1. The result of the Maclagan reaction is dependent on circumstances (accidents), and the test, therefore, unreliable.

2. It is not known what impurities are to be determined by this reaction. 3. It has been shown that there is no difference in physiological effect between a cocaine of the German Pharmacopoeia (D. A. B. III.) standard, which satisfies the Maclagan reaction, and a similar product which will not meet this reaction.

To this condemnation of the Maclagan test we feel obliged to answer, as we have for many years recognized the great value of this test for examining the cocaine of commerce, based on the fact that a cocaine which will not answer this test contains isatropylcocaine, a known poison, in larger amount than should be permitted at this date for medicinal use. This knowledge has long been current in interested circles, and for this reason it is the more surprising that a cocaine hydrochlorate containing a large percentage of isatropylcocaine, introduced by an otherwise reputable firm, should have found acceptance generally, it being represented that the other products of the factory referred to are excellent, and the assurance that this product met the requirements of the German Pharmacopoeia, In this speciously justifying the sale.

manner the endeavors of manufacturers to provide the purest possible products for physicians are simply nullified for years to come, until the Pharmacopoeia commission arrives at the revelation that something better than before is attainable, and then establishes more stringest methods and tests.

Value of the Maclagan Test.

We will attempt to adduce proof of the value of the Maclagan test, and to show how little tenable are the arguments of Dr. Guenther in favor of inferior products and against the generally esteemed test.

While Maclagan states that even 4 per cent of allied alkaloids (Maclagan did not know of the isatropylcocaine in 1887, when his test was published), will cause a turbid solution, manufacturers have long known that it is isatropylcocaine which prevents a crystalline separation of cocaine in the ammonia test.

To prove that this impurity is contained in the cocaine previously referred to, we purchased kg. indirectly and tested it.

100 Gm. of this cocaine hydrochlorate were dissolved in water, precipitated with soda solution and dried. The alkaloid was dissolved in absolute alcohol, the lye then separated from the pure cocaine after cooling, and evaporated to a dry residue. From this residue we obtained, by repeated treatment with petroleum ether (see Liebermann, Ber. d., Deutsch, Chem. Gesellsch., 1888, p. 2,343), 3.6 Gm. of an alkaloid almost insoluble in petroleum

* Pharmaceutische Centralhalle, 1898, No. 9.

ether. To prove the actual presence of isatropylcocaine, this resultant alkaloid was split up by the aid of concentrated muriatic acid, according to Liebermann's directions (Ber. d., Dtsch., Chem. Gesellsch., 1888, p. 2,346), the yield being 1.1 Gm. crude isatropic acid, which was readily converted, by treatment with barytes solution, into the readily soluble barytes salt of y-isatropic acid or into the difficultly soluble barytes salt of 8-isatropic acid. Acids isolated from both salts, on a single recrystallization from alcohol, showed the melting points established by Liebermann, 274°, for the y-acid and 206° for the -acid.

observation contains at least 3.6 per cent Thus it is proved that the cocaine under isatropylcocaine, and probably more. This cocaine does not stand the Maclagan test, and a milky-opalescent turbidity immediately follows the addition of ammonia to its solution, showing, according to Maclagan, a minimum constituent of 4 per cent side-alkaloid.

In order to determine the influence of isatropylcocaine on the Maclagan test, we prepared solutions of pure cocaine hydrochlorate1 with isatropylcocaine hydrochlorate2, 0.1 Gm. to 87 Cc. water, as has been our custom, and tested each one after addition of 4 drops ammonia (sp. gr. 0.96), the solution in a thick glass container being stirred energetically with a glass-rod and the sides of the container scraped at intervals. The following reactions were noted:

Per Cent.

appropriately large drops must be taken. According to our experience, exercised daily on our own product, a cocaine containing less than 0.2 per cent isatropylcocaine will meet the Maclagan test on addition of 3 to 4 drops of ammonia. This will give a considerable crystalline precipitate, which, at the moment of separation, fills the entire solution (4 drops from the ammonia bottle used by us equal 0.2 Cc.).

Maclagan (we quote from commercial organic analysis, Allen, Vol. III., part II., p. 280) himself directs that 2 drops stronger ammonia be taken for 1 grain (0.0648 Gm.). He must evidently mean the stronger ammonia water of the United States Pharmacopoeia, sp. gr. 0.901=28 per cent. It then follows that for 0.1 Gm. 3 drops of 28 per cent ammonia must be taken or about 8 to 9 drops of a 10 per cent ammonia (sp. gr. 0.96) according to the German Pharmacopoeia, while in our experience 0.2 Cc. (4 drops) of the 10 per cent ammonia will suffice, or much less than Maclagan directs, which shows that the size of the drop is of little moment. Of course, sufficient ammonia must be present to liberate the base.

Summary of Views.

To summarize our views of the Maclagan test, it affords an accord control of the isatropylcocaine admixture in cocaine hydroclorate, if these conditions are closely observed:

1. In testing 0.1 Gm. cocaine hydro

Solution clear at first.

1.

2.

0.1

212

66

This exhibit demonstrates that a cocaine containing no isatropylcocaine, or only a very little (less than 0.2 per cent) can be clearly distinguished from a cocaine containing more of this impurity, by means of the Maclagan test.

cocaine.

A cocaine containing 0.2 per cent isatropylcocaine will not show much apparent difference compared to one with 1 per cent of the impurity; this is the cause of the so-called irregularity of the test: it requires an extremely pure A pure product is distinguished by reacting very promptly (within 1 to 3 minutes -possibly even within 5 minutes, dependent on the energy of the stirring) with a considerable precipitate.

With a larger content than 1 per cent isatropylcocaine (up to 4 per cent) the solution remains clear after the addition of ammonia, but no apparent crystalline precipitate will show even after the most energetic agitation and stirring for onequarter hour. With 4 per cent isatropylcocaine the addition of ammonia causes a slight opalescence; with 5 per cent the solution becomes distinctly opaque.

Regarding the size of the drops of ammonia, to which Dr. Guenther attributes a considerable influence on the test, we will say:

Theoretically 0.1 Gm. cocaine hydrochlorate requires 0.05 Gm. ammonia of 0.96 sp. gr. (=10 per cent ammonia); 3 drops, commonly equal three times this amount =0.15 Cc. (20 drops=1 Cc.).

This amount will therefore suffice, and

chlorate, at least 0.15 to 0.2 Cc. (3 to 4 drops) of ammonia (0.96 sp. gr.) must be employed.

2. The solution must be stirred with much energy in a strong glass container; we have observed that without stirring even a chemically pure (produced synthetically from ecgonin) cocaine rarely yields a precipitate. Rubbing (or scraping) the sides of the container about ten times around should follow immediately after addition of the ammonia, and then stir the solution with the glass rod.

By this method, cocaine containing less than 0.2 per cent isatropylcocaine will positively yield the precipitate.

We wish to mention here that the proposition of 0.1 Gm. cocaine hydrochlorate to 100 Gm. water, as stated by Dr. Guenther, does not coincide with Maclagan's directions. It is true the complicated English and American designation for ounces, fluid ounces, avoirdupois weight, medicinal weight, etc., make it difficult to transcribe the directions into metric weights. But a grain is ever 0.0648 Gm., and 2 ounces of water equal 2×31.104 Gm. by weight, giving the proportion:

0.0648 62.208-0.1 : 96.0.

:

We have found that, on the one hand, an increase of the quantity of water retards the separation (or precipitation) in pure cocaine also, and on the other hand, insufficient stirring of the solution (0.1: 100) of pure cocaine even will delay the precipitation beyond five minutes.

Now, in order to promote the adoption of a practical and accurate standard of the Maclagan test, we suggest: Dissolve 0.1 Gm. cocaine hydrochlorate in 85 Cc. water and add as many drops of ammonia (0.96 sp. gr.) as equal 0.2 Cc.

It remains now to discuss the third point of Dr. Guenther's condemnation of the Maclagan test, the physiological effect of a cocaine containing the impurity, isatropylcocaine.

The statement of Dr. Guenther, that there is no difference in physiological effect between a cocaine which meets and one that does not meet the requirements of the Maclagan test, is purely unfounded, and not a single medical authority is quoted in the article to sustain the claim.

There is no doubt as to the toxic properties of isatropylcocaine, for shortly after its discovery by Prof. Liebermann, Prof. Dr. O. Liebreich experimented with this alkaloid and Prof. Liebermann incorporates the report in his own treatise (Ber. d. Deutsch, Chem. Gesellsch., 1888, p. 2,344) as follows:

Prof. Dr. O. Liebreich kindly examined the alkaloid with regard to its physiologi cal effects. He informed me that this alkaloid is of interest because very toxic, and that probably the frequently noted toxic side-effects from not perfectly pure cocaine are due to its presence. In its effect, isatropylcocaine resembles neither cocaine nor atropine; it is rather a powerful cardiac poison; a reduction of sensibility could not be substantiated either on local application or as a general effect.

Despite the fact that the toxic effect of this side-alkaloid is known, cocaine containing 3 to 4 per cent of it is introduced commercially and is sold without hesitation for use by the physician, although testing the product and the procuring of actually pure cocaine are equally easy.

A conscientious manufacturer of cocaine should aim to furnish only a pure product; this is not expecting too much; and as a matter of fact all leading brands of cocaine are pure.

The control necessary to demonstrate the absence of this dangerous impurity, isatropylcocaine, from cocaine hydrochlorate, is amply provided for in Maclagan's test, so that anyone handling cocaine and particular to have only the purest possible product, may employ this test with perfect assurance that it will guarantee safety.

We believe the foregoing arguments fully demonstrate the importance and necessity for testing all cocaine of commerce by the Maclagan test.

Compound Spirit of Ether Deficient

in Strength.

Geo. W. Kennedy, of Pottsville, Pa., stated in an address, recently delivered by him before the local druggists' association, that he had examined ten samples of spirit of nitrous ether, only two of which complied with the Pharmacopoeial requirements. Six of the samples proved to be merely mixtures of ether and alcohol of the proper specific gravity, but devoid of any oil of wine, and two samples were mixtures of ether, alcohol and water without any oil of wine.

HOSPITAL FORMULARY.

Preparations Used in the Hospitals of New York.

or

The fifth revised edition of the "Hospital Formulary of the Department of Public Charities of the City of New York" has just been issued to the apothecaries of the Department. Dr. Charles Rice, the editor, prefaces the work with the following explanation: The present edition, he says, will be found to vary materially from the preceding. Many formulae have been omitted, either because they had become obsolete, because they may now be found either in the United States Pharmacopoeia or in the National Formulary, or because they were in use only in the insane asylums and the correctionary institutions, both of which are no longer connected with the Department of Public Charities. Among miscellaneous subjects, various tables and chapters have also been discarded, and replaced by subjects and tables believed to be of more practical utility.

The editor says: "The formulae, particularly those for internal medicines, have been given in a new manner, making them more perspicuous both for the prescriber and dispenser. In giving the quantities of the ingredients in terms of the metric system, it was not intended to make the latter, in all cases, the exact equivalents of the corresponding terms of apothecaries' weight and measure, as this would have produced awkward fractions. The aim was to preserve the relative proportions of the ingredients, and at the same time to obtain products of volume or weight as simple and rounded-off as possible."

The book is divided into two parts. Part I. is taken up with the formulae and descriptions of the galenical preparations in use in the several hospitals and outdoor dispensaries of the Department. Part II. is given over to "Miscellaneous Subjects" and contains a mass of valuable notes on the preparation of gauzes, antiseptic dressings, catgut, disinfectants, preservative liquids, percentage solutions and specific gravity tables. Below we give a selection from the Formulary:

Before the sodium arsenate is weighed, a sufficient quantity of it should be powdered and dried at 100 deg. C., until it ceases to lose weight. It will then still contain 2 molecules of water, which cannot be driven out at a temperature below 148 deg. C. If a perfectly crystalline salt, without any trace of efflorescence, is available, this may be used. In this case 134 grains of the crystallized salt are substituted for the 14 grains of the dried, or 0.48 Gm. of the former for 0.34 Gm. of the latter.

Tinct. iodi

10 Cc.

10 Cc.

80 Cc.

Aquae ammon....of each 4 fl. drs. Linimenti sapon q. s. ad 4 fl. ozs. Add the chloroform and tincture of aconite to the soap liniment; then add the

** This preparation is supplied, ready made, by the general drug department. It is tinted with fuchsine so that the solutions, and any dressings prepared with them. may have a light pinkish tint to distinguish them from others. A table for readily preparing aqueous solutions of corrosive sublimate of any strength likely required, by means of the glycerite, will be found further on. This table is also printed on cards, for hanging up, which may be obtained from the General Drug Department.

This preparation is also used in its undiluted state for destroying bed-bugs in bedsteads, cots,

etc.

It is freely painted into cracks and upon places where the insects are prone to gather, and will remain effective for a long time.

COLD.

From 3,000 Deg. F. to -320 F.

Experiments with the Electric Furnace and Liquid Air at a Meeting of the Society of Chemical Industry.

E

XTREMES of temperature met in the demonstrations given at the regular monthly meeting of the New York Section of the Society of Chemical Industry, held in the main lecture room of Havemeyer Hall, Columbia University, on Friday evening, March 25th. The two principal papers presented were by W. H. Birchmore and Charles E. Tripler on "The Liquefaction of Air on a Commercial Scale (with experiments)." The liquefaction of air was really only a means to an end-that end being "experiments," which, while full of interest on account of their novelty, were presented in a manner more suggestive of a "show" than of a demonstration before a scientific body.

The interesting items on the programme brought out a large attendance of the members at the dinner in the University restaurant, which was presided over by Professor Chandler, and which was admirably served and unusually good. An informal vote of thanks for Professor Chandler for courtesies extended to the diners was passed before they adjourned to Havemeyer Hall.

THE ELECTRICAL FURNACE FOR

LABORATORY WORK.

On convening the meeting in Havemeyer Hall, Dr. Chandler called on W. H. Birchmore, who delivered a brief address on the general principles involved in the use of the electrical furnace. Mr. Birchmore referred at some length to the work done by Moissan and the experiments performed by him in the course of his lecture in New York City some years since. (See AMERICAN DRUGGIST of November 10, 1896, page 287). Mr. Birchmore stated that in using the form of electrical furnace devised by Moissan, great difficulty was experienced in governing the distance between the two carbons which represented the different poles of the current. It was practically necessary for the operator to keep both these carbons in his hands all the time, and it would thus be seen that the operator was very much handicapped in ordinary laboratory work, as one man could not handle the carbons and at the same time manipulate the substance operated on. Mr. Birchmore has, with the assistance of an electrical engineer, succeeded in overcoming the mechanical imperfections experienced with the Moissan furnace. The perfected furnace, as shown by Mr. Birch more, consisted of a box of wrought iron, some eight inches square, the lid of which opens upwards. The interior of this box is lined throughout with what is commercially known as asbestos stove lining, which is applied in the form of a paste and which Mr. Birchmore found would stand very high temperatures.

In the Moissan furnace, the carbons

are inserted horizontally, one on either side. Mr. Birchmore has the carbons inserted perpendicularly, one carbon being connected with the graphite crucible and the other being suspended above the crucible. The point of greatest importance in the furnace was the apparatus for regulating the distance between the two poles in the arc. This distance is regulated by a contrivance, the details of which were not described, but which acts automatically.

For the purposes of this demonstration, one side of the furnace was fitted with a magnifying lens, which projected on a screen a brilliantly illuminated image of the crucible, showing the effect of the very high heat on the various substances subjected to its influence. The first experiment was made with a mixture of chromium oxide and coke, and the brilliant reflection on the screen showed how the oxide was reduced to the molten state and gradually gave off its oxygen, the result being a button of metallic chromium, which was viewed with much interest by the members. During the process of reduction a Nichol's prism was interposed between the lens and the screen, and a beautiful and brilliant spectrum thrown on another screen, which developed the groupings of the dark lines which characterize chromium.

was

Calcium oxide and coke were then fused together, calcium carbide being formed. The calcium spectrum was shown very vividly. The speaker called attention to a grouping of the dark lines in the green, which was generally said to be distinctively characteristic of calcium, but which he had observed in the spectrum of the arc light alone when no calcium whatever was present.

The final experiment made was with a mixture of carbon and silica. Mr. Birchmore said he did not expect to produce silicon carbide, but that the effect of the very high temperature was interesting as showing the fusing of the mass to a puttylike consistency, which was very clearly shown on the screen.

Mr. Birchmore said that where the operator could have at his command only one form of current, the continuous current was to be preferred, but that the alternating current possessed certain advantages and could with profit be resorted to in certain conditions.

The temperatures reached were so high as to fuse the ends of the carbons. The experiments were performed in the most interesting manner and evoked frequent rounds of applause.

EXPERIMENTS WITH LIQUID AIR.

After extending to Mr. Birchmore the thanks of the society for his interesting demonstration, Professor Chandler introduced Chas. E. Tripler, who had been detained by other engagements until rather late in the evening. Mr. Tripler proceeded to give his demonstrations in a manner which was highly entertaining to the large and somewhat mixed audience present. Notwithstanding the title of the paper, "The Liquefaction of Air on a Commercial Scale," Mr. Tripler said absolutely nothing as to the methods pursued in liquefying the air nor as to the practical uses to which it might be put. The "experiments" were many of them ingenious and well calculated to demonstrate the startling effect of the extremely low temperatures produced by the evaporation of liquid air.

Mr. Tripler said in the beginning of his lecture that the question of temperature was wholly a relative one, and that the behavior of substances at the very low temperatures which he proposed to show differed as widely from that at the normal temperature as it did at the temperatures several thousand degrees above freezing point which had been shown by the gentleman who preceded him.

Mr. Tripler was provided with a fivegallon tin can filled with liquid air, which was packed in felt, so as to insulate it as much as possible, and covered with a piece

He carried out a number of demonstrations which seemed almost on a par with those of a vaudeville conjurer. A glass of whisky was frozen sol by pouring liquid air into it, and stirring the mixture, and the solid whisky was turned out on a platter and passed around to the audience. Absolute alcohol was also frozen with astonishing rapidity and facility, as was also hydrochloric acid, sulphuric acid and a flask of bromine. The latter substance showed a very marked change of color under the influence of the extreme cold. turning from its well-known red color

of globules, but the gas forming rapidly on the surface of these globules caused them rapidly to rise to the surface of the water, and as soon as the gas was given off, the globules again sank until within a few moments all the liquid air was wholly dissipated. The effect is shown in Fig. 11.

The striking effects of the very low temperature produced by the expansion of the liquefied air were then shown by the lecturer in various ways, among which the following were particularly interesting. Eggs, fruit, and vegetables were

of felt. It was difficult for a moment for the audience to comprehend that the liquid which was handled in an ostentatiously careless manner by himself and his assistants was liquid air. The lecturer dipped a tin dipper into the liquid and threw it on the floor, when a dense white steam arose which was rapidly dissipated as the air assumed its normal condition. He made no effort to give any scientific description of the phenomena involved, and indeed when asked to state the latent heat of liquid air, the lecturer waived the question aside with the statement: "Oh, you will find that up there somewhere," referring to the blackboard, where Prof. Chandler had written a table of the physical constants of air and some other gases.

to a yellowish pink, the red color reappearing when the temperature rose.

Pure Liquid Oxygen.

The boiling point of nitrogen is thirteen centigrade degrees lower than that of oxygen, and as a consequence, when a mixture of the elements in the liquid form is allowed to evaporate, the nitrogen evaporates first, leaving the oxygen. The lecturer poured a quantity of liquid air into a flask half filled with water. The mixed elements in liquid form are lighter than water and consequently floated on its surface. As the nitrogen was dissipated, and the heavier oxygen left behind, this element sunk downward through the water in the form

frozen by being plunged into liquid air and were then easily pulverized by even a slight blow. A beefsteak was plunged into the fluid and soon assumed a very pale, pink color and became even more brittle than ordinary ice. A tin dipper immersed in the liquid became so brittle that slight pressure crumbled it, as shown in Fig. 3. A few ounces of metallic mercury poured into a paper mould were frozen by pouring liquid air upon it, and this was used, as shown in Fig. 10, to suspend a weight of seventy-five pounds, the screw eyes being frozen in the mercury. Another paper mould was filled with mercury, a wooden handle thrust into the mould, liquid air poured on it, and the mercury frozen so that with the

it burst, when dropped, as though made of glass. One of the most interesting experiments consisted in showing the paradoxical action of heat when applied to th liquid air. Some of the liquid was poured into an ordinary tin tea-kettle, which was placed over a bunsen burner. The effect of the heat seemed to be to decre se the amount of vapor given off, instead of increasing it, while the carbon dioxide formed by the burning of the gas was solidified all over the exterior of the kettle. The flame was then removed an a glass of water was thrown into the kettle, the latent heat of which caused the air to come off in great volumes.

Experiments with Liquid Air.

! Fig. 15.

10, Frozen bar of mercury. 11, Liquid oxygen in water. 12, Frozen whisky. 13, Carbonic acid snow. 14, Burning carbon in liquid air. 15, Steel tube burst by explosion of liquid air.

resulted in the formation of particles cf solid carbon dioxide, giving the effect of snow. Fig. 8 shows a flask devised by Dewar consisting of two flasks, one inside the other, with a high vacuum existing between the two. By this means the contents of the flask were so completely insulated that eight ounces of liquid air were passed around to the audience, and after an hour it was not wholly evaporated; the evaporation from the surface of the air in this flask was so slow that only a slight and very superficial motion was noticeable. A rubber ball plunged into a glass of the liquid was frozen almost instantly, and became so brittle that

Burning Steel in a Cup of Ice. Probably the most striking experiment of the evening consisted in burning a steel pen in the liquid oxygen contained in a cup of ice, which is illustrated in Fig. 2. The cup of ice was formed around an ordinary tumbler as a mould. The tumbler was removed, the ice cup half filled with liquefied air; the nitrogen allowed to evaporate and in the liquid oxygen left, an ordinary steel pen was plunged after being heated in the flame of a match. The steel of the pen burned with great brilliancy as soon as it was plunged into the oxygen, while the lecturer directed attention to the wide con

trast of temperature represented, stating that the temperature of burning steel was 2,000 degrees above zero, while the temperature of liquid air was some 312 degrees below zero.

A striking demonstration of the effect of the presence of liquid oxygen on combustion was shown by the sudden and brilliant explosion which took place when a piece of felt saturated with the liquid was touched off by a match. The high degree of force exerted by the expansion of the liquid air was shown by partially filling a copper tube with the liquid and driving a plug into one end and standing the tube upright on the lecture table. The expansion of the gas soon drove the plug out with a terrific report. This experiment is illustrated in Fig. 4. The terrific force which is exerted by the ignition of a piece of cotton wooi saturated with the liquid oxygen was shown by an exhibition of the wrought steel tube in which the experiment had been made. Into this tube, which was open at both ends, a small plug of cotton wool was inserted which had previously been saturated with the liquid oxygen. When a light was applied this tube burst, although the plug had been lightly inserted and both ends of the tube were open.

In concluding, the lecturer made a brief reference to the history of liquid air from the time, in 1878, when Pictet first demonstrated that it was not a permanent gas, down to the experiments of Prof. Dewar.

Mr. Tripler said that the question of the utilization of the liquid was a problem he would have to leave to the members of the society for solution. He, himself, believes that it has a brilliant future.

Owing to the lateness of the hour, the following papers were read by title, namely: "Process for the production of photographic prints on textile fabrics by means of adjective colors (demonstration of specimens)," by Robert Job; "The determination of tin in tinplate and roofing tin," by Stewart F. Carter.

Election of Officers.

Dr. Woodcock, who acted as secretary in the absence of Dr. Schweitzer, announced that the following had been elected by the Governing Committee as officers for the New York Section to take office on July 1st:

Chairman, Thomas J. Parker; vicechairman, Clifford Richardson; treasurer, R. C. Woodcock; secretary, H. Schweitzer. Messrs. H. Endemann and James Hartford were retired from the Committee for seniority of service. The following members of the committee were also retired: Wm. Jay Schieffelin, Virgil Coblentz and R. C. Schupphaus. To fill the vacancies thus created in the committee the following new members were named: Professor Chas. E. Pellew, Dr. Claude Rosell, H. T. Jarrett, Jacob Hasslacher, Byron B. Goldsmith.

TRIPLER'S METHOD OF LIQUE-
FYING AIR.

The reference made by Mr. Tripler to the method used by him for liquefying the air was so scanty that an AMERICAN DRUGGIST reporter interviewed him at his laboratory, on West Eighty-ninth street, with a view of learning something more definite about the method employed. We present herewith an illustration showing the interior of Mr. Tripler's laboratory and the apparatus used by him in the preparation of liquefied air.