SURFER (the Surfaces Analyzer) Draft product specifications

Transcription

1 SURFER (the Surfaces Analyzer) Draft product specifications ThermoFisher Scientific Surfer applies the principle of static volumetric gas adsorption (physical and chemical adsorption) under controlled conditions (temperature and pressure) to determine micro structural properties of solids and powders. Surfer will determine, depending on the configuration and the type of experiment, the following physical properties: Specific surface area (m2/g) Pore size distribution in the meso, micro, ultra-micro and extended mesopore ranges Total pore volume (cc/g) Exposed metal surface area and metal dispersion in catalysts Surfer is the ultimate evolution for surface area determination. The new Surfer features a number of unmatched advantages and features. Improved design of stainless steel manifold to reach unmatched vacuum degree over the sample thus permitting investigation on new ultra-micro porous materials Extremely reduced manifold dead volume and new design sample temperature coolant level control permit to improve gas detection sensitivity by extreme pressure stabilization. Reduced necessary sample load (i.e. special requirements in the pharmaceutical field, in metal powder and catalysts applications) reduces by almost 50% the experiment time New gas injection system based on a proprietary design to introduce precisely extremely small as well as very large amount of adsorptive. The injection system does not add any dead volume to the system during the gas equilibration. New long lasting liquid coolant level control for best stabilization of the pressure in the system Wide range of available configurations: o Surfer Rapid (low cost mostly for QC/QA applications: surface area and mesopore size) o Surfer STD (for most of applications: surface area and mesopore size) o Surfer Micro (for microporous materials or experiments using Kr with very low surface areas) o Surfer Ultra (top of the line for ultra-microporous materials characterization & Kr) Page 1 of 8

2 New gas injection algorithm allows completely automatic analytical parameters setup. Available in these modes: o Mode Auto Surfer takes care automatically of the analytical set up adjusting the acquisition parameters in function of the sample nature and mass o Mode Choose Points User defines pressures steps at which data must be collected o Mode Micropores Automatic special operation to give best resolution for micro and ultramicroporous materials New instrument design, bench top, chassis optimization reduces space on the bench New electronic allows complete instrument control by a PC connected through LAN/Serial port New A/D converter 24 bit, 6 channels for highest resolution in pressure reading New and improved pumping system permits to reach unmatched vacuum degree in the sample area thus enabling the investigation of ultra micropores Availability of a dry primary vacuum pump in alternative to the standard oil pumps for clean and precise investigation of ultra-micropores avoiding possible sample contamination The degasser (part of Surfer) Extremely reduced bench space due to independent degasser (can be placed aside or under the Surfer bench or in a different lab) Degasser connectable to Surfer primary vacuum or to external vacuum system giving more possible customization Sample degasser with three stations up to 450 C with independent vacuum access and temperature control Two valve system permits to evacuate safely very fine powders in the degasser Page 2 of 8

3 Analytical capability Physisorption System capacity Analysis Sample Preparation Measurement ranges Specific surface area Surfer Rapid Surfer Standard Surfer Micro Surfer Ultra Specific surface area, mesopore size distribution, total specific pore volume One analysis port connected to the manifold, one saturation pressure sensor, one liquid nitrogen level resistive sensor Preparation unit with three degassing ports (separate vacuum access) From 0.1 m 2 /g using nitrogen or argon. No upper limit. Specific surface area, mesopore size distribution, total specific pore volume One analysis port connected to the manifold, one saturation pressure sensor, one liquid nitrogen level resistive sensor Preparation unit with three degassing ports (separate vacuum access) From 0.01 m 2 /g using nitrogen or argon. No upper limit. Specific surface area, mesopore size distribution, micropore size distribution, total specific pore volume, extremely low surface areas (using krypton) One analysis port connected to the manifold, one saturation pressure sensor, one liquid nitrogen level resistive sensor Preparation unit with three degassing ports (separate vacuum access) From 0.01 m 2 /g using nitrogen or argon. From m 2 /g using krypton. No upper limit. Specific surface area, mesopore size distribution, ultra-micropore size distribution, total specific pore volume, extremely low surface areas (with krypton) One analysis port connected to the manifold, one saturation pressure sensor, one liquid nitrogen level resistive sensor Preparation unit with three degassing ports (separate vacuum access) From 0.01 m 2 /g using nitrogen or argon. From m 2 /g using krypton. No upper limit. Specific pore volume From cm 3 /g From cm 3 /g From cm 3 /g From cm 3 /g Pore size range Typical range is from 2 to 100 nm Typical range is from 2 to 100 nm. (pore range can be extended by the micropore and ultra-micropore configurations or up to 500 nm by a suitable calculation software) Typical range is from 0.35 to 100 nm (pore range can be extended by a suitable calculation software up to 500 nm) Reproducibility Analysis time Better than 1% (according to sample nature and the applied calculation model) About 10 minutes for surface area measurement (for a complete isotherm the required time depends on the selected number of experimental points for every cycle and the sample nature) Better than 1% (according to sample nature and the applied calculation model) About 15 minutes for surface area measurement (for a complete isotherm the required time depends on the selected number of experimental points for every cycle and the sample nature) Better than 1% (according to sample nature and the applied calculation model) About 15 minutes for surface area measurement (for a complete isotherm the required time depends on the selected number of experimental points for every cycle and the sample nature) Typical range is from 0.35 to 100 nm (pore range can be extended by a suitable calculation software up to 500 nm) Better than 0.2% (according to sample nature and the applied calculation model) About 15 minutes for surface area measurement. For a complete isotherm the required time depends on the selected number of experimental points for every cycle and the sample nature (equilibrium time required to reach the equilibrium pressure). Gas inlets Adsorbate Four inlet ports selectable automatically and independently. Four inlet ports selectable automatically and independently. Four inlet ports selectable automatically and independently Four inlet ports selectable automatically and independently Inlet pressure Maximum inlet pressure 200 KPa Maximum inlet pressure 200 KPa Maximum inlet pressure 200 KPa Maximum inlet pressure 200 KPa Accepted adsorbates Physisorption N 2, Ar, CO 2, He, N 2, Ar, CO 2, He,... N 2, Ar, CO 2, He, Kr... N 2, Ar, CO 2, He, Kr,... Chemisorption H 2, O 2, CO, CH 4, light hydrocarbons, any non-condensable gas in the operating conditions H 2, O 2, CO, CH 4, light hydrocarbons, any non-condensable gas in the operating conditions Page 3 of 8

4 Sample holders Standard Vacuum system Primary vacuum Small size (about 10 cc), inlet Medium size (about 15 cc), inlet Final vacuum for manifold degassing by rotative double stage pump Small size (about 10 cc), inlet Medium size (about 15 cc), inlet Final vacuum for manifold degassing by rotative double stage pump Optional dry vacuum Final vacuum for manifold degassing by scroll dry pump Small size (about 10 cc), inlet Medium size (about 15 cc), inlet Final vacuum for manifold degassing by rotative double stage pump Final vacuum for manifold degassing by scroll dry pump Secondary vacuum Turbo molecular drag pump, final vacuum measured on the sample better than According to manufacturer specification: compression ratio for N , for Ar Vacuum measurement Optional Vacuum measurement Filters Resistive vacuum gauge (from 0.1 to 100 Pa) Active alumina filter between vacuum pump and manifold Manifold Manifold temperature controlled at temperature 37 C +/- 0.1 C Pressure measurement Injection transducer Absolute piezo transducer from 0.1 to 1000, accuracy better than 1% of reading, displayed resolution 0.1 Equilibrium transducer Optional equilibrium transducer Absolute piezo transducer from 0.1 to 1000, accuracy better than 1% of reading, displayed resolution 0.1 Resistive vacuum gauge (from 0.1 to 100 Pa) Micro Pirani gauge from 1x 10-5 to atmospheric pressure Active alumina filter between vacuum pump and manifold Manifold temperature controlled at 37 C +/- 0.1 C Absolute capacitive from 0.1 to 1000, accuracy 0.15% of reading, displayed resolution 0.01 Absolute capacitive from 0.1 to 1000, accuracy 0.15% of reading, displayed resolution 0.01 Absolute capacitive from 0.01 to 100, accuracy 0.15% of reading, displayed resolution Micro Pirani gauge from 1x 10-5 to atmospheric pressure Active alumina filter before manifold Manifold temperature controlled at 37 C +/- 0.1 C Absolute capacitive for 0.1 to 1000, accuracy 0.15% of reading, displayed resolution Absolute capacitive for 0.1 to 1000, displayed resolution 0.01 accuracy 0.15% of reading 2 - Absolute capacitive to 10, displayed resolution , accuracy 0.15% of reading Absolute capacitive from 0.01 to 100, accuracy 0.15% of reading, displayed resolution Small size (about 10 cc), inlet Medium size (about 15 cc), inlet Final vacuum for manifold degassing by scroll dry pump Turbo molecular drag pump, final vacuum measured on the sample better than According to manufacturer specification: compression ratio for N , for Ar Micro Pirani gauge from 1x 10-5 to atmospheric pressure (no need in case of dry scroll primary vacuum pump) Manifold temperature controlled at 37 C +/- 0.1 C Absolute capacitive for 0.1 to 1000, accuracy 0.15% of reading, displayed resolution Absolute capacitive for 0.1 to 1000, displayed resolution 0.01 accuracy 0.15% of reading 2 - Absolute capacitive to 10, displayed resolution , accuracy 0.15% of reading 3 - Absolute capacitive to 1, displayed resolution , accuracy 0.12% of reading Page 4 of 8

5 Saturation pressure Built-in A/D converter Coolant system Accepted coolants By temperature sensor, resolution better than 0.01K, pressure resolution 0.1, calibrated for liquid nitrogen and liquid argon boiling temperatures 24 bit A/D converter, 8 channels 12 bit A/D converter, 4 channels Automatic calibration and linearization routines Liquid nitrogen with automatic level control. Motor driven Dewar raising and lowering Level control Measured by a level sensor. Level control of coolant +/ mm from set point Analysis Dewar Single 3 litres by spherical low capacity evaporation rate Dewar Lasting time Minimum 60 hours maximum 120 hours (for nitrogen, according to manufacturer s specifications and according to sample nature) Physical Power supply Dimensions Weight Environment Temperature from 10 to 38 Celsius, humidity from 20 to 80 % By temperature sensor, resolution better than 0.01K, pressure resolution 0.1, calibrated for liquid nitrogen and liquid argon boiling temperatures 24 bit A/D converter, 8 channels 12 bit A/D converter, 4 channels Automatic calibration and linearization routines Liquid nitrogen and liquid argon with automatic level control. Motor driven Dewar raising and lowering Measured by a level sensor. Level control of coolant +/ mm from set point Single 3 litres by spherical low evaporation rate Dewar Minimum 60 hours maximum 120 hours (for nitrogen, according to manufacturer s specifications and according to sample nature) Temperature from 10 to 38 Celsius, humidity from 20 to 80 % By temperature sensor, resolution better than 0.01K, pressure resolution 0.1, calibrated for liquid nitrogen and liquid argon boiling temperatures 24 bit A/D converter, 8 channels 12 bit A/D converter, 4 channels Automatic calibration and linearization routines Liquid nitrogen and liquid argon with automatic level control. Automatic Dewar raising and lowering Measured by a level sensor. Level control +/ mm from set point Single 3 litres by spherical low evaporation rate Dewar Minimum 60 hours maximum 120 hours (for nitrogen, according to manufacturer s specifications and according to sample nature) Temperature from 10 to 38 Celsius, humidity from 20 to 80 % By temperature sensor, resolution better than 0.01K, pressure resolution 0.1, calibrated for liquid nitrogen and liquid argon boiling temperatures 24 bit A/D converter, 8 channels 12 bit A/D converter, 4 channels Automatic calibration and linearization routines Liquid nitrogen and liquid argon with automatic level control. Automatic Dewar raising and lowering Measured by a level sensor. Level control +/ mm from set point Single 3 litres by spherical low evaporation rate Dewar Minimum 60 hours maximum 120 hours (for nitrogen, according to manufacturer s specifications and according to sample nature) Temperature from 10 to 38 Celsius, humidity from 20 to 80 % Page 5 of 8

6 The degasser specifications Sample pre-treatment Degassing ports Three degassing ports with independent direct access to vacuum. Max vacuum degree depends on the vacuum system installed. Soft start vacuum generation prevents fine powder samples elutriation Maximum vacuum for degassing Degasser can be connected to the main vacuum source of Surfer or to an external and completely independent vacuum source. Temperature Accuracy Heating procedures Degassing time Backfill gas From room temperature up to 723 K (450 C) steps of 1 K +/- 1 % of full scale temperature Heating procedures: 1. ballistic operates on two degassing stations 2. programmable rates from 1 to 10 C/min with multiple cycling operates on a single station Manual (unlimited) or automatic selectable from 1 to 18 hours No need. Sample is kept under vacuum conditions during transfer in case of sample holder with vacuum stopcock Physical Power supply Dimensions Weight Environment Temperature from 10 to 38 Celsius, humidity from 20 to 80 % Page 6 of 8

7 Calculation Models for Surfer Standard software Main function Specific surface area Pore size distribution Available graphs Available reports Available data format ADP Software Main function Specific surface area Standard isotherms for t calculation Mesopore size distribution Micropore size distribution Available potential functions Chemisorption Available graphs Available reports Control the instrument, set the analytical parameters, display the isotherm during the analysis, display the liquid coolant level, performs main calculations and reporting BET 2 parameters Dubinin Radushkevitch-Kaganer Langmuir Dollimore-Heal Barrett Joyner-Halenda Horvath-Kawazoe Saito-Foley Isotherm Surface area Pore size distribution (histograms or derivative) 20 different report types can be memorized in the software Data can be exported in text, Excel or other electronic formats Advanced data processing Advanced Data Processing software encloses the most up-to-date calculation models for surface area and pore size determination. It also permits the creation of customized graphics format to be enclosed directly in scientific publications BET 2 parameters BET full equation (3 parameters) with non linear regression function Langmuir model Dubinin-Radushkevitch-Kaganer Excess Surface Work (ESW) model t-plot alpha-s-plot (Sing) MP-Plot (Mikhail-Brunauer-Bodor) Halsey Fransil Harkins-Jura De Boer Halenda Lecloux Hydroxylated silica User defined standard Barrett-Joyner-Halenda Dollimore-Heal Cranston-Inkley Modeless method Horvath-Kawazoe Saito-Foley Dubinin-Stoeckli Nitrogen Graphite (@ 77K) Argon Graphite (@ 77K, 87K) Carbon dioxide Graphite (194K, 273K, 298K) Argon Zeolite (@ 87K, 77K) Nitrogen Zeolite (@ 77K) User defined Subtraction procedure of isotherms for strong and weak chemisorption Back extrapolation to zero pressure for metal surface and dispersion calculation Langmuir model at variable exponent All calculations are applicable in graphic format. All graphs can be edited in almost all their components and exported in high resolution graphic file Three main reports are available: summary, standard and extended. Each report type can be manually edited by the user Page 7 of 8

8 NLDFT Software Module Main function Available pore models Pore size ranges Non Local Density Functional Theory The solver will minimize the free energy functional Ω [ρ(r)] with respect to ρ(r), using the Non Local Density Functional Theory (NLDFT method in the smoothed density approximation) for the determination of micropore and mesopore size distribution Infinite slit and cylindrical shape Set of pore sizes: 100 steps from 0.3 nm to 500 nm 20 steps range 0.3 nm to 1 nm 40 steps range from 1 nm to 10 nm 40 steps range from 10 nm to 500 nm For the infinite slit these numbers refer to the width of the slit For the cylindrical pores these numbers refer to the diameter Parameters for N 2 carbon at 77K based on a slit-pore model intermolecular N 2 carbon at 77K based on a cylindrical pore model potentials N 2 silica at 77K based on a cylindrical pore model Ar silica at 87K based on a cylindrical pore model Ar carbon at 87K based on a cylindrical pore model Ar carbon at 87K based on a slit-pore model CO 2 carbon at 273K based on a slit-pore model Data display Theoretical isotherm and calculated isotherm are overlaid in linear and logarithmic plot Pore size distribution function in linear and logarithmic plot Results export format Direct graph printing graph export in electronic format copy the graph on the clipboard and paste on a document or spreadsheet Data export in tabbed text file Operative system The solver run on a Windows (XP) based OS machine as a standalone application Page 8 of 8