Micromeritics Instrument Corporation


ASAP 2020C V2.00 G Unit 1 Serial #: 1309 Page 1

Sample: 5%Pd/TiO2
Operator: MN
Submitter: Prof. Karski
File: C:\...\PROF~1.KAR\000-036.SMP

Started: 2011-02-16 8:42:55 Analysis Gas: CO
Completed: 2011-02-16 17:11:39 Analysis Temp: 35.0 °C
Report Time: 2011-03-17 11:01:43 Equilibration Interval: 10 s
Sample Mass: 0.9999 g Low Pressure Dose: None
Measured free space: 15.6720 cmł Automatic Degas: No







Isotherm Tabular Report


Analysis Data

Repeat
Quantity Quantity
Adsorbed Repeat Adsorbed
Pressure (cmł/g Time Pressure (cmł/g Time
(mmHg) STP) (hh:mm) (mmHg) STP) (hh:mm)
------
103.4727 1.5081 00:28 95.2798 1.0026 01:46
154.4042 1.7277 00:31 154.4154 1.2451 01:48
205.1508 1.8979 00:33 205.3671 1.4042 01:51
255.5422 2.0348 00:35 255.6294 1.5312 01:53
305.9841 2.1497 00:38 305.7535 1.6395 01:55
355.8499 2.2464 00:40 356.0938 1.7324 01:58
406.0942 2.3326 00:42 406.2187 1.8137 02:00
456.1547 2.4111 00:44 456.2852 1.8854 02:02


Micromeritics Instrument Corporation


ASAP 2020C V2.00 G Unit 1 Serial #: 1309 Page 1

Sample: 5%Pd/TiO2
Operator: MN
Submitter: Prof. Karski
File: C:\...\PROF~1.KAR\000-036.SMP

Started: 2011-02-16 8:42:55 Analysis Gas: CO
Completed: 2011-02-16 17:11:39 Analysis Temp: 35.0 °C
Report Time: 2011-03-17 11:01:43 Equilibration Interval: 10 s
Sample Mass: 0.9999 g Low Pressure Dose: None
Measured free space: 15.6720 cmł Automatic Degas: No






Isotherm Plot


5%Pd/TiO2 - First analysis data point
Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
103.473 1.50807
154.404 1.72772
205.151 1.89789
255.542 2.0348
305.984 2.14971
355.85 2.24644
406.094 2.33263
456.155 2.41111

5%Pd/TiO2 - Repeat analysis data point
Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
95.2798 1.00256
154.415 1.24509
205.367 1.40425
255.629 1.53118
305.754 1.63952
356.094 1.73242
406.219 1.81373
456.285 1.88538



Micromeritics Instrument Corporation


ASAP 2020C V2.00 G Unit 1 Serial #: 1309 Page 1

Sample: 5%Pd/TiO2
Operator: MN
Submitter: Prof. Karski
File: C:\...\PROF~1.KAR\000-036.SMP

Started: 2011-02-16 8:42:55 Analysis Gas: CO
Completed: 2011-02-16 17:11:39 Analysis Temp: 35.0 °C
Report Time: 2011-03-17 11:01:43 Equilibration Interval: 10 s
Sample Mass: 0.9999 g Low Pressure Dose: None
Measured free space: 15.6720 cmł Automatic Degas: No






Analysis Summary

Percent of Atomic
Sample Atomic Stoichiometry Cross-Sectional Density
Element Weight (%) Weight Factor Area (nm²) (cmÅ‚/g)
------
palladium 5.000 106.400 1.000 0.0787 12.020

Analysis Results

Metal Dispersion: 13.6166 %
Metallic Surface Area: 3.0331 m²/(g of sample)
Metallic Surface Area: 60.6617 m²/(g of metal)
Crystallite Size (6.000 V / A): 8.22871 nm
Y-Intercept Quantity Adsorbed: 1.4342 ą 0.0442 cmł/g STP
Slope: 0.002225 Ä… 0.000137
Correlation Coefficient: 9.90607E-01

Difference Results

Metal Dispersion: 4.4209 %
Metallic Surface Area: 0.9848 m²/(g of sample)
Metallic Surface Area: 19.6951 m²/(g of metal)
Crystallite Size (6.000 V / A): 25.34483 nm
Y-Intercept Quantity Adsorbed: 0.4656 ą 0.0035 cmł/g STP
Slope: 0.000135 Ä… 0.000011
Correlation Coefficient: 9.84019E-01


Micromeritics Instrument Corporation


ASAP 2020C V2.00 G Unit 1 Serial #: 1309 Page 1

Sample: 5%Pd/TiO2
Operator: MN
Submitter: Prof. Karski
File: C:\...\PROF~1.KAR\000-036.SMP

Started: 2011-02-16 8:42:55 Analysis Gas: CO
Completed: 2011-02-16 17:11:39 Analysis Temp: 35.0 °C
Report Time: 2011-03-17 11:01:43 Equilibration Interval: 10 s
Sample Mass: 0.9999 g Low Pressure Dose: None
Measured free space: 15.6720 cmł Automatic Degas: No






Analysis Tabular Report

Quantity Quantity
Adsorbed Adsorbed 1st -
Pressure (cmł/g Pressure (cmł/g Repeat
(mmHg) STP) (mmHg) STP) (cmł/g STP)
-- -- -
103.4727 1.5081 95.2798 1.0026 0.5055
154.4042 1.7277 * 154.4154 1.2451 * 0.4826 *
205.1508 1.8979 * 205.3671 1.4042 * 0.4936 *
255.5422 2.0348 * 255.6294 1.5312 * 0.5036 *
305.9841 2.1497 * 305.7535 1.6395 * 0.5102 *
355.8499 2.2464 * 356.0938 1.7324 * 0.5140 *
406.0942 2.3326 * 406.2187 1.8137 * 0.5189 *
456.1547 2.4111 * 456.2852 1.8854 * 0.5257 *


* Included in calculation of line fit and difference data.



Micromeritics Instrument Corporation


ASAP 2020C V2.00 G Unit 1 Serial #: 1309 Page 1

Sample: 5%Pd/TiO2
Operator: MN
Submitter: Prof. Karski
File: C:\...\PROF~1.KAR\000-036.SMP

Started: 2011-02-16 8:42:55 Analysis Gas: CO
Completed: 2011-02-16 17:11:39 Analysis Temp: 35.0 °C
Report Time: 2011-03-17 11:01:43 Equilibration Interval: 10 s
Sample Mass: 0.9999 g Low Pressure Dose: None
Measured free space: 15.6720 cmł Automatic Degas: No






Line Fit Plot


Selected first analysis data
Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
154.404 1.72772
205.151 1.89789
255.542 2.0348
305.984 2.14971
355.85 2.24644
406.094 2.33263
456.155 2.41111

Selected repeat analysis data
Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
154.415 1.24509
205.367 1.40425
255.629 1.53118
305.754 1.63952
356.094 1.73242
406.219 1.81373
456.285 1.88538

Difference
Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
154.404 0.482636
205.151 0.49364
255.542 0.503622
305.984 0.510195
355.85 0.514021
406.094 0.518902
456.155 0.525726


Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
103.473 1.50807
154.404 1.72772
205.151 1.89789
255.542 2.0348
305.984 2.14971
355.85 2.24644
406.094 2.33263
456.155 2.41111

Non-selected first analysis data
Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
103.473 1.50807


Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
95.2798 1.00256
154.415 1.24509
205.367 1.40425
255.629 1.53118
305.754 1.63952
356.094 1.73242
406.219 1.81373
456.285 1.88538

Non-selected repeat analysis data
Pressure (mmHg) Quantity Adsorbed (cmł/g STP)
95.2798 1.00256



Micromeritics Instrument Corporation


ASAP 2020C V2.00 G Unit 1 Serial #: 1309 Page 1

Sample: 5%Pd/TiO2
Operator: MN
Submitter: Prof. Karski
File: C:\...\PROF~1.KAR\000-036.SMP

Started: 2011-02-16 8:42:55 Analysis Gas: CO
Completed: 2011-02-16 17:11:39 Analysis Temp: 35.0 °C
Report Time: 2011-03-17 11:01:43 Equilibration Interval: 10 s
Sample Mass: 0.9999 g Low Pressure Dose: None
Measured free space: 15.6720 cmł Automatic Degas: No







Options Report


Task Summary

Task Temp Rate Time Pressure
Number Task
Name Gas (°C) (°C/min) (min) (mmHg)
-------
1 Evacuation He 300 10.0 60
2 Flow H2 300 10.0 60
3 Evacuation 300 10.0 120
4 Evacuation 35 10.0 10
5 Leak Test 35 10.0
6 Analysis CO 35 10.0



Task Number: 6
Adsorptive: Carbon Monoxide
Temperature: 35.0 °C
Heat rate: 10.0 °C/min
Equilibration interval: 10 s
Relative target tolerance: 5.0 %
Absolute target tolerance: 5.000 mmHg

Repeat analysis: Yes
Fast evacuation: No
Unrestricted evac. pressure: 30.0 mmHg
Evacuation time: 30 min

Free space group: Measured
Estimated free space: 18.0000 cmł

Incremental dosing: No

Experiment Log

Start Furnace Sample
Task Task Time Temp Temp Time Pressure
Number Name (h:min) Gas (°C) (°C) (min) (mmHg)
--------
1 EVAC 0:02 Hel 332.0 299.8 60
2 FLOW 1:54 H2 338.0 299.5 60 769.0609
3 EVAC 2:55 332.0 300.4 120
4 EVAC 4:57 30.0 33.3 10
5 LEAK 5:45 30.0 33.2 1 0.1497
6 ANL 5:50 CO 34.0 34.8 158 421.1644

Leak Test Results

Maximum
Allowed Observed
Start Outgas Outgas
Time Rate Rate
(min) (µmHg/min) (µmHg/min) Status
----
350 50 1 Pass