During the digestion process, the oil sample should be carbonized at a low temperature for a specific duration before gradually increasing the heat for boiling digestion. If the temperature is too high too soon, the sample may spill over, leading to inaccurate results. To ensure complete digestion, it is important to continue the digestion for two hours after the solution becomes clear. This step guarantees that all organic matter is fully broken down.
Once the digestive solution has cooled in an ice bath, an excess of alkali solution is added. At this stage, the mixture separates into two distinct layers. It is crucial to handle this carefully before distillation to avoid mixing the layers prematurely, which could cause ammonia (NH3) to escape early and result in lower readings. When performing the distillation, once the distillation unit is connected, heating should begin immediately to prevent boric acid in the condensation tube from absorbing any ammonia due to cooling. Proper heating ensures that NH3 is effectively captured by the boric acid. As the solution approaches boiling, the heat should be reduced to maintain a steady boil and prevent rapid evaporation of ammonia, which could lead to incomplete absorption and lower test results.
The addition of sodium sulfide (Naâ‚‚S) serves to precipitate mercury (Hg), a highly toxic substance. Therefore, after the experiment, the waste liquid must not be disposed of in the sewer. Instead, it should be collected and properly treated to minimize environmental and health risks.
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This procedure highlights the importance of careful handling, precise timing, and safety measures in chemical analysis to achieve accurate and reliable results. Each step plays a critical role in ensuring the integrity of the final data. By following these guidelines, researchers can enhance the quality of their experiments while maintaining a safe working environment.
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