STI OPENING THE DOORS TO TEMPERATURE PROGRAMMING- A NEW FRONTIER IN HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

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1 OPENING THE DOORS TO TEMPERATURE PROGRAMMING- A NEW FRONTIER IN HIGH PERFORMANCE LIQUID CHROMATOGRAPHY Extended range HPLC has been investigated for many years; however, progress was delayed because of instrumentation and column limitations. With the introduction of temperature programmable instrumentation from Selerity Technologies Inc. and columns that are stable to temperatures as high as 200 C, it is now possible to develop HPLC methods that take full advantage of the benefits of extended temperature for your separations. A significant increase in speed is the most apparent benefit of elevated temperature HPLC. Furthermore, selectivity changes that can impact separations occur along with the polarity changes of reversed-phase solvents. As the temperature increases, aqueous mobile phases exhibit less polar character. Consequently, programmed temperature gradients mimic solvent gradients in most cases. The benefits of temperature programmed liquid chromatography (TPLC): Speed. (Higher practical linear velocities) Decrease or eliminate the use of organic solvents. At high temperatures water becomes less polar and behaves more like a moderately polar solvent making it possible to reduce or completely eliminate organic modifier in your mobile phase. This makes your laboratory environmentally friendly. Reduced viscosity of the mobile phase. Elevated temperature produces a reduction in mobile phase viscosity. This means lower back-pressure so that you can use the smallest particle size column packings without paying the pressure penalty, resulting in higher efficiencies, faster run times and overall better chromatography. At high temperatures, column efficiencies are not significantly reduced as the flow velocity increases. As a result flow rates well beyond the optimum velocity can be used without significant losses in efficiency. HPLC becomes really fastup to 10 times faster than at typical ambient conditions. Increased efficiencies. Rapid column re-equilibration between runs. Temperature programming provides the ability to perform analyses isocratically. This involves only a physical parameter change - with the rapid cool-down features of the Polaratherm TM Series 9000, your system is ready for another run in less than three minutes. You will immediately see an increase in efficiency and improvement in peak symmetry at higher temperatures. The result - better performance and better sensitivity for easier quantitation. Summarizing the use of high temperature in liquid chromatography, the chromatographer will be able to decrease analysis times, reduce organic solvent usage and produce better chromatographic results, saving both time and money. Is this important to you? Reference Application Notes

2 DYNAMIC MOBILE PHASE PREHEATING IS AN INTEGRAL PART OF THE TEMPERATURE PROGRAMMING PACKAGE Why Preheat the Mobile Phase? Heating the mobile phase before it enters the column is essential for good chromatography at high temperatures whether in isothermal or programmed temperature gradient mode. Solvent preheating eliminates peak band broadening due to thermal mismatch. It is essential even at temperatures as low as 50 C. Better chromatography and improved sensitivity comprise the value of dynamic preheating Heating Zone Temperature Sensing Zone The non-invasive, highly responsive preheater is an elegant solution to making temperature programming possible. 1 Stainless Steel Tubing 2 Heater 3 Thermocouple Sensor 4 Temperature Controller 5 Column 6 From Pump Convenient, easy-to-use, compact design. Non-invasive, non-contaminating. Versatile heat capacity for use with microbore to 4.6 mm columns. Easy internal preheater calibration. Preheater temperature calibrated to the column compartment for precise temperature control. Control of preheater temperature independent from column compartment allowing peak focusing. Available in 0.005, and internal diameters. Reference Technical Notes 803, 805 Rev 2 3/10/2005 Selerity Technologies Inc.

3 THE CALORATHERM MOBILE PHASE CONDITIONER CONTROL THE TEMPERATURE OF THE MOBILE PHASE - BECAUSE YOU CAN! Appealing to the masses, Improve your chromatography in just one simple step Insert mobile phase preheater assembly on existing tubing directly before the column. Eliminate thermal mismatch and improve peak shape by matching the mobile phase temperature to the column temperature. Decrease analysis time by increasing pump flow rates and changing selectivities. Stabilize baselines by controlling the eluent temperature before it enters the detector. Caloratherm TM Features Dynamic mobile phase preheater assembly to overcome peak band broadening due to thermal mismatch. Precise Peltier effluent assembly (optional) for detector stability. Small footprint control box for convenient, easy to use operation. Mobile phase preheater calibrated to oven cavity or laboratory environment for efficient, repeatable results. Communication options for pump shutdown to maintain lab safety.

4 CHANGING THE RULES FOR HPLC ANALYSIS THE CALORATHERM TM PROVIDES DRAMATIC IMPROVEMENTS EVEN AT 60 O C Specifications Temperature range: Temperature range w/peltier option: Dimensions (l x h x d): Weight: Mobile phase: Power requirements: Communication: 40 o C to 100 o C, isothermal 0 o C to 50 o C, isothermal 6.0 x 3.0 x 4.5 inches (15.2 x 7.6 x 11.4 cm) 16 oz. (0.45 kg) Any HPLC mobile phase VAC, 60VA Smart system with microprocessor control to communicate with the assembly sensors and HPLC equipment.

5 AT THE HEART OF SUCCESSFUL TEMPERATURE PROGRAMMED LIQUID CHROMATOGRAPHY- THE POLARATHERMTM SERIES 9000 TOTAL TEMPERATURE CONTROLLER Enhance your laboratory s capability with the Polaratherm TM Series 9000 Total Temperature Controller -A stand alone column compartment compatible with any existing HPLC system. Replace solvent gradients with temperature gradients. Shorten run times with temperature programming. Perform subzero analyses with ease. Simplify method development. Decrease solvent usage. Increase throughput. Polaratherm TM Features Forced air oven essential for precise temperature control. Cryo cooling option for subzero analysis. Automatic pump and instrument shutdown for laboratory safety. Organic vapor sensor for aditional security from possible mobile phase leakage. Low dead volume Secure-Fit TM connectors for superior chromatographic performance. Two-stage effluent conditioning for extreme temperature capability. Precise Peltier effluent control for detector stability. Dynamic mobile phase preheater to overcome peak band broadening due to thermal mismatch. Mobile phase preheater calibrated to oven cavity for efficient, repeatable results. Conveniently controlled oven programming by computer or through the front panel keypad. Compatible drivers for control with Agilent and Waters HPLC systems. Stable Blaze C 8 silica columns for high temperature use.

6 SELERITY TECHNOLOGIES TAKES HPLC TO THE EXTREMES SUBZERO TO 200 C WITH THE POLARATHERM TM SERIES 9000 Column compartment features for extreme temperature operation Isothermal and thermal gradient operation. Uniform temperature programs. Forced air oven provides rapid column recycling. Independent temperature programming controls for the column compartment and the preheater assembly. Accommodates columns from microbore to 4.6 mm ID up to 25 cm long. Peltier effluent conditioning for detector stability. Oven Specifications Operating range: 5 C above ambient to 200 C, ±0.5 C accuracy Operating range w/cryo option: Subzero (-20 C) to 200 C, ±1.0 C accuracy Temperature programming rates: 1-30 C/min when ramping up to 130 C 1-25 C/min when ramping up to 160 C 1-20 C/min when ramping up to 200 C Cool down rate: From 200 C to 50 C in 3.5 minutes, ready in 4.5 minutes From 50 C to 5 C above ambient 2.5 minutes, ready in 3.5 minutes Rev 2 3/10/2005 Selerity Technologies Inc.

7 TWO-STAGE EFFLUENT CONDITIONING ADDS THE FINISHING TOUCH FOR TEMPERATURE PROGRAMMED OPERATION Conditioning the effluent for detector stability. Cooling the effluent before it enters the detector is necessary when running at high temperatures. This is a two step procedure in the Series 9000 Total Temperature Controller. The effluent first passes through a passive heat exchanger lowering the temperature before it passes through the precisely controlled Peltier assembly. The Peltier assembly is actively controlled and responds to changing flow rates and mobile phase composition. This cool down process makes temperature programmed liquid chromatography possible with any HPLC detection method. Is versatility Important to you? Active effluent sensing. The temperature on the Peltier assembly can be set between 0 and 50 C to accommodate changing conditions. To monitor the temperature at the outlet of the column and before the detector, sensors have been placed on the outlet tubing after the column and after the conditioning assembly. This feature not only informs the user of the temperature at the outlet of the column and the temperature of the mobile phase before it enters the detector, but also can be used to determine column equilibration. Reproducibility is a critical parameter of any HPLC method. Rev 2 3/10/2005 Selerity Technologies Inc.

8 SAFETY FEATURES DINGUISH THE SELERITY HIGH TEMPERATURE SYSTEMS Automatic Safety Features Detecting flammable vapors triggers of a sequence of events that assures safe operation. Heating zones shut down. Vent flaps open to rapidly expel vapors. A signal is sent to initiate pump shut-off. Inert cryo fluid is injected into the oven cavity (when cryo option is installed). Watchdog system monitoring Flammable Vapor Sensor Computer program continuously monitors system functions. Prevents runaway of the temperature-controlled zones. Initiates oven shut-off when flammable vapor is detected. Audible alarm alerts operator when vapor is detected. Rev 2 3/10/2005 Selerity Technologies Inc.

9 SS THE AQUACHROM SERIES 8000 HIGH TEMPERATURE HPLC OVEN SUPERHEATED WATER AND UNIVERSAL DETECTION! Incorporate an environmentally friendly instrument into your laboratory. The Aquachrom high temperature HPLC oven was designed to combine the benefits of temperature programming with the use of superheated water as the mobile phase and flame ionization detection (FID). This multifunctional system can also be used with organic mobile phase compositions like the Polaratherm. Convert methods to environmentally friendly separations Gain the use of universal detection Eliminate organic solvent usage Take advantage of the changes in the dielectric constant (polarity) of water with changes in temperature Aquachrom Features Flame ionization for universal detection. Forced air oven essential for precise temperature control and temperature programming capabilities. Automatic pump and oven shut-off for laboratory safety. Organic vapor sensor assures safe operation at high temperatures. Low dead volume Secure-Fit TM connectors for superior chromatographic performance. Dynamic mobile phase preheater to overcome peak band broadening due to thermal mismatch. Independent control of mobile phase preheater and oven zones for efficient, repeatable results. Conveniently controlled oven programming by computer or through the front panel keypad. Stable Blaze silica columns for high temperature use.

10 FLAME IONIZATION DETECTION AND SUPERHEATED WATER- A HOT COMBINATION! The Aquachrom FID provides sensitive, stable universal detection Standard with all Aquachrom systems. Traditional FID design with grounded flame jet. Stable with up to 100µL/min of superheated water flowing directly into the flame jet. Capable of detecting low nanogram levels. Operates at temperatures up to 400 o C. Selerity FID Restrictor The Selerity column to detector interface provides the key to baseline stability All metal design. Elutes superheated water to the detector in aerosol formation. Maintains column back-pressure to minimize detector spiking. Pressure drop region remains short (2-5mm) and is positioned in the heated region of the FID.

11 THE AQUACHROM DESIGN ACCOMMODATES DUAL DETECTION MODE An added benefit of using the Aquachrom is obtained by routing the eluent as it exits the column into a post column splitter assembly, sending the sample to both a flame ionization detector and another detector of your choice. To stabilize the baseline of the second detector, the aquachrom features a post column cooling device directly outside of the oven cavity. Cooling the effluent to a constant temperature allows the use of any HPLC detector. Convenient, compact design makes it easy to regulate.

12 FOR MAXIMUM PERFORMANCE TRY THE SELERITY BLAZE FAMILY OF SILICA COLUMNS Blaze columns Polydentate polymer protects silica particles against hydrolytic breakdown providing a very stable, highly efficient column. Withstand temperatures up to 200ºC under reversed phase conditions. High temperature, low dead volume column housings. 1mm, 2mm and 4.6 mm ID column sizes. 5 cm, 10 cm and 15 cm column lengths. 3 µm particle size. 100 angstrom pore size. Other high temperature columns High temperature analyses have proven to be successful on polymer, carbon and zirconia columns with stainless steel housings. Selerity is actively evaluating columns for high temperature use from many sources and continues to develop new stationary phases in-house. For a list of the latest results visit our website at Reference Technical Note 804

13 ELIMINATE THE DEAD VOLUME CURSE WITH THE SELERITY TECHNOLOGIES PATENTED SECURE-FIT COLUMN CONNECTOR Significantly improves chromatographic performance. Zero dead-volume connections obtained by applying finger-tight tension. Self-adjusting within any depth and any type of acceptor fitting. The spring tension automatically positions the end of the tubing against the inside fitting face. Finger-tight tension, no wrenches needed. Holds pressures up to 10,000 psi. U.S. Patent 6,193, Silver soldered stainless steel washers 2 Stainless steel spring 3 Polymeric Ferrule Reference Technical Note 101 Rev 2 3/10/2005 Selerity Technologies Inc.