Dry Assay.—There is no dry assay in use. Any method which may be adopted will necessarily be applicable only to special compounds.
WET METHODS.
There are several methods in use which leave little to be desired either in speed or accuracy. We will give (1) a gravimetric method in which the estimation may be made directly by weighing the carbonic acid, or, indirectly, by estimating the carbon dioxide from the loss; (2) a volumetric one, by which an indirect determination is made of the gas; and (3) a gasometric method, in which the volume of carbon dioxide given off is measured, and its weight deducted.
Direct Gravimetric Method.—Fit up the apparatus shown in the diagram (fig. 79). The various tubes are supported by a fixed rod with nails and wire loops, and connected by short lengths of rubber-tubing. The first tube contains soda-lime. The small flask is fitted with a rubber-stopper perforated with two holes, through one of which passes the tube of a pipette holding 25 or 30 c.c. This pipette is to contain the acid. The substance to be determined is weighed out into the flask. The second tube contains strong sulphuric acid; the third, pumice stone, saturated with copper sulphate solution, and dried until nearly white (at 200° C.); the fourth contains recently fused calcium chloride; and the fifth, which is the weighed tube in which the carbonic acid is absorbed, contains calcium chloride and soda-lime,[120] as shown in fig. 80. The sixth also contains calcium chloride and soda-lime; its object is to prevent the access of moisture and carbonic acid to the weighed tube from this direction; it is connected with an aspirator.
Having weighed the U-tube and got the apparatus in order, weigh up 1, 2, or 5 grams of the substance and place in the flask. Fill the pipette with dilute acid, close the clamp, and cork the flask. Then see that the apparatus is tight. Open the clamp and allow from 10 to 20 c.c. of the acid to run on to the assay. Carbonic acid will be evolved and will be driven through the tubes. The gas should bubble through the sulphuric acid in a moderate and regular stream. When the effervescence slackens the clamp is opened and the greater part of the remaining acid run in. When the effervescence has ceased the clamp is opened to its full extent and a current of air drawn through with an aspirator. A gentle heat is applied to the flask; but it should not be prolonged or carried to boiling. After the removal of the heat a gentle current of air is drawn through the apparatus for 30 or 40 minutes. The weighed U-tube, which in the early part of the operation will have become warm if much carbonic acid was present, will by this time be cold. It is disconnected, plugged, and weighed. The increase in weight is due to the carbon dioxide of the sample.
Example.—Ore taken 1 gram.
| Weight | of tube, | before | 42.6525 | grams |
| " | " | after | 43.0940 | " |
| ———- | ||||
| Increase | equals CO2 | 0.4415 | " |
