差热扫描分析仪培训教程(TA DSC trianing).ppt

Hermetic Pans (Sealed) Hermetic Pans are available in: Aluminum – 600°C; 3 atm (300 kPa gage) Alodined Aluminum - 600°C; 3 atm (300 kPa gage) (For aqueous samples) Gold – 725°C, 6 atm (600 kPa gage) Specialized Sealed Pans High Volume - 100μL; 250°C; 600 psig(4.1 MPa) High Pressure - 35μL; 300°C; 1450 psig(10 MPa) Note: 3 atm is approximately 44 psig It Does Matter What Pan you use Monohydrate Pharmaceutical sample Sample Shape Keep sample thin Cover as much as the bottom of pan as possible Sample Shape Cut sample to make thin, don’t crush If pellet, cut cross section Sample Shape Cut sample to make thin, don’t crush If pellet, cut cross section If powder, spread evenly over the bottom of the pan Using Sample Press When using crimped pans, don’t over crimp Bottom of pan should remain flat after crimping When using Hermetic pans, a little more pressure is needed Hermetic pans are sealed by forming a cold wield on the Aluminum pans Crimped Pans Hermetic Pans Good Bad Sealed Not Sealed Sample Size Larger samples will increase sensitivity but……………. Larger samples will decrease resolution Goal is to have heat flow of 0.1-10mW going through a transition Sample Size Sample size depends on what you are measuring If running an extremely reactive sample (like an explosive) run very small samples (1mg) Pure organic materials, pharmaceuticals (1-5mg) Polymers - ~10mg Composites – 15-20mg Purge Gas Purge gas should always be used during DSC experiments Provides dry,inert atmosphere Ensures even heating Helps sweep away any off gases that might be released Nitrogen Most common Increases Sensitivity Typical flow rate of 50ml/min Purge Gas Helium Must be used with LNCS High Thermo-conductivity Increases Resolution Upper temp limited to 350°C Typical flow rate of 25ml/min Air or Oxygen Used to view oxidative effects Typical flow rate of 50ml/min Sample Temperature Range Rule of Thumb Have 2-3 minutes of baseline before and after