The oxidation product was heated on a watch crystal and the sublimate allowed to collect on a funnel. The first sublimate gave a melting point of 109 degrees Centigrade.
Combustions were made on this sublimate with the following results.
| (1) | C | 66% |
| H | 4.7% | |
| (2) | C | 65.7% |
| H | 4.8% | |
| (3) | C | 65.15% |
| H | 4.8% | |
| (4) | C | 65.8% |
| H | 4.85% |
The neutralization equivalent was obtained by titrating an alcoholic solution of the sublimate with standard sodium hydroxide. The following results were obtained on two different lots of the sublimed oxidation product.
| Wt. of substance | .09 | .1006 |
| Cc. of alkali N/10 | 7 cc | 7.9cc |
| Neutralization equiv. | 128.6 | 127.3 |
Using a third sample the neutralization equivalent was obtained from the analysis of the silver salt. The silver salt was formed by adding silver nitrate solution to a carefully neutralized solution of the sublimate. The insoluble silver salt was filtered off, washed with water to remove the excess of silver nitrate, and dried in a vacuum over sulphuric acid for several days. A weighed quantity of the silver salt was ignited in a platinum crucible and the residue of metallic silver was weighed. The following data were obtained using material from the same sample for each analysis.
| Wt. of dish | 12.8825 | 12.8826 |
| Wt. of dish and substance | 13.0060 | 13.1310 |
| Wt. of substance | .1235 | .2484 |
| Wt. of dish and silver | 12.9400 | 12.9980 |
| Wt. of silver | .0575 | .1154 |
| Neutralization equiv. | 125 | 125.3 |
Using the same sample, a neutralization equivalent was obtained by titration with standard NaOH.
| Wt. of substance | .0912 |
| N/10 NaOH | 7.25cc |
| Neutralization equiv. | 125.8 |
The above data shows that the sublimate is a mixture. No empirical formula can be calculated from the combustions, and different samples give different neutralization equivalents although the duplicate determinations on the same sample showed good agreement thus demonstrating the reliability of the methods.