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This eBook from the Gutenberg Project consists of approximately 188 pages of information about An Introductory Course of Quantitative Chemical Analysis.

Platinum crucibles have the advantage that they can be employed at high temperatures, but, on the other hand, these crucibles can never be used when there is a possibility of the reduction to the metallic state of metals like lead, copper, silver, or gold, which would alloy with and ruin the crucible.  When platinum crucibles are used with compounds of arsenic or phosphorus, special precautions are necessary to prevent damage.  This statement applies to both fusions and ignitions.

Fusions with sodium carbonate can be made only in platinum, since porcelain or silica crucibles are attacked by this reagent.  Acid sulphate fusions, which require comparatively low temperatures, can sometimes be made in platinum, although platinum is slightly attacked by the flux.  Porcelain or silica crucibles may be used with acid fluxes.

Silica crucibles are less likely to crack on heating than porcelain crucibles on account of their smaller coefficient of expansion.  Ignition of substances not requiring too high a temperature may be made in porcelain or silica crucibles.

Iron, nickel or silver crucibles are used in special cases.

In general, platinum crucibles should be used whenever such use is practicable, and this is the custom in private, research or commercial laboratories.  Platinum has, however, become so valuable that it is liable to theft unless constantly under the protection of the user.  As constant protection is often difficult in instructional laboratories, it is advisable, in order to avoid serious monetary losses, to use porcelain or silica crucibles whenever these will give satisfactory service.  When platinum utensils are used the danger of theft should always be kept in mind.

PREPARATION OF CRUCIBLES FOR USE

All crucibles, of whatever material, must always be cleaned, ignited and allowed to cool in a desiccator before weighing, since all bodies exposed to the air condense on their surfaces a layer of moisture which increases their weight.  The amount and weight of this moisture varies with the humidity of the atmosphere, and the latter may change from hour to hour.  The air in the desiccator (see above) is kept at a constant and low humidity by the drying agent which it contains.  Bodies which remain in a desiccator for a sufficient time (usually 20-30 minutes) retain, therefore, on their surfaces a constant weight of moisture which is the same day after day, thus insuring constant conditions.

Hot objects, such as ignited crucibles, should be allowed to cool in the air until, when held near the skin, but little heat is noticeable.  If this precaution is not taken, the air within the desiccator is strongly heated and expands before the desiccator is covered.  As the temperature falls, the air contracts, causing a reduction of air pressure within the covered vessel.  When the cover is removed (which is often rendered difficult) the inrush of air from the outside may sweep light particles out of a crucible, thus ruining an entire analysis.

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