QUADRASORBevo surface area & pore size analyzer

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Joshua Carr
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Features & Specifications Quantachrome s Quadrasorb evo TM Surface Area and Pore Size Analyzer P/N 02136-1, is a four sample station, bench-top, fully automated, vacuumvolumetric gas sorption system.

New samples may be added at each port as soon as previous measurements are completed thereby providing an analytical platform for many samples or multiple users.

1 Features & Specifications Quantachrome s Quadrasorb evo TM Surface Area and Pore Size Analyzer P/N , is a four sample station, bench-top, fully automated, vacuumvolumetric gas sorption system. The QUADRASORB evo TM is a high-throughput, cost-effective system featuring four separate and independent measurement ports allowing for simultaneous analysis of four samples. New samples may be added at each port as soon as previous measurements are completed thereby providing an analytical platform for many samples or multiple users. System is supplied complete with QuadraWin software for instrument control, report generation and file management including searchable results database (PC supplied separately), and full set of standard parts and accessories. System is suitable for operation with nitrogen, argon, carbon dioxide, and other non-corrosive gases for a wide range of applications. Quadrawin software ver 3.0+ can operate up to 3 QUADRASORB evo TM units simultaneously, from one PC. New Features in the BET QuickMode - For industrial high throughput settings- Time savings up to 50%: By passes most initialization, extended evacuation, and transducer zeroing sequences. Samples can run synchronously. Capable of running 4 samples in as little as 25 minutes. Dedicated Po transducer and manifold provides uninterrupted dosing of samples during measurements: P o can be continually measured. No need to stop measurement to update P o. No slow down in analysis to measure P o. Flexible Po Modes: P o can be estimated from ambient atmospheric pressure. P o can be entered as fixed value. P o can be analytically measured. New Hardware Features: Soft closing protective door with pneumatic hinges for operator safety. Integrated insulated dewar covers incorporated in lift mechanism to extend the life and insulating the dewar content. Smooth belt drive dewar lift for precise control of Quantachrome s novel cold zone. New 1 torr low pressure transducer for krypton and micropore measurements. Stainless steel gas paths including metal to metal seals for optimal vacuum performance. New Dose Wizard Flexibility: Can use a previously measured sample as a dosing template for reduced analysis time. Can be used with or without QuickMode EVO Rev A 1

2 QUADRASORB evo Features & Specifications Secure System for Pharmaceutical Industry The Quadrasorb evo TM, is available configured as a 21 CFR Part11 compliant BET Surface Area and Pore Size Analyzer system, P/N P. It is designed to help meet the regulatory requirements for electronic records within the pharmaceutical industry as set forth by the US Food and Drug Administration (FDA). Compliant software (QuadraWin CFR) allows for secure operation of the instrument, data acquisition and report generation. Among the functionalities included are: Tamper resistant data files Required login with unique user name / password combination Fully detailed audit trail integrated into data files Accessibility level programmable by system administrator Programmable session time-out (auto logoff ) Unique report identification; and a host of other features to ensure full compliance Upgradeable 2- and 3- Station Versions The Quadrasorb evo TM, is available with just 2 or 3 analysis stations for laboratories with smaller throughput requirements, but who still require independent operation of multiple stations. These versions are fully upgradeable to three or four stations in the future to meet growing needs. Base models are also field upgradeable to micropore (MP) capability for low pressure low surface area analysis using Krypton and micropore analysis with Argon. Available versions: : Three station MP-1 : Three station with micropore / Krypton capability MP-1-P : Three station Quadrasorb evo TM with micropore / Krypton capability (CFR)* P : Three stationquadrasorb evo TM, Secure System (CFR)* : Two station Quadrasorb evo TM MP-1 : Two station Quadrasorb evo TM with micropore / Krypton capability MP-1-P : Two stationquadrasorb evo TM with micropore / Krypton capability (CFR)* P : Two station Quadrasorb evo TM, Secure System (CFR)* *21 CFR Part 11 compliant 2

3 Analysis Features / Specifications Independent analysis stations, each consisting of: sample cell, P o cell, pressure transducer, dewar bath and automatic dewar lift drive, coolant level sensor. Dedicated P o manifold and P o transducer for continual P o. updates. Pressure Transducers: Six* 1000 torr transducers (one on each sample station, plus dosing manifold and P o manifold) plus one # 1 torr transducer (dosing manifold) Transducer Accuracy: 1000 torr: 0.11% full scale 1 torr: 0.15% reading Pressure Resolution: torr (1000 torr range) torr (1 torr range). Measurement Modes: Patented NOVA method for helium free analysis. Classical helium void volume measurement. QuickMode for high BET surface area throughput Sensitivity: < 1 x 10-7 moles adsorbed/ desorbed gas. Gas Dosing Methods: Standard-Intelligently adjusts dose pressure according to sample demands. Vector Dosing user selectable dose volumes from 0.25 to 10cc per point. Delta (volume) Max adds data points in regions of large uptake so pore filling step is never missed. Dose Wizard - can be used with or without QuickMode TM enabled. This allows the instrument to dose more aggressively, saving significant analysis time. Ultimate Vacuum: <1x10-2 torr achieved by dedicated two (2) stage rotary, direct drive pump. 1x10-9 torr achieved by turbo-molecular vacuum pump in QUADRASORB evotm - Kr/MP. Adsorbate: Nitrogen and any other non-corrosive gas with appropriate coolant. Surface Area Range: 0.01m 2 /g to no known upper limit (nitrogen) m 2 /g to no known upper limit (krypton) Kr/MP model only. Pore Volume: Detectable limit less than cc/g. Pore Size Range: 3.5 to >4000Å / 0.35 to >400nm. Number of independent Dewar (coolant) baths: Four* Coolant Level: Automatically maintained at a level around the sample cell to minimize cold zone volume. Maximum Analysis Time >30 hours on uninterrupted/unattended operation with LN 2 in standard dewar. Dewars (coolant baths): Number: Four (one per sample station) Nominal Capacity: 1000ml (each) * Full Quadrasorb evo model. 2- and 3-station versions have 4 and 5 respectively. # Kr/MP version only. Full Quadrasorb evo model. 2- and 3-station versions have 2 and 3 respectively. 3

4 QUADRASORB evo QuadraWin Data Reporting Capabilities Database Functionality: Build and maintain database of all analysis files, searchable by sample i.d., description, operator (user), comment or date range. Isotherms: User-selectable number of data points at any desired target pressures adsorption data points may be selected independently of desorption data points. BET Surface Area: Single point, multi-point, slope, intercept, C constant, correlation coefficient, tabular and graphic format. Langmuir Surface Area: Multi-point, slope, intercept, correlation coefficient, tabular, and graphic format. BJH Pore Size Distribution: Volume, area, adsorption, desorption, cumulative, derivative (linear and logarithmic), interpolated, tabular and graphic format. Dollimore-Heal Pore Size Distribution: Mesopore volume, area, adsorption, desorption, cumulative, derivative (linear and logarithmic), tabular and graphic format. Dubinin-Radushkevich Micro Pore Area: Slope, intercept, correlation coefficient, average pore size, micropore volume, average adsorption energy, tabular and graphic format. Total Pore Volume: At user-selectable P/P o. Average Pore Size: Radius, diameter. Statistical Thickness (t-plot): de Boer, Halsey or Carbon Black models t-method: Micropore area, mesopore area, micropore volume, correlation coefficient, tabular and graphic format. 4 Micropore Size Distribution: DFT (Density Functional Theory), HK (Horvath-Kawazoe), SF (Saito-Foley), DA (Dubinin-Astakhov), MP method; tabular and graphic format. NLDFT-Methods: N2 at 77K on carbon (slit pore, equilibrium model) N2 at 77K on carbon (cylindrical pore, equilibrium model) N2 at 77K on carbon (slit & cylindrical pores, equilibrium model) Ar at 77K on carbon (slit pore, equilibrium model) Ar at 87K on carbon (slit pore, equilibrium model) Ar at 87K on carbon (cylindrical pore, equilibrium model) CO2 at 273K on carbon (slit pore, equilibrium model) N2 at 77K on silica (cylindrical pore, equilibrium model) N2 at 77K on silica (cylindrical pore, adsorption branch model) N2 at 77K on silica (cylindrical and spherical pores, adsorption branch model) Ar at 87K on zeolites/silica (spherical/cylindrical pore, equilibrium model) Ar at 87K on zeolites/silica (spherical/cylindrical pore, adsorption branch model) Ar at 87K on zeolites/silica (cylindrical pore, equilibrium model) Ar at 87K on zeolites/silica (cylindrical pore, adsorption branch model) GCMC Method: CO2- carbon at 273K based on a slit-pore model Fractal Dimension: Neimark-Kiselev (NK), Frenkel-Halsey-Hill (FHH)

5 Data Reporting Capabilities General Specifications QSDFT: QSDFT N2 carbon equilibrium transition kernel at 77K based on a slit-pore model. QSDFT Ar carbon equilibrium transition kernel at 87K based on a slit-pore model. QSDFT N2 carbon adsorption branch kernel at 77K based on a cylindrical pore model. QSDFT N2 carbon adsorption branch kernel at 77K based on a cylindrical pore model. Physical & Utilities: Dimensions (WxDxH) 63.7 cm x 53.3 cm x 73.6 cm (inches: x 21.0 x 29.0) Depth Open x Height Open 66.5cm x cm (inches: 26.2 x 44) Weight 57.5 kg (127 lbs.)* * Four (4) station standard model not KR/MP mode QSDFT N2 carbon equilibrium transition kernel at 77K based on a slitpore model. QSDFT, N2, carbon equilibrium transition kernel at 77K based on a slit pore model (pore diameter <2nm) and a cylindrical pore model (pore diameter > 2 nm). QSDFT, N2, carbon adsorption branch kernel at 77K based on a slitpore model (pore diameter < 2 nm) and cylindrical pore model (pore diameter > 2 nm). QSDFT, N2, carbon adsorption branch kernel at 77K based on a cylindrical pore model (pore diameter < 5 nm) and spherical pore model (pore diameter > 5 nm). QSDFT, N2, carbon adsorption branch kernel at 77K based on a slitpore model (pore diameter <2 nm) and a cylindrical pore model (pore diameter 2 5 nm) and a spherical pore model (pore diameter > 5 nm). Tech Notes For a full explanation of data reduction, and QSDFT capabilities, please reference. #53 Application of Quenched Solid Density Functional Theory (QSDFT) for Pore Size Analysis of Cylindrical and Spherical Pore Carbons. Electrical VAC, 50/60 Hz Environmental C operating range at 90% maximum relative humidity. Gases (not supplied) All gases, adsorbate(s) and helium (if classical He void volume method used), shall be % purity or higher, and regulated to 8-10 psig (55 70k Pa). Cryogen (not supplied) Typically liquid nitrogen (though may vary according to specific applications). Initial requirement ~2 liters per station. Sample Preparation (Degassing) Options (Sold Separately) Four different Quantachrome degasser models available to meet virtually any sample preparation need in the R&D or quality control laboratory. They are: MasterPrep Degasser, XeriPrep Degasser, FloVac Degasser, and Flow Degasser. See recommended accessories for details. 5

6 QUADRASORB evo Included Standard Accessories The Quadrasorb evo TM is supplied with the following items at no additional charge according to number of analysis stations: Qty Description P/N #: Stations Dewar Sample cell, 9mm o.d. stem, long, large bulb Cell, 6mm o.d. stem, long, bulbless (for Po station) Sample cell, 9mm o.d. stem, long, bulbless Filler rod, 6mm x 268.5mm long (w/mushroom head) L LN 2 coolant level sensor (RTD) LN2-RTD All QuadrasorB evo TM models are supplied with the following further items at no additional charge. Please note there are minor differences in supplied items between the 2, 3 and 4 station Quadrasorb evo TM. Supplied Items: 2 Station - P/N : Stock Code Description Qty UOM Comments LN2-RT RTD assembly, ASI, 1,3,6 4 ea Input line 5 copper 2 ea Nut & ferrule set 1/8 brass 2 ea AS1, quartz cal. cell assembly 1 ea Adapter, sample cell 12mm 1 ea Funnel, sample cell 1 ea Manual Quadrasorb 1 ea Label attention loosen garvity 1 ea EV Quick Guide/Quad EV instruments 1 ea Fuse 5A, 250 Vac, 5 x 20mm 2 ea 6 Continue.

7 Standard Accessories Supplied Items: 2 Station - P/N : Stock Code Description Qty UOM Comments Power cord V 1 ea For volt v replace with # Cable DB9 M/F 10 RS232 1 ea QWCD S/W QuadraWin V ea for CFR model use # QWCFRCD SIUGD F/W QuadraWin V ea Flange stub, alum. hose FTG 1 ea Installed on # Centering ring assy, SS 1 ea Installed on # Clamping, vacuum ring DN16 1 ea Installed on # Hose vacuum Vardex 3/4 I.D. 5 FT mm O-Ring Viton 12mm brown 1 PR Clamp, Hose 1 ID 1 ea Installed on # Sample cell long LG bulb 9mm 3 ea Pellet long cell 6mm 3 ea Pellet long cell 9mm 3 ea L Filler rob 6mm x 268.5mm 2 ea Dewar vessel QC 10K, 105 x 300mm 2 ea Pellet cell undimpled 6mm 1 ea mm filler rod undimpled 270mm 1 ea TNT DOS license (100 Pieces) 1 ea Stem Cleaner 6mm x 12 1 ea 7

8 QUADRASORB evo Standard Accessories Supplied Items: 3 Station - P/N : Stock Code Description Qty UOM Comments LN2-RT RTD assembly, ASI, 1,3,6 5 ea Input line 5 copper 2 ea Nut & ferrule set 1/8 brass 2 ea AS1, quartz cal. cell assembly 1 ea Adapter, sample cell 12mm 1 ea Funnel, sample cell 1 ea Manual Quadrasorb EVO 1 ea Label attention loosen garvity 1 ea EV Quick Guide/Quad EV instruments 1 ea Fuse 5A, 250 Vac, 5 x 20mm 2 ea Power cord V 1 ea for volt v replace with # Cable DB9 M/F 10 RS232 1 ea QWCD S/W QuadraWin V ea for CFR model use # QWCFRCD SIUGD F/W QuadraWin V ea Flange stub, alum. hose FTG 1 ea installed on # Centering ring assy, SS 1 ea installed on # Clamping, vacuum ring DN16 1 ea installed on # Hose vacuum Vardex 3/4 I.D. 5 FT mm O-Ring Viton 12mm brown 1 PR Clamp, Hose 1 ID 1 ea installed on # Sample cell long LG bulb 9mm 4 ea Pellet long cell 6mm 4 ea Pellet long cell 9mm 4 ea L Filler rob 6mm x 268.5mm 3 ea Dewar vessel QC 10K, 105 x 300mm 3 ea 8 Continue

9 Standard Accessories Supplied Items: 3 Station - P/N : Stock Code Description Qty UOM Comments Pellet cell undimpled 6mm 1 ea mm filler rod undimpled 270mm 1 ea TNT DOS license (100 Pieces) 1 ea Stem Cleaner 6mm x 12 1 ea Supplied Items: 4 Station - P/N : Stock Code Description Qty UOM Comments LN2-RT RTD assembly, ASI, 1,3,6 6 ea Input line 5 copper 2 ea Nut & ferrule set 1/8 brass 2 ea AS1, quartz cal. cell assembly 1 ea Adapter, sample cell 12mm 1 ea Funnel, sample cell 1 ea Manual Quadrasorb 1 ea Label attention loosen garvity 1 ea EV Quick Guide/Quad EV instruments 1 ea Fuse 5A, 250 Vac, 5 x 20mm 2 ea Power cord V 1 ea for volt v replace with # Cable DB9 M/F 10 RS232 1 ea QWCD S/W QuadraWin V ea for CFR model use # QWCFRCD SIUGD F/W QuadraWin V ea Flange stub, alum. hose FTG 1 ea installed on # Centering ring assy, SS 1 ea installed on #46025 Continue 9

10 QUADRASORB evo Standard Accessories Supplied Items: 4 Station - P/N : Stock Code Description Qty UOM Comments Clamping, vacuum ring DN16 1 ea installed on # Hose vacuum Vardex 3/4 I.D. 5 FT mm O-Ring Viton 12mm brown 1 PR Clamp, hose 1 ID 1 ea installed on # Sample cell long LG bulb 9mm 6 ea Pellet long cell 6mm 6 ea Pellet long cell 9mm 6 ea L Filler rob 6mm x 268.5mm 4 ea Dewar vessel QC 10K, 105 x 300mm 4 ea Pellet cell undimpled 6mm 1 ea mm filler rod undimpled 270mm 1 ea TNT DOS license (100 Pieces) 1 ea Stem Cleaner 6mm x 12 1 ea 10

11 Required Accessories (not included with ) Qty description P/N #: 1 (for adsorbate) Gas Regulator Assembly Complete with CGA fitting and isolation valve. To control 8-10 psig output. Suitable for use with N 2, Ar, He etc. Note: Additional regulator assembly required for classical He void volume mode. 1 Vacuum Pump two stage, direct drive, capable of ~1 x 10-3 torr, for V operation, or Vacuum pump, two stage, direct drive, capable of ~1 x 10-3 torr, for V operation 1 Windows PC PC control module (for use with one QuadrasorB unit) Minimum specifications 1.6GHz processor, 256MB RAM 80GB hard drive, CD-ROM drive Microsoft Windows 17in Monitor, keyboard, mouse, USB ports 11

12 QUADRASORB evo Optional Accessories (not included with ) Qty Description P/N#: 1 Standard Reference Materials; available with nominal surface areas 0.5, 2, 10, 30, 100, 165, 275 m 2 /g 1 CellSeal TM Kit CellSeal check valve with integral frit fits into neck of 9mm o.d. cell. Kit consists of valve, two sample cells and all necessary fittings. Used to protect samples that are sensitive to the atmosphere from coming in contact with the atmosphere. Non-elutriating plug kits, prevents powder from becoming fluidized or elutriated to the instrument s manifold. Kit consists of cell, filter plug (Filter plug fits into neck of cell stem) and specially shortened filler rod (cell insert). 1 Non-elutriating plug kits, 6mm o.d. stem, small bulb Non-elutriating plug kits, 6mm o.d. stem, large bulb Non-elutriating plug kits, 9mm o.d. stem, small bulb Non-elutriating plug kits, 9mm o.d. stem, large bulb Non-elutriating plug, replacement, for 6mm o.d. stem Non-elutriating plug, replacement, for 9mm o.d. stem Multiple Sample Cell Holding Rack Uninterruptible Power Supply (110V only) Storage Dewar, 5 liter Storage Dewar, 10 liter Storage Dewar, 30 liter Trolley for 30 liter Dewar LN 2 Transfer Device for 30 liter Dewar

13 Recommended Accessories (not included with ) Choose one: An external preparation unit is required to use the. If you do not own a Quantachrome degasser unit, please talk to your sales representative to help choose a preparation unit to best suit your needs. Qty Description PN#: ( V operation) or ( V operation) Temperature control and logging via PC software (included). 1 MasterPrep Degasser* Six Station System for Flow or Vacuum Degassing. Temperature: Evacuation Rates: Back-fill Gas: Vacuum Display: Flow Rate: Programmable Digital Control, Ambient to 425ºC. Individually adjustable for each station. User-selectable, user-selectable Digital display 0 to 100 cc/minute, individually adjustable for each station. 1 Flow Degasser* Six heating and six cooling stations. PC Temperature Control Software included. Temperature: Back-fill Gas: Input Pressure: Flow rate: digital Control, Ambient to 400ºC in 1ºC steps. any dry, non-corrosive gas. 5 to 10 psi. 0 to 100cc/minute. 1 FloVac Degasser* Six Station System for Flow or Vacuum Degassing. PC Temperature Control Software included ( V operation) or ( V operation) Temperature: Evacuation Rates: Back-fill Gas: Vacuum Display: Flow Rate: digital Control, Ambient to 450ºC in 1ºC steps. User-selectable. Any dry, non-corrosive gas. digital display. 0 to 100 cc/minute. 1 XeriPrep Degasser * Six vacuum degassing stations, each consisting of sample cell port, heating mantle, independent temperature control, and isolation valve. PC control of all heating zones with individual heating ramps and times. Temperature: 350 C standard, 450 C optional. Evacuation Rates: Fine, Medium & Coarse Back-fill Gas: User preference-typically nitrogen. * vacuum pump not included 13

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