasted coffee. This is sold as a mixture of chicory and coffee." It had been held by a metropolitan magistrate, in a recent case, that if coffee was asked for, the purchaser was defrauded if any other article was supplied, however it might be labelled. He would further call the attention of the magistrate to the case of Liddle v. Reese, and the judgment of Justices Lush and Manisty, the protection afforded to the vendor by the giving of a label, referred to in section 8 of the Act, applied to the sale of compounded articles of food mixed with any matter or ingredient not injurious to health, and not intended fraudulently to increase its bulk, weight, or measure. Coffee was not necessarily a compounded article, and where chicory was added, which could be purchased separately at about one-fourth the price, he respectfully submitted that the effect was fraudulently to increase its bulk and weight, and that, consequently, an offence had been committed against the statute. Mr. Bushby said, after hearing the evidence, that he was of opinion that the vender had complied with the statute by giving a label, and that the case could not be sustained. If, however, a point of law were submitted to him, he would consider whether he should state a case for an appeal to a superior court.

INTERESTING CASES OF THE ADULTERATION OF OLIVE OIL.-At the Wandsworth Police Court, on the 17th ult., J. Palmer and Sons, Balham, were charged by Inspector Smith with selling olive oil so adulterated as to be indigestible, and consequently dangerous to health. The Inspector produced Dr. Muter's certificate, which showed that the oil was chiefly mineral oil, so prepared as to resemble olive oil in appearance. The defendant was fined £10 and costs.

At the same court, on the 1st of May, W. Taylor, jun., of Clapham, was charged by Inspector Smith with selling adulterated olive oil. Dr. Muter's certificate showed the article to contain not less than 50 per cent. of ground nut oil. The defendant pleaded entire ignorance, and the magistrate seeing that the article was not dangerous to health, let him off with 1s. fine and costs.

At the Southwark Police Court, on Wednesday, the 15th ult., before W. Slade, Esq., E. R. Goodrich, wholesale and retail oilman, 35, Old Kent Road, appeared in answer to a summons taken out by John Edwards, the Inspector for the District of St. George the Martyr, S.E. (on the certificate of Dr. Muter), for selling olive oil adulterated with 20 per cent. of cotton-seed oil. The defendant's counsel stated that he would plead guilty as he had had the oil analysed and found the certificate to be correct. The defendant had called in all the oil he sent out as olive oil as soon as he knew it to be impure, and he urged the magistrate to impose only a small fine. The Inspector stated to his worship that it was labelled "Finest Lucca Oil." The magistrate imposed a penalty of £5, and 12s. 6d. as costs.

CORRESPONDENCE.

[The Editor is not in any way responsible for opinions expressed by his correspondents.]
To the Editor of the ANALYST.

"NOTES ON LACTOSE."

SIR, I very much regret that I was prevented from attending the March meeting of the Society when Mr. E. W T. Jones read a paper upon Lactose," as I certainly should have pointed out that a considerable portion of the results contained in his paper had already been published in the ANALYST, Vol. xi., page 27.

Yours, etc.,

Mr. Jones' results, however, corroborate those obtained by myself. Thanking you beforehand for insertion of the above in your next issue. 13, Fish Street Hill, Eastcheap, London, 6th May, 1889.

WILLIAM JOHNSTONE.

ABNORMAL BUTTERS.

To the Editor of the ANALYST.

SIR,-I was under the impression that Mr. Estcourt was himself the authority for my statement that he had habitually employed, with his Westphal balance, a thermometer-plummet of which the bulb was broken, and which, therefore, gave him only arbitrary figures. I presume I may take Mr. Estcourt's last letter as an indication that I misunderstood him, but the use of a broken thermometerplummet for observations at the boiling point of water is quite compatible with the simultaneous possession of an undamaged plummet for use at ordinary temperatures.

I did not give up quoting specific gravities of melted fats at 100° F. at the suggestion of Mr. Estcourt; but I did adopt the use of the Westphal balance, in place of the Sprengel tube I had previously employed, at his suggestion. Mr. Estcourt employed a bath of heated paraffin, instead of one of boiling water as adopted by me.

ALFRED H. ALLEN.

May 14th, 1889.