Porous Materials, Inc.

PMI Automated BET Sorptometer

Instruction Manual

Porous Materials, Incorporated

20 Dutch Mill Rd
Ithaca, New York 14850
(607) 257-5544

1-800-825-5764 (in continental US and Canada)

POROUS MATERIALS INC. • 1

Table of Contents

EQUIPMENT INFORMATION 4

Shipment Inspection....................................................................................................................... 4

Notes on Installation ...................................................................................................................... 4

Specifications .................................................................................................................................. 5

BACKGROUND 6

Physical Adsorption: Surface Area Measurements ......................................................................... 7

Physical Adsorption: Isotherms and Pore Size Distribution .................................................... 10

Chemisorption............................................................................................................................... 14

PRINCIPLES OF OPERATION 15

Adsorption Measurements ........................................................................................................... 17

Calibration .................................................................................................................................... 19

Computer Hardware & Software Requirements ........................................................................ 20

OPERATING PROCEDURE 22

Start Up......................................................................................................................................... 23

Automated Tests ........................................................................................................................... 25

Installation/Removal of Sample Cell ........................................................................................... 27

Installation/Removal of Dewar Flask .......................................................................................... 28

Installation/Removal of Heating Mantle..................................................................................... 29

DO's and DON'Ts.......................................................................................................................... 30

BETWIN SOFTWARE SYSTEM 31

Introduction .................................................................................................................................. 31

Main Menu Screen........................................................................................................................ 32

File Menu ...................................................................................................................................... 33

Select User ....................................................................................................................... 33
New User .......................................................................................................................... 34
Select Gas ......................................................................................................................... 36

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 Select Units ...................................................................................................................... 37
Exit ................................................................................................................................... 38
Execute Menu ............................................................................................................................... 39
Automated Test ............................................................................................................... 39
Advanced Settings .............................................................................................. 42
Test Status Screen .............................................................................................. 49
Automated Test Description ............................................................... 54
Manual Control ................................................................................................................ 56
Calibrate Gauges ............................................................................................................. 64
Calibrate Sample Chamber............................................................................................. 66
Calibration Status Screen ............................................................... 67
Description of Sample Chamber Calibration.......................................... 71
Calibrate Instrument ...................................................................................................... 73
Description of Instrument Calibration ................................................. 74

Report Menu ................................................................................................................................. 75

Execute Report................................................................................................................. 75
Graph Setup ............................................................................... 77
Output Device ............................................................................. 77
Report Setup .............................................................................. 78
Multi-Graphic Option ..................................................................... 81
Report Cover Page ....................................................................... 81
Alter Cover ....................................................................................................................... 82
Modify Menu ................................................................................................................................. 83
Edit Auto Parameters ..................................................................................................... 84
Manually Create File ...................................................................................................... 88
Curve Fit .......................................................................................................................... 93
Interpolate........................................................................................................................ 95
Edit Old Gas..................................................................................................................... 96
Setup Menu ................................................................................................................................... 97
New Multipoint List ........................................................................................................ 98
New Isotherm List ......................................................................................................... 100
New Pretreatment List ................................................................................................. 102
Create New Gas ............................................................................................................. 105
Pressure Units ............................................................................................................... 109
Hardware Protocol ......................................................................................................... 111
Help Menu ................................................................................................................................... 112
About BETWIN .............................................................................................................. 112
Help ................................................................................................................................ 112

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EQUIPMENT INFORMATION

Shipment Inspection
Your PMI Automated BET Sorptometer was carefully inspected and
tested prior to shipping. Please make sure that the instrument and accessories
have arrived in good condition. Claims for any damage must be made against the
delivering carrier, but PMI should also be notified so that we can assist you as
much as possible.

Porous Materials, Inc. warrants each new instrument against defects in

materials and workmanship for one year from the date of delivery. Please contact
us if you have any questions or problems.

Notes on Installation
This manual is not designed to be a tutorial on the operation of the BET
Sorptometer, but rather is designed as a reference manual and a guide to the
theory of operations. (Though it has been found to be adequate in certain cases
where installation was not requested by the end user.) All automated BET
Sorptometers come with on-site installation by a factory representative within the
continental United States. It is recommended that the manual be read by the
people who are to operate the instrument before the installer arrives, but that they
do not attempt to actually operate the instrument until guided by the installer. If,
when reading the manual, you have any questions about the instrument, don't
hesitate to contact PMI for further information. The installer is well versed in all
aspects of the instrument and can best answer your questions.

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Specifications
Sample volume: up to 10 cc for sample cells provided (others available)

Adsorbate: any non-corrosive gas

Pressure transducer: 0-1000 Torr

resolution 1 part in 20,000
accuracy 0.15% of reading

0-10 Torr
resolution 1 part in 20,000
accuracy 0.15% of reading

Adsorption temperature: -196°C (liquid nitrogen) to 300°C

Surface area range: 0.01 m2 and higher

Pore diameter range: 10-500 Å

Power requirements: 110 VAC, 50/60 Hz

Size: 82"H x 44"W x 36"D

Weight: 600 lbs

Vacuum pump: Edward's RV12

Diffusion pump optional
Turbo pump optional

Controlling computer: Windows based computer with monitor.

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BACKGROUND

The adsorption of gases on solid surfaces is of interest in numerous

applications, and serves as the basis for some well-established techniques for the
characterization of materials. Physical or chemical adsorption can occur,
depending upon the nature of the solid adsorbent and gaseous adsorbate, and on
the temperature and adsorbate pressure. In physical adsorption, there is a
relatively weak van der Waal's-type interaction between the solid and the
adsorbed gas molecules; multiple layers of adsorbate can result, akin to
condensation of vapor on the solid surface. Chemisorption, on the other hand,
involves relatively strong chemical bonding between the solid and the adsorbate,
and is, therefore, limited to monolayer coverage (an adsorbed layer one molecule
thick). Although any gas will physically adsorb on any solid at appropriate
temperatures and pressures, chemisorption can only occur with certain solids and
reactive gases (or liquids).

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Physical Adsorption: Surface Area Measurements
Physical adsorption can occur over the entire surface of any solid, if the
adsorbate molecules are small enough to enter essentially all pores that may be
present. Thus, the total surface area of a solid can be determined from physical
adsorption measurements. The Brunauer-Emmett-Teller (BET) method is most
commonly employed, and utilizes the following adsorption isotherm for analysis
of experimental data:
P
=
1
+
(C - 1)P [1]
N(P0 - P) N m C N m CP0
where P = adsorbate gas pressure
P0 = saturation pressure of adsorbate gas at the system temperature
N = equilibrium amount of gas adsorbed
Nm = amount of gas adsorbed in monolayer
C = dimensionless constant that depends on the temperature and
on the gas-solid system.
Here, N and Nm will be expressed as moles of gas, but they could also be
expressed as masses of gas or as volumes of gas at standard temperature and
pressure (STP) -- 0°C and 1 atm. If the BET equation [1] is obeyed, a plot of
P/N(P0 - P) versus relative pressure P/P0 should give a straight line with a slope
of (C - 1)/NmC and an intercept equal to 1/NmC. The values of Nm and C are
then given by:
1
Nm = [2]
s + i
s
C = 1 + [3]
i
where s = slope from linear BET plot
i = intercept from linear BET plot.
Once the amount of adsorbed gas that corresponds to monolayer coverage has
been estimated, the total surface area per unit mass of sample can be calculated
from the effective cross-sectional area of the adsorbate molecule:
Nm N0 
Sg = [4]
Ws
where No = Avogadro's number, 6.02 x 1023 molecules/mole
 = effective cross-sectional area of adsorbate molecule (16.2 Å 2 for
nitrogen, 19.5 Å 2 for krypton)
Ws = mass of sample
Sg = total surface area per unit mass of sample.

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 In general, physical adsorption data are well correlated by the BET
equation for relative pressures (P/P0) between about 0.05 and 0.30, so this range
is used for surface area measurements. The standard adsorbate in the BET
method is nitrogen vapor, at liquid-nitrogen temperature (-195.8°C) and pressures
in the range of 0.05 to 0.30 atm (0.74 to 4.41 psia). For samples with relatively
low surface areas (< 5 m2/g), the sensitivity of the technique can usually be
improved by using krypton, rather than nitrogen, as the adsorbate. At
liquid-nitrogen temperature, krypton has a saturation pressure (P0) of 2.63 torr, so
pressures in the range of 0.132 to 0.789 torr should be employed. In either case, a
reliable multi-point BET surface area is obtained by making adsorption
measurements at several different adsorbate pressures (in the appropriate range)
and analyzing the data as outlined above.

If the constant C is sufficiently large (much greater than one), the BET
equation [1] can be simplified to obtain an estimate of Nm from a single
adsorption measurement:
 P P 1
N m,sp = N 1 - , for 1 > >> [5]
 P0  P0 C

where the subscript sp denotes the single-point BET method. The multi- and
single-point BET surface areas can be compared by substituting Nm (from
equation [1]) or Nm,sp into equation [4]:
Sg - Sg,sp 1 - (P P0 )
 sp = = [6]
Sg 1 + (C - 1)(P P0 )

where  sp is the relative error in the single-point BET surface area, and is
tabulated as a function of C and P/P0 in Table I. In the single-point method, the
adsorption measurement is made at a relative pressure between 0.2 and 0.3 so that
the error in the surface area will be only a few percent if C is greater than about
50 (as it often is for nitrogen adsorption). Thus, the additional time and effort
required in the multi-point BET method may not be justified for many
applications.

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 Table I
Relative Error (sp) in the Single-Point BET Surface Area
for Selected Values of C and P/P0
P/P0
C 0.1 0.2 0.3
1 0.90 0.80 0.70
5 0.64 0.44 0.32
10 0.47 0.29 0.19
50 0.15 0.074 0.04
5
100 0.083 0.038 0.02
3
500 0.018 0.008 0.00
5
1000 0.009 0.004 0.00
2

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Physical Adsorption: Isotherms and Pore Size Distribution
A porous solid can be further characterized by generating complete
physical adsorption and desorption isotherms, from which the pore size
distribution and pore volume can be determined. The adsorption/desorption
isotherms are obtained from measurements of the equilibrium amount of vapor
that is physically adsorbed as a function of increasing/decreasing adsorbate
pressure over the range 0 < P/P0 < 1, at constant temperature. As the relative
pressure P/P0 is increased, multilayer adsorption and capillary condensation
eventually occur. Vapor can condense within the pores at pressures below the
saturation pressure (where bulk condensation would occur), since the equilibrium
vapor pressure over a curved liquid meniscus in a pore is lower than that over a
planar liquid surface if the liquid wets the pore wall. The Kelvin equation relates
the vapor pressure of the liquid to the radius of curvature of a hemispherical
meniscus:
2  VL cos 
ln (P P0 ) = - [7]
rK RT
where P = vapor pressure over curved liquid surface (same as adsorbate gas
pressure, at equilibrium)
P0 = vapor pressure over planar liquid surface (same as saturation
pressure of adsorbate gas, at equilibrium)
 = surface tension of the liquid
VL = molar volume of the liquid
 = contact angle of the liquid with pore wall
rK = radius of curvature of the meniscus (positive for a concave liquid
surface)
R = gas constant
T = absolute temperature.
Note that rK increases as P/P0 increases; thus, capillary condensation can occur at
a lower relative pressure in a pore of smaller radius. For a given value of P/P0, all
pores whose radii are smaller than some critical pore radius rp,c should be filled
with liquid via capillary condensation. The thickness of the adsorbed layer (t) that
is present in all pores, independent of any capillary condensation, must be taken
into account to properly relate rp,c to P/P0:
2 VL cos 
rp,c = rK + t = - +t [8]
RT ln (P P0 )

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 For nitrogen adsorption,  = 0° so cos  = 1, and the thickness of the adsorbed
layer is given by the following correlation:
1
 
3
5
t (in ? = 3.54   [9]
 ln (P0 P )

The adsorption measurements are usually made at -195.8°C (the normal boiling
point of nitrogen), and substitution of numerical values into equation [8] gives the
corresponding relationship between the critical pore radius and the relative
pressure:
-1 − 13
 P   P 
rp,c (in ? = 9.57 ln  0  + 6.05ln  0  [10]
 P   P 

Values of the adsorbed film thickness, Kelvin radius, and critical pore radius
calculated from these equations are tabulated as a function of relative pressure in
Table II.

For an adsorption or desorption isotherm, the difference in the moles of

gas adsorbed at different relative pressures can be expressed as an equivalent
volume of liquid ( VL), which corresponds to the difference in the volume of
capillary condensed liquid within the pores plus the difference in the volume of
the adsorbed film on the walls of the pores that remain unfilled:
2
 rK 
VL = (N )VL  (Vp )  + (t ) rp rp,c (Sp )
rp - t
[11]
 rp,c  rp
where r K, t , r p,c = average values of the Kelvin radius, adsorbed film
thickness, and critical pore radius for the relative pressure
interval
t = change in adsorbed film thickness resulting from the
change in relative pressure
Vp = volume of pores with radii in a specified interval (here, the
interval in critical pore radius corresponding to the relative
pressure interval)
Sp = surface area of pores with radii in a specified interval (here,
all radii greater than r p,c)
rp = average pore radius for a specified interval.
This equation can be used to calculate the pore size distribution from an isotherm;
however, rK, t, and rp,c must be known as a function of the relative pressure, so
the usual adsorbate is nitrogen at its normal boiling point. Equation [11] should
be applied to small decrements in P/P0, starting at the highest P/P0 (slightly less

POROUS MATERIALS INC. • 11

 than 1) where essentially all pores are filled by capillary condensation. For the
first decrement, the summation in equation [11] can be neglected and Vp is
readily calculated. The corresponding value of Sp (for use in subsequent
calculations) can be estimated by assuming that the pores are cylindrical:
2(Vp )
Sp = [12]
rp

In this way, Vp and Sp can be determined for each decrement in P/P0 (which
corresponds to a certain range of pore radii) so that the pore volume and pore
surface area distributions are obtained. The total pore volume (Vp) and total
surface area (Sp) are then given by:
Vp =  (Vp ) [13]
rp

S p =  (S p ) [14]
rp

This total surface area is based upon the assumption that the pores are cylindrical
and does not include any contribution from pores smaller than about 15 Å in
diameter (for which the Kelvin equation should not be applied); thus, it is less
reliable than the BET surface area.

Hysteresis effects (differences between the adsorption and desorption

isotherms) are often observed for porous solids, and can provide additional insight
into the pore structure. The desorption isotherm is generally preferred for
calculation of the pore size distribution, since the conditions are usually closer to
those assumed in the Kelvin equation.

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 Table II

Critical Pore Radius as a Function of Relative Pressure

for Nitrogen

Adsorption/Desorption at -196°C
P/P0 t(Å) rK(Å) rp,c(Å)

0.30 5.7 7.9 13.6

0.40 6.2 10. 16.
4 6
0.50 6.8 13. 20.
8 6
0.60 7.6 18. 26.
7 3
0.70 8.5 26. 35.
8 4
0.80 10.0 42. 52.
9 9
0.90 12.8 90. 104
8
0.95 16.3 187 203
0.98 22.2 474 496
0.99 28.0 952 980

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Chemisorption
In contrast to physical adsorption, which is nonspecific and typically
observed at low temperatures, chemisorption occurs with gases that are
sufficiently reactive to chemically bond onto certain solids or onto specific
surface sites of a solid, and is usually observed at elevated temperatures.
Chemisorption can be activated or non-activated, the latter type resembling
physical adsorption in that equilibrium is achieved quite rapidly (adsorption and
desorption are fast). Activated chemisorption proceeds more slowly, and in some
cases, equilibrium cannot be established within a reasonable time.

The Langmuir isotherm is often useful in the analysis of chemisorption

data, and relates the equilibrium amount of gas adsorbed to the gas pressure:
N KP
= [15]
Nm 1 + KP

where N/Nm is the fractional coverage of adsorption sites and K is the adsorption
equilibrium constant, which is a function of temperature. Note that 0 < N/Nm < 1
since chemisorption is limited to monolayer coverage.

Selective chemisorption can sometimes be used to determine the surface

area corresponding to a particular type of site, rather than the total (BET) surface
area of the solid. The characterization of a supported metal catalyst, for example,
may involve hydrogen chemisorption measurements to determine the exposed
metal surface area (hydrogen adsorption on the support is usually negligible), as
well as BET surface area measurements for the metal and support combined.
Chemisorption conditions should be chosen to provide monolayer coverage
(N/Nm = 1), and it is necessary to know the number of surface metal atoms
covered for each hydrogen molecule adsorbed and the surface area per metal atom.
Hydrogen usually dissociates on most catalytic metals, so that one hydrogen atom
is adsorbed on a metal atom. For all metals, there are approximately 1019 atoms
per square meter of surface; the exact number varies somewhat for different
metals and, to a lesser extent, for different crystallographic planes. In addition to
hydrogen, carbon monoxide and oxygen have also been used for selective
chemisorption -- the choice depending upon the particular catalyst under study.

POROUS MATERIALS INC. • 14

PRINCIPLES OF OPERATION

The PMI Automated BET Sorptometer is a precision volumetric sorption

instrument in which any non-corrosive gas can be used as the adsorbate. The
equilibrium amount of gas adsorbed on the sample at a controlled temperature and
pressure is calculated from the measured drop in pressure of a known quantity of
adsorbate gas when it is allowed to expand from a reference volume into the
sample cell, which is initially evacuated. Adsorbate gas can then be transferred to
or from the sample cell to obtain additional data at different pressures. Sample
pretreatment (such as outgassing) is carried out in situ, so there is no need to
transfer the sample and risk contamination during a test. The instrument is well
suited for both chemisorption studies and the physical adsorption measurements
from which BET surface areas (single- or multi-point), adsorption/desorption
isotherms, and pore size distributions can be determined. Gas pycnometry can
also be performed to measure the absolute (true) density of a sample.

A schematic of the Automated BET Sorptometer is shown in Figure 1.

The sample cell is a removable glass U-tube that mounts vertically on the
instrument. The bottom portion of the U-tube, which contains the sample, can be
immersed in a Dewar flask containing liquid nitrogen (or other coolant) for low-
temperature adsorption measurements, or it can be heated to a specified
temperature by means of a heating mantle and temperature controller that is
incorporated into the instrument. An external vacuum pump is used to evacuate
the system, which can be monitored with the low pressure vacuum gauge. Both
the sample chamber and the reference volume can be isolated by means of the
shut off valves. The reference volume is enclosed by valves 1 through 4, with
valve 5 open, and serves as a reservoir for the adsorbate gas. The gas pressure in
the reference volume is measured with a pressure transducer. Adjustable
metering valves are located in the inlet line to the sample cell and in the adsorbate
gas inlet line to prevent ellutriation of powder samples and to make it easier to
pressurize the reference volume to the desired level. Valve 5 is closed only when
it is necessary to pretreat a sample under flowing gas, as is sometimes desired in
chemisorption tests. The temperature within the instrument, where the reference
volume and connecting lines are located, is held constant by means of a

POROUS MATERIALS INC. • 15

 temperature controller that should be set several degrees higher than the normal
room temperature.

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Adsorption Measurements
The test is started by placing a known mass of sample in the sample cell
and connecting it to the instrument. Before any adsorption measurements are
made, the sample should be pretreated -- usually by outgassing at elevated
temperature under vacuum, to drive off any moisture or adsorbed gases. After the
sample has been pretreated and the sample chamber and reference volume have
been evacuated, the desired sample temperature for adsorption is established and
the sample chamber is isolated by closing valves 1 and 2. The reference volume
is pressurized with adsorbate gas and is then isolated, so that the resulting gas
pressure (Pi) can be measured. This gas is allowed to expand into the sample
chamber by opening the isolation valves (1 and 2), and after the system has
equilibrated, the final gas pressure (Pf) is measured. The amount of gas adsorbed
on the sample can be calculated from the following equation, which makes use of
the ideal gas law:
Pi VA Pze Vit Pze (Vtt - Vs ) Pf (VA + Vit ) Pf (Vtt - Vs )
+ + = + + N [16]
Rit Rit Rtt Rit Rtt
where it = instrument temperature
tt = sample or adsorption testing temperature
VA = reference volume
Vit = volume within the top portion of the sample cell and the
connecting lines, at temperature it
Vt = volume within the bottom portion of the empty sample cell, at
temperature tt
Vs = true volume of solid in the sample
R = gas constant
Pze = zero error of the pressure transducer used to measure Pi and Pf
(this correction is the transducer reading when the system is
evacuated)
N = moles of gas adsorbed on the sample at temperature tt and
adsorbate gas pressure P (= Pf - Pze).
After this initial adsorption data point has been obtained, adsorbate gas can be
transferred to or from the sample cell via the reference volume, to generate
additional data at different pressures along the adsorption or desorption isotherm.
This is accomplished by isolating the sample chamber, and then pressurizing or
evacuating the reference volume to establish a new Pi. The system will
equilibrate at a new Pf after valves 1 and 2 are opened, and the incremental
amount of gas adsorbed or desorbed is given by:

POROUS MATERIALS INC. • 17

 V V -V 
N n - N n-1 = (Pi,n - Pf,n ) - (Pf,n - Pf,n-1 ) it + tt s  [17]
VA
Rit  Rit Rtt 

where the subscripts n-1 and n denote any two consecutive data points. This
generalized equation reduces to equation [16] when n=1 (i.e. for the first data
point after the system has been evacuated), since Pf,0 = Pze = 0 and N0 = 0.

The system volumes VA, Vit, and Vtt are determined through calibration
tests (described below), while Vs can be calculated from the mass of the sample if
its true (absolute) density is known or can be measured via gas pycnometry. Gas
pycnometry is conveniently performed at room temperature prior to the
adsorption measurements. Although helium is recommended, other gases such as
nitrogen or krypton can be used for pycnometry since they behave nearly ideally
and are essentially non adsorbing at room temperature and low pressures. The
procedure is quite simple: the system is evacuated to a residual gas pressure Pr,
the reference volume is pressurized to Pi, and the isolation valves are opened to
allow the gas to equilibrate at Pf. The true volume of solid in the sample can then
be obtained from the following equation:
Pi - Pf
Vs = Vit + Vtt - VA [18]
Pf - Pr

POROUS MATERIALS INC. • 18

Calibration
Values for VA and VB (the volume in the connecting lines, as shown in
Figure 1) are included in the specifications for each instrument, and were
determined at PMI by conducting a calibration test with each of two empty
sample cells having different but known internal volumes. These tests were
carried out at room temperature using the same procedure as that employed for
gas pycnometry. The following equation applies to each of the two tests, with
different values for VC (empty sample cell volume) and the corresponding
pressures, so that VA and VB could be calculated:
(Pi - Pf )VA = (Pf - Pr )(VB + VC ) [19]

If desired, the user can repeat these tests to verify the instrument calibration.

Values for Vit and Vtt must be determined by the user for each sample cell
and adsorption temperature of interest. This calibration is performed prior to the
adsorption test, using an empty sample cell and the appropriate adsorbate gas.
With the sample cell at room temperature (it), the system is evacuated to
essentially zero pressure (Pze), the reference volume is pressurized to Pi, and the
isolation valves are opened to allow the gas to equilibrate at Pf,it. The empty
sample cell is then cooled or heated to the desired adsorption temperature (tt), and
the new equilibrated gas pressure Pf,tt is measured. Simultaneous solution of the
following equations yields the values for Vit and Vtt:
(P - P )V = (P
i f,it A f,it - Pze )(Vit + Vtt ) [20]

Vit Vtt
(P - P ) V
i f,tt
A
= (Pf,tt - Pze ) + [21]
it it tt

It is important to note that each set of values for Vit and Vtt applies to a specific
sample cell and adsorption temperature, and must be used accordingly. The
following equation may also be useful:
Vit + Vtt = VB + VC [22]

This provides a check on the sample cell calibration if VC is measured directly, as

by weighing the sample cell before and after it is filled with water. Note that the
actual formulas used in the programs differ somewhat as they take into account
that the room temperature may be different from the instrument temperature.

POROUS MATERIALS INC. • 19

Computer Hardware & Software Requirements
The Automated BET Sorptometer is operated via the mouse and keyboard
of the Personal Computer (henceforth referred to as PC) attached to your BET
Sorptometer. This PC also collects and analyzes the test data acquired during an
automated test. Menus are displayed on the PC's monitor to guide the user
through the various options available, such as during an automated test ; the user
is instructed when to provide input data (e.g. sample identification and weight),
and when to perform the necessary manual operations such as installing or
removing the sample cell and setting up the dewar flask or heating mantle to
control the adsorption temperature. The computer performs all valve operations in
the proper sequence, determines when equilibrium has been established, and
acquires the test data automatically. An information screen displays the
instrument status throughout the test. The computer also performs all calculations
necessary to reduce the raw data to the final results, which are presented in report
quality tables or graphs as specified by the user. The instrument can be operated
in manual mode via the mouse or from the PC's keyboard, which allows the user
to open and close the valves as desired.

With the implementation of the BETWIN Software System, the computer

requirements to control the BET Sorptometer have increased. The requirements
to run the new software system are as follows:
• Microsoft Windows 3.x & a Mouse (Serial or BUS)
• 2 Megabytes RAM
• Color VGA video (640 x 480 resolution)
• 2 Serial Ports for a Serial Mouse or 1 Serial Port and a BUS Mouse
• 1 Parallel Port

There are a large number of computers, either an IBM PC or compatible, that you
can choose from to run the software. The minimum system required to run the
BETWIN Software System is an 80286. This will slow down the speed of the
software considerably, but it is a valid system.

We recommend that you have at least a 80386sx-20 (the 20 stands for the
processor speed 20 MHz). This gives you more processing power and the
BETWIN Software System runs much faster.

POROUS MATERIALS INC. • 20

 The computer system we would suggest to you if you wish a system that
would perform well would be as follows:
• an IBM PC or compatible with an 80386DX-33
• 4 Megabytes RAM
• VGA video (640 x 480)
• 2 Serial Ports
• 1 Parallel Port

To further increase system performance you might wish to consider the following
options:
• a more powerful computer system (e.g., an 80486DX-50)
• a math co-processor (this should be matched to your computer system
and include: 80287, 80387sx, Wietek, etc.)
• more memory (the performance of Windows improves with an
increase in memory)
• a GUI Accelerator (Graphical User Interface) (these are new graphics
cards available to increase the speed of graphics display)
All of the above items will increase your computer's interaction with Windows,
thus increasing the speed at which your software runs.

POROUS MATERIALS INC. • 21

OPERATING PROCEDURE

Note regarding pressure units:

Throughout the rest of this manual it will be assumed that your BET
Sorptometer software has been set up to use PSIA as the default pressure units.
The user may change the pressure units used. This process will be explained later
in the manual.

POROUS MATERIALS INC. • 22

Start Up
The following start up procedure must be completed before any tests can
be performed with the Automated BET Sorptometer. During periods of heavy use,
the instrument and vacuum pump should not be shut down; instead, they should
be left in a standby status that corresponds to the completion of this start up
procedure. Tests can then be performed much more quickly.
A1. Connect a source of compressed gas(ses) (to be used as the adsorbate or
for pycnometry) to the gas inlet(s) on the side of the instrument. This gas
must be clean, dry, and non-corrosive, and the pressure at which it is
supplied to the instrument should be regulated at approximately 25 psia
(10 psig). More than one gas can be connected at one time. The gas
connected to gas inlet A (the top one) will be used for sample volume
measurement and for bringing the system back to atmospheric pressure at
the end of the test. (Normally this would be Nitrogen.) If a different gas
is to be used for either pre-treatment or for performing the actual test,
connect this gas to inlet B (the second one from the top). Inlet C is
normally reserved for the P0 tube, which is used to determine the actual
P0 pressure of the gas being used before the actual test is run. If it is not
being used, a third gas may be connected to inlet C (the third down from
the top and directly above the vacuum connector). If the optional
continuous P0 system is installed, inlet C will never be used for the P0
tube and can be used for a third gas while still determining the actual P0
pressure.
A2. Use a vacuum hose to connect the vacuum pump to the vacuum fitting
(nipple) on the side of the instrument. A suitable trap can be placed in
this vacuum line to prevent pump oil from entering the instrument in case
of misoperation or pump malfunction.
A3. Make the appropriate electrical connections (see Figure 2) between the
instrument and the IBM-PC controlling computer and peripherals
(computer monitor, instrument status display, and graphics printer).
A4. Plug the power cords for the instrument, vacuum pump, computer,
monitor, display, and printer into 120 VAC (60 Hz) outlets. (Note: some
instruments are designed to operate at 240 VAC and should be connected
to appropriate power source.)
A5. Turn on the vacuum pump.
A6. Turn on the instrument and the instrument status display. After several
seconds, the display should show that valves 1, 2, and 3 are closed and
that valves 4, 5 and 7 are open (so that the reference volume can be
evacuated). On multi-chamber instruments, the valves should be in this
position on all chambers.

POROUS MATERIALS INC. • 23

 After the start up procedure has been completed, commence with the appropriate
test procedure as described below. Note, however, that before adsorption
measurements are made, the reference volume should be evacuated to within one
count of the zero point of the lowest gauge. It may be necessary to leave the
system overnight to accomplish this after a long shutdown.

POROUS MATERIALS INC. • 24

Automated Tests
The Automated BET Sorptometer is operated via the keyboard or mouse
of the controlling computer, even when the instrument is controlled manually.
The test procedure is as follows:
B1. Complete the start up procedure (steps A1 through A7). Make sure that
the appropriate gas is supplied to the instrument.
B2. Turn on the printer, computer, and monitor. If your computer is set up to
enter Windows and the BETWIN Software System automatically, simply
wait for the computer to boot up and start the necessary programs.
If your computer system presents you with a C:\ > or similar prompt type
'win' and press ENTER. This starts the Windows operating system. If
Windows does not start or has not yet been installed on you computer
please see your Windows manual on the proper steps to install the
Windows software.
If the BETWIN Software System does not start automatically upon
entering Windows, double clicking on the BETWIN icon that appears on
the Windows Program Manager screen will start BETWIN. If the
BETWIN Software System does not appear on you screen please see the
section entitled BETWIN Software Installation below. The instructions
within that section explain how to install BETWIN on you computer.
B3. Follow the instructions that appear on the computer monitor, and enter the
appropriate data and menu selections via the keyboard or mouse. The user
will be guided through the test that is selected, and will be instructed when
to perform the necessary manual operations such as installing or removing
the sample cell and setting up the Dewar flask or heating mantle (these
procedures are given in the following sections). The instrument status
display indicates whether each valve is open or closed and shows the
system pressure from two different gauges, one marked P and one marked
V (P is for high pressure, V is for near vacuum), and heating mantle
temperature (in C), throughout the test. The different versions of the BET
Sorptometer hardware a varying number of valves which are numbered
from 1 to 9 and V (valve V is present in version 5.2 and later machines),
the pressure gauge P and the vacuum gauge V. If the optional continuous
P0 system is installed, there will be another valve labeled P0 and another P
gauge.
B4. After the test has been completed, select the desired report format from the
menus on the computer monitor.
The instrument can also be controlled manually, if desired, by selecting
that option from the main menu or by putting an automated test in hold mode (by
entering an H from the keyboard or clicking on the HOLD button) and then
entering an M from the keyboard or clicking on the Manual Mode button. While
in hold mode you may also abort the automated test by entering an A or clicking

POROUS MATERIALS INC. • 25

 on the Abort Test button, leave hold mode and continue with the test by pressing
R or clicking on Resume, control the dewar lifter by pressing L or clicking the
Move Lifter button, or turn the test around (end adsorption and begin desorption)
by pressing T or clicking on the Turn Around button. These steps will be further
described in the section on the automated test and manual control procedures.

POROUS MATERIALS INC. • 26

Installation/Removal of Sample Cell
The procedure for installing a sample cell at the start of a test is as follows:
(Duplicate this for each chamber on a multi-chamber system)
C1. Weigh the empty sample cell (which must be clean and dry), place the
sample in the cell, and then measure their combined weight. The
difference between these measurements is the initial weight of the sample.
(The easiest way to do this is with a digital electronic balance. Put the
empty chamber in the balance, record the empty weight, zero the balance,
add the sample, and read the weight of the sample. The empty weight is
necessary if you want to determine the final sample weight after the test is
over.)
C2. Make sure that a filter is inserted into each of the two sample cell fittings
on the instrument.
C3. Clean the O-ring contacts with a Q-tip.
C4. Lightly coat two O-rings with vacuum grease. Use the clamps provided to
fasten the sample cell (containing the sample) and the O-rings onto the
appropriate fittings on the instrument.

After the test, the final sample weight can be determined by re-weighing
the sample cell immediately after removing it from the instrument (the initial and
final sample weights may differ somewhat, due to the removal of moisture and
adsorbed gases during pretreatment). The gas pressure within the sample cell
should always be adjusted to essentially atmospheric pressure before attempting
to remove the cell from the instrument. This is done automatically by the
computer at the end of any automated test.

POROUS MATERIALS INC. • 27

Installation/Removal of Dewar Flask
The Dewar flask is used in conjunction with a liquid coolant (usually
liquid nitrogen) during low-temperature adsorption measurements and the
corresponding calibration tests. The procedure for setting up the Dewar flask is as
follows:
D1. Fill the Dewar flask with coolant. Make sure that the Dewar jack is in its
full down position. Hold the Dewar at an angle and position it so that the
sample chamber and the two temperature probes go inside the flask. Be
careful not to put any pressure on the sample chamber. Raise the Dewar
around the sample chamber and turn it fully upright. Lower the Dewar
onto the jack.
D2. If you are controlling the instrument manually, you can control the dewar
lifter using the Dewar Lifter Control section of the Manual Control
Screen. If your BET Sorptometer is a version 3.1 or 3.0, make sure that
the AC is turned OFF and that the MODE is set to COLD.

The sample cell should always be evacuated before removing the Dewar
flask after the test, to prevent the potential buildup of pressure due to desorption
of gas from the sample as it warms to room temperature. This is done
automatically by the computer at the end of any automated test.

POROUS MATERIALS INC. • 28

Installation/Removal of Heating Mantle
The heating mantle is used during sample pretreatment, and for
high-temperature adsorption measurements and the corresponding calibration
tests. We have recently begun using a new style of heating mantle. The
instructions below include the procedures for both the old (E1a & E2a) and new
(E1b & E2b) style heating mantles.
E1a. Carefully position the heating mantle around the bottom portion of the
sample cell and then slide the manually adjustable lab jack underneath to
support the heater. Make sure that the lower temperature probe is inside
the mantle, next to the bottom of the sample cell. The bottom of the
sample cell should not be touching the bottom of the mantle. If it is, lower
the mantle slightly to provide a gap between the mantle and the bottom of
the sample cell. The sides of the mantle must completely cover the section
of the sample cell that contains the sample.
E1b. Make sure the Dewar Lifter is at its lowest point. Place the heating mantle
on the lifter making sure to line the oval in the top of the heater insulation
with the sample chamber. If this is not done, the sample chamber and
heater could become wedged together and break the sample chamber.
E2a. Plug the heater into the appropriate outlet on the instrument. Note that
each chamber of a multi-chamber instrument has its own heater outlet.
The outlet is located on the top inside panel behind the connections for the
sample chamber. Carefully place two pieces of insulation over the heating
mantle and around the sample cell.
E2b. Raise dewar lifter until the top of the insulation is above the area of the
sample chamber that contains the sample. Stop the lifter and install the
two halves of the heater cover. The cover halves have two semi-circular
notches and a long groove in them. The long groove is for the temperature
probe, and the two notches coincide with the sample chamber tubes.
E3. Specify the desired sample temperature (between room temperature and
300°C), to be maintained by the heating mantle and temperature controller,
at the proper line of the test setup list.

POROUS MATERIALS INC. • 29

DO's and DON'Ts
F1. Don't install the instrument near "noisy" electrical equipment, or where
there is excessive vibration, dusty or smoky air, or extreme temperature
changes (such as near a heater or outside doorway).
F2. Never use the instrument without filters in the sample cell fittings.
Replace the filters if they become clogged or dirty.
F3. Use vacuum grease sparingly on the O-rings, which should then appear
glossy but not sticky. Make sure you use only high vacuum grease.
F4. Don't overfill the sample cell, or it will not be possible to surround the
entire sample with the heating mantle or liquid-nitrogen bath. There must
be a clear passage connecting the two side tubes of the sample cell so that
gas can flow over the sample.
F5. Don't over tighten the sample cell clamps, which should only be finger
tight.
F6. When operating the instrument in manual mode:
(a) Always open the isolation valves (valves 1 and 2) by opening valve
1 first, since the in-line metering valve will prevent ellutriation of
powder samples. After the initial gas surge has subsided, valve 2
can be opened.
(b) Always evacuate the sample cell before removing the liquid-nitrogen
bath (Dewar flask), to prevent a potential buildup of pressure.
(c) Always adjust the gas pressure within the sample cell to essentially
atmospheric pressure before attempting to remove the cell from the
instrument.
(d) Never leave the heating mantle turned on (AC on in HOT mode)
when the instrument is unattended.
F7. Never turn the vacuum pump off without first disconnecting it from the
instrument.
(As an alternative, you can turn the vacuum pump off when valves 1, 2, 4,
and 5 are open and the sample chamber is removed from the instrument.
This will vent the vacuum pump to the atmosphere. When the pump has
shut down, and is no longer drawing air, you can close the valves.)

POROUS MATERIALS INC. • 30

BETWIN SOFTWARE SYSTEM

Introduction
The BETWIN Software System was developed by Porous Materials, Inc.
in response to an increasing number of requests for a software package that would
run under the Microsoft Windows 3.x environment. For a more detailed
description of the requirements needed to make use of BETWIN please see the
section of this manual entitled Computer Hardware and Software
Requirements.

The following portion of this manual describes the various functions of the
BETWIN Software System and how to make use of them. This information is
also available from within the BETWIN Software System by using the Help
menu or buttons found on many of the screens within BETWIN.

POROUS MATERIALS INC. • 31

Main Menu Screen

The above image is a copy of the Main Screen for the BETWIN Software
System. It displays information on the current user, default gas, and default units,
as well as the menu bar that controls the software system itself.

Each item along the menu bar (File, Execute, Report, Modify, Setup,
Help) when activated displays a menu of further options which control the BET
Sorptometer, report on collected data, modify testing parameters, etc. These
menus will be explained in detail below.

POROUS MATERIALS INC. • 32

File Menu
This menu contains options that allow you to customize the system for use
by multiple users. This feature allows the BET Sorptometer to be used by more
than one person, with each person having a different setup (gas, output units,
automatic test options, etc.).

Select User

Using the Select User option, you may switch between existing users'
settings. For more information regarding what a user is, please see New User
below.

The Select User option gives you a list of all existing users and asks you
to select one of these to attain a list of system defaults.

The two buttons also located on the form are:

CANCEL - leaves Select User without changing the current user.
CONTINUE - changes the current user to the one highlighted on the list
above.

POROUS MATERIALS INC. • 33

 New User

The BETWIN software system now supports multiple users, each one
capable of setting some of the machine parameters to deal with the type of test
they wish to run. This saves setup time and effort when a different user wishes to
run a test.
The computer stores the default directories, top temperature, the settings
of the last test run by that user, etc. for each user.
When creating a new user you are asked to enter a name by which the
system may identify this person (the name must be eight letters or less). This
name is used to create a sub-directory within the USERS directory (i.e. if you
entered the name SAM and your BETWIN directory was C:\BETWIN the
computer would create the directory C:\BETWIN\USERS\SAM). The computer
then copies the needed default files into the new user's directory.
You are also asked to select which of the defined gasses you wish to use
as this user's default gas. The gasses you have to select from are stored in the
GASSES sub-directory of your BETWIN directory. Any gas supplied with the
BETWIN Software system, or created using the utility Create a New Gas, and
stored within the GASSES sub-directory is available for selection as your default
gas.
Finally you are asked to select the units you wish your pressure values to
be displayed in. The three most often used pressure units are Torr, PSIA, and
kiloPascals.
There are also three buttons at the bottom of the New User form. They
are:
CANCEL - this aborts the user creation process.

POROUS MATERIALS INC. • 34

 CONTINUE - when you have entered the user's name, default gas, and
pressure units, pressing Continue will set the system up for
the new user.
HELP - calls the help facility and displays the information you are
currently reading.

POROUS MATERIALS INC. • 35

 Select Gas

This option allows you to change the default gas for the current user.
Because different gasses have different characteristics, this may affect the options
available on other forms (i.e. the Automatic Test).

You are asked to select the name of the gas you wish to use from the
supplied list (these gas files are stored in the GASSES sub-directory within your
BETWIN directory). This gas will be the one used by the system for tests and
calibrations unless changed before the test starts or you again change the default
gas.

The two buttons at the bottom of the form are:

CANCEL - leaves Select Gas without changing the system's default
gas
CONTINUE - change the default gas to the gas you selected from the list.

POROUS MATERIALS INC. • 36

 Select Units

The Select Units option allows you to select a different unit of pressure.
The selected unit of measure (i.e., PSIA, Torr, etc.) is used to display pressure
values. For more information on what these units mean please see the section
entitled Pressure Units.

The form itself consists of a list box and two buttons. The list box allows
you to select from any of the previously created pressure units. To select a unit
highlight the pressure units you wish to use by clicking on that unit name.

The two buttons perform the following tasks:

Continue - makes the selected pressure unit active and returns control
to the main screen.
Cancel - returns control to the main screen without changing the active
pressure unit.

POROUS MATERIALS INC. • 37

 Exit

This option, when selected, exits the BETWIN Software System and
returns control to the Microsoft Windows 3.x environment.

When this option is selected, the user is presented with the above form to
confirm the fact that he/she wishes to leave the BETWIN Software System.

POROUS MATERIALS INC. • 38

Execute Menu
The Execute menu contains the options that directly control the BET
Sorptometer. These options allow you to run an automated test, control the
instrument manually, or calibrate various portions of the instrument.

Automated Test

An automated test is used to gather data on a sample which you wish to

test. It requires that you have a previously calibrated sample chamber into which
to place the sample. If you have not yet done an Instrument Calibration on a
new instrument and/or a Sample Chamber Calibration on a new sample
chamber, so that the chamber you will be using is calibrated correctly, you will
not get accurate results.

If you have a previously calibrated sample chamber you may proceed.

The Automatic Test Settings screen is the screen that appears when
Automated Test is selected from the Execute Menu unless there is currently no

POROUS MATERIALS INC. • 39

 information on the last test run using the default gas. If this is the case, the
system switches to the Advanced Settings screen and you are asked to select the
test options that you wish run.

The sample screen above differs from the actual screen for a single
chamber BET. The box near the top which indicates the testing unit for which the
settings are being displayed is not normally present on a single chamber BET. It
is visible in the form above for display purposes.

The Automatic Test Settings screen allows the user to run a test using the
previously selected options with a minimum of input. The information requested
is as follows:
The following information is for sample chamber -
This frame is visible only on multiple unit BET's. The numbers
visible coincide with the testing units on the BET. If the circle
beside a given number is displayed with a dot in it as in the
example above the information being displayed is for that unit. To
switch units simply click on the desired unit number.
Weight of Sample (gm) -
The weight of the sample to be tested is entered here. The weight
displayed when the form is first displayed is that of the last sample
on that unit.
Sample ID -
This field contains the ID of the previous sample that was tested on
this unit. It allows you to identify individual samples by giving
them unique ID's.

The section below this consists of a series of command buttons and a

display of what the current setting for the Output Data File. The Change
Output Data File Name button calls the File Selector so that you may enter a
new file name to which BETWIN will store the data attained during the test. The
other buttons perform the following tasks:
Advanced Settings - unloads the Automatic Test Settings screen and
displays the Advanced Settings Screen. For more
information on the Advanced Settings screen please
see the following section.
Start Test(s) - clicking on Start Test(s) switches you to the Test
Status screen which allows you to keep track of what
the test running on each unit is doing. If there is a
problem with the setup for the test(s), the Advanced

POROUS MATERIALS INC. • 40

 Settings screen will be loaded so that you may correct
it.
Cancel - ends the Automated Test without performing a test.
Help - calls the BETWIN Help System and displays
information on the Automatic Test Settings screen.

POROUS MATERIALS INC. • 41

 Advanced Settings

The black bar in the center of the screen divides the information displayed
into that which deals with individual test units and that which deals with all tests.
The information above the bar, which selects which unit you are working with,
deals with the entire unit. These include Instrument Temperature, Room
Temperature, whether you wish to calibrate the instruments gauges before
proceeding with the test, etc.

The information below the bar deals with the unit you are currently
working with. This information includes the sample chamber data file, the name
of the file you wish to use to store test data, whether or not you wish to take
intermediate data points, etc.

The exact options available to you depend upon the version number of
your BET Sorptometer and the gas you are using to run the test. Listed below are
all the options available when running an Automatic Test.

The following options affect the test on all units (for multiple unit
systems):
Instrument Temperature -
This is the internal temperature of the BET Sorptometer.

POROUS MATERIALS INC. • 42

 Room Temperature -
The current temperature of the room the BET Sorptometer is
located in.
P0 Value -
The contents of this frame depend on the type of gas being used. If
the gas is capable of calculating pore size, the frame will list the P0
value of the gas, otherwise it will display information on Surface
Area Factor. When set to AUTO, the P0 value will be determined
through the use of the P0 tube connected to gas inlet C. If you
have the optional continuous P0 system installed, P0
measurements will be made through the P0 inlet, and not through
gas inlet C. With this optional system, there will also be a third
setting to this line, CONTINUOUS, that will calculate the P0 value
at the beginning of the test, just like AUTO, but will also re-check
the P0 value before taking each data point.
Calibrate Gauges -
If you wish to re-calibrate the pressure gauges before you start the
test select Yes. If you wish to use the current calibration
information select No. If your system contains the optional
continuous P0 system, and you selected either Auto or Continuous
P0 calculations, AND you select Yes to re-calibrate the pressure
gauges, then the P0 gauge will also be re-calibrated right before
using it to measure the P0 value.
Outgassing Time -
This is the time that the sample will be held under vacuum at the
outgassing temperature. The time will start when all the samples
are at their outgassing temperature.
Pre-treatment Gas -
When you double click on this box the program will display the
File Selector so that you may select from the available gasses.
The default directory will be the one that was last used to attain a
gas file. The gas you select will be used in the pre-treatment
process.
Main Das- (Pre-treatment Gas Valve)
This allows you to select which gas valve is connected to the
pretreatment gas.
Test Gas – (Gas Inlet Valve)
The gas valve which is connected to the gas to be used for the test
itself.

POROUS MATERIALS INC. • 43

 The black frame near the center of the screen controls which unit you are
setting the test options for. If your BET Sorptometer is a multiple unit machine,
simply click on the proper unit number to set up a test for that unit. If you have a
multiple unit machine and do not make changes to the test information for any but
the first unit, the program will use the settings for the last test for the other units.
The following options affect individual units of the BET Sorptometer:
Sample Chamber Data File -
The file listed in this box contains the information on a sample
chamber. To change sample chambers double click on the box.
This will bring up the File Selector so that you may choose the
data file on the sample chamber you are using to run this test.
Weight of Sample -
How much does the sample you are testing weigh before the test?
Outgassing Temperature -
At what temperature do you wish to outgas the sample? The BET
Sorptometer will first attempt to reach the outgassing temperature
then wait for the amount of time given in Outgassing Time.
Testing Temperature -
This is the temperature at which the test is run. If the gas you
selected is a COLD gas, then the testing temperature will always
be -195.76 and should not be changed. If you do give a different
temperature you must maintain that temperature manually during
the test.
Pore Volume -
If you select Yes, your report will calculate the pore volume from
the isotherm data. If the gas is not capable of generating this result,
this option will not be visible.
Density of Sample -
This option allows you to enter the known density of a sample or
to determine the density automatically. When the AUTO option is
selected, the density of the sample will be determined before the
test begins by performing gas pycnometry on the sample using the
gas at inlet A. If the density of the sample is already known, select
the other option button and enter the density into the box provided.
Take Intermediate Data Readings -
This setting determines how the test is to treat intermediate data
points. The testing procedure tries to reach target pressure values
listed in the controlling files by bringing in just the right amount of

POROUS MATERIALS INC. • 44

 gas as a PI value. If the sample adsorbs or desorbs more than
anticipated, then the PF value will fall too low (or too high for
desorption). If this line is set to Yes, then the program will wait
for the PF level to reach equilibrium, take a reading, and then try
once again to reach the target PF value. If this line is set to No,
then if it is determined that PF will not be reached, and the
minimum level of equilibrium has been reached, the isolation
valves will be closed, and another dose of gas brought in to try to
reach the target PF. No reading will be stored to disk until the
target PF value is reached, and the PI value that will be paired with
this PF value will be a composite of the initial PI plus all the
additional doses of gas used to reach PF.
Multipoint Test -
A multipoint test is used to measure surface area using three or
more data points. These data points are determined using partial
pressures whose ranges depend upon the gas you are using.
If you are not using a gas that is capable of doing surface area
(Krypton, Nitrogen, etc.) this option will not appear on the screen.
Note that multipoint files use a different extension from isotherm
files, and that you can only select a file that was defined under the
control of the gas you are using. To define a new multipoint
control file use the New Multipoint List in the Setup menu on the
main screen.
The options available for a multipoint test are: Skip, Single Point,
Same as Ads., and Multipoint Control File. When set to Skip, the
multipoint test will not be performed. When set to Single Point, no
controlling file will be used for the surface area section of the test,
and a single point of .25 P/P0 will be used. To perform a single
point test with a value other than .25, create a multipoint file that
contains only one point. When set to Same as Adsorption, the test
control program will use the same isotherm file that will be used
by the adsorption test. If the last option, Multipoint Control File, is
selected the multipoint test section will use the partial pressure list
defined in the selected file. To change the selected file, simply
double click on the box containing the file name (or blank box if
none was previously selected). This will call the File Selector and
allow you to select a multipoint control file to use during the test.
If the box was blank when you selected this option, the File
Selector will automatically be called.
Adsorption Test -
The adsorption test determines the amount of gas adsorbed by a
sample at increasing pressures. When you do run an adsorption
test you must have an isotherm list to control the test. If you do
not have one available that fits your needs you can create one by

POROUS MATERIALS INC. • 45

 using the New Isotherm List command which is under the Setup
menu item on the main screen.
You are given two options in the adsorption test section. You may
either Skip the adsorption test or select an Adsorption Control File.
If you select Skip, the test control program will not do an
adsorption test on the sample. If you select Adsorption Control
File, the control program will use the isotherm list you select to run
the adsorption test. If you wish to use a different adsorption
control file simply double click the box containing the file name.
This will call the File Selector which allows you to choose a
different isotherm file. If the adsorption control file field is blank
when you select this option it will automatically call the File
Selector.
Desorption Test -
The desorption test determines the amount of gas adsorbed by a
sample at decreasing pressures. When you do run a desorption test
you must have an isotherm list to control the test. If you do not
have one available that fits your needs you can create one by using
the New Isotherm List command which is under the Setup menu
item on the main screen.
The options available for a desorption test are: Skip, Same as
Adsorption, and Desorption Control File. If Skip is selected the
program will not run a desorption test. If Same as Adsorption is
selected and the adsorption test is set to skip, the control program
will skip the desorption test as well. If, however, you have
selected an isotherm for the adsorption test the control program
will use the same file as the adsorption test, but in reverse order. If
you wish to run a desorption that is different from the adsorption or
only run a desorption, you would select the final option which is
for the Desorption Control File. If the file name box is blank, it
will automatically call the File Selector so that you can select a
desorption isotherm. If there is a file listed in the box but you wish
to use a different isotherm, simply double click on the box to call
the File Selector to select a different isotherm.
Pre-treatment File -
The pretreatment section allows you to run a series of predefined
commands including evacuate, wait for specific vacuum, flow gas,
heat, and wait for a given amount of time. To define a
pretreatment file you would select the New Pretreatment File
option under the Setup menu on the main screen. (i.e. this allows
you to define an outgassing protocol that increases the temperature
over a given amount of time)

POROUS MATERIALS INC. • 46

 The two options you are given are Skip or pretreatment control file.
If you select Skip, the control program will skip the pretreatment
section even if a pretreatment gas was selected. If you select a
pretreatment control file the control program will run a
pretreatment of your sample based on the instructions stored in that
file. If no pretreatment control file name is currently displayed and
you select the later option, the program will automatically call the
File Selector so that you may select an existing pretreatment file.
If there is a file name displayed but you wish to use an different
file, simply double click on the box containing the file name. This
will also call the file selector and allow you to choose an different
file.
Estimated Surface Area -
This value is used only if you are doing a Multipoint Test. It is
used to control gas flow during the test. If you have no idea what
the surface area of your sample is, enter a 1.
Output File -
Double clicking on this box allows you to enter the name of the
file you wish to store the data from the test in. To do this it calls
the File Selector. Using the file selector you select the drive and
directory you wish to store the data file in and enter a new name or
select an existing file to replace it.
Sample ID, Line 1, and Line 2 -
These three lines contain user entered text that will be printed on
the report. The first line contains the sample ID. The next two
lines contain any information you choose, such as company name
and purchase order number.

You must have at least one of the three tests (adsorption, desorption, or
multipoint) set to a valid file for at least one of the sample chambers. Setting
them all to SKIP for all of the sample chambers will generate an error message
when you try to leave this screen.

The four command buttons in the lower right corner of the screen are used
for the following:
START TEST(s) -
When you are done setting up your test(s), clicking on Start
Test(s) switches you to the Test Status screen which allows you to
keep track of what the test running on each unit is doing.
RESET -

POROUS MATERIALS INC. • 47

 This button resets the values of the test options (settings below unit
bar), for the unit you are working on, to the settings they had when
you started the Automatic Test.
HELP -
This command calls the help system you are currently using and
sets the subject to this section of help.
CANCEL -
This button will cancel the automatic test.
For further information on the procedures involved in the actual test please
see the information on the Test Status screen.

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 Test Status Screen

The Test Status screen keeps you informed of what the test is doing at any
given point. The exact appearance of the screen depends upon how many testing
units your system has. There will be one column of information for each of the
units your BET Sorptometer has (i.e. 1-6).
To control the test there are a several command buttons located on the
screen. The major buttons are located along the bottom edge of the screen and
along the left edge. When the Test Status screen is loaded only two of these six
buttons will be active. The two are the BEGIN and HELP buttons. The others
will be inactive and the captions on them will be at half intensity and will remain
so unless you enter HOLD mode. There are also two other buttons located in the
left side of the screen, which, depending upon what version of machine you have
and whether or not you have a diffusion or turbo pump, may not be visible. The
following is a list of the these buttons and their functions:
BEGIN -
This button starts the actual test program using the options you set
earlier using the Automated Test Control Screen. This button is
the default button when the screen loads so that you only need to

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 press RETURN, the Space Bar, or click on the BEGIN button to
start the test. Once it is pressed this button becomes the HOLD
button.
HOLD -
This button causes the system to go into hold mode. This also
activates the other four buttons that are along the bottom of the
screen. It pauses the test at the point you have reached so that you
may use one of the other four functions called by Move Lifter,
Manual Control, Turn Around, and Abort Test. When you
enter hold mode this button becomes the RESUME button.
RESUME -
This button returns the test from hold mode to the point where the
test was placed in hold mode and resumes the test at that point.
The caption of this button is then changed to HOLD. It also
deactivates the control buttons listed above in HOLD.
Move Lifter -
This function allows you to control the lifters for each unit on your
machine. For more information see the section on Dewar Lifter
Control.
Manual Control -
This brings up the Manual Control Screen and allows you to
perform a variety of tasks.
Turn Around -
This is used to force a test that is doing adsorption to take the point
it is currently working towards and then start doing desorption. If
a desorption test was not set for that unit it will end the test for that
unit. For more information see Turn Around Screen.
Abort Test -
Aborts the test in one of two ways. If no data points have been
taken yet it will simply abort the test and leave the automated test
program. If data points have been taken, however, it will finish
taking the current data point then end the test. This will give you a
usable data file up to the point where you aborted the test.
HELP -
Starts the BETWIN Help System and displays information on the
Test Status Screen.
Cancel Wait -
Allows you bypass certain periods when it is required that you wait
a given period of time (i.e. the wait for maximum vacuum, the ten

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 minute wait when the sample has been immersed in liquid nitrogen,
etc.)
Evac. Fast -
This button only appears when the sample chamber is being
evacuated at the start of a test. When that section of the test is
complete the button will be deactivated and will no longer be
visible on the screen.
Diff. Pump Off / T. Pump Off – (Option for EL model))
This button turns the diffusion or turbo pump off earlier than
required by the program. If your BET Sorptometer is not equipped
with a diffusion pump or a turbo pump this button will not appear
on the screen.
Unit x - (Option for multi chamber)
These buttons located along the top of the form these buttons serve
a dual purpose. It's main purpose is as a label for each of the
columns of test information. During one of the tests (adsorption,
etc.), however, clicking on that button will cancel the stability wait
for that unit. The x in the heading is replaced with the unit number.
The following information is displayed during the course of the test as the
information changes:
Elapsed Time -
This is the amount of time that has past since you began the
automated test.
Current Time -
The current time according to your computer's internal clock.
Normal Stability Time -
The amount of time in seconds it normally takes for the BET
Sorptometer to stabilize for the particular section of the test you
are currently in.
Minimum Stability Time -
The program will wait for this amount of time before testing to see
if a point is within the proper bounds during a test for stability. If
the point is within the proper range it will continue the wait,
otherwise it will give you an out of bounds message and retry the
reading.
Stability Lower Limit -

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 The lower bound of a stability test. Depending upon which
direction a test is going (adsorption or desorption) the number
displayed will either be a -9999 or the specific limit.
Stability Upper Limit -
The upper limit of a stability test. Depending upon which direction
a test is going (adsorption or desorption) the number displayed will
be either 9999 or the specific limit.
Stability Time -
This field is used as the timer for all waits and stability tests.
Stability Pressure -
If the program is waiting for a stable pressure (i.e. when it is
getting maximum vacuum) the pressure that it has reached will be
displayed here.
Stability Status -
A variety of messages are printed here to inform you as to what the
unit is doing (i.e. waiting, out of bounds, take point, etc.).
PF Target -
The pressure value that is the PF that the program is trying to reach
for this particular point.
Minimum PI -
The minimum pressure value the program will accept as a valid PI
for the current data point.
Maximum PI -
The maximum pressure value the program will accept as a valid PI
for the current data point.
Last PI -
The last valid PI value the program attained.
Total Adjusted PI -
The total pressure used to reach the current PI value when the
system requires multiple doses of gas to reach the proper PI value.
PI of Last Point -
This is the PI value stored in the data file for the last point taken.
PF of Last Point -
This is the PF value stored in the data file for the last point taken.
Surface Area so Far -

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 This the surface area of the sample as calculated to the current
point in the test.
Units' Current Status -
This field contains abbreviated messages about what each of the
units is doing at the present moment. (i.e. Wait Temp [waiting for
temperature], Calc PF [calculate the target PF value], etc.)
All Units -
This field, as the name implies, deals with all units in a BET
Sorptometer. The messages here tell you what section of the test
the program is currently in.

For more information on the test procedures please see the next
section entitled Automated Test Description.

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 Automated Test Description
An Automated Test follows a set order to perform the tests and
procedures requested on the test setup screen. During the run of the test you may
be prompted to do additional tasks such as install the dewar, refill the dewar, etc.
These tasks take place at a variety of times depending upon the options you
selected for the test. The order in which the main tasks are performed is as
follows:
1. You are prompted to prepare everything, install the sample chamber(s),
heater(s), and P0 tube (only if there is an optional P0 system installed).
This gives you the opportunity to make sure that the proper gas(ses) are
attached to the appropriate inlets, in addition to installing the sample
chamber(s), heater(s), and P0 tube.
2. The system makes sure all valves are in the proper position. While this is
being done the All Units message field informs you that the 'Setting up
BET Sorptometer for Automatic Test'.
3. If you have selected the option to Calibrate Gauges, the BET
Sorptometer will now go through the steps necessary to calibrate the
instrument.
4. If you have selected the Auto option from the Density of Sample the BET
Sorptometer will run Pycnometry on the sample.
5. If you have chosen to Pretreat your sample, the commands in the
pretreatment file you chose will now be performed.
6. Next the sample will be heated to the temperature you selected for the
Outgassing Temperature and evacuated until the vacuum stays stable for
five minutes. If the temperature you selected is equal to or less than room
temperature no heating will take place.
7. If your Outgassing Temperature is higher than your Testing
Temperature, the software will pause to allow the sample to cool before
it continues.
8. The program will now bring the sample to the proper testing temperature
and begin the Multipoint and Adsorption tests, if you have chosen to do
either or both of these.
9. When BETWIN has completed the Adsorption test it will run the
Desorption test if one was requested.
10. The sample chamber is brought to approximately atmospheric pressure,
then sealed off and the rest of the BET Sorptometer is evacuated.

POROUS MATERIALS INC. • 54

 11. You are asked to enter the weight of the sample after the test. You may
enter a 0 to use the weight entered before the test started for calculations.
12. The rest of the information for the data file is now written out and you are
returned to the main menu.

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 Manual Control

Manual Control allows you to control the various valves, heaters, lifters,
etc. without actually running a test. You may also get feed-back from the
instrument on the pressure reading from various gauges, position of the lifter,
temperature, etc.

There are separate sections for controls that affect individual testing units
and for those that affect the entire instrument.

Not all options are available on all machines, so there may be what appear
to be blank spots on the control screen. As an example, if you do not have a
diffusion pump as part of your system, the Diffusion Pump controls will not be
visible when you start manual control. In the case of valves that are not present in
your BET (i.e. Valve V which is present only in Version 5.2 and later machines),
they will appear as only half intensity and you will not be able to select them.
This is also true of the Unit Number section if your BET Sorptometer has less
than six units.

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 Topics which deal with each individual unit:
Unit Number -
Some BET Sorptometers have the ability to test more than one
sample at a time. Each testing section is assigned a unit number
to distinguish one unit from another. This allows you to work with
each unit separately.
Valve Control -
The Valve Control section allows you to control the valves that
deal with individual units (1-7, 9, and V). Using the commands
located in this frame you can select the valve you wish to move
and either open, close, or pulse the valve.
The exact valves you can control depend upon the version of BET
Sorptometer you are using. Prior to Version 3.3 you do not have
any valve numbers greater than 5. Version 3.3 and later machines
add valves 6 and 7. Version 5.2 and later machines add valves 9
and V to the list. If your BET Sorptometer does not support a
given valve, that valve will not be available as a valid selection.
After selecting a valve you are given a choice of three commands
to perform using that valve. You may:
OPEN - opens the selected valve and leaves it open.
PULSE - causes the selected valve to open then close.
The amount of time between the open and close
commands are controlled from the All Units
section using the Valve Timing command.
CLOSE - closes the selected valve.
Valve 8 -
This control will only appear for BET Sorptometers of Version 4.0
and later.
Valve 8 is a different style of valve from the others in the BET
Sorptometer. The other valves (1-7, 9 and V) are solenoid valves,
as opposed to valve 8, which is motorized.
Valve 8 is used to restrict the flow of gas from the back manifold
into the testing area, thus controlling how fast the gas is allowed to
enter. This gives you five options for controlling valve 8 instead
of the three options for the other valves. They are as follows:
Full Open - fully opens valve 8.
Pulse Open - opens valve 8 for the length of time
specified in the Valve Timing section of All
Units.

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 Stop - only active when you are performing a valve 8
full open or close. Stop will be the only
command active during either of the two
commands and will cause the system to stop
valve 8 where it is at the time.
Pulse Close - closes valve 8 for the length of time
specified in Valve Timing from the All Units
section.
Full Close - close valve 8 all the way. This still allows
some gas to pass but the flow is greatly
restricted.
Lifter Control -
This control frame will not be visible for all versions of the BET
Sorptometer.
The unit of dewar lifter you wish to control is selected from the
Unit Number section in the upper left corner of the Manual
Control screen.
If your machine is a Version 3.1 or earlier BET Sorptometer, this
frame does not appear when you start Manual Control. To move
the lifter for Version 3.1 and earlier machines use the direction
switch on the BET Sorptometer itself to control the lifter direction
and the AC Power controls to start and stop the dewar.
If your machine is Version 3.2 or later the frame is visible but the
exact appearance will differ. For BET Sorptometers of Version 3.2,
3.3, and 3.4, only the direction buttons are visible. Machines of
Version 4.0 and greater also add the speed controls.
The speed controls are:
1 Low speed (1/4 of full speed)
2 (1/3 of full speed)
3 (1/2 of full speed)
4 High speed (full speed)
You can change the speed at any time, even when the lifter is in
operation.
The direction buttons are fairly self explanatory. Pressing Up
causes the lifter to rise, Down causes it lower, and Stop causes it
to stop where it is.
Test Mode -
There are two buttons within this frame. They tell the BET
Sorptometer and BETWIN Software System which testing mode it
is in, either Hot or Cold.

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 The mode you are in also affects the temperature displays in the
Reading Information section. If you are in Hot mode the
temperatures are listed in degrees Celsius, if you are in Cold mode
the readings will be in degrees Kelvin.
AC Power -
This control is visible for all versions of the BET Sorptometer.
This control turns on and off the AC Power outlet in the testing
chamber in all versions. In versions prior to 3.2, however, it serves
a dual purpose. In BET Sorptometers prior to Version 3.2, the AC
outlet was also used to power the dewar lifter with the direction of
the lifter travel controlled by a switch mounted on the BET's
cabinet or in the sample chamber area.
BET Sorptometers of Version 3.2 and later use a separate Lifter
Control system.
Sample Temperature -
This control frame is visible for BET Sorptometers of Version 5.2
and later. It allows you to set a specific temperature for the
temperature controller for the sample chamber to reach.
To set the temperature, enter the temperature you want to reach
and maintain into the box provided and click on the Set button.
The temperature controller will then bring the sample to that
temperature and maintain it there until you set a new temperature
or turn the heater off.
Gas Inject -
Using the Gas Inject controls you are able reach a target pressure
using the gas of your choice.
To reach a desired pressure follow the steps listed below:
1. Select the gas inlet valve that contains the gas you wish to
use A, B, C, or None (None means you wish to use the gas
already in the back manifold).
2. Enter the Target Pressure you wish to reach within the
allowed range.
3. Press the GO button.
When you press GO the BET will begin pressurizing in an attempt
to reach the Target Pressure. During this attempt the only
command active in manual control will be Terminate.
The Terminate button is used to stop the Gas Inject routine before
it reaches the Target Pressure. If Terminate is pressed prior to
the Target Pressure being reached the system will stop
pressurizing at the point it has reached.

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 In either case, target pressure reached or use of the Terminate
button, or if the system itself determines that it cannot reach the
Target Pressure, the other commands available on the Manual
Control screen will be reactivated.
The following topics have a bearing on the instrument as a whole:
Gas Valve Control -
This control frame is similar to the Valve Control section in that it
allows you to control a series of valves. In this case it allows you
to control the gas and P0 Valves.
First select the valve with which you wish to work (A, B, C, or P0).
Valves A, B, and C are the gas inlet valves. The P0 valve is the
valve that isolates the P0 Section from the rest of the BET
Sorptometer.
After selecting the valve you wish to move you are given a choice
of three commands to perform using that valve. You may:
OPEN - opens the selected valve and leaves it open.
PULSE - causes the selected valve to open then close.
The amount of time between the open and close
commands are controlled from the All Units
section using the Valve Timing command.
CLOSE - closes the selected valve.
Top Temperature -
This control is supported in Version 3.1 and later BET
Sorptometers. It allows you to set and control the temperature
inside the BET itself.
To reach and maintain a desired temperature simply enter the
desired temperature into the provided box and press Set. This will
instruct the BET's internal computer to have the instrument reach
and maintain this temperature.
Valve Timing -
Valve timing is used to set the length time a valve stays open when
it is pulsed, in the case of most valves, or how long valve 8 runs
when it is pulsed.
To set a new pulse length simply enter a valid value into the
provided box (this value must be between 1 and 255) and press the
Set button within the Valve Timing frame. This informs the BET's
internal computer to set the valve pulse width to (entered value/60)
seconds. (i.e. if you enter a value of 10 your new pulse width will
be 1/6th of a second)
Diffusion/Turbo Pump -

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 This control will only be visible if your BET Sorptometer is
equipped with either a diffusion pump or a turbo pump.
You can determine whether or not your system has one and which
it is by looking at your BET Sorptometer version number. If your
version number is of the form X.X, you do not have either type of
pump and this control frame will not be visible on your Manual
Control screen. If the version number is in the form of X.X1, your
system is equipped with a diffusion pump. If you have a version
number that is of the form X.X2, you have a turbo pump installed
in your system.
The two buttons that are part of this control frame turn the
appropriate pump ON or OFF depending upon which of the two
buttons you press.
Cold Cathode Control -
This control is available only on Version 5.2 and later BET
Sorptometers. It is used to turn the Cold Cathode high vacuum
gauge ON and OFF, If you turn the gauge on at a pressure that
could damage the gauge the internal computer will automatically
shut it down until the pressure drops low enough.
Reading Information -
Allows you to attain feedback from various parts of the BET
Sorptometer system. The items from which you can attain
information depends upon the version of the BET Sorptometer you
are using. The following items are available for all versions:
Auto Pressure -
Using this option displays the current pressure using
the best pressure gauge. If the pressure drops or
rises to the point where a different gauge would be
better, it will switch the better gauge automatically.
It also informs you of which gauge it is currently
reading.
Pressure Low Range -
This listing displays the current pressure using the
low range of the pressure gauge.
Pressure High Range -
This listing displays the current pressure using the
high range of the pressure gauge.
Vacuum High Range -
When selected, this option displays the current
pressure using the high range of the vacuum gauge.

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 Vacuum Low Range -
This option displays the current pressure using the
low range of the vacuum gauge.
Probe Temperature -
This selection causes the system to read the
temperature from the sample chamber area probes.
Ground Reference -
This selection causes the system to read the voltage
of the internal ground reference (this should always
be 500 counts and 0 volts).
+2 Volt Reference -
This selection sets the system to display the voltage
of the internal +2 volt reference.
If your system has an optional P0 system installed you are also
given these choices:
P0 Low Range -
The system displays the current pressure of the P0
system using the low range of the P0 system's
pressure gauge.
P0 High Range -
The system displays the current pressure of the P0
section using the high range of the P0 system's
pressure gauge.
If your system is a Version 4.0 or greater you may also attain
information on the following:
Close Limit -
The close limit of valve 8, which is the lowest
position value normally attainable, is displayed.
Open Limit -
The open limit of valve 8, which is the highest
position value normally attainable, is displayed.
Valve Position -
This selection displays the current position of valve
8 in percentage open which is the inverse of the
flow restriction of the system (100% = no
restriction, 0% = full restriction but some gas will
still pass).
Lifter Position -

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 Displays the percentage of full height the lifter for
the currently active unit.
For Version 5.2 and later machines you also add the following
items to the list:
Cathode VAC. Low Range -
Reads the current pressure using the low range of
the Cold Cathode Gauge.
Cathode Vac. High Range -
Displays the current pressure using the high range
of the Cold Cathode Gauge
Top Temperature -
Informs you of the temperature of the upper section
of the BET Sorptometer itself.
The two buttons that are located within the Read Information
command frame control the output boxes. These two buttons are:
Begin -
This button starts the continuous reading desired
gauge or device and displays the value in counts in
the upper display box and the appropriate units or
percentage value in the lower box with the third box
containing the units used or a % sign.
Stop -
This button ends the reading of the desired gauge or
device so that another may be selected. This button
only becomes active when the Begin button is
pressed and is deactivated again when it is pressed.

The two buttons in the lower right hand corner of the Manual Control screen are:
QUIT - returns you to the portion of the program from which Manual
Control was called.
HELP - calls the Help system.

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 Calibrate Gauges

Before you can run a test or even calibrate the internal volumes of a
machine you must have accurate gauge readings. This routine resets the zero
points and cross-over points of the gauges so that the readings you attain from
them are accurate.

All the activity for this section takes place on one form. You are first
asked to select which testing unit(s) that you wish to calibrate. If your BET
Sorptometer has more than one unit you may calibrate as many as you wish by
clicking on the appropriate unit's number. (Example: If your BET Sorptometer
has three units and you wish to calibrate units one and three but not two, you
would select those two units leaving unit two's check box empty. During the
calibration process unit two would be ignored.)

You are also asked whether or not you wish to do an absolute calibration.
If you select YES you are also asked to enter the current atmospheric pressure.
This entered pressure is used to gain a more accurate calibration of the
instruments by using this pressure value as a set point to calibrate the gauges.
Absolute calibration also requires that there NOT be a sample chamber
installed on the unit(s) that are being calibrated.

This routine brings the instrument to two different target pressures

(slightly below 200 Torr and slightly below 2 Torr, which are the dividing lines
for the pressure and vacuum gauge), and brings the system to maximum vacuum.

POROUS MATERIALS INC. • 64

 If you asked for absolute calibration, the system will now open valves one
and two which usually seal off the sample chamber. This brings the system to
atmospheric pressure. This gives a more accurate calibration of the instrument's
gauges because it uses the atmospheric pressure you enter as a set point to
calibrate the gauges.

POROUS MATERIALS INC. • 65

 Calibrate Sample Chamber

Before you can run a test on a sample you must place that sample into a
sample chamber. To attain accurate results from that test you must calibrate that
sample chamber so that the computer knows the proper volumes for that chamber.
This routine is used to determine the correct volumes needed by the program to
run a test using a new sample chamber.

To calibrate a new sample chamber you need to have a sample chamber

data file from a previously calibrated chamber. The values from this file are used
to calculate the new chambers volumes.

This procedure uses two separate screens. The first is used to set up the
procedure (which unit to use, gas inlet valve, etc.). The second is a status form
that allows the user to keep track of what the machine is doing and also displays
the results of the calibration when completed.

To setup the calibration you need to select which unit you will be
calibrating the sample chamber on (you may only run one calibration at a time),
which gas inlet valve to use, the PI pressure for the gas you are using (only if the
gas doesn't have a P0 value), room temperature, the instrument temperature, and
whether you are using liquid nitrogen (for cold gas), and if you are using a hot gas
or not liquid nitrogen, what the testing temperature is.

When you click BEGIN the first form will be unloaded and the
Calibration Status Screen will appear.

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 Calibration Status Screen

This form is used with both Instrument Calibration and Sample

Chamber Calibration procedures. The form's appearance will differ depending
upon the procedure it was called from. The main difference is the inclusion of a
second column to display information on the second sample chamber after
calibration is complete when called from Sample Chamber Calibration.
When the Status Screen is loaded, click on the BEGIN button or press
the Spacebar or RETURN key to start the actual calibration.
The following is a brief description of each of the fields and their
meanings. The upper section of the screen is identical no matter which procedure
this routine was called from. In both the left and right corners at the top of the
form are two fields containing times. The field on the left is the time since the
calibration process began. The field on the right is the current time according to
your PC's clock. The text between these two clock fields informs you of which

POROUS MATERIALS INC. • 67

 unit on your machine is being used to run this calibration. The other fields within
this upper section are as follows:
Unit Status -
This box displays information on the current state of the instrument.
Stability Status -
This box displays information on the current state of the calibration
procedure.
Target Pressure & Stability Pressure -
Both of these boxes are used during various portions of the
calibration to display pressure values being read by the BET
Sorptometer or that you are attempting to reach.
Wait Time -
This box and heading is only visible during the wait periods for
maximum vacuum and the 10 minute wait for the chamber to cool
or heat to the target temperature.
Time to Wait for Stability -
This box displays the timer during stability tests.
The bottom portion of the form consists of a series of labels, either one or
two columns of information, and a series of buttons. The labels are always visible,
although the Volume label is disabled during a Sample Chamber Calibration.
There is always one column of fields that display information on the sample
chamber at the end of the calibration. During an Instrument Calibration, there
are two columns so that information on both chambers can be displayed
simultaneously. The information that is displayed is as follows:
PI -
This box contains the gas pressure (in the default pressure units)
within the internal plumbing of the machine when brought to initial
pressure.
PFit -
This box displays the pressure within the BET Sorptometer when
the sample chamber valves are opened after the PI pressure has
stabilized.
PFtt -
This box displays the internal pressure of the BET after the sample
chamber has been allowed to cool or heat to the desired
temperature and been allowed to stabilize there.

POROUS MATERIALS INC. • 68

 Maximum Vacuum -
The lowest pressure value attained while the system was being
evacuated prior to the original pressurization is displayed in this
box.
Volume -
The previously entered volumes of the two sample chambers are
displayed in these boxes for Instrument Calibration. This
information is not displayed for Sample Chamber Calibration.
VA -
This box contains the volume of the internal plumbing of the BET
Sorptometer (in version 5.2 and later machines this is the volume
with valve 10 open and valves 3 and 4 closed).
Vit -
This box displays the volume of the internal plumbing and the
sample chamber at room temperature.
Vtt -
This box displays the volume of the internal plumbing and the
sample chamber at testing temperature.
Instrument Temperature -
This box displays the temperature of the upper section of the BET
Sorptometer.
Testing Temperature -
This box displays the target temperature for the Calibration process
to reach and maintain before taking the PFtt reading.
Room Temperature -
This box displays the ambient room temperature.

There are also six buttons that appear on the form, one of which is not always
visible, another which is used for four separate purposes. The buttons and their
meanings are as follows:
BEGIN - starts the actual calibration process. Once you have
clicked on BEGIN the caption for this button changes to
Hold.
Hold - places the BET Sorptometer into hold mode. This
pauses the calibration process, enables the Move Lifter,
Manual Control, and Abort Calibration buttons, and
changes the caption for this button to Resume.

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 Resume - restarts the calibration process at the point where it was
placed into hold mode. This deactivates the three
buttons that were activated when Hold was pressed. It
also switches the caption for this button back to Hold.
EXIT - displayed only after the calibration process is complete,
this is the same button as used by the above three
commands. Returns you to the calibration setup screen.
Move Lifter - only active when the BET Sorptometer is in Hold Mode,
this button calls the Dewar Lifter Control screen.
Manual Control - calls the Manual Control screen so that you may
make changes to the instrument. It is only active while
in Hold Mode.
Abort Calibration - like the previous two, this button is only valid while
the BET is in Hold Mode. It is used to prematurely end
the calibration process without storing the calibration
data to disk.
Cancel Wait - can be used during the wait for maximum vacuum or the
wait after the target temperature has been reached to end
the wait default wait periods prematurely.
HELP - calls the BETWIN Help System.

For further information on the actual steps used in an either an Instrument

Calibration or a Sample Chamber Calibration see the appropriate description
section below.

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 Description of Sample Chamber Calibration
When performing a sample chamber calibration the system calculates
three (five in the case of Version 5.2 and above BET Sorptometers) volumes by
using the attained pressure values. All versions attain volume readings for the
internal plumbing, the internal plumbing and sample chamber at room
temperature, and the internal plumbing and sample chamber at testing temperature.

Version 5.2 and later machines also have valve V which closes off the
vacuum valve so as not to damage it if the pressure is too high, and the P0 system
has been moved to between valves 4 and 7. The first of the additional volumes
includes the internal volume with valve V open. The second is similar to the first
but valve 7 is closed and valve 4 is open. This gives you the testing volume
including the P0 section up to the P0 valve.

To perform a sample chamber calibration the BET Sorptometer goes

through the following steps:
1. You are first prompted to install the sample chamber. This also gives
you the chance to make sure that the gas has been connected as well.
2. The BET Sorptometer will then reach maximum vacuum. This
process can be a lengthy one.
3. The upper system is pressurized to a calculated point and allowed to
stabilize.
4. Valves 1 and 2 which isolate the sample chamber are opened and the
pressure is again allowed to stabilize.
5. You are asked to install the Dewar (for a cold gas) or Heater (for a hot
gas) on the system.
6. The system then reaches the target temperature (i.e., for liquid nitrogen
the target temperature is -195.76 C) and waits for 10 minutes so that
the system may stabilize.
7. The pressure is again taken.
8. You are informed that you may now remove the dewar.
9. You are informed that you may now remove the sample chamber.
10. You are asked to select a previous Sample Chamber file to use as a
base for the needed calculations.
11. After the needed calculations have been completed you are asked to
select a file to output the new sample chamber information to.

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 12. Click on Exit to return to the Chamber Calibration setup screen.

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 Calibrate Instrument

This routine is used to calibrate the internal volumes of the BET

Sorptometer. Using two separate sample chambers, the Sorptometer calculates
the volumes of it's internal system and of the two sample chambers.

The two sample chambers that you use should be as different in size as
possible. The greater the difference, the better the results you will get. (Example:
if you use two chambers of 18.9 cc and 24.6 cc you will not get as accurate a
measure as if you had used one of 9.6 cc and another of 30.3 cc)

This procedure uses two separate screens. The first is used to set up the
procedure (which unit to use, gas inlet valve, etc.). The second is a status form
that allows the user to keep track of what the machine is doing and also displays
the results of the calibration when completed.

To set up the calibration you need to select which unit you will be
calibrating the sample chamber on (you may only run one calibration at a time),
which gas inlet valve to use, the PI pressure for the gas you are using (only if the
gas doesn't have a P0 value), room temperature, the instrument temperature, and
whether you are using liquid nitrogen (for cold gas), if you are using a hot gas or
not liquid nitrogen, what the testing temperature is, and the volumes of both
sample chambers in cc's.

When you click BEGIN the first form will be unloaded and the
Calibration Status Screen will appear. For more information on the Status
Screen see the above section entitled Calibration Status Screen.

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 Description of Instrument Calibration
The Instrument Calibration procedure is simply two Sample Chamber
Calibrations performed on two separate chambers to attain the two sets of values
needed for the volume calculations. To perform an Instrument Calibration the
BET Sorptometer goes through the following steps:
1. You are first prompted to install Sample Chamber 1. This also gives
you the chance to make sure that the gas has been connected as well.
2. The BET Sorptometer will then reach maximum vacuum. This
process can be a lengthy one.
3. The upper system is pressurized to a calculated point and allowed to
stabilize.
4. Valves 1 and 2, which isolate the sample chamber, are opened and the
pressure is again allowed to stabilize.
5. You are asked to install the Dewar (for a cold gas) or Heater (for a hot
gas) on the system.
6. The system then reaches the target temperature (i.e., for liquid nitrogen
the target temperature is -195.76 C) and waits for 10 minutes so that
the system may stabilize.
7. The pressure is again taken.
8. You are informed that you may now remove the dewar.
9. You are informed that you may now remove Sample Chamber 1.
10. Repeat steps 1 - 9 for Sample Chamber 2.
11. Select the file name you wish to use to store the information on
Sample Chamber 1.
12. Select the file name you wish to use to store the information on
Sample Chamber 2.
13. Click on Exit to return to the Instrument Calibration Setup screen.

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Report Menu
The options here deal with the output of reports based on data attained
during an Automated Test or entered manually by the user. The options available
are:

Execute Report

The Execute Report option allows you to attain printed reports on the
data collected during an Automated Test or entered using the Manually Create
a Data File option under the Modify Menu. The image above represents the
report form after the Advanced button has been pressed.

Starting with the BETWIN Software System you are now able to select
only those reports and/or graphs you wish to have printed (i.e. you can choose to
have only the adsorption graphs and the BET Surface Area Analysis report). This
saves printing time because it will only do the calculations for those sections that
you wish printed.

There are five options/sets of options that control what reports are printed,
where they are printed to, and, if you are doing graphs of any of the reports, the
appearance of those graphs. The five report options which need to be set are as

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 follows. The first two options are available when you first start the Execute
Report Section.

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 Graph Setup
The Graph Setup option allows you to determine how the graphs
you have selected, if any, will be scaled. Scaling in this case determines
the ranges of the different axis for each graph. The three scaling methods
available are:
Last Scale -
This setting uses the scaling information stored during the
last Manual Scaling or Maximum Scaling report. This
method may miss some points if the data does not fit the
same range as the last set of data.
Manual Scale -
This option allows you to adjust the settings for each graph
manually.
Auto Scale -
This selection uses the data to determine the scaling
necessary to display all the data on the graph.

Output Device
The Output Device option allows you to select where the reports
and graphs you select will be displayed or stored. The three options for
output are:
Printer -
Selecting Printer will send the report and graphics to the
systems default printer.
Screen -
This option causes the report and associated graphics to be
printed to the computer screen
Text File -
The report is stored as ASCII text to a disk file. The
computer will bring up the File Selector for you to choose
a file to store the report in or to enter a new file name.
Outputting to a Text File does not allow you to do graphics.
Plotter -
This selection will output only the graphs of the reports
selected. Currently the plotter must be a Hewlett-Packard
7475A or compatible.

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 Report Setup
The Report Setup section of the report form is used to set up
which reports and sets of graphs you wish to output. You are asked to
check the box corresponding to the report and/or set of graphs you wish to
have when the report is output. The reports and corresponding graphs you
have to choose from are:

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 BET Surface Area Analysis
This option reports on the surface area of the sample you
are generating the report on. Two methods are used to
calculate the Surface Area. These two methods are Single
Point and Multipoint.
If the data file you select consists only of Multipoint data,
you will be asked if you will be asked if you wish to
convert the data into Single point. If you select Yes, the
multipoint data will be compiled into a comparable single
point, where the initial pressure will be the first initial
pressure from the multipoint data, plus the difference
between each subsequent final pressure (except the last one)
and the next initial pressure, to give a resulting initial
pressure that represents the total amount of gas used in the
entire test. The final pressure will be the final pressure of
the last dose in the multipoint data. If your data file
contains data beyond the multipoint range (P/P0 of greater
than .35 for nitrogen) you should not use this option.
Horvath-Kawazoe Table
This report generates a listing of the points within your data
that fit within the Horvath table.
Micro Pore Calculations
This selection generates a report that displays the volume
of liquid, surface area, and pore volume of the sample
tested within given thickness ranges for the pores.
Micro Pore Volumes
Both of these reports, MPTPlot and TPlot, generate
reports on the thickness of the adsorbed layer on the surface
of the sample versus the total amount adsorbed. The
MPTPlot method uses the MEB equations.
Gas Adsorption (Pierce)
This selection generates a report that calculates the gas
adsorbed by the sample at increasing pressure values, using
the Pierce equations. This report is generated only if an
adsorption test was run on the sample.
Gas Desorption (Pierce)
This selection generates a report that calculates the gas
adsorbed by the gas at decreasing pressure values. This
report is generated using the Pierce equations. This report
is generated only if a desorption tests was run on the
sample.

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 Gas Desorption (BJH)
This selection generates a report that calculates the gas
adsorbed by the gas at decreasing pressure values. This
report is generated using the BJH equations. This report is
generated only if a desorption tests was run on the sample.

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 Multi-Graphic Option
When you select this option, you are allowed to select up to 10
data files, using the File Selector, with which to print the graphs for each
report selected. All data sets will be plotted on the same graph.

Each time you select a valid data file, the number of files you have
selected so far will be checked. If you have selected fewer than 10 data
files, a box will appear in the center of the screen asking you if you wish
to enter more reports. This box also includes the number of files you are
allowed to choose (10) and the number you have selected to that point.

If you wish to include another data file in this report click on Yes,
otherwise select No. If you select Yes, the File Selector will be displayed
again so that you may select another file.

Report Cover Page

This option turns the cover page for the report on and off. The
cover page displays information about the sample and the company that
ran the test.

There are also three buttons that appear on the left edge of the Report form.
These buttons perform the following tasks:
BEGIN - begins printing the report using the options selected by the user.
The program will first call the File Selector so that the user
may select a data file(s) from which to attain the data for the
report. It will then use that file(s) to generate the requested
reports and graphs, outputting them to the selected device.
HELP - calls the BETWIN Help System and displays information on
the Report Setup Screen.
CANCEL - cancels the report program without printing any reports and
returns you to the main screen for the BETWIN software
system.

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 Alter Cover
This option allows the user to modify the company information that
appears on the cover sheet for reports. This is an example of what may appear in
the company information:

POROUS MATERIALS, INC. ANALYTICAL SERVICES DIVISION

20 DUTCHMILL RD.

ITHACA, NY 14850 USA

PHONE (607)-257-5544 or 1-800-TALK-PMI

To do the actual editing, BETWIN calls the Windows NotePad accessory

and loads the existing cover file into this text editor. You are then able to edit the
existing Company Information to include the information you wish.

For more information on the Notepad program use the Help available
within Notepad application.

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Modify Menu
This menu allows you to modify a variety of files and options that control
the BET Sorptometer or the data acquired during an automated test or entered by
the user. The options available are:

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 Edit Auto Parameters

There are many factors that control an Automated Test. Some of these
factors have been put into a parameter list to allow easy user modification. For
each gas, there is a default parameter list that is used when running a test with this
gas, and other parameter lists that can be made default by using the parameter
editor.

This screen shows the current values of the parameters, preceded by a

brief description of the parameter. When this program is first run, the values on
the screen are taken from the default parameter file for the selected gas, and
represent the values that are currently being used to control tests run with this gas.
To change a value, simply press the TAB key until the value you wish to change
is highlighted or Click on the desired value.

The following are the options you are allowed to change which control an
Automated Test:
Minimum PI Undershoot Count & Maximum PI Undershoot Count -
When trying to reach a PI value, the optimal pressure is calculated,
and then allowable minimum and maximum pressures are

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 determined. The minimum pressure can not fall below the
previous PF (during pressurization). The minimum PI is
determined by the parameters for Minimum PI Undershoot and
Maximum PI Undershoot. At the low point of a gauge, the
minimum PI is Minimum PI undershoot counts below optimal PI.
At the high point it is Maximum PI Undershoot counts below,
with a linear scale in between. If the previous PF is below the
minimum PI, the point can not be taken because it is too close.
Parameters Minimum PI undershoot and Maximum PI
Undershoot are given in counts, which vary depending on which
gauge is used to read the pressure. In this way, they increase as the
pressure increases.
PI Overshoot Factor -
Maximum PI is set based on the minimum PI. It is set to
parameter PI Overshoot Factor times as far above optimal PI as
the minimum PI is below. If parameter PI Overshoot Factor is
1.5, then Maximum PI will be 1.5 times as far above optimal PI as
minimum PI is below optimal PI.
Maximum Pressure Cap & Minimum Pressure Cap -
When re pressurizing, subsequent PI values can be set to larger
than the initial PI calculation. When the initial PI is calculated, the
maximum pressure cap is set to twice PI. A subsequent PI value in
a secondary gas dose will be limited by this cap value. This cap is
further constrained by the parameters Maximum Pressure Cap
and Minimum Pressure Cap. It will not be set to lower than
Minimum Pressure Cap or greater than Maximum Pressure
Cap. Further, the parameter Maximum Pressure Cap is also the
absolute maximum pressure allowable at any time during the test.
Allowable PF Undershoot % Error -
When the isolation valves are opened and the test is trying to reach
PF, if the pressure falls more than the Allowable PF Undershoot
% Error away (below during pressurization) from the target PF
value, the point is said to be out of bounds and a secondary dose of
gas is required. If the test is being run with intermediate data
points, then the full equilibrium will still be obtained and the point
taken, but the target PF for the next dose will remain the same.
Otherwise a smaller equilibrium will be used and a new dose of
gas will be brought in trying to reach the same PF value.
Allowable PF Undershoot % Error is set in percent error, which
is calculated as the difference between the optimal PF and the
actual PF, divided by the optimal PF and multiplied by 100. If the
Allowable PF Undershoot % Error is .2 and optimal PF is .1,
then the actual PF will have to be above .0998 when doing
adsorption and below .1002 when doing desorption.

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 Initial Pressure Equilibrium Count, Final Pressure Equilibrium
Count,
Minimum PF Equilibrium Count & Re-pressurization Equilibrium
Count -
Before any pressure reading is taken, the pressure gauge is read
until it has remained stable for a certain number of seconds. The
Initial Pressure Equilibrium Count determines the number of
seconds required when reading the initial pressure. The Final
Pressure Equilibrium Count determines the number of seconds
when reading the final pressure (while the sample is adsorbing gas).
If the sample adsorbs too much gas, and the testing program is set
not to take intermediate readings, then after the Minimum PF
Equilibrium Count in seconds of equilibrium are met, the
isolation valves close and wait for the Re-pressurization
Equilibrium Count in seconds to determine the starting pressure
for adding another dose of gas.
Allowable Count Flicker Gauge 0 through Gauge 3 -
When reading a pressure gauge, it is said to be stable if it does not
vary more than a certain number of counts from its initial reading.
If it does, it is called unstable, and the next reading is used as the
new initial reading. Since the two pressure gauges each have two
ranges, and the smaller the range the greater the allowable flicker,
Allowable Count Flicker for Gauge 2 is usually larger than
Allowable Count Flicker for Gauge 1. Allowable Count
Flicker for Gauge 1 is the allowable flicker from the full scale
reading of the largest range gauge (Phi). Allowable Count
Flicker for Gauge 0 is for the one half range of that gauge (Plo),
Allowable Count Flicker for Gauge 3 is for the full scale reading
of the smallest range gauge (Vhi), and Allowable Count Flicker
for Gauge 2 is the one half range of that gauge (Vlo). Due to the
nature of the digitizing process, the smallest allowable flicker is 1.
Allowable Overshoot -
Allowable Overshoot is not used in the current system. It was
used in older systems that did not support multiple chambers. In a
multiple chamber system a cold probe trigger point is required for
each chamber, and therefore the cold probe value is stored in the
file BETSTUFF.DAT, along with all the gauge calibration data. It
is usually not necessary to change this value, but if it is, contact
PMI for help.

There is also a series of seven buttons down the right side of the form.
The buttons and their meanings starting at the top are:

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 Load New Parameters - allows you to load a previously created
parameter file other than the default parameters for
the current gas.
Save Current Settings - saves the values of the parameters to a file
for use at a later time. (Note: this does not make the
current values the default parameters)
(both of the previous two options use the File Selector to load
or save parameter file data)
Make These Default - makes the current parameter settings the
default parameters values. If you wish to save these
values to a file use the Save Current Settings
button before pressing this button.
Reset Values - resets the values to the default parameter values.
Help - calls the Help facility and displays information on
the Edit Auto Parameters Screen.
Cancel- ends the Automatic Test Parameter File Editor
without making any changes to the current settings.
Done - ends the Automatic Test Parameter File Editor
and saves the current settings as the default
parameters.

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 Manually Create File

Normally, a data file is created by testing a sample using the Automated

Test procedure. If, for some reason, you have data from a sample test performed
by some other procedure, or on some other instrument, you may use the
Manually Create Data File option from the Modify Menu to enter this data into
a standard data file for use with the report program. To create this data file, you
will need to know certain volumes and temperatures that are normally collected
automatically.
Manual creation of a data file consists of five separate sections. The first
is choosing a name for the data file you are about to create. This is done from the
File Selector.
The second section consists of a series of Yes or No questions that control
the output of the report. Depending upon the gas you are using as your default
gas, the number of questions may vary. (i.e. if your gas can not be used to
calculate Surface Area, you will not be asked if you wish to do Surface Area) A
complete list of questions is as follows:
Do you want to calculate Surface Area?
Do you want to calculate the Adsorption Isotherm?
Do you want to calculate the Pore Volume?

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 Do you want to calculate the Desorption Isotherm?
Simply answer Yes or No to each of the above questions. The Pore
Volume question will only be asked if you answer Yes to the Adsorption or
Desorption question and the gas is capable of doing Pore Volume.

The third section consists of the main form with a frame entitled Heading
Information and the following two buttons:
CANCEL - ends the creation of the data file without saving any
information to the file.
HELP - calls the BET Sorptometer Help system and displays
information on the steps necessary to Manually Create a Data
File.
The Heading Information is that information that appears at the top of a
data file before the data itself. The exact information requested depends upon the
gas you are using. The information requested is as follows:
Enter the P0 value, or 0 for default / Enter the Surface Area Factor,
or 0 to skip -
The first item you are asked to enter is the P0 Value for this test.
If you want to use the default value, enter a 0 instead. If the gas
you are using can not be used to calculate pore volume, it will not
have a P0 Value. In this case, enter the Surface Area Factor, or 0
to skip Chemisorption Surface Area calculations.
Enter the outgassing vacuum (microns) -
You are also asked to enter the outgassing vacuum in microns.
Normally, the automated system sets this value to 20. Enter
whatever value you like. This value is not used in calculations,
and is just printed on the report.
Enter the outgassing temperature (C) -
Next enter the temperature of the sample when the vacuum was at
the value previously entered, just before the test was started. As
with the vacuum reading, this value is not used in any calculations,
and is just presented in the report as information to the reader.
Enter the zero correct factor (0 for true pressure readings) &
Enter the scale correct factor (1 for true pressure readings) -
The next two inputs are for the zero correction factor and the
pressure scale factor. These are used for ease of entering pressure
values gathered on a unit that does not give direct readout in PSIA.
Note that if your software has been set for alternate units, such as
kPa, and you are entering data in these alternate units, then you
would set the pressure scale factor to 1.

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 The zero correction factor is the value of the pressure readout
when the actual pressure was zero (the system and sample were
under vacuum). Give this value in whatever units were used by the
pressure readout. This value is subtracted from all of the pressure
inputs before anything else is done to them. If your readout was a
negative number at vacuum, enter that negative number. If your
gauge gave readings in actual PSIA, enter 0 for the zero correction
factor.
The pressure scale factor is used if your readout is in some units
other than PSIA. When any pressure value is read into the report
program, the zero correction factor is first subtracted from it, and
the result is then multiplied by the pressure scale factor. If your
gauge read 1 at vacuum and 3 at 10 PSIA, then the zero correction
factor would be 1, as this was the reading at vacuum, and the
pressure scale factor would be 5, because the gauge read 5 times
less than the actual value once the zero correction factor had been
taken into account. Note that while the zero correction factor can
be any number, positive or negative, the pressure scale factor must
be a number greater than zero. If you are using a system which
gives lower numbers when the pressure increases, invert the sign
of all of the numbers first, and then calculate the zero correction
factor and the pressure scale factor. This insures a positive
pressure scale factor. Enter the pressure values with the sign
inverted as well. If your gauge reads in direct PSIA, or if the only
modification necessary is the zero correction factor, enter a 1 for
the pressure scale factor. After you enter the pressure scale factor,
and press return, it will be time to enter the PI and PF values taken
during the test. Enter them using the values actually read from the
gauge (or negative values if you had to invert them because of a
negative pressure scale factor).

When the entries for the above topic have been entered to your satisfaction,
click on the Done button within the Heading Information frame to continue to
the next section.

After clicking the Done key from the previous section, that frame will be
disabled and the items dealing with the fourth section will become visible. The
fourth section consists of a frame for use in entering data points and a list of PI
and PF values that have already been entered. The list is empty to begin with but
eventually fills up as you add points to the data file. If you enter more points than
there are room for in the list box, simply click on the arrows or bar that appear in
the list box. To enter data points follow the directions as they appear in the Data
Entry frame. Each time you click on ENTER, the data will be saved and a copy
of the point will be displayed in the list box.

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 Once you have clicked DONE on the Data Entry section, it will become
disabled and the fifth and final section dealing with the Footer Information will
become visible. Footer Information is the information that appears after the data
points in a data file. You are asked to enter the following information:
Enter VA value, Enter Vit value & Enter Vln value -
The VA value is the volume of the upper section of the machine,
above valves 1 and 2 but below valves 3 and 4. This value is taken
with all the valves closed except for valve 5. Enter the value, in cc,
and press return. You will next be asked for the Vit value. This is
the volume of the section below valves 1 and 2, including the value
added when valves 1 and 2 are opened, that is at the instrument
temperature. This will include some of the internal tubing, and the
part of the sample cell that is above the liquid nitrogen. Enter the
value, in cc, and press return. You will next be asked for the Vln
value. This is the volume of the portion of the sample cell that is at
the testing temperature (below the level of liquid nitrogen, or
surrounded by the heating mantle), and should include all of the
section of the sample cell that holds the sample. This volume
should be taken with no sample in the cell. The volume taken up
by the sample will be subtracted by the report program.
Enter the sample's weight before outgassing &
Enter the sample's weight after outgassing -
The report program needs to know the weight, in grams, of the
sample. Enter the weight before the test. You are also asked to
enter the weight of the sample after the test. If you only know the
weight before the test, enter a 0 in the after field, otherwise enter
the weight after the test, and press return. If you enter a 0 for the
Weight after Outgassing, the weight before the test will be used
in all calculations.
Enter the density of the sample -
You are now asked to enter the density of the sample for which
you are entering data.
Enter the instrument temperature & Enter the testing temperature -
Next you will be asked for the temperature of the upper portion of
the machine. This will be the temperature of the VA and Vit
volumes entered above. If your gas is not run at liquid nitrogen
temperature, you will be asked for the testing temperature. This is
the temperature of the bottom of the sample chamber during the
test. Enter both these values in degrees C.
Sample ID, Line 1, and Line 2 -

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 You will then be prompted for the Sample ID. This can be
anything, but shouldn't exceed 20 characters. This Sample ID is
used in the report to identify the sample that the report is being
printed for. There is also space for two lines of any descriptive
text you would like to appear with the Sample ID. This text is not
used in any calculations, and can be up to 80 characters in length
and contain any characters. They can be used for further
clarification of what the sample is, who ran the test, etc.
Enter the date the test was run -
You will next be prompted for the date of the test. Enter the date,
in any format you prefer.

After you have answered these questions and are satisfied with the
responses click on the DONE button within this section of the screen. This
finishes writing the test information to the data file.

You may now go to the Report Menu to setup and run a report using this
data.

Note: If the data you entered was not from a real test, strange
results can happen in the report program. You can also use any
text editor to edit a data file, which will have an extension .BDT,
but there are certain lines that are added by this program which
have to be the values they are. If you create or edit a data file
using a text editor, you may be stopped when submitting it to the
report program with a message to the effect that this data file was
not created on the system, and returned to the main menu.

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 Curve Fit

Use of the Curve Fit utility allows you to smooth out the curve of the data
collected during an Automated Test or manually entered using Manually Create
File.

You are first asked to enter the name of the data file you wish to curve fit.
The File Selector is called to allow you to do this. Once you have selected a
valid data file you are presented with a form and asked to set the following three
options:
Percentage Error Allowed (0-100) -
This is used to determine if a data point is within the allowed range
of difference from the norm.
Number of Points to Use for Fitting (3-10) -
This value is used to determine the number of points the program
will use to fit a point to the curve. The data points are taken on a
sliding selection from 3 to 10 points (i.e. if you enter a 5 the
program will first use points 1 through 5 then 2 through 6, etc.) and
a polynomial will be generated using these points.
Maximum Distance Between Any Two Data Points in _______ -
The label for this option depends upon whether the gas you used
for the test could do Pore Volume. If it could and you asked for
Pore Volume, you are asked to enter the maximum distance
between data points in P/P0. If you did not ask for, or the gas is
not capable of doing Pore Volume, you will be asked to enter the
distance in terms of the pressure units you have chosen to use. The
value you enter will be used to determine whether or not to
generate an interpolated data point.
You are also presented with three buttons. They perform the following tasks:
BEGIN - starts the actual Curve Fit procedure.

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 HELP - starts the BETWIN Help System and displays information on
the Curve Fit section of BETWIN.
CANCEL - ends the Curve Fit procedure without fitting the data file
you selected.

A good starting point is to use a percentage error of 0.1 and 5 for the
number of points used. This will use points 1 through 5 to fit points 1, 2 , and 3;
points 2 through 6 will be used to fit point 4, etc.

As the points are fit to the curve, the box at the bottom of the form labeled
Percent Complete will slowly change color to show you how much of the curve
fitting has been completed. When the program is finished curve fitting the data,
the File Selector is again displayed so that you may enter a file to output the
newly fitted data file into.

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 Interpolate
The Interpolate portion of BETWIN simply requires three calls to the
File Selector.

The first call to the File Selector is for the file which contains the raw data.
If this file already contains interpolated data, you will receive a warning message
and will be asked if you want to continue. It is best to interpolate only raw data.
Interpolating already interpolated data is less accurate, but can be done.

Next you will be asked for the interpolation list, which should already
have been created by using the New Isotherm List option from the Setup Menu.
After selecting the isotherm list file, the data will be interpolated and you will be
asked to enter the name of the new data file. It is best not to write over the old
data file in case you ever want to re-interpolate it, or show the raw data. When
done, you will be returned to the main menu. From there you can run a report on
your new interpolated data file.

When you print a report using an interpolated data file, a report is

generated in which the radius values are those in the interpolation list and the
volumes are derived from the data points found in the raw data file, but
interpolated to give the values that would have been found had the data been
taken at the interpolation list's radius values, instead of the radius values that were
actually taken.

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 Edit Old Gas
This procedure is almost identical to the Create New Gas option under
the Setup Menu. The only differences are that the user is not allowed to change
the single letter/number used to signify the gas and the name used to store the gas
file.

For more information on what each field means please see the section on
Create New Gas.

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Setup Menu
This menu contains options that allow you to create and/or modify files
that are used to control a test, define a gas, define pressure units for display
purposes, and system calibration information. The options available are:

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 New Multipoint List

The New Multipoint List option allows you to create a file containing a
list of P/P0 values to be used by BETWIN as target pressures when performing a
Multipoint Test during an Automated Test. If the gas you have selected as your
default gas is not capable of doing Surface Area calculations, you will be
presented with an error message to this affect and returned to the Main Menu.

If your gas is capable of doing Surface Area calculations, you will be

prompted for a name to store this file under using the File Selector. After
entering a valid file name, the form used to create a New Multipoint List will be
displayed.

The top half of the form consists of information dealing with the creation
of a Multipoint List including the valid range of P/P0 points for the default gas
(i.e. for Nitrogen the range is 0.04 to 0.35).

To create the list simply enter P/P0 values in ascending order within the
allowed range and either click on the Enter button or press the RETURN key on
the keyboard. For each value you enter in this manner the value will be stored in
the Multipoint List file and displayed in the Previous Values list box. This list
contains all of the previously entered P/P0 values.

The four command buttons that appear on the form perform the following
tasks:
HELP - calls the BETWIN Help system and displays information on
the New Multipoint List section.

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 ENTER - checks the value that has been entered into the P/P0 Value
box to see that it is within the valid range and is larger than
the previous value. If these conditions are met, the value is
accepted, stored to the Multipoint List file, and displayed in
the Previous Values list box.
DONE - causes the program to save the Multipoint List file and
returns control to the Main Menu.
CANCEL - aborts the creation of the Multipoint List file without
saving any information.

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 New Isotherm List

When creating a New Isotherm List File you must first enter the name
you wish to use to store this file. You are presented with the File Selector so that
you may enter a file name and where to store the file. After entering a valid file
name the main form for this option will be displayed.

The exact appearance of this form depends upon the current default gas. If
the gas you are using is not capable of doing Pore Radius calculations, a message
to this affect will appear at the top of the screen informing you of this fact and
telling you that you need to enter the raw PF values instead of Pore Radius values.
If the gas you are using can do Pore Radius calculations this message box will be
empty.

If your gas is not capable of doing Pore Radius calculations, the area
below the above mentioned box will be empty. If your gas is capable of doing
Pore Radius calculations, you are asked to select which form you wish to enter the
values in: Radius Values or P/P0 Values. You must select which type of value
you will be entering before you start entering value. Once you start entering
values you may not switch to the other style.

The next message box informs you of what type of values the program is
looking for (i.e. pressure targets, P/P0 Values, etc.) and the range of valid points.
Again, the exact contents of this field depend upon the gas you are using and/or
the type of value you have selected to enter.

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 The next item is used to enter the values that will be stored into the
isotherm file. The label for this field, like the message box above, depends upon
several different factors. The three labels possible are: P/P0, Radius Value, or
Pressure (????), where the ???? stands for the current default pressure units.
Enter the values for the list in order from smallest to largest. After entering each
number click on the Enter button. This stores the value you just entered and
displays it in the list box to the right of the Enter button. Until you have entered
a number into the data entry field, the Enter button will not be activated.

The actual values stored in the list are not the actual radius values, but the
P/P0 values that, when put through a complex formula, become the radius values.
This formula can not be inverted, so this program uses an approximating
algorithm for the conversion. It is done this way so that the two programs that
need this information do not have to go through this conversion process every
time they need radius values. The process does not take much time for an
individual point, and since each P/P0 is calculated when you enter a radius value,
the time used is minimal. You may notice that there is a slight delay after
entering each radius point before the next prompt appears. This conversion
process varies for each gas. A file created for tests using one gas can not be used
for tests using the other gas. If the gas you are using can not generate pore radius
values, then you will have to enter the values as direct pressure values (in PSIA).

As mentioned above, there is a list box just to the right of the Enter key
which keeps track of all the currently entered values.

The three other command buttons located on the right side of the form and
their meanings are as follows:
DONE - ends the isotherm file and saves it to the previously selected
file name. This will happen automatically if you enter a value
that is equal to the upper limit for entered values.
HELP - calls the BETWIN Help system and displays information on
the New Isotherm List section.
CANCEL - ends the Isotherm List File creation process without
saving the list to disk.

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 New Pretreatment List

Before a sample is outgassed, it can be put through an optional

pre-treatment procedure. The actual workings of this procedure are controlled
through a pre-treatment instruction list. To create such a list, select the New
Pretreatment File option from the Setup Menu on the main screen.
The gas used for the pretreatment is assumed to be the default gas you
currently have selected. If you wish to use a different gas, first use Select Gas
from the File Menu.
Next you will be asked to enter the name of your output file using the File
Selector.
You are then presented with a series of command buttons which control
the pretreatment process. Below is a list of these commands and what their effect
on the sample is:
EVACUATE -
This command is used to start evacuating the sample being tested.
This also causes the Wait for Vac. button to become visible. The
sample will continue to be evacuated until it either reaches a
pressure set using the Wait for Vac. command or until the Flow
Gas command is used. This causes the message, "Start
Evacuating.", to appear in the list box below the command
options.
WAIT FOR VAC. -

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 This button becomes visible only after the user has pressed the
evacuate button. After pressing this button you will be prompted
to enter the pressure in your default units that you wish to set as a
target pressure to evacuate to. Causes the message, "Maintain
vacuum until pressure = ??? (units).", to appear in the list box.
HEAT -
This button causes the sample to be heated to the temperature you
are prompted to enter. After you have entered the temperature to
which you wish to heat the sample to, the message, "Maintain
heat at ??? degrees C.", will be displayed in the list box.
FLOW GAS -
This command stops evacuation and starts flowing gas over the
sample. You are prompted for a maximum pressure. When it
flows gas, valves 1,2, and 3 are open, valve 5 is closed, and valve 4
is normally closed, but, if the maximum pressure is exceeded, is
opened (and closes again when this pressure is no longer exceeded).
After you have entered the maximum pressure, the message that
appears in the list box is in the form, "Flow gas at up to ??
(units)."
WAIT TIME -
This button causes the pretreatment to wait for the amount of time
you are prompted to enter (in minutes). After entering the amount
of time you wish to wait, the message, "Wait for ?? minutes.",
will appear in the list box below.
DONE -
This button ends the entry of commands into the pretreatment file
and saves the commands to the previously selected file name. You
are then returned to the main screen.
ENTER -
This button is used when you are prompted to enter any type of
value. After typing in the value you wish to use either click on the
Enter button or press the Enter key on the keyboard to accept it.

The list box mentioned above lists the commands in the order they have
been entered so that you may keep track of what commands you have already
entered.

Finally, there are two command buttons that do not enter commands into
the pretreatment file. They are:
CANCEL - ends the Pretreatment File Creation process and returns
you to the main screen without saving the pretreatment file.

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 HELP - calls the BETWIN Help system and displays information on
the New Pretreatment List section of BETWIN.

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 Create New Gas

Before any gas can be used with the system, either to run a test, create a
data file manually, or enter any form of parameter list, it must first be described
through this section. This form is also used for the option Edit Old Gas from the
Modify Menu, except that from the modify option you are not able to change the
name of the gas or the one letter extension assigned to it.

The following two questions are asked only if you are creating a new gas:
Enter the single letter or number to be used to signify this gas -
Each gas has a single letter or number that acts as its "handle".
This is usually the first letter of the name of the gas, though it can
be anything that is not already being used by another gas. This
handle is only used internally to designate different types of files.
(For example, isotherm list files all have the three letter extension
beginning IS, but the third letter is the handle of the gas for which
they were meant to be used.) You can see these handles being
used if you look at the three letter extensions on the files listed in
the automated test description list. You select each file by its name
(up to 8 letters), but when the full file name is displayed on the
screen, it also has the disk drive designation (and sub-directory, if
any), plus the extension, which usually contains the gas handle as
the last letter.
If the "handle" is already in use you will be informed of this later
and given the opportunity to change it.

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 Enter the filename for this gas using up to eight characters -
This file name is up to eight letters long, and is converted to all
upper case. This is the name that will show up on subsequent gas
selection menus. If you enter a name that is already being used,
you will get an error message and be asked to enter a different
name.

The next four questions deal with the gas and what type of sample it will be use
with:
Enter the Name of this Gas to be used in reports -
This name can be as long as you like, and contain virtually any
characters. This name will be used when printing the report. Only
the file name and the handle need to be unique. You can use the
same official name for more than one gas without causing any
problem with the program, though it may cause confusion when
comparing reports.
Enter the density of the gas at STP -
Simply enter the density at STP of the gas you are creating a file
for.
Enter the molecular weight of the gas -
Enter the molecular weight of the gas you are entering.
This gas is to be used with what type of sample -
This will determine the type of calibration used in sample
chambers. If you select Cooled, then this gas is assumed to be
used with liquid nitrogen. If you select Heated, then this gas is
assumed to be used with a heater.
The next two questions control other questions so they have been separated into
their own frames.
Can this gas be used to calculate Surface Area?
If the gas can be used to calculate surface area select Yes. If the
answer is Yes, you will need to answer four additional questions.
The three questions within the Surface Area Frame are:
Enter the cross-sectional area of one molecule (Sq. Ang)
-
Enter the cross-sectional area, in square angstroms,
of one molecule of the gas you are entering/editing.
Enter the lower range of P/P0 for multi-point &
Enter the upper range of P/P0 for multi-point -

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 These values determine the lower and upper ranges
of P/P0 values when creating New Multipoint Lists
for use during Automated Tests.
You are also asked to:
Enter the normal P0 pressure in ???? -
Enter the normal P0 pressure in your default
pressure unit (the ???? above stands for the current
units of pressure) for the gas you are currently
entering or editing.
Can this gas be used to calculate Pore Size?
If the gas you are working with can be used to calculate pore size
select Yes. If the answer is Yes, you will need to answer an
additional five questions. The three questions that appear in the
Pore Size frame are:
Enter Kelvin radius @ .1 P/P0, in Angstroms -
Enter the Kelvin Radius, in angstroms at .1 P/P0 for
the gas you are entering/editing.
Enter the Monolayer thickness (Tau), in Angstroms -
Enter the thickness of one unit layer of the gas you
are creating/editing.
Enter the volume ratio (liquid/gas) -
Enter the volume ratio liquid to gas for the gas you
are currently entering/editing.
You will also need to answer the following two questions which
become visible at the bottom of the Gas File Editor/Creation
form:
Enter the normal P0 pressure in ???? -
Enter the normal P0 pressure (the ???? stands for
the current pressure units), for the gas you are
currently entering or editing.
Enter the minimum pore radius for the Pore Volume
Report, in Angstroms -
Enter the minimum pore radius, in angstroms, of the
gas you are currently entering/editing for the pore
volume report.

There are also three command buttons on the right side of the form. These
buttons are:

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 OK - saves the information on the gas to the file listed in the file
name field.
CANCEL - ends the Gas File Editor/Creation Form without
saving/creating the gas file.
HELP - starts the BETWIN Help system and displays the information
you are currently reading.

If the single character you selected to designate this gas is already in use,
you will be informed of this fact and asked if you wish to replace the current gas.
If you select YES the old gas file is replace with the new information. If you
select NO you will be returned to the Gas Parameter File Editor/Creation form
so that you may change the designating character.
If you choose to replace an old designator, you will be asked if you wish
to erase the old Isotherm lists, Multipoint lists, etc. created under the old gas.
Simply check off those file types you wish to erase and click on the Continue
button. This will erase all existing files of the type you selected which use the
designator of the old gas. If this new gas file is for a totally new gas, you will
want to erase all the old isotherm lists, as they will no longer be valid. If the new
file is basically the same gas, with just something small (like the name) changed,
then the isotherm lists will still be valid.

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 Pressure Units

Using this option, a user may define a new unit of measure for pressure
readings. This unit of measure is what BETWIN uses to display pressure readings.
BETWIN comes with three previously created units of pressure. They are PSIA,
Torr, and KiloPascals.
The calculations that BETWIN performs, dealing with pressure, use the
pressure unit Torr. The pressure readings that are stored in a data file are in Torr.
The conversion factor is used when the pressure reading is to be displayed. Using
the currently defined pressure units, you get the following equivalencies: 760
Torr = 14.7 PSIA = 101 kiloPascals.
To define a new unit of pressure you need to enter a name, of exactly 4
characters in length without spaces, by which BETWIN will use as the pressure
label (i.e. Torr, Atms, k_Pa, etc.). This name is entered in the Unit Name field.
The Unit Conversion field is for the conversion value. Examples of
conversion values are displayed in the box at the top of the form. This is the
value that, when a Torr value is multiplied by this value, you get the equivalent
value in the unit you are creating.
Example: If you wish to measure pressure in Atmospheres, type
Atms (or similar name) into the Unit Name field. The Unit
Conversion field would contain the value attained from the
following formula:
Atmospheres 1 Atms
= = 0.001315789
Torr 760 Torr
There are also three command buttons located at the bottom of the form.
These buttons perform the following commands:
CANCEL - ends the creation process without saving the conversion
information.

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 HELP - calls the BETWIN Help system and displays information
on the Pressure Units section.
CONTINUE - saves the conversion factor to the BETWIN default
directory using the 4 character name you used to define the
unit of measure then returns you to the main screen.

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 Hardware Protocol
The Hardware Protocol option of the Setup Menu allows you to edit the
file BETSTUFF.DAT. This file contains calibration information on the various
gauges in your BET Sorptometer along with other information. You should be
very careful about any changes you make to this file as the contents control the
readings you receive from the pressure and vacuum gauges.

Editing is accomplished using the Notepad text editor that is provided

with Microsoft Windows. To move around within the editor you may use both
the cursor keys and the mouse. To change an existing value simply Delete or
Backspace over the character(s) you wish to replace and type the character(s) you
wish to insert. For more information on how to use the NotePad editor please see
the Help facility within the editor itself.

For further information on the information stored within the

BETSTUFF.DAT file see the section below entitled Explanation of
BETSTUFF.DAT.

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 Help Menu
This menu calls two sections of the on-line Help facility. The options
available are:

About BETWIN

This option displays a box on the screen which contains information on

the BETWIN Software System (i.e., title, version number, etc.) and information
on the Windows environment.

Help
Starts the BETWIN Help System and displays the main topics list. This
system allows you to attain help on a each of the major sections of the BETWIN
Software System as well as the associated programs.

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