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Experimental method

Design of experiment (Things that you can play around with your experiment)
**Typically, scope of study by experimentalist will fall on one of the following categories.
Minimum is you need to do for categories 2 & 5 in which you prepare your material and test its
performance.
1) Screening
- Finding the best raw material/chemical
2) Preparation
- Choose the best synthesis method
3) Optimization
- Optimize the synthesis condition to give the best performance
4) Characterization
- Investigate physical & chemical properties of developed products
5) Performance/process study
- Study the performance of the developed products
- Study the effect of each interested parameters
6) Modeling
- Come up with simple model to explain the phenomenon found in experiment
- Try to explain it based on some principles, laws and theories with complete math derivation
7) Scale-up
- Conduct the performance study in pilot plant scale
- To see the performance under field condition or large scale

Tips for each work flow


Screening
- Try to find those raw material from nature and the best are waste, non-toxic, recyclable,
abundant and easy to process.
- Or chemicals that are safe to use.
- Try to avoid using HF acid, dealing with H2S gases, radioactive material, and controlled
bacteria/virus.
- Go through MSDS to check the info on each chemicals
Preparation
- Look for plausible synthesis method that is doable at Curtin
- Calculate how many grams that you need for characterization and performance study.
- Make sure you know the amount required for each experimental run
- Make sure you have all glassware and equipment needed

Optimization
- Suggested to use the software of Design of Experiment (DOE) to help you to generate the
experimental matrix
- It will tell you how to set the condition for each experimental run
- Besides, it will also give you the optimized solution for best performance and which
parameters are significant to affect your performance

Characterization
- X-Ray diffraction (XRD) and crystal structure determination
- Field Emission Scanning Electron Microscope (FESEM) and surface morphology
observation
- Physical nitrogen adsorption and desorption analysis and Specific surface area
determination
- Fourier Transform Infrared Spectroscopy (FTIR) and IR active functional group
determination
- Nuclear Magnetic Resonance (NMR), and pore distribution and permeability
determination
- High Resolution Transmission Electron Microscope (HRTEM) and crystallographic
defects observation
- Energy Dispersive X-Ray Spectroscopy (EDS) and elemental analysis (XRF)
- Dynamic Light Scattering (DLS) technique and particles size distribution
- Gel Permeation Chromatography (GPC) and polymer molecular weight determination
- Ultraviolet-Visible Spectrophotometry (UV-Vis) and solution concentration
determination
- Conductivity measurements and micelles critical concentration determination
- Simultaneous Thermogravimetry and Differential Scanning Calorimetry (TGA/DSC)
analysis
- Drop Shape Analyzer (DSA) and contact angle measurement
- Rheology and viscosity profiling

Performance/process study
- Test the performance of your developed material (EOR, wettability, strength, elasticity,
etc)
- Study the effect of interested parameters (temperature, pressure, concentration, etc.)
Modeling
- Come up with a developed model to explain the rate of reaction based on maths.
- To study the dynamic of your system or reaction
- Able to predict the condition beyond your range of study

Scale-up
- Run in larger scale and investigate the decrease in performance
- Aim for commercialization

Lab skills
- Add in water first before adding any acid or bases (to avoid the glassware from being
cracked under excessive heat of dissolution)
- Make sure the sample is neutral before putting it in oven or furnace (corrosion problem)
- Wear proper protective equipments (glove, mask, goggle)

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