Copyright 2012 Micromeritics Instrument...
Transcript of Copyright 2012 Micromeritics Instrument...
Copyright 2012 Micromeritics Instrument Corporation
Quick application view of Micromeritics Gas Adsorption Instruments
Profile and Performance Features
• Three analysis ports with independent transducers• A Po port with a dedicated transducer• Inlet ports for helium and five analysis gases• 29 bit A/D conversion of pressure transducers • Stainless steel gas inlet and analysis manifolds• Hard seal valves• Minimum >70 hour useable Dewar life (3 sample
tubes, isothermal jacket, Po tubes and heated manifold)• Data reduction with MicroActive and new user defined
report options• The ability to control up to four instruments from one
computer• Built-in diagnostics for maximum uptime performance
Profile for the 3Flex
Manifolddesign
• Hard seals
• Welded components• VCR - component connections
• Highest quality available• Metal diaphragm - PCTFE valve seat
• Best available technology for use with VCR and welded components
Pressuremeasurement
Dosing manifold transducers
• 1000 torr• 10 torrPort (equilibrating) transducers
• 1000 torr (3)• 10 torr (2 or 3)• 0.1 torr (2 or 3)Psat port
• 1000 torrVacuum gauge
• Pirani• Cold cathode
DedicatedPo
VacuumgaugesDual gauge
• Pirani
• Cold cathode
Compensated for gas type
• Gas specific and updated for each gas used during an analysis
Unique Physical location
• Comparable to the sample location to provide measurements that are consistent with the sample, not measured at pump inlet as competition
Servocontrolfordosingandevacuationprovideshigherdegreeofgas
management
Review of PerformanceResults
Temperature control
Proprietary Micromeritics technology
• Developed by Micromeritics Benefit of integrating hardware, software
and control 3 strategic RTD locations
• Temperature control of +/- 0.05°C
Better control than provided by a temperature controlled transducer
Instrument Hardware Specifications
Competitor B Competitor Q 3Flex
Transducers 11 7 12
Transducer(temperature controlled)
2(manufacturer)
2(manufacturer)
12(proprietary Micromeritics)
Vacuum gauge Dual gauge Dual gauge Dual gauge
Manifold (temperature controlled)
40°C optional 45°C(proprietary Micromeritics)
Data acquisitionA/D
24 bit 24 bit 25 bit(29 bit a/d)
Dosing & Evacuation Needle valves Needle valves Servo
Hybrid turbo pump Elastomer seal CF(metal seal)
CF(metal seal)
Roughing pump 2 stage diaphragm 2 stage diaphragm 4 stage diaphragm
Diagnostics for system monitoring and performance
Operational Dashboard
Routine event monitoring
Number of analyses
Diaphragm pump life
Nitrogen Po
Manifold outgas rate
Reference material
User scheduled diagnostic testingBackground monitoring while the instrument is idle
Diagnostics
Full logging of all system events, calibration and error messages
Adsorptive properties
Standard library includes more than 30 fluids
• Inorganic gases: nitrogen, oxygen, argon, krypton ...
• Alkanes: methane, ethane, propane, butane, ...
• Alkenes: ethylene, propylene, ...
The 3Flex is designed with extensive chemical compatibility
• The large library allows the user to utilize the full instrument capabilities
Reduce the “user effort” to find information
• Do more faster
Adsorptive LibraryNitrogen MethaneArgon EthaneKrypton PropaneOxygen n-ButaneHelium i-ButaneNeon PentaneXenon HexaneHydrogen HeptaneDeuterium OctaneAmmonia NonaneSulfur hexafluoride DecaneCarbon dioxide EthyleneCarbon monoxide PropyleneNitrous oxide MethanolWater Ethanol
Acetone
Reports
Configurable Reports
Users can specify the reports and the order for presentation
Overlays (up to 25) to allow more and easier selection
Integration
MicroActive
• Select a script• Manipulate the model using
MicroActive controlsReport System
• Summary• Tabular• Graphics
Blank Tube and Reference Material Analyses
3Flex Sample Analysis Results
• Nitrogen adsorptive at LN2 Temperature
Nitrogen Blank Tube Isotherms
Relative Pressure (P/Po)0.10.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
-0.08-0.08
-0.06
-0.04
-0.02
0.00
0.02
Isotherm Linear Plot
003-009 : 003-009 Nitrogen blank 12 mm long 102 mm rod Setra 003-010 : 003-010 Nitrogen blank 12 mm long 102 mm rod Setra003-011 : 003-011 Nitrogen blank 12 mm long 102 mm rod Setra
Results are displayed at a magnified scale to show isotherm detail
• Nitrogen adsorptive at LN2 Temperature
Nitrogen Blank Tube Isotherms with Limits
Relative Pressure (P/Po)0.00.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
-0.2-0.2
0.0
0.2
Nitrogen Blank Isotherm Plot
C:\3Flex\data\data2\000-180.SMP C:\3Flex\data\data2\000-181.SMP C:\3Flex\data\data2\000-182.SMP
Results are displayed at a magnified scale to show isotherm detail
• Nitrogen adsorptive at LN2 Temperature
Silica-Alumina Isotherms
Relative Pressure (P/Po)0.00.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
00
100
200
300
400
Isotherm Linear Plot
000-183 : 000-183 Silica Alumina Tube 1 000-184 : 000-184 Silica Alumina Tube 2 000-185 : 000-185 Silica Alumina Tube 3
• Silica-Alumina Reference Material 004-16821-00 214 +/- 6 m2/g
Silica-Alumina BET Surface Area
BET Surface Area Report
BET Surface Area: 217.5052 ± 0.2739 m²/g Slope: 0.019841 ± 0.000025 g/cm³ STP
Y-Intercept: 0.000173 ± 0.000004 g/cm³ STP C: 115.822081 Qm: 49.9645 cm³/g STP
Correlation Coefficient: 0.9999960 Molecular Cross-Sectional Area: 0.1620 nm²
• Krypton adsorptive at LN2 Temperature
Krypton Blank Tube Isotherms
Relative Pressure (P/Po)0.000.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
-0.0002-0.0002
0.0000
0.0002
0.0004
Isotherm Linear Plot
000-144 : 000-144 Blank Krypton 000-145 : 000-145 Blank Krypton 000-146 : 000-146 Blank Krypton
Results are displayed at a magnified scale to show isotherm detail
• Krypton adsorptive at LN2 Temperature
Krypton Blank Tube Isotherms - Repeated
Relative Pressure (P/Po)0.000.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
-0.0002-0.0002
0.0000
0.0002
0.0004
Isotherm Linear Plot
000-144 : 000-144 Blank Krypton 000-145 : 000-145 Blank Krypton 000-146 : 000-146 Blank Krypton 000-147 : 000-147 Blank Krypton000-148 : 000-148 Blank Krypton 000-149 : 000-149 Blank Krypton
Results are displayed at a magnified scale to show isotherm detail
• Krypton adsorptive at LN2 Temperature
Krypton Blank Tube Isotherms – with Limits
Relative Pressure (P/Po)0.000.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
-0.002-0.002
0.000
0.002
0.004
Krypton Blank Isotherm Plot
C:\3Flex\data\data2\000-144.SMP C:\3Flex\data\data2\000-145.SMP C:\3Flex\data\data2\000-146.SMP C:\3Flex\data\data2\000-147.SMPC:\3Flex\data\data2\000-148.SMP C:\3Flex\data\data2\000-149.SMP
Results are displayed at a magnified scale to show isotherm detail
• Krypton adsorptive at LN2 Temperature
alpha-Alumina Isotherms
Relative Pressure (P/Po)0.000.00 0.05 0.10 0.15 0.20 0.25 0.30
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
0.000.00
0.02
0.04
0.06
0.08
Isotherm Linear Plot
000-150 : Alumina Reference Material With Krypton Tube A2 000-151 : Alumina Reference Material With Krypton Tube A3000-152 : Alumina Reference Material With Krypton Tube A4
• Alumina Reference Material 004-16816-00 0.28 +/- 0.03 m2/g
alpha-Alumina BET Surface Area
BET Surface Area Report
BET Surface Area: 0.2755 ± 0.0047 m²/g Slope: 19.931535 ± 0.346146 g/cm³ STP
Y-Intercept: 0.552528 ± 0.068085 g/cm³ STP C: 37.073343 Qm: 0.0488 cm³/g STP
Correlation Coefficient: 0.9990964 Molecular Cross-Sectional Area: 0.2100 nm²
• Nitrogen adsorptive at LN2 Temperature
13X Isotherm
Relative Pressure (P/Po)10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 100
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
00
50
100
150
200
250
Isotherm Log Plot
13x - Adsorption 13x - Desorption
• Nitrogen adsorptive at LN2 Temperature
13X Horvath-Kawazoe Pore Width
Pore Width (nm)0.00.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
Pore
Vol
ume
(cm
³/g)
0.000.00
0.05
0.10
0.15
0.20
0.25
dV/dw
(cm³/g·nm
)
0.00.0
0.5
1.0
Horvath-Kawazoe Cumulative Pore Volume Plot
Cylinder Pore Geometry (Saito-Foley)13x Smoothed dV/dw Pore Volume
• 004/16843/00 13X Reference Material – 0.80 +/- 0.02 nm
13X Horvath-Kawazoe Pore Width
Maximum Pore Volume: 0.212201 cm³/g at Relative Pressure: 0.165860101
Median Pore Width: 0.8189 nm Relative Pressure Range: 2.716e-008 to 1.659e-001
Diameter of Adsorptive Molecule: 0.3000 nm Adsorptive Density: 6.710e+014 molecules/cm²
Adsorptive Dispersion Constant: 7.777e-059 Diameter of Sample Atom: 0.3040 nm
Sample Density: 3.750e+015 molecules/cm² Sample Dispersion Constant: 7.923e-059
Density Conversion Factor: 0.0015476
• Nitrogen adsorptive at LN2 Temperature
Y Zeolite Isotherm
Relative Pressure (P/Po)10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 100
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
00
50
100
150
200
250
Isotherm Log Plot
Y zeolite - Adsorption Y zeolite - Desorption
• Nitrogen adsorptive at LN2 Temperature
Y Zeolite Horvath-Kawazoe Pore Width
Pore Width (nm)0.00.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6
Pore
Vol
ume
(cm
³/g)
0.000.00
0.05
0.10
0.15
0.20
0.25
dV/dw
(cm³/g·nm
)
0.00.0
0.5
1.0
Horvath-Kawazoe Cumulative Pore Volume Plot
Cylinder Pore Geometry (Saito-Foley)Y zeolite Smoothed dV/dw Pore Volume
• 004/16844/00 13X Reference Material – 0.74 +/- 0.02 nm
Y Zeolite Horvath-Kawazoe Pore Width
Maximum Pore Volume: 0.219492 cm³/g at Relative Pressure: 0.164575388
Median Pore Width: 0.7522 nm Relative Pressure Range: 4.209e-008 to 1.646e-001
Diameter of Adsorptive Molecule: 0.3000 nm Adsorptive Density: 6.710e+014 molecules/cm²
Adsorptive Dispersion Constant: 7.777e-059 Diameter of Sample Atom: 0.2760 nm
Sample Density: 1.310e+015 molecules/cm² Sample Dispersion Constant: 8.957e-059
Density Conversion Factor: 0.0015474
• Nitrogen adsorptive at LN2 Temperature
Y Zeolite Isotherm Overlay
Relative Pressure (P/Po)10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 100
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
00
50
100
150
200
250
Isotherm Log Plot
yzeolite-3 : Y zeolite yzeolite-4 : Y zeolite
• Nitrogen adsorptive at LN2 Temperature
Mesoporous Alumina Isotherm
Relative Pressure (P/Po)0.00.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
00
100
200
300
Isotherm Linear Plot
Aluminum Oxide Mesoporous MSU-X wormhole Tube #1 - Adsorption Aluminum Oxide Mesoporous MSU-X wormhole Tube #1 - Desorption
• Nitrogen adsorptive at LN2 Temperature
Mesoporous Alumina BJH Adsorption Pore Vol. Dist.
Pore Diameter (nm)1 2 4 6 8 10 20 40 60 80 100 200
Pore
Vol
ume
(cm
³/g)
0.00.0
0.1
0.2
0.3
0.4
0.5
dV/dlog(D
) Pore Volum
e (cm³/g)
0.00.0
0.5
1.0
BJH Adsorption Cumulative Pore Volume (Larger)
Harkins and Jura : Faas CorrectionBJH Adsorption Cumulative Pore Volume (Larger) BJH Adsorption dV/dlog(D) Pore Volume
• Nitrogen adsorptive at LN2 Temperature
Mesoporous Alumina BJH Desorption Pore Vol. Dist.
Pore Diameter (nm)1 2 4 6 8 10 20 40 60 80 100 200
Pore
Vol
ume
(cm
³/g)
0.00.0
0.1
0.2
0.3
0.4
0.5
dV/dlog(D
) Pore Volum
e (cm³/g)
0.00.0
0.5
1.0
1.5
2.0
2.5
BJH Desorption Cumulative Pore Volume (Larger)
Harkins and Jura : Faas CorrectionBJH Desorption Cumulative Pore Volume (Larger) BJH Desorption dV/dlog(D) Pore Volume
• Nitrogen adsorptive at LN2 Temperature
Three Mesoporous Aluminas Isotherm Overlay
Relative Pressure (P/Po)0.00.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
00
500
1,000
1,500
Isotherm Linear Plot
Al2O3-1 : Aluminum Oxide Mesoporous MSU-X wormhole Tube #1 Al2O3-2 : Aluminum Oxide mesoporous MSU-X (wormhole) Tube #2Al2O3-3 : Aluminosilicate, mesostructurerd AL-MSU-F Tube #3
• Nitrogen adsorptive at LN2 Temperature
Three Mesoporous Aluminas BJH Adsorption Overlay
Pore Diameter (nm)1 2 4 6 8 10 20 40 60 80 100 200
dV/d
log(
D) P
ore
Vol
ume
(cm
³/g)
00
5
10
15
BJH Adsorption dV/dlog(D) Pore Volume
Harkins and Jura : Faas CorrectionAl2O3-1 : Aluminum Oxide Mesoporous MSU-X wormhole Tube #1 Al2O3-2 : Aluminum Oxide mesoporous MSU-X (wormhole) Tube #2Al2O3-3 : Aluminosilicate, mesostructurerd AL-MSU-F Tube #3
• Nitrogen adsorptive at LN2 Temperature
Three Mesoporous Aluminas BJH Desorption Overlay
Pore Diameter (nm)1 2 4 6 8 10 20 40 60 80 100 200
dV/d
log(
D) P
ore
Vol
ume
(cm
³/g)
00
5
10
15
BJH Desorption dV/dlog(D) Pore Volume
Harkins and Jura : Faas CorrectionAl2O3-1 : Aluminum Oxide Mesoporous MSU-X wormhole Tube #1 Al2O3-2 : Aluminum Oxide mesoporous MSU-X (wormhole) Tube #2Al2O3-3 : Aluminosilicate, mesostructurerd AL-MSU-F Tube #3
• Nitrogen adsorptive at LN2 Temperature
Macroporous Silica Isotherm
Relative Pressure (P/Po)0.00.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
00
50
100
Isotherm Linear Plot
silica - Adsorption silica - Desorption
• Nitrogen adsorptive at LN2 Temperature
CarboPack F Isotherm
Relative Pressure (P/Po)10-6 10-5 10-4 10-3 10-2 10-1 100
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
0.001
0.01
0.1
1
10
100
Isotherm Log Plot
carbopack-F - Adsorption carbopack-F - Desorption
• Henry’s Law Linearity
CarboPack F Isotherm
Relative Pressure (P/Po)1 x 10-6 5 x 10-6 1 x 10-5 5 x 10-5 1 x 10-4
Qua
ntity
Ads
orbe
d (c
m³/
g ST
P)
0.001
0.005
0.01
0.05
0.1
0.5
1
Isotherm Log Plot
carbopack-F - Adsorption carbopack-F - Desorption
3Flex Sample Analysis Results vs. Competition
• 3Flex versus Competitor B and Competitor Q
Nitrogen Blank Tube Isotherms with Limits
-0.4
-0.3
-0.2
-0.1
0
0.1
0.2
0.3
0.4
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
cc/g
P/P0
N2 Blank Tube
3Flex Upper Limit Lower Limit BEL iQ N2 BlankComp B Comp Q
Results are displayed at a magnified scale to show isotherm detail
• 3Flex versus Competitor B and Competitor Q
Silica-Alumina Isotherms
0
50
100
150
200
250
300
350
400
450
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
cc/g
P/P0
Silica Alumina Reference Material
3Flex BEL iQComp B Comp Q
• 3Flex versus Competitor B and Competitor Q
alpha-Alumina Isotherms
0
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
0.045 0.095 0.145 0.195 0.245
Qua
ntity
Ads
orbe
d
Relative Pressure
Alpha Alumina Krypton Analysis
BEL Kr Alumina 3Flex Kr Alumina iQ Kr AluminaComp B Comp Q
• 3Flex versus Competitor Q
Y Zeolite Isotherms
0
20
40
60
80
100
120
140
160
1.00E-08 1.00E-07 1.00E-06 1.00E-05 1.00E-04 1.00E-03 1.00E-02
cc/g
log P/P0
Y-Zeolite
3Flex AS iQComp Q
3Flex with 0.1 Torr transducerComp Q with 1.0 Torr transducer
• 3Flex versus Competitor Q
13X Zeolite Isotherms
020406080
100120140160180200
1.000E-08 1.000E-07 1.000E-06 1.000E-05 1.000E-04 1.000E-03 1.000E-02
cc/g
P/P0
13x: 3Flex vs Competitor Q
Autosorb iQ 3FlexComp Q
3Flex with 0.1 Torr transducerComp Q with 1.0 Torr transducer