F-Sorb X400 User Guide

Gold APP Instruments
2012
F‐Sorb X400 Specific Surface Area Analyzer User Guide
Sales Service Department
www.jinaipu.com
GOLD APP INSTRUMENTS CHINA
Lead You to Particles World Better
F-Sorb X400 Specific Surface Area Analyzer
1 Summary........................................................................................................................................................ 1
1.1 Models and versatility……………………………………………………………………………………1
1.2 Analyzer overview…………………………………………………………………………………………1
1.3 Pressure regulator………………………………………………………………………………………….3
2 Analyzer installation processes .... …………………………………………………………………………4
2.1 Intordution of the analysis system…………………………………………………………………………4
2.2 Samples filling and cells installation ... ……………………………………………………………………4
3 Software installation and instruction .. ……………………………………………………………………6
3.1 Software installation ………………………………………………………………………………………6
3.2 Software overview ... ………………………………………………………………………………………8
4 Surface area analysis instruction... ………………………………………………………………………12
4.1 Standard sample reference (SSR) method procedure ……………………………………………………12
4.2 BET surface area analysis method procedure ……………………………………………………………14
4.3 Notes during analysis processes………………………………………………………………………….16
4.4 How to calibrate the calibrator tube volume .. ……………………………………………………………16
5 Sample degassing recommendation.......................... …………………………………………………….17
6 Faults handling……………………………………………………………………………….………….17
6.1 Electric relay control……………………………………………………………………………………..17
6.2 Gas leak…………………………………………………………………………………………………..17
6.3 System time change………………………………………………………………………………………18
7 Reference table…………………………………………………………………………………………..18
Address: floor 6th, Tianli Building, NO.56th, Zhichun Rd., Haidian Dist., Beijing 100098, CHINA http://www.jinaipu.com
Tel: (+8610)-82133318 Mobile: +86-18210009838 Fax: +8610-82118197 Email: [email protected]
1 Summary
1.1 F-Sorb X400 series models and versatility
Models
F-Sorb 1400 F-Sorb 2400 F-Sorb 3400
Versatility
Standard Sample Reference √ √ √
Langmuir Method x √ √
BET Surface Area x √ √
BJH Pore Size Distribution x x √
Adsorption Constant C x √ √
Carbon Black External Surface Area x √ √
1.2 analyzer overview
Power
Cell Connector
Port 4, Port 3, Port 2, Port 1
Elevator
Front View
Communication Connector
Power Line Connector

N2 Input
Gas Outlet He Input
Back View
1.3 pressure regulator
Isolation Valve Pressure Gauge Pot Valve

5 4 1
3 Cylinder Outlet Regulator 2
Gas Container
3
Table one:
Mark Name Function description
① Pot Valve To switch on or off the gas pot
To Adjust the pressure into the analyzer
② Regulator
“DEC” means decrease and “INC” means increase
③ Cylinder Connector To connect the regulator with the analyzer inlet port
④ Pressure Gauge To display gas pressure in the pot
To display gas pressure into the analyzer.
⑤ Isolation Valve
And must both be equal to 0.16MPa for Nitrogen and Helium
Operation Notices:
※ The regulator is precise part and should be operated slowly and carefully;
※ Check and make sure the pressure regulator is switched off before switching one the gas pot valve;
※ Switch on the gas pot valve by anticlockwise. Pressure gauge displays the real pressure, will decrease
when using, in the pot; The outlet pressure cannot over 0.2Mpa, 0.16Mpa is suitable for analysis;
※ Keep pressure regulator in natural loose condition when switch to DEC direction. If too tight, the
regulator may be damaged;
※ After switched off the pressure regulator, little gas stays in it and will escape gradually;
※ Switch off the pressure regulator after using is a must.
2 Analyzer Installation Processes

2.1 introduction of the absorbent N2 and carrier He analysis system
1) Connect the gas N2 and He regulators with the gas pots respectively.
2) Connect the gas flow controllers to the outlets of reducers through diameter-altering connectors.
3) Connect the gas supplies with the analysis system by provided metal pipes (please make sure the right inlets for
N2 and He pot)
4) Open the gas pot valves and adjust the pressure around 0.16MPa by the regulators.
5) Make sure no air leak from the connecting points.
Notice: please guarantee the gas pressure into the analyzer is always keeping at 0.16MPa around as the equipment is
designed and tested in this parameter.
2.2 samples filling and sample cells installation

1) Use the provided funnel to fill samples into the cells and prevent samples adhered to the cells’ wall;
2) Filled sample volume should limit in 2/3 of cell bottom volume, in case block gas flow;
3) Use a needle item to thrust sample if it is chocked in funnel;
4) Filled sample mass depends on its surface area. The larger surface area is, the less sample quantity is. Generally,
(9.1 m2/g≈1g);
5) Should use a 0.0001 precision balance to eliminate weighting errors;

6) Prevent samples adhered to cells’ walls as these samples can’t soaked into liquid nitrogen bath;
7) Circle the nut on cell, then the rubber O-ring. The O-ring against the cell mouth is about 5mm which can get an
ideal airproof effect;
8) Carefully screw two pressing nuts concurrently to keep them pressing the rubber O-ring tightly to achieve a high
airproof effect.
9) ALL four rows of sample stations should be mounted with sample cells no matter how many rows of
samples are analyzed at one time, shown as figure above. It is because these four stations are parallel
pipeline and will be analyzed simultaneously. Empty cells should be installed if measured samples are less
than four rows.
10) Be aware that the sample cells are fragile and have to treat them carefully.
3 Software Installation and Instruction

3.1 software installation
1) Make sure your computer installed with windows 2000 or XP English version system.
2) Have the analyzer get ready for measuring and connect computer and the analyzer with COM cable.
3) Find and run the analysis software named as “APDSetup_EN-090723.msi” on the CD enclosed
with your analyzer package.
4) Click “Next” button and continue.
5) Select the folder where you want the software be installed and click “Next”.
6) Click the “Next” button to finish the installation.
7) Click the “Close” button to complete the installation.

8) Copy the full folder named as “APP F-Sorb X400 analysis software updated” to your computer anywhere you
AppDetect_EN-090723.exe
want and run the program named as “AppDetect_EN-090723.exe “.
9) ※ PLEASE DON’T CLICK & RUN THE ”AppDetect.exe” WHICH IS AN OLD VERSION AND JUST
IGNORE IT.
7
3.2 software overview
1) Above is the initial interface of the analysis software.
Click the button and analyzer will

self-check to find COM port on computer
that connected with it. 1 8
2) Go to the COM port configuration interface from Menu: SetupCOM Settings. Must keep the COM settings
parameters as it is except the COM item, which depends on your computer’s COM port available. Click the
“Check” button to find or find it by yourself.
3) Go to the above password input interface from Menu: SetupInstrument Parameters. THE PASSWORD IS
“admin”. PLEASE KEEP IT IN YOU MIND.
Limit the maximum curve peak
2 value when begin to do adsorption
Limit the longest desorbing span
equilibrium detecting action
time to the value indicated in the 3
box.
1
Indicate if the adsorbing or
desorbing equilibrium is achieved.
The less the value is, the more
difficult to achieve equilibrium.
4
Indicate the waiting time after the
sample adsorption or desorption
equilibrium has been completed.
5
Indicate the sensor signal volt when
the gas flow rate is about equal to
zero. If the default value 1.1V
doesn’t work, set it as 0.9V
6
Limit the interval between
Indicate the flow rate permissible
two gas flow adjusting
variance value when running gas
actions.
helium or nitrogen flow adjusting. 7
9
4) Notice: all the parameters in the above “Instruments parameters” interface are critical for the analyzer running
functionally well. Wrong settings may cause analyzer malfunction or damage. The default is ok. So the setup
interface is not accessible for users and just for manufacture purpose. Password is required.
2
Select the analysis Click the button to
method you want. start the analysis
when ready
1
5 Calibrator tube volume. 3

It is about 2.94 for your
Station No.1
analyzer
Station No.2
No use for your
Station No.3
analyzer, please don’t
Station No.4
4
check.
Type in the boxes

6 according to your
P/Po point set for your analysis cases.
selecting when doing
7
BET analysis.
Total mixture gas
flow rate, keeping at
70 ml/min 8
5) Refer to above illustrations for explanation of parameters used in the software.
10
Station No.3 Station No.1
Station No.4 Station No.2
6) Refer to above illustrations for sample No. stations which are corresponding with analyzer software interface.
11
4 Surface Area Analysis Instruction

4.1 standard sample reference (SSR) method procedure
1) Degassing samples and gets them ready for analysis.
2) Mount sample tubes on the analyzer’s station ports
NOTICE: four stations must all be mounted with tubes even if just run one station sample analysis, as shown above
illustration.
3) Adjust gas valves to input gas into the analyzer. Keep the gas regulators both for Nitrogen and Helium at
0.16MPa shown as above illustration.
4) Get ready the analyzer for analysis and run the analysis software.
5) Click above button to warm up the system for 15-30min.
12
Select the SSR

method first
1 Not necessary
for SSR Method.
3
Standard Sample
SSA Value
2
Fill in samples 4
qualities respectively.
6) Fill in the analysis parameters as shown above example.

7) MUST MOUNT STANDARD SAMPLE AT STATION No.1, and matching with “Standard ID” column at
software interface above.
8) Could run most up to three set of samples analysis simultaneously with standard sample mounted at station No.1.
9) Also, you could select to run one or two set of samples analysis. In this case, just fill in the sample quality column
with the number “0” at above interface corresponding to the analyzer’s station with no sample analysis running.
10) When above all are ready, prepare liquid nitrogen flasks for every ongoing analysis stations (refer to operating
video) and click the “analysis” button to start the analysis, and waiting for the analysis completed.
13
11) SSR surface area analysis report showed as above.
4.2 BET surface area analysis method procedure

1) Samples and analyzer preparation operations are same as SSR method illustrated above.
Calibrator volume value. It is

Select the BET
2.94 for your analyzer. The
method first
value need to be calibrated
1
about every three months.
Check the box

when doing low
SSA samples
analysis.
4
Select the BET P/Po sets,
normally selecting sets of
0.25/0.20/0.15/0.10/0.06
2) Type in the analysis parameters showed as above example.

3) Following procedures are same as SSA method illustrated above.
4) Final BET surface area report displayed as below.
14
Double click
the toggle on or
off (Yes->No) 1
15
Click the button

to recalculate the
BET result.
2
5) Double click the individual P/Po row to alter the calculating toggle on or off (Yes->No) to have it included or
excluded in final BET calculation.
6) Click “Cal Refresh” button to recalculate the BET result when toggling on or off alteration, or changes calibrator
volume value.
4.3 notes during analysis processes

1) Should fill the liquid nitrogen when half left. Generally, fill in liquid nitrogen when the elevator comes down;
2) Cannot adjust the pressure regulator at random, even there is a slightly fluctuations displayed.
3) Forbid heavily shake for the connecting pipes and analyzer.
4) If malfunctions or abnormal phenomena (such as abnormal peak, pipe broken) occurred, pls shut down the software
and turn off power.
5) Show down analyzer power, then gas supply after analysis finished.
6) Must turn off pressure regulator if do not analysis.
4.4 how to calibrate the calibrator tube volume

1) Run BET surface area analysis with standard samples (Reference Materials) enclosed with your analyzer package
correctly, and get good coefficient of the line at BET plot.
Try to change the value to

let BET result of standard
sample analyzed be about
equal to its approval
result as possible.
1
2) Try to change the value to let BET analyzed results of standard sample (Reference Materials) as equally as
possible. Then you can use the “New” calibrator volume value as it is amended.
16
3) Do the calibrating practices every 3 months.
5. Sample Degassing Recommendation

1) The degassing temperature for provided standard samples is about 105℃ and degassing time is about 1-2 hours.
Also the vacuum is advised. So can be treated in any heating devices available for you.
2) The degassing temperature for measured samples heavily depends on the samples properties. But, generally, it
should be over 100℃ which benefits for water vapor degassing. The degassing time is about 3-5 hours normally.
6. Faults Handing
6.1 electric relay control
Two reasons for above fault:

1) No or little gas input. Pls refer to analysis log;
2) At least one parameter did not type in for analysis parameters. Pls check analysis log and find the blank textbox,
type in the correct parameters.
6.2 gas leak

1) Reasons: electric bridge cannot get balance for a long time; the adsorption isotherm stays below the base line for a
long while and cannot rise up; abnormal desorption isotherm.
Reverse sorption phenomena usually occurs 3-5 mins during adsorption process, if took too long time (as above pic) that
shows gas leak had happened and maybe caused by sample cell loosen. At this moment, forced to stop analysis, save
document and contact us in case man-made faults happened.
17
6.3 system time change

Forbid to change computer system time during analysis, because the analyzer adopts computer time to operate and
record log. Analysis will fail when PC system time changed. Pls refer below pic.
7. Reference Table
Appendix I
ASTM D-24
Standard Reference Carbon Black 8#(SRB-8) Value
Standard Reference Carbon Black NSA(m2/g) STSA(m2/g)
A-8(N326) 76.2(74.93~77.55) 76.7(75.58~77.91)
B-8(N134) 142.6(141.11~144.15) 133.3(130.93~135.66)
C-8(HS-Tread) 126.3(124.72~127.92) 115.9(114.40~117.46)
D-8(LS-Carcass) 21.6(20.92~22.20) 21.1(20.27~21.94)
E-8(N660) 36.5(35.88~37.14) 35.6(34.60~36.61)
F-8(N683) 36.8(36.26~37.41) 35.5(34.38~36.53)
G-8(N990) 9.1(8.74~9.46) 8.4(7.80~9.00)
Note: CTAB value be calculated by CTAB=STSA×1.017+2.6434, only for reference.
18
AppendixⅡ
rpi(nm)(Pore real dpi(Pore
P/P0 rk(Pore Semi-diameter)（nm） Adsorption film thickness t(nm)
semi-diameter) Diameter）
0.414/LOG(P0/P) (0.354*POWER(-5/LN(p/p0),1/3)) rpi=rki+ti dpi=2*rpi(nm)
0.990 94.84958935 2.805001332 97.65459068 195.3092
0.985 63.07351284 2.448331724 65.52184457 131.0437
0.980 47.18527144 2.222576609 49.40784804 98.8157
0.975 37.65216282 2.061505809 39.71366863 79.4273
0.970 31.29661955 1.938297328 33.23491688 66.4698
0.960 23.35187782 1.758039074 25.1099169 50.2198
0.950 18.58469494 1.629194989 20.21388993 40.4278
0.940 15.40628701 1.53045506 16.93674207 33.8735
0.920 11.43261974 1.385595635 12.81821538 25.6364
0.900 9.047698965 1.281643682 10.32934265 20.6587
0.880 7.457131242 1.201651452 8.658782695 17.3176
0.850 5.865595051 1.109239379 6.97483443 13.9497
0.820 4.803556157 1.037788557 5.841344713 11.6827
0.800 4.272004380 0.998002931 5.27000731 10.5400
0.780 3.836694089 0.962883278 4.799577367 9.5992
0.750 3.313624031 0.916971133 4.230595164 8.4612
0.700 2.672658242 0.853563292 3.526221533 7.0524
0.650 2.212878443 0.801506606 3.014385049 6.0288
0.600 1.866136279 0.757243764 2.623380042 5.2468
0.550 1.594532000 0.71856435 2.31309635 4.6262
0.500 1.375278231 0.683992663 2.059270894 4.1185
0.450 1.193814703 0.652479535 1.846294239 3.6926
0.400 1.04035782 0.623230691 1.663588511 3.3272
0.350 0.908030233 0.595600001 1.503630234 3.0073
0.300 0.791770566 0.569011492 1.360782058 2.7216
0.250 0.687639116 0.542885336 1.230524452 2.4610
0.200 0.592300095 0.516537498 1.108837593 2.2177
0.150 0.502482835 0.488984392 0.991467227 1.9829
0.100 0.41400000 0.458410652 0.872410652 1.7448
0.060 0.31820942 0.419912624 0.738122043 1.4762
19

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Gold APP Instruments

Sales Service Department

F-Sorb X400 Specific Surface Area Analyzer

Standard Sample Reference √ √ √

BET Surface Area x √ √

BJH Pore Size Distribution x x √

Carbon Black External Surface Area x √ √

1.2 analyzer overview

Port 4, Port 3, Port 2, Port 1

Power Line Connector

Gas Outlet He Input

1.3 pressure regulator

Isolation Valve Pressure Gauge Pot Valve

3 Cylinder Outlet Regulator 2

2 Analyzer Installation Processes

2.2 samples filling and sample cells installation

5) Should use a 0.0001 precision balance to eliminate weighting errors;

3 Software Installation and Instruction

4) Click “Next” button and continue.

6) Click the “Next” button to finish the installation.

7) Click the “Close” button to complete the installation.

3.2 software overview

1) Above is the initial interface of the analysis software.

Click the button and analyzer will

5 Calibrator tube volume. 3

Type in the boxes

5) Refer to above illustrations for explanation of parameters used in the software.

Station No.3 Station No.1

Station No.4 Station No.2

4 Surface Area Analysis Instruction

5) Click above button to warm up the system for 15-30min.

Select the SSR

6) Fill in the analysis parameters as shown above example.

11) SSR surface area analysis report showed as above.

4.2 BET surface area analysis method procedure

Calibrator volume value. It is

Check the box

2) Type in the analysis parameters showed as above example.

Click the button

4.3 notes during analysis processes

4.4 how to calibrate the calibrator tube volume

Try to change the value to

3) Do the calibrating practices every 3 months.

5. Sample Degassing Recommendation

Two reasons for above fault:

6.2 gas leak

6.3 system time change

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