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Elements of Chemistry Part 30

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This apparatus cannot be used in very accurate experiments, when the substances intended to be operated upon have a very rapid action upon each other, or when one of them can only be introduced in small successive portions, as in such as produce violent effervescence when mixed together. In such cases, we employ a tubulated retort A, Pl. VII.

Fig. 1. into which one of the substances is introduced, preferring always the solid body, if any such is to be treated, we then lute to the opening of the retort a bent tube BCDA, terminating at its upper extremity B in a funnel, and at its other end A in a capillary opening.

The fluid material of the experiment is poured into the retort by means of this funnel, which must be made of such a length, from B to C, that the column of liquid introduced may counterbalance the resistance produced by the liquors contained in all the bottles, Pl. IV. Fig. 1.

Those who have not been accustomed to use the above described distilling apparatus may perhaps be startled at the great number of openings which require luting, and the time necessary for making all the previous preparations in experiments of this kind. It is very true that, if we take into account all the necessary weighings of materials and products, both before and after the experiments, these preparatory and succeeding steps require much more time and attention than the experiment itself.

But, when the experiment succeeds properly, we are well rewarded for all the time and trouble bestowed, as by one process carried on in this accurate manner much more just and extensive knowledge is acquired of the nature of the vegetable or animal substance thus submitted to investigation, than by many weeks a.s.siduous labour in the ordinary method of proceeding.

When in want of bottles with three orifices, those with two may be used; it is even possible to introduce all the three tubes at one opening, so as to employ ordinary wide-mouthed bottles, provided the opening be sufficiently large. In this case we must carefully fit the bottles with corks very accurately cut, and boiled in a mixture of oil, wax, and turpentine. These corks are pierced with the necessary holes for receiving the tubes by means of a round file, as in Pl. IV. Fig. 8.

SECT. II.

_Of Metallic Dissolutions._

I have already pointed out the difference between solution of salts in water and metallic dissolutions. The former requires no particular vessels, whereas the latter requires very complicated vessels of late invention, that we may not lose any of the products of the experiment, and may thereby procure truly conclusive results of the phenomena which occur. The metals, in general, dissolve in acids with effervescence, which is only a motion excited in the solvent by the disengagement of a great number of bubbles of air or aeriform fluid, which proceed from the surface of the metal, and break at the surface of the liquid.

Mr Cavendish and Dr Priestley were the first inventors of a proper apparatus for collecting these elastic fluids. That of Dr Priestley is extremely simple, and consists of a bottle A, Pl. VII. Fig. 2. with its cork B, through which pa.s.ses the bent gla.s.s tube BC, which is engaged under a jar filled with water in the pneumato-chemical apparatus, or simply in a bason full of water. The metal is first introduced into the bottle, the acid is then poured over it, and the bottle is instantly closed with its cork and tube, as represented in the plate. But this apparatus has its inconveniencies. When the acid is much concentrated, or the metal much divided, the effervescence begins before we have time to cork the bottle properly, and some gas escapes, by which we are prevented from ascertaining the quant.i.ty disengaged with rigorous exactness. In the next place, when we are obliged to employ heat, or when heat is produced by the process, a part of the acid distills, and mixes with the water of the pneumato-chemical apparatus, by which means we are deceived in our calculation of the quant.i.ty of acid decomposed.

Besides these, the water in the cistern of the apparatus absorbs all the gas produced which is susceptible of absorption, and renders it impossible to collect these without loss.

To remedy these inconveniencies, I at first used a bottle with two necks, Pl. VII. Fig. 3. into one of which the gla.s.s funnel BC is luted so as to prevent any air escaping; a gla.s.s rod DE is fitted with emery to the funnel, so as to serve the purpose of a stopper. When it is used, the matter to be dissolved is first introduced into the bottle, and the acid is then permitted to pa.s.s in as slowly as we please, by raising the gla.s.s rod gently as often as is necessary until saturation is produced.

Another method has been since employed, which serves the same purpose, and is preferable to the last described in some instances. This consists in adapting to one of the mouths of the bottle A, Pl. VII. Fig. 4. a bent tube DEFG, having a capillary opening at D, and ending in a funnel at G. This tube is securely luted to the mouth C of the bottle. When any liquid is poured into the funnel, it falls down to F; and, if a sufficient quant.i.ty be added, it pa.s.ses by the curvature E, and falls slowly into the bottle, so long as fresh liquor is supplied at the funnel. The liquor can never be forced out of the tube, and no gas can escape through it, because the weight of the liquid serves the purpose of an accurate cork.

To prevent any distillation of acid, especially in dissolutions accompanied with heat, this tube is adapted to the retort A, Pl. VII.

Fig. 1. and a small tubulated recipient, M, is applied, in which any liquor which may distill is condensed. On purpose to separate any gas that is absorbable by water, we add the double necked bottle L, half filled with a solution of caustic potash; the alkali absorbs any carbonic acid gas, and usually only one or two other ga.s.ses pa.s.s into the jar of the connected pneumato-chemical apparatus through the tube NO. In the first chapter of this third part we have directed how these are to be separated and examined. If one bottle of alkaline solution be not thought sufficient, two, three, or more, may be added.

SECT. III.

_Apparatus necessary in Experiments upon Vinous and Putrefactive Fermentations._

For these operations a peculiar apparatus, especially intended for this kind of experiment, is requisite. The one I am about to describe is finally adopted, as the best calculated for the purpose, after numerous corrections and improvements. It consists of a large matra.s.s, A, Pl. X.

fig. 1. holding about twelve pints, with a cap of bra.s.s a b, strongly cemented to its mouth, and into which is screwed a bent tube c d, furnished with a stop-c.o.c.k e. To this tube is joined the gla.s.s recipient B, having three openings, one of which communicates with the bottle C, placed below it. To the posterior opening of this recipient is fitted a gla.s.s tube g h i, cemented at g and i to collets of bra.s.s, and intended to contain a very deliquescent concrete neutral salt, such as nitrat or muriat of lime, acet.i.te of potash, &c. This tube communicates with two bottles D and E, filled to x and y with a solution of caustic potash.

All the parts of this machine are joined together by accurate screws, and the touching parts have greased leather interposed, to prevent any pa.s.sage of air. Each piece is likewise furnished with two stop-c.o.c.ks, by which its two extremities may be closed, so that we can weigh each separately at any period of the operation.

The fermentable matter, such as sugar, with a proper quant.i.ty of yeast, and diluted with water, is put into the matra.s.s. Sometimes, when the fermentation is too rapid, a considerable quant.i.ty of froth is produced, which not only fills the neck of the matra.s.s, but pa.s.ses into the recipient, and from thence runs down into the bottle C. On purpose to collect this sc.u.m and must, and to prevent it from reaching the tube filled with deliquescent salts, the recipient and connected bottle are made of considerable capacity.

In the vinous fermentation, only carbonic acid gas is disengaged, carrying with it a small proportion of water in solution. A great part of this water is deposited in pa.s.sing through the tube g h i, which is filled with a deliquescent salt in gross powder, and the quant.i.ty is ascertained by the augmentation of the weight of the salt. The carbonic acid gas bubbles up through the alkaline solution in the bottle D, to which it is conveyed by the tube k l m. Any small portion which may not be absorbed by this first bottle is secured by the solution in the second bottle E, so that nothing, in general, pa.s.ses into the jar F, except the common air contained in the vessels at the commencement of the experiment.

The same apparatus answers extremely well for experiments upon the putrefactive fermentation; but, in this case, a considerable quant.i.ty of hydrogen gas is disengaged through the tube q r s t u, by which it is conveyed into the jar F; and, as this disengagement is very rapid, especially in summer, the jar must be frequently changed. These putrefactive fermentations require constant attendance from the above circ.u.mstance, whereas the vinous fermentation hardly needs any. By means of this apparatus we can ascertain, with great precision, the weights of the substances submitted to fermentation, and of the liquid and aeriform products which are disengaged. What has been already said in Part I.

Chap. XIII. upon the products of the vinous fermentation, may be consulted.

SECT. IV.

_Apparatus for the Decomposition of Water._

Having already given an account, in the first part of this work, of the experiments relative to the decomposition of water, I shall avoid any unnecessary repet.i.tions, and only give a few summary observations upon the subject in this section. The princ.i.p.al substances which have the power of decomposing water are iron and charcoal; for which purpose, they require to be made red hot, otherwise the water is only reduced into vapours, and condenses afterwards by refrigeration, without sustaining the smallest alteration. In a red heat, on the contrary, iron or charcoal carry off the oxygen from its union with hydrogen; in the first case, black oxyd of iron is produced, and the hydrogen is disengaged pure in form of gas; in the other case, carbonic acid gas is formed, which disengages, mixed with the hydrogen gas; and this latter is commonly carbonated, or holds charcoal in solution.

A musket barrel, without its breach pin, answers exceedingly well for the decomposition of water, by means of iron, and one should be chosen of considerable length, and pretty strong. When too short, so as to run the risk of heating the lute too much, a tube of copper is to be strongly soldered to one end. The barrel is placed in a long furnace, CDEF, Pl. VII. Fig. 11. so as to have a few degrees of inclination from E to F; a gla.s.s retort A, is luted to the upper extremity E, which contains water, and is placed upon the furnace VVXX. The lower extremity F is luted to a worm SS, which is connected with the tubulated bottle H, in which any water distilled without decomposition, during the operation, collects, and the disengaged gas is carried by the tube KK to jars in a pneumato-chemical apparatus. Instead of the retort a funnel may be employed, having its lower part shut by a stop-c.o.c.k, through which the water is allowed to drop gradually into the gun-barrel.

Immediately upon getting into contact with the heated part of the iron, the water is converted into steam, and the experiment proceeds in the same manner as if it were furnished in vapours from the retort.

In the experiment made by Mr Meusnier and me before a committee of the Academy, we used every precaution to obtain the greatest possible precision in the result of our experiment, having even exhausted all the vessels employed before we began, so that the hydrogen gas obtained might be free from any mixture of azotic gas. The results of that experiment will hereafter be given at large in a particular memoir.

In numerous experiments, we are obliged to use tubes of gla.s.s, porcelain, or copper, instead of gun-barrels; but gla.s.s has the disadvantage of being easily melted and flattened, if the heat be in the smallest degree raised too high; and porcelain is mostly full of small minute pores, through which the gas escapes, especially when compressed by a column of water. For these reasons I procured a tube of bra.s.s, which Mr de la Briche got cast and bored out of the solid for me at Strasburg, under his own inspection. This tube is extremely convenient for decomposing alkohol, which resolves into charcoal, carbonic acid gas, and hydrogen gas; it may likewise be used with the same advantage for decomposing water by means of charcoal, and in a great number of experiments of this nature.

FOOTNOTES:

[60] The representation of this apparatus, Pl. IV. Fig. 1. will convey a much better idea of its disposition than can possibly be given by the most laboured description.--E.

CHAP. VII.

_Of the Composition and Application of Lutes._

The necessity of properly securing the junctures of chemical vessels to prevent the escape of any of the products of experiments, must be sufficiently apparent; for this purpose lutes are employed, which ought to be of such a nature as to be equally impenetrable to the most subtile substances, as gla.s.s itself, through which only caloric can escape.

This first object of lutes is very well accomplished by bees wax, melted with about an eighth part of turpentine. This lute is very easily managed, sticks very closely to gla.s.s, and is very difficultly penetrable; it may be rendered more consistent, and less or more hard or pliable, by adding different kinds of resinous matters. Though this species of lute answers extremely well for retaining ga.s.ses and vapours, there are many chemical experiments which produce considerable heat, by which this lute becomes liquified, and consequently the expansive vapours must very readily force through and escape.

For such cases, the following fat lute is the best hitherto discovered, though not without its disadvantages, which shall be pointed out. Take very pure and dry unbaked clay, reduced to a very fine powder, put this into a bra.s.s mortar, and beat it for several hours with a heavy iron pestle, dropping in slowly some boiled lintseed oil; this is oil which has been oxygenated, and has acquired a drying quality, by being boiled with litharge. This lute is more tenacious, and applies better, if amber varnish be used instead of the above oil. To make this varnish, melt some yellow amber in an iron laddle, by which operation it loses a part of its succinic acid, and essential oil, and mix it with lintseed oil.

Though the lute prepared with this varnish is better than that made with boiled oil, yet, as its additional expence is hardly compensated by its superior quality, it is seldom used.

The above fat lute is capable of sustaining a very violent degree of heat, is impenetrable by acids and spiritous liquors, and adheres exceedingly well to metals, stone ware, or gla.s.s, providing they have been previously rendered perfectly dry. But if, unfortunately, any of the liquor in the course of an experiment gets through, either between the gla.s.s and the lute, or between the layers of the lute itself, so as to moisten the part, it is extremely difficult to close the opening.

This is the chief inconvenience which attends the use of fat lute, and perhaps the only one it is subject to. As it is apt to soften by heat, we must surround all the junctures with slips of wet bladder applied over the luting, and fixed on by pack-thread tied round both above and below the joint; the bladder, and consequently the lute below, must be farther secured by a number of turns of pack-thread all over it. By these precautions, we are free from every danger of accident; and the junctures secured in this manner may be considered, in experiments, as hermetically sealed.

It frequently happens that the figure of the junctures prevents the application of ligatures, which is the case with the three-necked bottles formerly described; and it even requires great address to apply the twine without shaking the apparatus; so that, where a number of junctures require luting, we are apt to displace several while securing one. In these cases, we may subst.i.tute slips of linen, spread with white of egg and lime mixed together, instead of the wet bladder. These are applied while still moist, and very speedily dry and acquire considerable hardness. Strong glue dissolved in water may answer instead of white of egg. These fillets are usefully applied likewise over junctures luted together with wax and rosin.

Before applying a lute, all the junctures of the vessels must be accurately and firmly fitted to each other, so as not to admit of being moved. If the beak of a retort is to be luted to the neck of a recipient, they ought to fit pretty accurately; otherwise we must fix them, by introducing short pieces of soft wood or of cork. If the disproportion between the two be very considerable, we must employ a cork which fits the neck of the recipient, having a circular hole of proper dimensions to admit the beak of the retort. The same precaution is necessary in adapting bent tubes to the necks of bottles in the apparatus represented Pl. IV. Fig. 1. and others of a similar nature.

Each mouth of each bottle must be fitted with a cork, having a hole made with a round file of a proper size for containing the tube. And, when one mouth is intended to admit two or more tubes, which frequently happens when we have not a sufficient number of bottles with two or three necks, we must use a cork with two or three holes, Pl. IV. Fig. 8.

When the whole apparatus is thus solidly joined, so that no part can play upon another, we begin to lute. The lute is softened by kneading and rolling it between the fingers, with the a.s.sistance of heat, if necessary. It is rolled into little cylindrical pieces, and applied to the junctures, taking great care to make it apply close, and adhere firmly, in every part; a second roll is applied over the first, so as to pa.s.s it on each side, and so on till each juncture be sufficiently covered; after this, the slips of bladder, or of linen, as above directed, must be carefully applied over all. Though this operation may appear extremely simple, yet it requires peculiar delicacy and management; great care must be taken not to disturb one juncture whilst luting another, and more especially when applying the fillets and ligatures.

Before beginning any experiment, the closeness of the luting ought always to be previously tried, either by slightly heating the retort A, Pl. IV. Fig. 1, or by blowing in a little air by some of the perpendicular tubes S s s s; the alteration of pressure causes a change in the level of the liquid in these tubes. If the apparatus be accurately luted, this alteration of level will be permanent; whereas, if there be the smallest, opening in any of the junctures, the liquid will very soon recover its former level. It must always be remembered, that the whole success of experiments in modern chemistry depends upon the exactness of this operation, which therefore requires the utmost patience, and most attentive accuracy.

It would be of infinite service to enable chemists, especially those who are engaged in pneumatic processes, to dispense with the use of lutes, or at least to diminish the number necessary in complicated instruments.

I once thought of having my apparatus constructed so as to unite in all its parts by fitting with emery, in the way of bottles with cristal stoppers; but the execution of this plan was extremely difficult. I have since thought it preferable to subst.i.tute columns of a few lines of mercury in place of lutes, and have got an apparatus constructed upon this principle, which appears capable of very convenient application in a great number of circ.u.mstances.

It consists of a double necked bottle A, Pl. XII. Fig. 12.; the interior neck bc communicates with the inside of the bottle, and the exterior neck or rim de leaves an interval between the two necks, forming a deep gutter intended to contain the mercury. The cap or lid of gla.s.s B enters this gutter, and is properly fitted to it, having notches in its lower edge for the pa.s.sage of the tubes which convey the gas. These tubes, instead of entering directly into the bottles as in the ordinary apparatus, have a double bend for making them enter the gutter, as represented in Fig. 13. and for making them fit the notches of the cap B; they rise again from the gutter to enter the inside of the bottle over the border of the inner mouth. When the tubes are disposed in their proper places, and the cap firmly fitted on, the gutter is filled with mercury, by which means the bottle is completely excluded from any communication, excepting through the tubes. This apparatus may be very convenient in many operations in which the substances employed have no action upon Mercury. Pl. XII. Fig. 14. represents an apparatus upon this principle properly fitted together.

Mr Seguin, to whose active and intelligent a.s.sistance I have been very frequently much indebted, has bespoken for me, at the gla.s.s-houses, some retorts hermetically united to their recipients, by which luting will be altogether unnecessary.

CHAP. VIII.

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