What is the method of measuring sulfur for minerals such as metal oxide or molybdenum oxide through Leco furnace (or similar furnaces) at different temperatures, times and weights after leaching and after cleaning by titration method (gravimetry)?
You can use TG (Thermogravimetric) analysis for measuring the amount of mass losses during the thermal cycle. After the analysis, you should determine the main reactions which are probably responsible for that mass losses. It can be followed by the calculation based on the stoichiometry. I guess after that you will be able to predict which reactions occur during the thermal cycle.
The measurement of sulfur content in molybdenum oxide can be crucial for quality control and process optimization in industries such as metallurgy and catalyst manufacturing. One common method for measuring sulfur in molybdenum oxide is the combustion/infrared (IR) detection method. Here's a general guide:
### Combustion/Infrared (IR) Detection Method:
#### Materials and Equipment:
1. **Sulfur Analyzer:**
- An elemental analyzer specifically designed for sulfur determination.
2. **Molybdenum Oxide Sample:**
- The molybdenum oxide sample with a known mass.
3. **Combustion Tube:**
- A combustion tube capable of withstanding high temperatures.
4. **Oxygen Source:**
- A source of high-purity oxygen to support combustion.
5. **Infrared Detector:**
- An infrared detector capable of measuring sulfur dioxide (SO2) produced during combustion.
6. **Furnace:**
- A high-temperature furnace for combusting the sample.
7. **Sample Boat or Boat Combustion System:**
- A sample boat or boat combustion system for introducing the molybdenum oxide sample into the combustion tube.
8. **Gas Purification System:**
- A gas purification system to remove impurities.
#### Procedure:
1. **Sample Preparation:**
- Weigh a known mass of the molybdenum oxide sample.
2. **Combustion:**
- Introduce the sample into the combustion tube or boat combustion system.
3. **Combustion Reaction:**
- Initiate the combustion reaction by supplying high-purity oxygen to the sample in the presence of a combustion catalyst.
4. **Sulfur Oxidation:**
- The sulfur in the sample oxidizes to form sulfur dioxide (SO2) during combustion.
5. **Gas Separation:**
- After combustion, separate the combustion gases, including sulfur dioxide, from other combustion byproducts.
6. **Infrared Detection:**
- Direct the separated gases to the infrared detector, which measures the concentration of sulfur dioxide.
7. **Quantification:**
- The concentration of sulfur dioxide is used to calculate the sulfur content in the molybdenum oxide sample.
8. **Calibration:**
- Calibrate the sulfur analyzer using known sulfur standards to ensure accurate measurements.
9. **Quality Control:**
- Implement quality control measures to verify the precision and accuracy of the sulfur measurements.
10. **Data Analysis:**
- Analyze the data and report the sulfur content in the molybdenum oxide sample.
It's important to note that the specific details of the method may vary based on the sulfur analyzer used and the instrument's manufacturer. Always follow the manufacturer's guidelines and best practices for sample preparation, combustion, and detection. Additionally, consult relevant standards or methods such as ASTM or ISO for guidance on sulfur determination in specific materials.