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قراءة كتاب The Elements of Blowpipe Analysis

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The Elements of Blowpipe Analysis

The Elements of Blowpipe Analysis

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دار النشر: Project Gutenberg
الصفحة رقم: 4

Intumescence is the swelling of the substance upon heating.

Decrepitation is the crackling of a substance due to the sudden expansion of combined water upon heating.

Deflagration is the burning of a substance with explosive violence, generally due to excess of oxygen.

Incandescence is the white light emitted by a substance that is infusible when subjected to a high temperature.

Examination on Charcoal alone.—The size of the assay should be about that of a mustard seed. This is sufficiently large to show all of the reactions clearly, and though a larger piece would exhibit the characteristic phenomena, yet much more effort is required. A very small, shallow hole should be cut in the Ch. to receive the assay. The Bp. flame should be directed at an angle of about 30° with the surface of the Ch. Considerable care must be taken lest the hole in the Ch. is burned too deep and the assay lost in the coal.

The force of the air from the jet must also be borne in mind for a strong blast, or sudden puffs may blow the substance away.

The following changes are to be looked for:—

a. Whether the substance is volatile or non-volatile.

Illustrations. Examine before the Bp. on Ch. some arsenious oxide, As2O3, also some alumina, Al2O3.

b. Whether the substance is fusible or infusible.

Illustrations. Examine before the Bp. on Ch. some silver oxide, AgO, also some zinc oxide, ZnO.

c. Whether the substance is alkaline or non-alkaline when placed upon moistened red litmus.

Illustrations. Ignite some calcium carbonate, CaCO3, before the Bp. on Ch., and place residue on moistened red litmus. In like manner, examine some magnesium carbonate, MgCO3.

d. Color of coating on Ch. caused by combination of metal and oxygen due to heat of Bp. flame.

Illustrations. Examine some oxide of lead, PbO, before the Bp. on Ch., also some oxide of cadmium, CdO.

e. Decrepitation.

Illustration. Examine some sodium chloride, NaCl, before the Bp. on Ch.

f. Deflagration.

Illustrations. Examine some potassium nitrate, KNO3, before the Bp. on Ch., also some ammonium nitrate, NH4NO3.

g. Intumescence.

Illustration. Examine some alum,

K2Al2(SO4)4,

before the Bp. on Ch.

h. Incandescence.

Illustration. Examine some oxide of barium, BaO, before the Bp. on Ch.

i. Formation of a metallic bead—color and malleability.

Illustration. Examine some silver oxide, AgO, before the Bp. on Ch.

Examination on Charcoal with Na2CO3.—Metallic compounds are often difficult to reduce with the blowpipe flame alone, and hence no bead is obtained. In order to facilitate reduction and the obtaining of a metallic bead, the substance in a finely powdered condition is mixed with four parts of sodium carbonate, Na2CO3, and ignited before the Bp. on Ch. The metallic compound is decomposed, the metal being transformed into the carbonate, which in turn, through the agency of the Ch. and the heat of the flame, is reduced to the free metal. Sometimes the reduction is made easier by adding to the substance about its own bulk of potassium cyanide, KCN, which takes up oxygen from the compound and is converted into potassium cyanate, KCNO.

The reactions in reducing copper sulphate, CuSO4, with Na2CO3 and with KCN before the blowpipe, are here given:—

CuSO4 + Na2CO3 = CuCO3 + Na2SO4 } (1)
2CuCO3 + C = 3CO2 + 2Cu }
 
CuSO4 + Na2CO3 = CuCO3 + Na2SO4 }
CuCO3     = CuO + CO2 } (2)
CuO + KCN = Cu + KCNO }

After obtaining beads, it is well to obtain their coatings, for oftentimes it is only in this way that we can distinguish between the metals.

Examination in Tube with Na2CO3 and Charcoal.—If the substance in a finely pulverized condition be mixed with twelve parts, Na2CO3, and six parts of charcoal powder and the mixture be placed in an ignition tube and subjected to heat, the acid of the substance combines with the soda and the metal is set free.

If this metal is volatile, a sublimate is formed in the upper end of the tube.

Mercury deposits in minute globules, which may be seen with the magnifying glass. Arsenic forms a ring, which, when examined with the magnifying glass, is seen to be made up of minute crystals. Ammonia is recognized by its characteristic odor, and also by its turning a slip of moistened red litmus (held over the mouth of the tube) blue.

Examination on Platinum Wire.—Many substances possess the property of imparting to the colorless flame of the Bunsen burner characteristic colors.

The chlorides of these substances exhibit these flame reactions best, and hence before applying the flame tests we dip the wire which serves as a support into hydrochloric acid and then into the substance. When the substance has been taken up on the wire, it is placed in the edge of the long colorless flame of the Bunsen burner near the apex, when instantly the flame becomes tinged with the characteristic color of the substance.

Illustrations. Sodium compounds color the flame yellow, and a crystal of potassium dichromate appears colorless in the sodium light.

This sodium reaction is extremely delicate, it being possible to detect with ease a quantity of a sodium salt less than 1/3000000 of a milligram in weight.

Potassium colors the flame purplish-violet.

Barium colors the flame apple-green.

Strontium colors the flame crimson.

Calcium colors the flame orange-red, distinguished from strontium, by appearing gray when seen through blue glass.

Boracic acid colors the flame green when the substance has been moistened with glycerine.

Examination in Borax Bead.—Borax, Na2B4O7, and microcosmic salt,

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