ASAP 2420 surface area analyzer Operation precautions 112.05.

01

1. A sample tube set consists of sample tube, seal frit and filler rod.
2. We provide filler rods, seal frit and long funnel. Please buy your own sample tubes.
Purchase information: Lind ID Weien 0928887887 email: weiencafe@meritscience.com.tw
3. After experiment, take off the seal frits, and put them back in the drawer. Don’t take
them out of the lab and wash the seal frits.
4. The filler rod help ensure accuracy in samples with lower total surface by reducing the
free-space volume. It is generally a good practice to use filler rods for samples having
less than 100 m2. Clean and dry the filler rods then put back in the drawer after used.
5. Sample tubes and filler rods must be thoroughly clean and dry before samples are
added and weighed.
6. If you use the filler rod, place the filler rod in sample tube by holding the sample tube
horizontally and sliding the filler rod into the sample tube slowly.
7. Determining amount of sample to use:
A sample providing 40-120 m2 of total surface area is recommended for nitrogen
analysis. Less than this may cause variability of results; considerably more than this
extends unnecessarily the time required for analysis.
(1) 1000 < Sample has high surface areas ----- 0.08-0.1g.
(2) 10 < Sample has high surface areas < 1000 ------0.1- 0.5g.
(3) Sample has high surface areas <1------ more than 1g, even up to 5g
8. Samples should be put in oven(105℃) overnight.
9. Degas time is suggested over 12 hr.
10. Please check the liquid Nitrogen is enough, one sample 2.7L for 40hr.
11. When finish the analysis, please take of the sample tube and recycle the liquid Nitrogen.

If necessary, log in to ASAP2420 computer through anddesk.

Anydesk Information
ID : 680395786
Password : ASAP2420

BET and Meso-pore analysis : Chapter 1+Chapter 2+ Chapter 6

Micro-pore analysis : Chapter 1+Chapter 3+ Chapter 4+ Chapter 5+ Chapter 6
 Chapter 1 Create new sample file and Degas 112.05.01
※ Sample should be put in oven overnight (100℃) before degassing.
Most solid materials absorb moisture and other contaminants when expose to the
atmosphere. The sample must be clean when an analysis is performed. The sample is
heated and placed under vacuum to remove moisture and other contaminants. This
process is referred to as degassing the sample.

一、 Weigh and load sample

1. Weigh the sample tube set: sample tube+ filler rod (if needed)+ seal frit ->W1.
2. Weigh the sample tube set with sample : sample tube+ filler rod( if needed)+seal
frit+ sample (before degas：W2)
3. Tyr using a long funnel to ensure the sample id loaded toward the bottom bulb and
not sticking to the walls.

二、Install sample tubes to degas ports

1. Hold the degas port plug, loosen, then remove the connector nut and plug from
the degas port by turning the connector nut counterclockwise.
2. Place the degas port connector nut, ferrule, and O-ring onto the sample tube set as
the picture.(The o-ring should to smoothly around the tube at 3mm from the top of
the glass. Too low and the tube will not seal correctly in the port).
3. Carefully push the tube up into the port. Be sure to push the sample tube in to a full
stop. Secure the sample tube in place by sliding the connector nut, ferrule, and O-
ring up onto the degas port and turning the connector nut clockwise. Tighten the
nut securely by hand.
*** If not handled carefully, the tube can and does easily crack at the top and must
then be replaced.
4. Carefully place a heating mantle over the bulb of the sample tube and fasten the
mantle with the mantle clip.
三、 Using the Software：
1. Click ASAP 2420 to show instrument schematic
FileOpenSample information

b.
2. Create a new sample file:
a. Click ﹝…﹞ to previous folder
and to select your folder a.
b. File name doesn’t need to be changed.
c. Click OK

d. Click YES to create new file. d. c.

3. Settings for sample information file

a. Click Replace All to replace the current file containing the values you wish to use.
b. Double-click to move up one level in the selected directory, to find
C:\2420\method
c. Choose the method
d. Click OK

c.
b.

a.
d.

e. Sample identification:
(1) In the sequence field specify a default string for the sample file number.
(2) In the right-side field of the sample line, enter a format for the sample’s
identification. The weigh will need to be edited later after degassing.

e.
4. Sample Tube properties file: filler rod information (use or not use)

5. Degas Condition file contain degassing information for preparing samples.

a. Input the temperature and hold time (input in minutes) for second stage at
which to degas the sample. It should be a high temperature to help remove
any impurities, but the sample must be safe (under vacuum) for long times
at this temperature. Typical degas times are on the order of ~hours and are
typically left over night.
b. Click Save, then Close

a.

b.

6. Analysis Conditions file : Dependent on where you expect to see key features in your
measurement.
a. Pressures: The method has been set up the relative pressure points. If you want to
insert or delete relative pressure point, you can use the right side icon to adjust.

a.

a. b.

c. d.
 b. Options:
(1) Tick the checkbox of low pressure incremental (only for micro-pore analysis),
and enter the dose mount (Estimate BET/100), Click OK
(2) It is not necessary to tick the checkbox of low pressure incremental for BET or
mesopore analysis.

Micro-pore settings
BET & meso-pore setting

c. Free space setting

BET and meso micro+meso+enter free space Tick

Tick the Measure theenter

d. Backfill setting：
(1) Degas on analysis port should not perform backfill sample at start.

(2) No degas on analysis port should tick the backfill sample at start of analysis.

No degas on analysis port Degas on analysis port

7. Adsorptive Properties file：Nitrogen

8. Report Options：

9. Click to save the sample file, and to create the next one.
a.
10. Degas
a. Click Unit 1 Start Multiple Degas
b. Make sure the degas port number.
c. Click Browse for the SMP file you set up.
d. Click Start to start.
b. c.
Wait the designated time.
Typically, at least overnight

d.

11. When the degas operation is complete, a message dialog is displayed. Click OK to
close the message box.

12. Allow the sample tube to cool before removing it.

13. After the sample has cooled, remove the sample tube to reweight and transfer to the
analysis port to start degas on analysis port or analysis.
 Chapter 2 BET or Meso-pore Analysis 112.05.01

1. Carefully remove the heating mantle clip and the heating mantle from the sample tube
and allow the sample tube to cool to room temperature.
2. While holding the sample tube, loosen the port connector nut and remove the sample
tube form the degas port.

3. Take your sample back to the balance to reweigh the sample tube set. Edit the weight
information in the sample file.
4. Slide an isothermal jacket down over the sample tube stem until it touches the sample
tube bulb.
5. Place the connector nut, ferrule, and O-ring on to the sample tube stem.

6. Attach the sample tube to the analysis port, pushing it fully up. Turn the connector nut
clockwise to hand-tighten.
7. Make sure the P0 tube is next to the sample tube.
8. Put the Dewar cover over the sample stem just above the isothermal jacket.
9. Fill LN2 in the Dewar. (Get LN2 from LN2 container nearby)
a. Protect yourself by wearing insulated gloves.
b. Pour the LN2 from one container to another slowly to prevent splashing.
c. To check the fluid level, insert the dipstick in the Dewar as shown below.
d. The volume for a full Dewar is about 2.7 L, last 40 hours.
e. Place the safety shield over the sample tube and Dewar.
10. Open sample file, edit the information of weigh.
a. File Open Sample Information
b. Sample Information
c. Click Calculate, input the weight of empty tube set before degassing(W1) and
weight of sample tube set after degassing(W3).
d. Click SAVE and close the window.
b.

a.
c. W1
W3

d
.
11. Please carefully verify the parameters and changes necessary for analysis conditions.
12. Performing an Analysis 1.
1. Click Unit 1
2.
2. Click Start High Throughput Analysis
3. For each port on which you want
to start an analysis, Click Browse 3.
4. Select the SMP file you set up
5. Click OK 4.
6. Click Start to begin the analysis 5.
6.

*As date are collected, a graph is drawn in

the window.

13. The analysis time will depend on your procedure but can take on average 3-8 hours.
Primarily determined by # of analysis points, but higher surface area samples will take
longer.
14. When analysis is complete, the Status shows IDLE, then remove the tube and install the
protect tube back.
15. Click Close to exit.
 Chapter 3 Degas on analysis port
(for micro-pore analysis sample) 112.05.01

The characterization of microporous materials may by significantly improved by

starting the analysis with the sample pre-evacuated. To avoid exposure to
contaminants, it is often best to degas a microporous sample on the same port that
will be used for analysis.
1. Carefully remove the heating mantle clip and the heating mantle from the sample tube
and allow the sample tube to cool to room temperature.
2. While holding the sample tube, loosen the port connector nut and remove the sample
tube form the degas port.

3. Take your sample back to the balance to reweigh the sample tube set. Edit the weight
information in the sample file.
4. Install the sample tube on the sample port and position the P0 tube so that is away
from the sample tube.
5. Slide the isothermal jacket up to the top of the sample tube. (The isothermal jacket fits
tightly on the sample tube to ensure thermal stability. Use care when sliding it up or
down)
6. Loosen the lace on the heating mantle and slide the side-lacing heating mantles
around the sample tube, then tighten the lace.
7. Secure the heating mantle with a mantle clip.
8. Select Unit 1>Evacuate Analysis Port. The Evacuate Analysis Port dialog is displayed.
9. Select the port to which the sample tube is attaced,
10. Select the evacuation parameters. 8.
(Should not tick the box of Fast evacutation)
Unrestricted evac pressure usually use 5 mmHg/s
If the sample is fine, use 1 or 3 mmHg/s
11. Click Start.
9.

10.

11.

12. When the port evacuation is completed, the window will close automatically and the
valve 8 is left open. .
13. Repeat Step 8 through 12 for each sample to be degassed.
14. Select Unit 1> Show Analysis Schematic, then select Unit> Enable manual control. The
Manual Control screen is displayed. (All Valves color is yellow)
15. Double clicks to open the sample port which are in use.

16. Gently heat the sample：

a. Select Unit 1Show Degas Schematic to display the Degas Schematic
b. Right-Click on the degas port to which the heating mantle are used, then select
Set.

b.
a.
 c. Enter 90℃ for Target temperature and click OK to begin to heat.
d. When the temperature raise to 90℃, and hold 30min, Use Anydesk to change
the Target temperature to the second stage target temperature.(usually the
degas temperature - 50℃.
e. Remember to close the function of Enable Manual Control，Click Unit1Enable
Manual Control to cancel (Untick the Enable Manual Control).

c. e.

17. Allow the sample to degas for a minimum of 3hrs (Additional time may be required
to fully degas the sample)
a. Click Unit 1Enable Manual Control
b. Right-click on the degas port sample tube, then select Disable.
c. Remember to close the function of Enable Manual Control，Click Unit1Enable
Manual Control to cancel (Untick the Enable Manual Control).

a.

b.

18. When the heating mantle is cool enough to handle (the red light turns green),
remove it from the sample tube and allow the sample to cool to room temperature.

Anydesk informaiton
ID : 680395786
Password : ASAP2420
Chapter 4 Micro-pore + Measure Free Space 112.05.01

1. Carefully remove the heating mantle clip and the heating mantle from the sample tube.
2. Carefully slide the isothermal jacket down over the sample tube stem until it touches
the sample tube bulb.
3. Make sure the P0 tube is next to the sample tube.
4. Place the Dewar cover over the sample stem just above the isothermal jacket.
5. Fill LN2 in the Dewar. (Get LN2 from LN2 container nearby)
a. Protect yourself by wearing insulated gloves.
b. Pour the LN2 from one container to another slowly to prevent splashing.
c. To check the fluid level, insert the dipstick in the Dewar as shown below.
d. The volume for a full Dewar is about 2.7 L, last 40 hours.
e. Place the safety shield over the sample tube and Dewar.

6. Open sample file, edit the information of weigh

a. File Open Sample Information
b. Sample Information
c. Click Calculate, input the weight of empty tube set before degassing(W1) and
weight of sample tube set after degassing(W3)

d. Click save
b.
a.

c.

d.
 e. Please carefully verify the parameters and changes necessary for analysis
e.
conditions.
i. Options: Tick Low pressure incremental
i.
with dose amount (surface area/100)
1
ii. iii.
ii. Free space: Tick Enter
iii. Sample Backfill Options:

iii
i. .
ii.

7. Performing an Analysis
a. Click Unit 1
b. Click Start Micro-pore Analysis
c. For each port on which you want to start an analysis, Click Browse to select the SMP
file you set up, then Click OK
d. Click Start to begin the analysis
a.

b. c.

d.
 8. When analysis is finished, we need to get the data of free space to get the correct
Isotherm.
a. Create a new sample file in your folder
i. Click File Open Sample Information
ii. Click﹝…﹞ to up level the find your folder
iii. Click OK
iv. Click Yes to create a new SMP file.

a.
b.

d.

c.

9. Replace Method:
a. Click Replace All
b. Click ﹝…﹞ to C:\2420\method
c. Select 1 point BET Method
d. Click OK to replace the parameters
e. Sample ID enter free space for which SMP file
f. Verify Analysis Conditions file, the box of
Measure is ticked. a.
g. Click OK
h. Click SAVE
i. Then create the SMP file for the other samples.

c. b.

f.
d.

e.

g.
h.
10. Perform Analysis
a. Click Unit1 Select Start High Throughput Analysis
b. Select the Analysis port you want to analyzed.
c. Click Browse to select the SMP file your just create for measure free space and
click OK
d. Click Start to begin analysis.

b. c.
a.

d.

2. The analysis time is about 3 hours. When the analysis is completed, you can get the
data for warm/cold free space.
3. When the status shows IDLE, you can remove the sample and clean and recycle the
LN2 in the Dewars
 Chapter5 Clean and recycle LN2 in the Dewar
1. When the analysis is completed, the View of Status, the Details shows Idle, then you
can take off the sample tube.

2. Move the P0 tube away to make sure that when we raise the Dewar, it would not hit the
P0 tube.
3. Click Unit 1Enable Manual Control (Ticked) ，the color of all valves change to yellow.

4. Right-Click the Dewar, select Raise and the Dewar starts to raise. When it is easy to lift
the Dewar, then you can select Stop to stop raising.

5. Take the Dewar out of instrument, pour the LN2 in the plastic beaker, and use the
strainer to remove the ice and to the container.
6. Remember to cancel the function of Enable Manual Control(Unticked), the color of all
valves change to green.
7. Remember to write down the use record.
 Chapter 6 Data Process
Please copy your SMP file to your folder, then Use MicroActive to edit the SMP
fil.
1. Click MicroActive
2. Click File  Open 2. 3.
3. Select your SMP file
4. Click Open to open the file

4.

5. The window displays

6. Click the Isotherm then you can select Advanced

7. Enter free space data (Micropore analysis- you need to the measure free space SMP to get the free
space data.
a. Click Isotherm， b. Enter Free space data
(If you are doing BET or mesopore analysis, you can ignore this step)

b.

a.
8. BET report
a. Select BET
b. Isotherm curve (bottom right picture), drag the left blue line to 0.0
c. The top left picture (BET Surface Area Plot), drag the blue line to C is positive. And
correlation coefficient
d. Bottom left picture, don’t select the point which is trend down.

c.

d.
b.

a.

9. Langmuir report
a. Select Langmuir
b. Isotherm curve (bottom right picture) adjust the pressure range same as the
pressure of BET report

b
.

a
.
10. t-Plot report
a. Click t-Plot
b. Isotherm drag the left blue line to 0.0
c. 4 point, correlation coefficient higher is better
d. Y-intercept should be positive

b
.

a
.
11. BJH adsorption and desorption :

一般用 H &J 模式

12. HK

13. DFT and NLDFT

a. Sample Geometry select Slit, Model select N2@77 on carbon silt pores
b. Drag Isotherm left blue line to the left to whole relative pressure
c. Bottom left picture (Goodness of Fit vs. Regularization), adjust the blue line to
the point next to the cross.
a.

b.

C.調整解析度

14. Click Save to save the file

 b.
15. Print the Report
a. Select Advanced
b. Select Report Options
c. Double clicks Summary c.
d. You can select the summary report data you need
On first page.
e. If pore volume the relative pressure is 0.995
f. Click OK
g. Tick the Reports you want to show in your report.
h. Click Preview a.
i. Click Save As
j. Select the file type (excel or PDF)
k. Click Save

d.
e.
g.

f. h.
 Refill the liquid Nitrogen
If your analysis is over 30 hours, you need to go to lab to refilled the Nitrogen. Or the

analysis will fail because temperature is not low enough.

a. Click Suspend

b. b-1 Select the no. of Port which detail is not show Rate of Change

b-2 Click Yes (In these case, you should choose port 3.
a.
b-1.

Can not Suspend

b-2.
c.
Can Suspend

c. Enable Manual Control

Unit 1 (tick )Enable Manual Control

d. Move the mouse to the Dewar you want to lower and right click, choose Lower to

let the elevator starts to lower. When you see the top of the white isothermal jacket

shows up, then right click and choose Stop.

(If the Dewar is too low, the analysis will fail because temperature of the sample is

not low enough) e.

D.

e. Take off the shield and white cover, use the funnel and adjust the angle, it will be

easier to refill the liquid Nitrogen (Wearing the glove is necessary).

f. Move the mouse to the Dewar and right click, and select Raise.
f.
g. Wait for 5 minutes to let the temperature to stabilize  Click Resume Choose

the Port YES

g-1.

g-2.

g-3.

h. Disable manual Control : Unit 1 (untick )Enable Manual Control

i. Remember to put back the cover and the shield.

j. Make sure the Cylinder is back to safe place.