copyright 2012 micromeritics instrument...

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 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



Silica-Alumina Isotherms


Qua

ntity

Ads

orbe

d (c

m³/

g ST

P)

00

100

200

300

400


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


Qua

ntity

Ads

orbe

d (c

m³/

g ST

P)

-0.0002-0.0002

0.0000

0.0002

0.0004


000-144 : 000-144 Blank Krypton 000-145 : 000-145 Blank Krypton 000-146 : 000-146 Blank Krypton



Krypton Blank Tube Isotherms - Repeated


Qua

ntity

Ads

orbe

d (c

m³/

g ST

P)

-0.0002-0.0002

0.0000

0.0002

0.0004


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



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



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


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


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


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


Y Zeolite Isotherm


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


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


Y Zeolite Isotherm Overlay


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


Mesoporous Alumina Isotherm


Qua

ntity

Ads

orbe

d (c

m³/

g ST

P)

00

100

200

300


Aluminum Oxide Mesoporous MSU-X wormhole Tube #1 - Adsorption Aluminum Oxide Mesoporous MSU-X wormhole Tube #1 - Desorption


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


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


Three Mesoporous Aluminas Isotherm Overlay


Qua

ntity

Ads

orbe

d (c

m³/

g ST

P)

00

500

1,000

1,500


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


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


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


Macroporous Silica Isotherm


Qua

ntity

Ads

orbe

d (c

m³/

g ST

P)

00

50

100


silica - Adsorption silica - Desorption


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



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


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

copyright 2012 micromeritics instrument...

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