SOP TriStar3000 (BET)

GENERAL

The TriStar 3000 provides high-quality surface area and porosimetry measurements on solid
materials by using the technique of gas adsorption. This easy-to-operate, tabletop instrument is
designed to analyze up to three samples simultaneously for optimum throughput. Its speed and
accuracy make it an ideal instrument for research and quality control applications, as well as for
industries that include pharmaceuticals, cosmetics, paints, pigments, food products, and high-
tech ceramics.

The TriStar 3000 Analyzer uses physical adsorption and capillary condensation principles to
obtain information about the surface area and porosity of a solid material. The analytical
technique is simple: a sample contained in an evacuated sample tube is cooled (typically) to
cryogenic temperature, then is exposed to analysis gas at a series of precisely controlled
pressures. With each incremental pressure increase, the number of gas molecules adsorbed on
the surface increases. The equilibrated pressure (P) is compared to the saturation pressure (Po)
and their relative pressure ratio (P/Po) is recorded along with the quantity of gas adsorbed by
the sample at each equilibrated pressure.

As adsorption proceeds, the thickness of the adsorbed film increases. Any micropores in the
surface are filled first, then the free surface becomes completely covered, and finally the larger
pores are filled by capillary condensation. The process may continue to the point of bulk
condensation of the analysis gas. Then, the desorption process may begin in which pressure
systematically is reduced resulting in liberation of the adsorbed molecules. As with the
adsorption process, the changing quantity of gas on the solid surface at each decreasing
equilibrium pressure is quantified. These two sets of data describe the adsorption and
desorption isotherms. Analysis of the shape of the isotherms yields information about the
surface and internal pore characteristics of the material.

Standard Operating Procedure (SOP) for the TriStar 3000 Page 1

SAMPLE PREPARATION

For the sample preparation you can use the “FlowPrep 060”, a heating block that goes up to
400 °C and can be set under vacuum or purged with N 2. Make sure the sample is dried
properly, because if the sample is still too wet, starting the measurement will be harder. A
common use is to dry the samples overnight.

MEASURMENT

To start a measurement, open the TriStar 3000 Software.

- Select „Unit 1‟  „Sample Analysis’: a screen pops up where you can insert up to 3
samples (it‟s also possible to measure 1 or 2 samples)

Standard Operating Procedure (SOP) for the TriStar 3000 Page 2

 - Select „Options‟  ‘Sample Defaults’: a screen pops up where you can insert the
conditions for your samples. Several tabs guide you through the conditions:

o SAMPLE INFORMATION

 The sequence number (xxx-xxx) is selected automatically

 Insert your sample name, the operator and the mass of your sample
 Leave the density at 1 g/cm3 and enter a comment if needed.

o SAMPLE TUBE

 All the tubes for the TriStar3000 are 3/8 inch tubes. Leave the other
conditions untouched.

o DEGAS CONDITIONS

 Here u can insert your conditions of the sample preparation (Soak

Temperature, Soak Time and Heating Rate). These values don‟t influent
your measurement.

Standard Operating Procedure (SOP) for the TriStar 3000 Page 3

 o ANALYSIS CONDITIONS

 Select „Adsorption – Desorption CARL 5‟ for a normal measurement. If

this is not sufficient enough, it is possible to create your own pressure
table.
 Preparation – Free Space – Po and Temperature Options – Equilibration:
(Leave the conditions selected as in the print screen).

Standard Operating Procedure (SOP) for the TriStar 3000 Page 4

 o ADSORPTIVE PROPERTIES

 Leave the conditions selected as in the print screen if you are working
with N2

o REPORT OPTIONS

 Select the „Full Report Set‟

- Press „Save‟, press „Close‟

Standard Operating Procedure (SOP) for the TriStar 3000 Page 5

 - In the „sample analysis‟-screen you can now insert your created file
- Click „Browse…‟ from Port 1 and click „OK‟
- The system asks now to create the file, click „Yes‟

- REPEAT THE SAMPLE DEFAULTS STEP FOR THE OTHER SAMPLES (For Port 2 and 3) !

- Installation of the sample tubes:

o Move the isotherm jacket over the sample tube (at the red mark line)

o Move the sample tube through the dewar cover on the TriStar

o Add the sample tube ferrule and O-ring and attach the tube to the TriStar

- Press „Start‟ to start the measurement

GENERAL REMARKS

o If the 3 sample tubes are installed, push the dewar cover up to the top (so the
dewar is covered when going up.
o When filling the dewar with LN2, fill it exactly so the LN2 reaches
the hole (red line on the picture) of the depth gauge

Standard Operating Procedure (SOP) for the TriStar 3000 Page 6