A System of Instruction in the Practical Use of the Blowpipe
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A System of Instruction in the Practical Use of the Blowpipe - DigiCat
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A System of Instruction in the Practical Use of the Blowpipe
EAN 8596547377603
DigiCat, 2022
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Table of Contents
PREFACE.
THE BLOWPIPE.
Part First.
THE USE OF THE BLOWPIPE.
B. UTENSILS.
VARIOUS APPARATUS NECESSARY.
THE REAGENTS.
Part II.
INITIATORY ANALYSIS.
1. EXAMINATIONS WITH THE GLASS BULB.
2. EXAMINATIONS IN THE OPEN TUBE.
3. EXAMINATIONS UPON CHARCOAL.
4. EXAMINATIONS IN THE PLATINUM FORCEPS.
5. EXAMINATIONS IN THE BORAX BEAD.
6. EXAMINATIONS IN MICROCOSMIC SALT.
TABLE I.
A. BORAX
A. BORAX
B. MICROCOSMIC SALT.
B. MICROCOSMIC SALT.
TABLE II.
7. EXAMINATIONS WITH CARBONATE OF SODA.
Part III
SPECIAL REACTIONS; OR, THE BEHAVIOR OF SUBSTANCES BEFORE THE BLOWPIPE.
A. METALLIC OXIDES.
CLASS II.
CLASS III.
NON-METALLIC SUBSTANCES.
TABULAR STATEMENT OF THE REACTIONS OF MINERALS BEFORE THE BLOWPIPE.
POTASH.
SODA.
BARYTA AND STRONTIA.
LIME.
MAGNESIA.
ALUMINA.
SILICATES.
TABLE II.
URANIUM.
IRON.
MANGANESE.
NICKEL AND COBALT.
ZINC.
BISMUTH.
LEAD.
COPPER.
ANTIMONY.
ARSENIC.
MERCURY.
SILVER.
THE END.
PREFACE.
Table of Contents
It is believed the arrangement of the present work is superior to that of many of its predecessors, as a vehicle for the facilitation of the student's progress. While it does not pretend to any other rank than as an introduction to the larger works, it is hoped that the arrangement of its matter is such that the beginner may more readily comprehend the entire subject of Blowpipe Analysis than if he were to begin his studies by the perusal of the more copious works of Berzelius and Plattner.
When the student shall have gone through these pages, and repeated the various reactions described, then he will be fully prepared to enter upon the study of the larger works. To progress through them will then be but a comparatively easy task.
The arrangement of this little work has been such as the author and his friends have considered the best that could be devised for the purpose of facilitating the progress of the student. Whether we have succeeded is left for the public to decide. The author is indebted to several of his friends for valuable contributions and suggestions.
S.
CINCINNATI, June, 1857.
THE BLOWPIPE.
Table of Contents
Part First.
Table of Contents
THE USE OF THE BLOWPIPE.
Table of Contents
Go to TOC
Perhaps during the last fifty years, no department of chemistry has been so enriched as that relating to analysis by means of the Blowpipe.
Through the unwearied exertions of men of science, the use of this instrument has arrived to such a degree of perfection, that we have a right to term its use, "Analysis in the dry way, in contradistinction to analysis
in the wet way." The manipulations are so simple and expeditious, and the results so clear and characteristic, that the Blowpipe analysis not only verifies and completes the results of analysis in the wet way, but it gives in many cases direct evidences of the presence or absence of many substances, which would not be otherwise detected, but through a troublesome and tedious process, involving both prolixity and time; for instance, the detection of manganese in minerals.
Many substances have to go through Blowpipe manipulations before they can be submitted to an analysis in the wet way. The apparatus and reagents employed are compendious and small in number, so that they can be carried easily while on scientific excursions, a considerable advantage for mineralogists and metallurgists.
The principal operations with the Blowpipe may be explained briefly as follows:
(a.) By Ignition is meant the exposure of a substance to such a degree of heat, that it glows or emits light, or becomes red-hot. Its greatest value is in the separation of a volatile substance from one less volatile, or one which is entirely fixed at the temperature of the flame. In this case we only take cognizance of the latter or fixed substance, although in many instances we make use of ignition for the purpose of changing the conditions of a substance, for example, the sesquioxide of chromium (Cr²O³) in its insoluble modification; and as a preliminary examination for the purpose of ascertaining whether the subject of inquiry be a combination of an organic or inorganic nature.
The apparatus used for this purpose are crucibles of platinum or silver, platinum foil, a platinum spoon, platinum wire or tongs, charcoal, glass tubes, and iron spoons.
(b.) Sublimation is that process by which we convert a solid substance into vapor by means of a strong heat. These vapors are condensed by refrigeration into the solid form. It may be termed a distillation of a solid substance. Sublimation is of great consequence in the detection of many substances; for instance, arsenic, antimony, mercury, etc.
The apparatus used for the purposes of sublimation consist of glass tubes closed at one end.
(c.) Fusion.—Many substances when exposed to a certain degree of heat lose their solid form, and are converted into a liquid. Those substances which do not become converted into the liquid state by heat, are said to be infusible. It is a convenient classification to arrange substances into those which are fusible with difficulty, and those which are easily fusible. Very often we resort to fusion for the purpose of decomposing a substance, or to cause it to enter into other combinations, by which means it is the more readily detected. If insoluble substances are fused with others more fusible (reagents) for the purpose of causing a combination which is soluble in water and acids, the operation is termed unclosing. These substances are particularly the silicates and the sulphates of the alkaline earths. The usual reagents resorted to for this purpose are carbonate of soda (NaO, CO²), carbonate of potash (KO, CO²), or still better, a mixture of the two in equal parts. In some cases we use the hydrate of barytes (BaO, HO) and the bisulphate of potash (KO, 2SO³). The platinum spoon is generally used for this manipulation.
Substances are exposed to fusion for the purpose of getting a new combination which has such distinctive characteristics that we can class it under a certain group; or for the purpose of ascertaining at once what the substance may be. The reagents used for this purpose are borax (NaO, 2BrO³) and the microcosmic salt (NaO, NH⁴O, PO⁵, HO). Charcoal and the platinum wire are used as supports for this kind of operation.
(d.) Oxidation.—The chemical combination of any substance with oxygen is termed oxidation, and the products are termed oxides. As these oxides have qualities differing from those which are non-oxidized, it therefore frequently becomes necessary to convert substances into oxides; or, if they are such, of a lower degree, to convert them into a higher degree of oxidation. These different states of oxidation frequently present characteristic marks of identity sufficient to enable us to draw conclusions in relation to the substance under examination. For instance, the oxidation of manganese, of arsenic, etc. The conditions necessary for oxidation, are high temperature and the free admission of air to the substance.
If the oxidation is effected through the addition of a substance containing oxygen (for instance, the nitrate or chlorate of potash) and the heating is accompanied by a lively deflagration and crackling noise, it is termed detonation. By this process we frequently effect the oxidation of a substance, and thus we prove the presence or the absence of a certain class of substances. For instance, if we detonate (as it is termed by the German chemists) the sulphide of antimony, or the sulphide of arsenic with nitrate of potash, we get the nitrate of antimony, or the nitrate of arsenic. The salts of nitric or chloric acid are determined by fusing them with the cyanide of potassium, because the salts of these acids detonate.
(e.) Reduction.—If we deprive an oxidized substance of its oxygen, we term the process reduction. This is effected by fusing the substance under examination with another which possesses a greater affinity for oxygen. The agents used for reduction are hydrogen, charcoal, soda, cyanide of potassium, etc. Substances generally, when in the unoxidized state, have such characteristic qualities, that they cannot very readily be mistaken for others. For this reason, reduction is a very excellent expedient for the purpose of discerning and classifying many substances.
B. UTENSILS.
Table of Contents
Go to TOC
We shall give here a brief description of the most necessary apparatus used for analysis in the dry way, and of their use.
FIG 1The Blowpipe is a small instrument, made generally out of brass, silver, or German silver, and was principally used in earlier times for the purpose of soldering small pieces of metals together. It is generally made in the form of a tube, bent at a right angle, but without a sharp corner. The largest one is about seven inches long, and the smallest about two inches. The latter one terminates with a small point, with a small orifice. The first use of the blowpipe that we have recorded is that of a Swedish mining officer, who used it in the year 1738 for chemical purposes, but we have the most meagre accounts of his operations. In 1758 another Swedish mining officer, by the name of Cronstedt, published his Use of the Blowpipe in Chemistry and Mineralogy,
translated into English, in 1770, by Van Engestroem. Bergman extended its use, and after him Ghan and the venerable Berzelius (1821). The blowpipe most generally used in chemical examinations is composed of the following parts: (Fig. 1.) A is a little reservoir made air-tight by grinding the part B into it. This reservoir serves the purpose of retaining the moisture with which the air from the mouth is charged. A small conical tube is fitted to this reservoir. This tube terminates in a fine orifice. As this small point is liable to get clogged up with soot, etc., it is better that it should be made of platinum, so that it may be ignited. Two of these platinum tubes should be supplied, differing in the size of the orifice, by which a stronger or lighter current of flame may be projected from it. Metals, such as brass or German silver, are very liable to become dirty through oxidation, and when placed between the lips are liable to impart a disagreeable taste. To avoid this, the top of the tube must be supplied with a mouthpiece of ivory or horn C. The blowpipe here represented is the one used by Ghan, and approved by Berzelius. The trumpet mouthpiece was adopted by Plattner; it is pressed upon the lips while blowing, which is less tiresome than holding the mouthpiece between the lips, although many prefer the latter mode.
Dr. Black's blowpipe is as good an instrument and cheaper. It consists of two tubes, soldered at a right angle; the larger one, into which the air is blown, is of sufficient capacity to serve as a reservoir.
A chemist can, with a blowpipe and a piece of charcoal, determine many substances without any reagents, thus enabling him, even when travelling, to make useful investigations with means which are always at his disposal. There are pocket blowpipes as portable as a pencil case, such as Wollaston's and Mitscherlich's; these are objectionable for continued use as their construction requires the use of a metallic mouthpiece. Mr. Casamajor, of New York, has made one lately which has an ivory mouthpiece, and which, when in use, is like Dr. Black's.
The length of the blowpipe is generally seven or eight inches, but this depends very much upon the visual angle of the operators. A short-sighted person, of course, would require an instrument of less length than would suit a far-sighted person.
The purpose required of the blowpipe is to introduce a fine current of air into the flame of a candle or lamp, by which a higher degree of heat is induced, and consequently combustion is more rapidly accomplished.
FIG 2By inspecting the flame of a candle burning under usual circumstances, we perceive at the bottom of the flame a portion which is of a light blue color (a b), Fig. 2, which gradually diminishes in size as it recedes from the wick, and disappears when it reaches the perpendicular side of the flame. In the midst of the flame there is a dark nucleus with a conical form (c). This is enveloped by the illuminating portion of the flame (d). At the exterior edge of the part d we perceive a thin, scarcely visible veil, a, e, e, which is broader near the apex of the flame. The action of the burning candle may be thus explained. The radiant heat from the flame melts the tallow or wax, which then passes up into the texture of the wick by capillary attraction until it reaches the glowing wick, where the heat decomposes the combustible matter into carbonated hydrogen (C⁴H⁴), and into carbonic oxide (CO).
While these gases are rising in hot condition, the air comes in contact with them and effects their combustion. The dark portion, c, of the flame is where the carbon and gases have not a sufficiency of air for their thorough combustion; but gradually they become mixed with air, although not then sufficient for complete combustion. The hydrogen is first oxidized or burnt, and then the carbon is attacked by the air, although particles of carbon are separated, and it is these, in a state of intense ignition, which produce the illumination. By bringing any oxidizable substance into this portion of the flame, it oxidizes very quickly in consequence of the high temperature and the free access of air. For that reason this part of the flame is termed the oxidizing flame, while the illuminating portion, by its tendency to abstract oxygen for the purpose of complete combustion, easily reduces oxidated substances brought into it, and it is, therefore, called the flame of reduction. In the oxidizing flame, on the contrary, all the carbon which exists in the interior of the flame is oxidized into carbonic acid (CO²) and carbonic oxide (CO), while the blue color of the cone of the flame is caused by the complete combustion of the carbonic oxide. These two portions of the flame—the oxidizing and the reducing—are the principal agents of blowpipe analysis.
If we introduce a fine current of air into a flame, we notice the following: The air strikes first the dark nucleus, and forcing the gases beyond it, mixes with them, by which oxygen is mingled freely with them. This effects the complete combustion of the gases at a certain distance from the point of the blowpipe. At this place the flame has the highest temperature, forming there the point of a blue cone. The illuminated or reducing portion of the flame is enveloped outside and inside by a very hot flame, whereby its own temperature is so much increased that in this reduction-flame many substances will undergo fusion which would prove perfectly refractory in a common flame. The exterior scarcely visible part loses its form, is diminished, and pressed more to a point, by which its heating power is greatly increased.
The Blast of Air.—By using the blowpipe for chemical purposes, the effect intended to be produced is an uninterrupted steady stream of air for many minutes together, if necessary, without an instant's cessation. Therefore, the blowing can only be effected with the muscles of the cheeks, and not by the exertion of the lungs. It is only by this means that a steady constant stream of air can be kept up, while the lungs will not be injured by the deprival of air. The details of the proper manner of using the blowpipe are really more difficult to describe than to acquire by practice; therefore the pupil is requested to apply himself at once to its practice, by which he will soon learn to produce a steady current of air, and to distinguish the different flames from each other. We would simply say that the tongue must be applied to the roof of the mouth, so as to interrupt the communication between the passage of the nostrils and the mouth. The operator now fills his mouth with air, which is to be passed through the pipe by compressing the muscles of the cheeks, while he breathes through the nostrils, and uses the palate as a valve. When the mouth becomes nearly empty, it is replenished by the lungs in an instant, while the tongue is momentarily withdrawn from the roof of the mouth. The stream of air can be continued for a long time, without the least fatigue or injury to the lungs. The easiest way for the student to accustom himself to the use of the blowpipe, is first to learn to fill the mouth with air, and while the lips are kept firmly closed to breathe freely through the nostrils. Having effected this much, he may introduce the mouthpiece of the blowpipe between his lips. By inflating the cheeks, and breathing through the nostrils, he will soon learn to use the instrument without the least fatigue. The air is forced through the tube against the flame by the action of the muscles of the cheeks, while he continues to breathe without interruption through the nostrils. Having become acquainted with this process, it only requires some practice to produce a steady jet of flame. A defect in the nature of the combustible used, as bad oil, such as fish oil, or oil thickened by long standing or by dirt, dirty cotton wick, or an untrimmed one, or a dirty wickholder, or a want of steadiness of the hand that holds the blowpipe, will prevent a steady jet of flame. But frequently the fault lies in the orifice of the jet, or too small a hole, or its partial stoppage by dirt, which will prevent a steady jet of air, and lead to difficulty. With a good blowpipe the air projects the entire flame, forming a horizontal, blue cone of flame, which converges to a point at about an inch from the wick, with a larger, longer, and more luminous flame enveloping it, and terminating to a point beyond that of the blue flame.
To produce an efficient