OptiMelt Automated Melting Point System - Stanford Research ...
OptiMelt Automated Melting Point System - Stanford Research ... OptiMelt Automated Melting Point System - Stanford Research ...
48 Melting Point Determination Chapter 3If your sample is hygroscopic, or sublimates at high temperatures, the open end of thecapillary tube must be sealed by heating. Hygroscopic samples must be stored in adessicator between tests, this is particularly critical in humid environments or duringrainy days.The sample tubes are loaded into the OptiMelt by inserting them into one of the sampleposition slots located on top of the instrument. Up to three samples can be accommodatedby the heating block simultaneously. Loading three capillaries with the same substanceand melting them at the same time and averaging their melting points provides the fastestand simplest way to improve the repeatability and accuracy of melting pointdeterminations.Figure 29. Loading capillaries into OptiMelt.Tips• Most pharmacopeias list recommended drying procedures for melting point samplesand certified reference standards.• Make sure the OptiMelt is plugged in and set to a Start temperature below theexpected melting point of the sample(s) before placing any capillaries into the sampleslots.• Use the same batch of capillaries for calibration and for high accuracy measurementsto assure the repeatability of results. NOT ALL CAPILLARIES ARE MADEEQUAL!• The standard OptiMelt package includes a vial of precision melting point capillariesspecifically designed to (1) fit the OptiMelt heating stand and (2) provide the mostuniform and repeatable results. Replacement capillaries can be purchased directlyfrom SRS (SRS Part# O100MPC).• Never force a capillary into the heating block! Once the capillary is inserted into asample hole, it should literally drop down to the bottom of the stand.OptiMelt Automated Melting Point System
Chapter 3 Melting Point Determination 49• Some chemists choose to make their own capillary tubes. This is not recommendedfor accurate and reproducible results. The use of commercial capillaries, with tightmanufacturing tolerances, is strongly recommended instead.• For precision measurements, the optimum filling height of 2-3 mm must be strictlyobserved.• The use of a packing wire to compact a sample can lead to excessive bubbleformation and trapping during the phase transition. Do not use a packing wire ifexcessive bubble formation interferes with the detection of the meniscus and clearpoints of your sample.Tube CleaningFailure to clean the glass tubing before making capillary tubes is one of the chief causesof low melting points and wide melting ranges. The presence of alkali on the surface ofthe sample tubes is one of the main problems. This is generally not an issue with premade,commercially available melting point capillaries.ImportantIf you must make your own tubes, make sure the glass stock is cleaned by rubbing theinside with dilute solution of a neutral detergent, rinsing with dilute (10%) HCl, andfinally rinsing thoroughly with distilled water.OptiMelt Automated Melting Point System
- Page 12 and 13: xBack Panel OverviewPrinterOptiMelt
- Page 14 and 15: xiiSpecificationsOptiMelt Automated
- Page 16 and 17: 2 Getting Started Chapter 1• Repl
- Page 18 and 19: 4 Getting Started Chapter 1Ceramic
- Page 20 and 21: 6 Getting Started Chapter 1Principl
- Page 22 and 23: 8 Getting Started Chapter 1Quick St
- Page 24 and 25: 10 Getting Started Chapter 18. Preh
- Page 26 and 27: 12 Getting Started Chapter 1Touch t
- Page 28 and 29: 14 Getting Started Chapter 1If none
- Page 30 and 31: 16 Getting Started Chapter 1• Tou
- Page 32 and 33: 18 Getting Started Chapter 1OptiMel
- Page 34 and 35: 20 Displays and Menus Chapter 2Nume
- Page 36: 22 Melt Screen Chapter 2Melt Screen
- Page 39 and 40: Chapter 2 Melt Screen 25Touch the T
- Page 41 and 42: Chapter 2 Melt Screen 27Select Newe
- Page 43 and 44: Chapter 2 Melt Screen 29Select Came
- Page 45 and 46: Chapter 2 Melt Screen 31Options Men
- Page 47 and 48: Chapter 2 Melt Screen 33The thermod
- Page 49 and 50: Chapter 2 Timer Screen 35ResetTouch
- Page 51 and 52: Chapter 2 T Meter Screen 37Alarm Lo
- Page 53 and 54: Chapter 2 System Screen 39System Sc
- Page 55 and 56: Chapter 2 System Screen 41The Print
- Page 57 and 58: Chapter 2 System Screen 43Screen Me
- Page 59 and 60: Melting Point Determination 45Chapt
- Page 61: Chapter 3 Melting Point Determinati
- Page 65 and 66: Chapter 3 Melting Point Determinati
- Page 67 and 68: Chapter 3 Melting Point Determinati
- Page 69 and 70: Chapter 3 Melting Point Determinati
- Page 71 and 72: Chapter 3 Melting Point Determinati
- Page 73 and 74: Chapter 3 Melting Point Determinati
- Page 75 and 76: Chapter 3 Melting Point Determinati
- Page 77 and 78: Maintenance and Calibration 63Chapt
- Page 79 and 80: Chapter 4 Maintenance and Calibrati
- Page 81 and 82: Chapter 4 Maintenance and Calibrati
- Page 83 and 84: Chapter 4 Maintenance and Calibrati
- Page 85 and 86: Chapter 4 Maintenance and Calibrati
- Page 87 and 88: Chapter 4 Maintenance and Calibrati
- Page 89 and 90: Chapter 4 Maintenance and Calibrati
- Page 91 and 92: Pharmacopeia vs. Thermodynamic Melt
- Page 93 and 94: Appendix A Pharmacopeia vs. Thermod
- Page 95 and 96: Appendix A Pharmacopeia vs. Thermod
- Page 97 and 98: Appendix A Pharmacopeia vs. Thermod
- Page 99 and 100: Melting Point Certified Reference S
- Page 101 and 102: Appendix B Melting Point Certified
- Page 103 and 104: Appendix B Melting Point Certified
- Page 105 and 106: Using Melt Graphs 91Appendix CUsing
- Page 107 and 108: Appendix C Using Melt Graphs 93The
- Page 109 and 110: OptiMelt Remote Programming 95Appen
- Page 111 and 112: Appendix D OptiMelt Remote Programm
48 <strong>Melting</strong> <strong>Point</strong> Determination Chapter 3If your sample is hygroscopic, or sublimates at high temperatures, the open end of thecapillary tube must be sealed by heating. Hygroscopic samples must be stored in adessicator between tests, this is particularly critical in humid environments or duringrainy days.The sample tubes are loaded into the <strong>OptiMelt</strong> by inserting them into one of the sampleposition slots located on top of the instrument. Up to three samples can be accommodatedby the heating block simultaneously. Loading three capillaries with the same substanceand melting them at the same time and averaging their melting points provides the fastestand simplest way to improve the repeatability and accuracy of melting pointdeterminations.Figure 29. Loading capillaries into <strong>OptiMelt</strong>.Tips• Most pharmacopeias list recommended drying procedures for melting point samplesand certified reference standards.• Make sure the <strong>OptiMelt</strong> is plugged in and set to a Start temperature below theexpected melting point of the sample(s) before placing any capillaries into the sampleslots.• Use the same batch of capillaries for calibration and for high accuracy measurementsto assure the repeatability of results. NOT ALL CAPILLARIES ARE MADEEQUAL!• The standard <strong>OptiMelt</strong> package includes a vial of precision melting point capillariesspecifically designed to (1) fit the <strong>OptiMelt</strong> heating stand and (2) provide the mostuniform and repeatable results. Replacement capillaries can be purchased directlyfrom SRS (SRS Part# O100MPC).• Never force a capillary into the heating block! Once the capillary is inserted into asample hole, it should literally drop down to the bottom of the stand.<strong>OptiMelt</strong> <strong>Automated</strong> <strong>Melting</strong> <strong>Point</strong> <strong>System</strong>