CH4407_Lab Manual

CH4407 Process Technology 4 LABORATORY MANUAL

General Laboratory Safety Rules - Dept. of Chemical Sciences
Experiment Manual
- Exp. 1: Extraction of Copper Sulphate from Impregnated Vermiculite
- Exp. 2: Absorption of Carbon Dioxide (CO2) by Water in a Packed Column
- Exp. 3: Separation of Methanol-Water Mixture in a Plate Distillation Column
Interactive Questions
Guide to Lab Report (Lab Report Template)

Note: Safety Data Sheets for all chemicals are available for inspection in the laboratory.

Personal Protective Equipment (PPE):
- Safety glasses are mandatory; prescription glasses are inadequate for eye protection.
- Lab coats must be buttoned and closed shoes worn; legs and ankles must be covered; long hair should be tied back.
Food and Drink Prohibition:
- Eating, drinking, and chewing in the lab area is strictly prohibited.
Mobile Devices:
- Mobile phones are prohibited in undergraduate labs; these must remain in the cloakroom.
Operating Equipment:
- Do not operate any apparatus without training or instructions from the person in charge.
Waste Disposal:
- Broken glass must be disposed of in designated broken glass bins; sharps in sharps bins only.
- Clearly label, store, and transport samples and containers safely.
Fume Hood Use:
- Ensure fume hood extraction is active before work; operate with the sash at 1/3 height or lower.
- Avoid placing your head inside a fume hood.
Accident Reporting:
- Report all accidents, equipment breakages, or health concerns immediately.
Safety Equipment:
- Tampering with safety equipment is not tolerated.
Work Policy:
- No solo work; ensure work outside normal hours is authorized.
Cleanliness:
- Keep work areas tidy and walkways clear of obstructions; clean and return all glassware and equipment after use.
Consultation:
- Always consult an instructor if in doubt.
Consequences of Infringement:
- Breach of any rule may result in suspension or expulsion from the lab.

Familiarize with the experimental set-up before the experiment.
Control valves and switches: V1 & V5 fully open; V7 directs the extract to tank R2; V2, V4 & V9 closed.

The solubility and extraction from solid depend on solvent type and process conditions (flow, temperature).
The concentration of the extract decreases over time; determining the economic extraction point is critical.

Impregnated and dried Vermiculite with copper sulphate.
Terylene sample bag, CuSO4 stock solution, UV-Vis spectrophotometer.
Various glassware including volumetric flasks, pipettes, beakers, and distilled water.

Preparation:
- Fill the Terylene bag with vermiculite and place in the extractor vessel.
- Fill solvent tank R1 with 5 L distilled water.
- Check and prepare the UV-Vis spectrophotometer to measure at 820nm.
- Set the water pump at the prescribed rate; record initial sample weights and levels.
Sampling:
- Begin sampling after 3-4 minutes; record absorbance (ABS) values.
- Dilute samples as required for accurate readings.
- Record observations, temperatures, and ABS readings in Table 1.1.
Calibration and Measurements:
- Prepare calibration solutions using provided CuSO4 stock.
- Plot calibration curve for ABS versus concentration to determine sample concentrations from their absorbance.
Process Shut Down:
- Switch off equipment, collect extracts, and record final measurements.
- Arrange for the drying and weighing of samples.

CO2 exhibits moderate solubility in water, while air (mainly N2 and O2) does not.
Efficient gas absorption occurs in packed columns due to large interfacial areas and concentration differences.

pH probes, distilled water, 0.1 M NaOH, graduated cylinders, thermometer, barometer.

Set up includes monitoring pH changes throughout the experiment.
Record actions, observations, and pH in real time, ensuring appropriate adjustments are made based on readings.
Calculate dissolved CO2 concentrations from recorded pH values.

Compile data and findings for lab reports, including calculations, observations, and error analysis for all experiments.