™

TAM III
TAM Assistant Software

Getting Started Guide

Issued June 2012

 Notice

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Page 2 TAM Assistant Software Getting Started Guide

Introduction

Important: TA Instruments Manual Supplement

Please click the TA Manual Supplement link to access the following important information supplemental
to this Getting Started Guide:
• TA Instruments Trademarks
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TAM Assistant Software Getting Started Guide Page 3

Notes, Cautions, and Warnings
This manual uses NOTES, CAUTIONS, and WARNINGS to emphasize important and critical
instructions. In the body of the manual these may be found in the shaded box on the outside of the page.
NOTE: A NOTE highlights important information about equipment or procedures.

CAUTION: A CAUTION emphasizes a procedure that may damage equipment or cause loss of data if not fol-
lowed correctly.

A WARNING indicates a procedure that may be hazardous to the operator or to the environment if
not followed correctly.

Page 4 TAM Assistant Software Getting Started Guide

 Table of Contents

Introduction ................................................................................................................................................. 3
Important: TA Instruments Manual Supplement ................................................................................... 3
Notes, Cautions, and Warnings .............................................................................................................. 4

Table of Contents ........................................................................................................................................ 5

Chapter 1: Introducing TAM Assistant ................................................................................................... 9

Overview ....................................................................................................................................................... 9
TAM Assistant Plot Windows .................................................................................................................... 12
Curve Fitting Functions ........................................................................................................................ 14
Exponential Fit Functions .................................................................................................................... 15
Exponential Pulse Fit Functions ........................................................................................................... 18
Logistic Sigmoid Fit Functions ............................................................................................................ 20
Integrate Functions ............................................................................................................................... 23
Integrate against baseline and Integrate two curves ...................................................................... 23
Integrate against extrapolated fit ................................................................................................... 23
Integrate against integral ............................................................................................................... 24
Additional Signal Selections ......................................................................................................... 24
The Devices Explorer ................................................................................................................................. 26
The Thermostat Device ........................................................................................................................ 26
Changing Temperature Using the Control Tab ............................................................................. 26
Setting a Safety Range Using the Settings Tab ............................................................................. 27
The 4 mL Multicalorimeter Device ...................................................................................................... 27
The Signals Tab ............................................................................................................................. 28
Controlling the Calorimetric Calibration Heaters ......................................................................... 29
The 3201 Nanocalorimeter / 3220 Microcalorimeter Device .............................................................. 31
The Control Tab............................................................................................................................. 31
Heat Pulse ...................................................................................................................................... 32
Activate Heat Sink Control............................................................................................................ 32
The Settings Tab............................................................................................................................ 33
The 20 mL Multicalorimeter Device .................................................................................................... 34
The Overview Tab ......................................................................................................................... 35
The Signals Tab ............................................................................................................................. 35
Analyze Peak Function ........................................................................................................................ 37
The 3811 Flow Control Device ............................................................................................................ 38
Setting Up a Ramp......................................................................................................................... 38
Controlling the RH Perfusion Ampoule ........................................................................................ 40
The Experiment Explorer ........................................................................................................................... 41
The Results Explorer .................................................................................................................................. 42
The Report Explorer ................................................................................................................................... 43
Creating a Results File Report ............................................................................................................. 43
The Graph Group (TAM Assistant Embedded) ............................................................................ 45
Creating a Results File ................................................................................................................................ 46
Results Report Wizard ......................................................................................................................... 46
Creating and Manipulating an Overlay Plot or Report ........................................................................ 48
TAM Assistant in Network ......................................................................................................................... 53
Connecting TAM Assistant to a TAM III System ............................................................................... 53
Chapter 2: Calibrating the TAM III Calorimeter ................................................................................. 55
Background ................................................................................................................................................. 55
The Gain Factor .................................................................................................................................... 56
Calibration with TAM Assistant ................................................................................................................. 56

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 Calibration Procedures ......................................................................................................................... 56
Calibration Directly from the Device Control............................................................................... 56
Calculation of the Calibration Constants....................................................................................... 58
Calibration in a Generic Experiment ............................................................................................. 58
Manual Calibration ........................................................................................................................ 59
Dynamic Calibration ............................................................................................................................ 64
Performing a Dynamic Calibration................................................................................................ 64

Chapter 3: Running Experiments ........................................................................................................... 68

Experimental Practices ............................................................................................................................... 68
Sample Ampoules and Reference Inserts ............................................................................................. 68
The Reference Inserts of the 3206 Minicalorimeter...................................................................... 68
The Sample Ampoules................................................................................................................... 69
Balancing the 3206 Minicalorimeter .................................................................................................... 69
Common Heat Capacities .............................................................................................................. 71
An Example ................................................................................................................................... 71
Balancing the 3226 Minicalorimeter .................................................................................................... 72
Choosing the Correct Reference for the 20 mL Minicalorimeter.................................................. 72
An Example ................................................................................................................................... 72
Sealing a Glass Ampoule ..................................................................................................................... 73
Running Experiments ................................................................................................................................. 75
Starting a New Experiment .................................................................................................................. 75
Running Generic Experiments ............................................................................................................. 76
Setting Up a Generic Experiment.................................................................................................. 76
Adding Additional Devices .................................................................................................................. 79
Setting the Experiment Start ................................................................................................................ 79
Finalizing a Generic Experiment ................................................................................................................ 80
Ampoule Experiments .......................................................................................................................... 80
The Ampoule Wizard .................................................................................................................... 81
Ampoule Wizard Results Tab........................................................................................................ 83
Normalization Criteria for the Signal ............................................................................................ 83
Decide about Initial Baseline......................................................................................................... 84
Thermal Equilibration of the Sample ............................................................................................ 86
Insertion into the Calorimetric Measuring Position ...................................................................... 88
Managing the Main Part of the Experiment .................................................................................. 90
Decide about Final Baseline .......................................................................................................... 91
Decide on Experimental Data Reduction ...................................................................................... 95
Ampoule Experiment–STANAG 4582 ......................................................................................... 96
Preparing the sample and filling the ampoule ............................................................................. 100
Loading, equilibration, and measurement ................................................................................... 101
Non-Isothermal Measurements.................................................................................................... 103
Setting Up a Temperature Profile................................................................................................ 104
Defining a Baseline ..................................................................................................................... 106
Starting the Non-Isothermal Experiment..................................................................................... 107
RH Perfusion Experiments ................................................................................................................. 107
Initiating an RH Perfusion Experiment ....................................................................................... 108
Setting Up the RH Ramp ............................................................................................................. 109
Baseline Definitions .................................................................................................................... 111
Start the RH Control Experiment ................................................................................................ 112
Titration Experiments ......................................................................................................................... 113
The Titration Experiment Wizard................................................................................................ 113
Downloading Results Files ....................................................................................................................... 120
Run Sequences .......................................................................................................................................... 122
Using the “Action” Option ................................................................................................................. 124
Using the “Wait For” Option ............................................................................................................. 126
Using the “Repeat” Option ................................................................................................................. 127
Using the “If” Option ......................................................................................................................... 128
Option Overview ................................................................................................................................ 129
Actions......................................................................................................................................... 129

Page 6 TAM Assistant Software Getting Started Guide

 Wait For/If Conditions................................................................................................................. 130

Chapter 4: Data Handling & Analysis .................................................................................................. 132

Data Handling ........................................................................................................................................... 132
Downloading Results Files ................................................................................................................ 132
Exporting Data ................................................................................................................................... 134
Exporting Data During an Experiment........................................................................................ 137
Results Analysis ........................................................................................................................................ 137
Gain Validation .................................................................................................................................. 137
General Performance .......................................................................................................................... 139
Ligand Binding ................................................................................................................................... 140
Choosing a Binding Model.......................................................................................................... 143
Ligand Binding Simulation ................................................................................................................ 144
Heat Capacity Analysis ...................................................................................................................... 145
Compatibility ...................................................................................................................................... 147
Loading Compatibility Data ........................................................................................................ 147
Kinetic Analysis ................................................................................................................................. 153
Arrhenius Analysis ............................................................................................................................. 155
STANAG 4582 Analysis .................................................................................................................... 157
Add propellant ............................................................................................................................. 161

Chapter 5: TAM Assistant Security ...................................................................................................... 163

Introduction ............................................................................................................................................... 163
Setting up TAM Assistant Security .......................................................................................................... 164
Using TAM Assistant Security on a TAM III Instrument ................................................................. 164
Installing TAM Assistant Security on a Standalone Computer ......................................................... 166
Connecting a TAM III Instrument to a Standalone Security System ................................................. 169
Connecting External Computers Running TAM Assistant to the Security System ........................... 172
TAM Assistant Security Manager ............................................................................................................ 174
Connecting to a Security Server ......................................................................................................... 174
The Security Manager Window ......................................................................................................... 174
Apply ........................................................................................................................................... 175
Cancel .......................................................................................................................................... 175
Security Server Settings ..................................................................................................................... 175
Users and Groups ............................................................................................................................... 176
Enable Active Directory Integration............................................................................................ 177
Default Domain ........................................................................................................................... 177
Use All Users and Groups from Active Directory ...................................................................... 177
Only Use Selected Users and Groups from Active Directory ..................................................... 177
Users ............................................................................................................................................ 177
Hide Inactive Users ..................................................................................................................... 177
Groups ......................................................................................................................................... 178
Adding New Users....................................................................................................................... 178
Logon Name ................................................................................................................................ 178
Full Name .................................................................................................................................... 178
E-mail .......................................................................................................................................... 178
Password/Confirm Password....................................................................................................... 179
User Must Change Password at the Next Logon......................................................................... 179
Password Never Expires.............................................................................................................. 179
Editing Users ............................................................................................................................... 179
Logon Name ................................................................................................................................ 180
Full Name .................................................................................................................................... 180
E-mail/Company/Department/Title/Location/Street address/PO box/City/State/Postal code/Coun-
try/Telephone Number.............................................................................................................................. 180
Active........................................................................................................................................... 180
Locked out ................................................................................................................................... 180
Password never expires ............................................................................................................... 180
Reset Password ............................................................................................................................ 180
User Must Change Password at Next Logon............................................................................... 180

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 Member of ................................................................................................................................... 180
Working with User Groups.......................................................................................................... 181
Creating a New User Group ........................................................................................................ 181
Adding Members to a Group ....................................................................................................... 181
User and Group Selection .................................................................................................................. 182
Searching for Users and Groups.................................................................................................. 182
Selected Users and Groups .......................................................................................................... 182
Check Names............................................................................................................................... 182
Permissions and Roles ................................................................................................................. 183
Users and Groups List ................................................................................................................. 184
Permissions List........................................................................................................................... 184
Available Roles............................................................................................................................ 184
Available Permissions ................................................................................................................. 185
Audit Trail .......................................................................................................................................... 186
Audit Entries Filter ............................................................................................................................. 186
Show Entries for User(s) ............................................................................................................. 186
Show Entries Added During........................................................................................................ 187
Show Entries in Categories.......................................................................................................... 187
Minimum Audit Level ................................................................................................................. 187
Show Entries for Children ........................................................................................................... 187
Show Most Recent Entries First .................................................................................................. 187
Show Oldest, Show Older, Show More Recent, Show Most Recent .......................................... 187
Exporting Audit Trails ....................................................................................................................... 188
Printing Audit Trails .......................................................................................................................... 188
Commands in TAM Assistant Security Manager ..................................................................................... 188
Security System Access in TAM Assistant .............................................................................................. 188
Security Settings ................................................................................................................................. 189
Automatically Login at Startup ................................................................................................... 189
Use Current Windows Credentials When Logging In................................................................. 189
Automatically Connect to Devices at Login................................................................................ 189
Security in Property Windows .................................................................................................................. 190
Commands in TAM Assistant .................................................................................................................. 190
Commands on the TAM III Instrument (TAM Assistant Embedded) ...................................................... 191
Security Considerations and Backup of Security Data ............................................................................. 191
Backup ................................................................................................................................................ 191

Appendix: STANAG 4582 ...................................................................................................................... 192

Measurement Duration and Heat Flow Limits ......................................................................................... 192
STANAG Safety Issues ............................................................................................................................ 193
References ................................................................................................................................................. 193

Page 8 TAM Assistant Software Getting Started Guide

Chapter 1:
Introducing TAM Assistant

Overview
In this manual, TAM Assistant (the dedicated software to TAM III), the third generation TAM, and the
TAM 48-channel calorimeter are described in detail.

Two versions of the software for TAM III exist:

• TAM Assistant Embedded

• TAM Assistant (external version)
Both versions are essential for running the TAM III. The two versions are similar in appearance and many
features are common, but the external version has more functionality with report functions, data analysis,
etc. TAM Assistant Embedded is pre-installed on the TAM III system when delivered, while the TAM
Assistant is intended for an external computer connected to the TAM III and/or a local network (e.g. an
office computer).

Figure 1 TAM Assistant Embedded Software program interface.

TAM Assistant Software Getting Started Guide Page 9

The Group field in the left panel of the program main window contains a number of fields that are some-
what different for TAM Assistant as compared to TAM Assistant Embedded; see Table 1 below.
Table 1: TAM Assistant Embedded vs. TAM Assistant
TAM Assistant Embedded TAM Assistant
Devices explorer Devices explorer
Experiment explorer Experiment explorer
Results explorer Results and data files
Graph Report
Group Field Group Field

By clicking a group header, a list of mini-view buttons is shown that is specific for each group. For
instance, clicking the Device group displays a list of the connected devices (e.g. the thermostat and calo-
rimeters in the TAM III) or selecting the Results group lists saved results files.

TAM Assistant Software Getting Started Guide Page 10

The device structure for TAM 48 Channel is shown below.

Figure 2 Device structure for TAM 48.

The calorimeters for the TAM 48 Channel or the multicalorimeter of the TAM III may be regarded as sub
devices under the Multicalorimeter main device, and a software control interface exists for each of them.
Device windows for the individual calorimetric channels are accessed through the multicalorimeter main
device button (i.e., the mini-view button). A unique device interface exists for the thermostat. The number
of connected calorimeter sub devices is always a multiple of 6 for the multicalorimeter TAM III or 12 for
TAM 48 Channel (with n=1, 2, 3 or 4).

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TAM Assistant Plot Windows
Plot windows in TAM Assistant can be viewed in a variety of situations. For example, a plot can be viewed
under the Overview tab associated with a connected device under the Devices group, or when showing the
results in a saved experiment file accessed from the Results group in TAM Assistant Embedded or from the
Results and data Files group in TAM Assistant external version. Interactive graphs appear also in TAM
Assistant report files..

Figure 3 Plot window for a multicalorimeter device.

The scale bars on the horizontal and vertical directions of the plot window are used to change the scale of
the x and y axes and also move along an axes in the x or y direction without changing the scale.
For example, clicking on the left side of the horizontal scale bar (x-axis) and dragging to the left will scale
down the time axis towards earlier time values. Up-scaling from low time values is achieved when drag-
ging to the right. Clicking on the middle part of the scale bar and dragging to the left or right simply moves
the time axis toward lower or higher time values with the time scale preserved.

Figure 4 Plot Tool bar.

The tool bar above the plot contains a number of tools you can use to control the plot window. See Table 2
below for an explanation of each button.
Table 2: Tool bar buttons

Button Description

Use the selection tool to choose a curve when creating a report or graph.

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 Button Description

Activating the plus sign (Zoom Mode) allows you to manually zoom in on events on
the graph by clicking and dragging.

Press the sight sign (Data Reader Mode) to show the value of the x and y axis in a pop
up text box when the cursor is within the bounds of a curve. It is the position of the cur-
sor along the x axis that determines the chosen x,y point. The color of the curve turns
white when sighted. If the left mouse button is pressed down while moving the cursor,
the change in heat flow and time between marked points will be seen.

The reset zoom button (Scale to show all) scales the plot to a predefined scale. The
predefined scale may be considered as 100% magnification.

Use the undo zoom button to recapture the last magnification. Press this button several
times to recapture subsequent plots.

Auto scale right side x (left icon) and lock x-axis range (right icon) work as check
boxes. Select one of the two functions.

The auto scale y button auto scales the y-axis according to a defined magnification,
which is dependent on the min/max range of the graph.

The Multiple Offset button changes the offset of each individual curve so that it is
positioned approximately in the middle of the screen. This is useful for comparison of
curves positioned far from each other. The absolute values of the curves are the same,
but the offset differs, i.e., it will not have a value, only a plus sign below on the x-axis.

Normally the scale is the same for several graphs in common plot. Press the Multiple
Scales button to create individual scales for each graph. The magnification will hence
be 100% for each graph. Use this function when comparing the signal quality between
graphs as generated by signals of different absolute values.

Use the curve fitting buttons to fit a mathematical model to a chosen part of a curve.
Use the first button to choose between linear fit and a constant fit (i.e., zero slope). Use
the second button to choose between a number of exponential equations. Use the third
button to fit dual exponentials. Use the fourth to fit different sigmodials, see below for
more details.

Select a curve then use the Integrate button to perform a peak integration analysis. You
can click the arrow to the right of the button to integrate in different ways, see below
for more details.

Select a curve then use the Analyze Peak button to obtain the peak’s range, integral,
width, height, inflection, half-height, amplitude, etc.

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 Button Description

Use the set signal offset and define signal gain buttons to define the signal offset as
well as the calorimeter gain factor. These operations can be used to perform a calibra-
tion manually.

NOTE: A single plot can be chosen among several plots in the graph.

Curve Fitting Functions

The curve fitting buttons can be used in the graphs of the Devices group, in a Results file, or in a Report.
The examples shown here are given from a results file, but would be identical to that of signals displayed
in the devices group. Results windows remain only temporarily when analyzed in a Results file or from the
devices window. When data is analyzed inside of a report a text box with the results will remain displayed
within the plot window. Please refer to the section covering reports and plot window for more specific
examples.
1 Click on the down arrow and choose the model of interest, e.g., Linear slope fit.

Figure 5 Select model.

2 Move the cursor to the plot in the graph that is of interest.

3 The broken lines appear on both sides of the curve, click the left mouse button to mark the curve. To
make fitting move the cursor to the initial time, click and drag the cursor over along the curve over the
time interval that is to be fitted.
The results of the regression are displayed in the text field on the upper left side of the graph. Beside the
estimated fitting parameters (slope, k and intercept, C in Figure 6) the initial time, x0, is given. This time
corresponds to x = 0 in the equation. The assignment Std. dev is the standard deviation of the residuals, i.e.
the difference between the calculated values with the estimated model parameters and the experimental
points. NDF is the number of data points used in the regression.

Figure 6 Regression results.

NOTE: A single curve can be chosen among several in the graph.

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Exponential Fit Functions
There are four different exponential fits available for either exponential decay or exponential growth. In
the options with zero offset, the fitting function assumes the decay to go to zero heat flow or the growth to
origin from zero heat flow.

Figure 7 Exponential fits available.

A fit could look like Figure 8 (blue line) and the results are given in the small window appearing when
clicking the fit button. The function fitted is shown in the results box.

Figure 8 Fit results.

A: the signal amplitude at time x.

τ: the time constant for the decay (growth).
C: the offset. It will not be shown if the zero offset function is used.
x: the start time of the fit.
Std.dev: the standard deviation of the residuals i.e. the difference between the calculated values with the
estimated model parameters and the experimental points. This is also referred to as the signal noise level.
NDF: the number of data points used in the regression excluded the number of unknowns.

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If the Extrapolate button is pressed, the exponential fit will be extended in both ends.

Figure 9 Extended exponential fit.

1 From the toolbar click on the down arrow and choose the fit desired.

Figure 10 Exponential Fit functions

2 Move the cursor to the plot in the graph, select the curve, then click and drag the cursor over the curve
to make the fit.

Figure 11 Make the fit by selecting the curve.

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3 Exponential decay fit will display the pre exponential constant, A, and also constant, C, which is the
value of infinite decay. Time constant (τ) and initial time (x0) are also shown along with Std. dev and
NDF. Full equations utilized to create the fits are listed in the table below.
Table 3: .Equations for exponential fit functions

Model Fit Equation

Exponential Decay

Exponential Decay
(zero offset, C = 0)

Exponential Growth

Exponential Growth
(zero offset, C = 0)

TAM Assistant Software Getting Started Guide Page 17

Exponential Pulse Fit Functions
There are three options for Exponential Pulse Fit functions–Exponential pulse fit, Exponential sloped
pulse fit, and Dual exponential fit.
1 From the toolbar click on the down arrow and choose the desired exponential pulse fit function.

Figure 12 Exponential Pulse Fit functions.

2 Move the cursor to the plot in the graph, select the curve, then click and drag the cursor over the curve
to make the fit.

Figure 13 Make the fit by selecting the curve.

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3 Exponential pulse fit will display time of peak along with peak amplitude. Also listed are two constants,
C and A followed by two time constants (τ1 and τ2), initial time (x0), Std. dev, and NDF. Full equations
utilized to create the fits are listed in the table below.
Table 4: Equations for exponential pulse fit functions

Model Fit Equation

Exponential Pulse

Exponential Sloped Pulse

Dual Exponential

TAM Assistant Software Getting Started Guide Page 19

Logistic Sigmoid Fit Functions
There are multiple options for Logistic Sigmoid Fit functions. The Logistics and the Pythagorean sigmoids
are calculated in two different ways. The function is shown in the results window. You will define the base-
line sigmoid. Each of these models allows constant or sloping baseline sections to be fitted.
1 From the toolbar click on the down arrow and choose Logisitc sigmoid fit..

Figure 14 Logistic Sigmoid Fit functions.

2 Move the cursor to the plot in the graph, select the curve, then click and drag the cursor over the curve
to make the fit.

Figure 15 Make the fit by selecting the curve.

TAM Assistant Software Getting Started Guide Page 20

Logisitc sigmoid fit will display constants, C and A followed by the time constant (τ) and initial time (x0).
Std. dev is the standard deviation of the residuals and NDF is the number of data points used in the regres-
sion. Full equations utilized to create the fits are listed in the table below.
Table 5: .Equations for sigmoid fit functions

Model Fit Equation

Logistic Sigmoid

Sloped Logistic Sigmoid

Pythagorean Sigmoid

Sloped Pythagorean Sigmoid

3 From the toolbar, click on the down arrow and choose Baseline sigmoid (Figure 14 above). Move the
cursor to the plot and select a baseline section on the left side of the transition.
4 Click and drag the cursor over the curve and release the mouse button.

Figure 16

TAM Assistant Software Getting Started Guide Page 21

5 Now select the baseline on the right side of the transition in the same manner.

Figure 17 Select the baseline.

6 A baseline will now be displayed and the cursor will change to a hand. Click on the hand icon and drag
the vertical line to the midpoint of the transition. The baseline sigmoid fit displays and the integration
value calculated from that baseline displays in the window to the left of the graph.

Figure 18 Baseline Sigmoid Fit results.

TAM Assistant Software Getting Started Guide Page 22

Integrate Functions
There are five options for Integration functions.

Figure 19 Integration options.

1 From the toolbar click on the down arrow and choose the desired integrate function.
2 Move the cursor to the plot and select the curve then click and drag a region to integrate.

Figure 20 Select curve and integrate region; red shading indicates exothermic and green indicates
endothermic.

3 A linear baseline will be used with the basic integration function and the total integration of the curve
with respect to this line will be displayed in the window. Please note that if the curve is exothermic (or
up) relative to the integration baseline the shading will be red in color and if endothermic (or down) the
shading will be green (see Figure 20).

Integrate against baseline and Integrate two curves

Integrate against baseline works very similar to the two curve function (shown in “Additional Signal
Selections”); however, the integration is calculated relative to an extrapolated line defined by a baseline
section collected during an experimental wizard.

Integrate against extrapolated fit

Integrate against extrapolated fit will utilize any sigmoidal baseline analyzed like shown above; however,
the user will have the option to choose new x-axis or time limits of integration.

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Integrate against integral
Integrate against integral will integrate the curve using the running integral (or heat value) from time zero
of the selected range as the baseline for integration.
NOTE: Watch the sign for integrated values. Values for an exothermic integral will be displayed as posi-
tive values in TAM Assistant software; however, exothermic heat should be negative when used for calcu-
lation purposes.

Additional Signal Selections

All of the curve fit functions on the tool bar operate in the same manner as described above. However,
there are integration options that may require additional signal selections. One example shown here
describes the Integrate two curves function. Before proceeding, make sure all signals of interest are dis-
played on the plot.
1 From the toolbar click the down arrow of the integration icon and select Integrate two curves.
2 Move the cursor to the plot and select the positive curve, which is the curve of interest.

Figure 21 Select the positive curve.

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3 Select the negative curve, which is the curve that should be integrated against (e.g. a blank or baseline
curve).

Figure 22 Select the negative curve.

4 Once both curves are selected the cursor will change to an integration symbol. Now click and drag the
cursor over the curve and release the mouse button.

Figure 23 Integrated curves.

5 A value of the total integration with respect to selected curves will be displayed in the window. Please
note that if the curve is exothermic (or up) relative to the integration baseline the shading will be red in
color and if endothermic (or down) the shading will be green (see Figure 20 above).
NOTE: The color of the integral shading will depend on the order in which the two curves are selected for
analysis.

TAM Assistant Software Getting Started Guide Page 25

The Devices Explorer
In the Device group, the connected devices are listed in the group area. Different auxiliary devices like
pumps, mass flow controllers, etc. may be included, depending on the TAM configuration.
Click on a mini-view button under the Device group to open a new window in the view area, which is spe-
cific for the chosen device. If the chosen device is of a type that generates an output signal, the signal is
shown in a plot window with a graph of the signal evolution as a function of time.

The Thermostat Device

In normal operator mode, the thermostat device interface consists of three views accessed through the
Overview, Control, and Settings tabs.
Under the Control tab, the signal evolution of the thermostat temperature, as a function of time, is shown in
a plot window. See the previous section in this chapter, “TAM Assistant Plot Windows” for a description of
the plot window.

Changing Temperature Using the Control Tab

Follow these steps to change the temperature setting of the thermostat:
1 Access the temperature settings of the thermostat using the Control tab, see the figure below. The
temperature of the thermostat can be set to any value within 15 to 150°C for the oil based thermostat.
When using the water thermostat, the range is 15 to 90°C.
2 Enter the new value in the text box marked Temperature in the Set target temperature box to change the
temperature.
3 Click the arrow [->] button. The new temperature will appear in the corresponding text box under the
Current target temperature box, and the thermostat will start to adjust itself to the chosen temperature.

Figure 24 Control tab.

4 To decrease the time for the calorimeters to come to thermal equilibrium at a new temperature, click
Coax instead of the arrow. By doing this the temperature of the thermostat will be overset for a short
period of time, then decreased to the set temperature
5 To change the temperature in a controlled way, check the box Scan to target. There is now an option
to set the change rate or the time to reach a new temperature.

TAM Assistant Software Getting Started Guide Page 26

The target temperature will be reached within 10 to 60 minutes, depending on the magnitude of the temper-
ature jump. The rate of the temperature change is between 2 to 10 K h-1, depending somewhat on the abso-
lute value of the temperature.
If you attempt to change the temperature from the current value to an arbitrary value outside the specified
interval, an error message will appear and the command will not be implemented.

Setting a Safety Range Using the Settings Tab

Select the Settings tab to set a safety range of the thermostat temperature. If the Enable critical watchdog
box is checked, the thermostat will shut itself off, providing the temperature is outside this range. TAM III
will not restart after that. If the thermostat is shut down by the critical watchdog, it needs to be reactivated
when TAM III is manually started again.
NOTE: When loading an ambient temperature ampoule into a warm calorimeter (> 70°C) it is important to
utilize the temporary watchdog disable function shown in Figure 25 so that the TAM III does not automat-
ically shut down.

Figure 25 Settings tab.

The 4 mL Multicalorimeter Device

When you select the Multicalorimeter device in the Devices group, a view opens that lets you chose
between a number of views associated with the 3206 calorimeters.
In normal mode you can access three main views through the tabs—Overview, Signals, and Control.
Under the Overview tab the signal evolution can be followed as a function of time in a plot. See the previ-
ous section in this chapter, “TAM Assistant Plot Windows” for a description of the plot window.

TAM Assistant Software Getting Started Guide Page 27

The Signals Tab
Click on the Signals tab to display the following view for TAM 48 calorimeters. A similar view appears
for the TAM III 3208 Multicalorimeter .

Figure 26 Signals tab (TAM 48 calorimeter).

Each rectangle in the figure represents a calorimeter. In Figure 26 (above) there are 48 calorimeter chan-
nels installed on the system, and the current signal is displayed for each channel.
A red rectangle indicates that the signal from the calorimeter is not stable according to a specified stability
criterion. When the signal becomes stable according to the given criterion, the rectangle changes color to
green.
The criterion can be defined in the drop-down menu named Indicate signal stability. The signal stability
conditions include Low, Moderate, and High. The default value is Moderate. This is a criterion that
should be fulfilled by all calorimeters in a TAM III system. Stability criteria are given in Table 6.
Table 6: Stability criteria for 4 mL minicalorimeter device(s)

Slopemin Slopemax Deviation Window

/nW h -1
/nW h -1 /nW /min

High 50 500 100 30

Moderate 250 3000 200 20

Low 1000 5000 500 15

A stability criterion is composed of the three parameters shown in the table above.
• Slope is a fitted straight line (polynomial of order 1) by a minimization procedure.
• Deviation is the standard deviation of the residuals with respect to a fitted straight line.
• Window is the time interval for which the slope and deviation are calculated. The window is moving
stepwise with an interval of one second.

TAM Assistant Software Getting Started Guide Page 28

When the value for the slope is found to be below the Slopemin, the calorimetric signal is considered sta-
ble. After the value for Slopemin and Deviation have been met, the signal is considered unstable whenever
the slope is higher than Slopemax. In order for the signal to be considered stable, after it has become unsta-
ble, the criterion for Slopemin has to be met again.
In addition to the Slope, the criterion for the Deviation has to be fulfilled at all times in order for the signal
to be considered stable.
When None is chosen all rectangles changes color to white.
NOTE: The criterion chosen here acts locally, together with the diagram, and will not affect an ongoing
experiment since baseline criterions, etc. are chosen uniquely for each experiment during the start-up
phase. The purpose of this diagram is for information only.
The values of the Gain and Offset from the latest performed calibration are shown in the corresponding
text boxes only when one minicalorimeter channel is chosen in the drop-down list. The time for the last
calibration is also displayed.

Figure 27 Gain and offset values and time displayed in the control tab.

Controlling the Calorimetric Calibration Heaters

Under the Control tab of a calorimeter device, a form representing a user interface from which manual con-
trol actions of calibration heaters and calibrations according to a defined protocol can be made.
The channels to be included are selected from the drop-down list by clicking the down arrow on the right
side of the text field.
There are two calibration heaters for each calorimeter, one on the sample side (A) and the other on the ref-
erence side (B). A prefix, e.g., m, µ, n, etc., is entered automatically according to the magnitude of the
given heat effect, or it can also be inserted manually. The magnitude and duration of the heat pulse is
entered in the text boxes in the frame labeled Heater pulse.

TAM Assistant Software Getting Started Guide Page 29

Click Perform gain calibration in the Gain calibration section to initiate an electrical calibration. The cal-
ibration will run according to a defined protocol; see Chapter 2 for a detailed description.

Figure 28 Control tab.

The Gain and Offset values, from the latest performed calibration, are shown in the corresponding text
boxes only when one calorimeter channel is chosen in the drop-down list.

TAM Assistant Software Getting Started Guide Page 30

The 3201 Nanocalorimeter / 3220 Microcalorimeter Device
Select the calorimeter device in the Devices group to choose between a numbers of views associated with
the 3201 Nanocalorimeters (or the 3220 20-mL Microcalorimeter device).
There are three main views that can be accessed through the tabs—Overview, Control, and Settings.
The Overview tab allows you to follow the signal evolution as a function of time in a plot. See the previous
section in this chapter, “TAM Assistant Plot Windows” for a description of the plot window. The Control
tab is explained in the next section.

The Control Tab

The Control tab of the 3201 Nanocalorimeter Device (Figure 29) is used for manual control of the calibra-
tion heaters, and for performing calibrations according to a defined protocol. Other functions include con-
trols of Measuring principle and the Peltier regulator (or active heat sink control), which are described
below.

Figure 29 The Control tab.

TAM Assistant Software Getting Started Guide Page 31

Heat Pulse
Refer to Chapter 2, “Calibrating the TAM III Calorimeter,” for information on the Heater pulse functions.

Figure 30 Heater pulse function.

Activate Heat Sink Control

The Peltier regulator consists of a thermopile and a feedback mechanism. The thermopile thermally con-
nects the heat sink of the 3201 Nanocalorimeter and the 3220 Microcalorimeter to the thermostat liquid.
The thermopile senses whenever there is a measurable temperature difference between the surface of the
heat sink and the liquid in the thermostat. The feedback mechanism then sets in. The thermopile then
works as a Peltier element that “pumps” thermal energy to or from the heat sink to even out the tempera-
ture differences and reach thermal equilibrium between the thermostat and the calorimeters faster. This
function significantly speeds up the time needed for the calorimetric signal to stabilize after a temperature
change.
When changing the temperature of TAM III, click Activate Heat Sink Control. The button name changes
to Deactivate Active Heat Sink Control. Once the calorimeter has reached the set temperature, click the
button again to deactivate.
Measurement Principles
The 3201 Nanocalorimeter can be operated in accordance with three different measurement principles—
Heat flow (most common), Dynamic correction, and Feedback.

Figure 31 Measurement principles.

Use the Heat flow mode whenever processes have slow conversion rates, or when it is the thermodynamics
of the reaction that is of interest rather than the rate. If you are using the calorimeter as a titration calorim-
eter (or ITC, isothermal titration calorimetry), this mode should not be used.
In ITC experiments, you can operate the instrument in Dynamic correction mode to gain speed. Both the
Dynamic correction and Feedback modes use a mathematical procedure to correct for the thermal inertia of
the calorimeter. These modes, therefore, reflect the true heat production rate in the sample closer than the
heat flow mode.

TAM Assistant Software Getting Started Guide Page 32

You will need to perform a dynamic calibration when using the Dynamic correction mode to get time con-
stants for the instrument. This is not necessary for the Feedback mode, which uses counter power of the
calibration heaters. All measuring modes may use the same calibration, or gain factors. See below on how
to calibrate the heat flow.
Heatflow Calibration
Refer to Chapter 2, “Calibrating the TAM III Calorimeter,” for information on the Heatflow calibration and
Heater pulse functions.

Figure 32 Gain calibration.

The Settings Tab

Figure 33 The Settings tab.

Gain Selection
Gain selection has two options as seen in the figure below—Automatic gain selection and Low gain
always.

Figure 34 Set gain selection.

TAM Assistant Software Getting Started Guide Page 33

Automatic gain selection is used to help regulate the heat flow values. When the heat flow value, in abso-
lute terms, becomes larger than approximately 500 µW (or 480-580 µW depending on the calorimetric
temperature), the software will automatically turn to lower gain (i.e., lower resolution). When the absolute
heat flow decreases and becomes lower than 500 µW, the software automatically turns to a higher gain.
This option ensures that the highest resolution is given when measuring in the nanoWatt range. The resolu-
tion as given from the A/D converter is then approximately 0.2 nW.
When the software changes the Gain from high to low or vice versa, a minor disturbance in the heat flow
signal can occur. In order to avoid this, you can select Low gain always so that the low-resolution mode is
always on. However, this is not suitable for highly sensitive measurements, and should be used only when
signals higher than 2 µW are of interest. For most applications with the 3201 Nanocalorimeter, Automatic
gain selection is the preferred option.
Set Gain Calibration Settings
Refer to Chapter 2, “Calibrating the TAM III Calorimeter,” for information on gain calibration.

The 20 mL Multicalorimeter Device

When the 20 mL Multicalorimeter device is selected in the Devices group, a window opens that let you
choose between a numbers of views associated with the 3226 20 mL Minicalorimeters.

Figure 35 Views window.

To view and control features of the 3228 Multicalorimeter device in TAM Assistant, enter the Devices
explorer to the left of the TAM Assistant window and click the Device Mini-view button.
There are three main views that can be accesses through the tabs: Overview, Signals, and Control.

TAM Assistant Software Getting Started Guide Page 34

The Overview Tab
Under the Overview tab, the signal evolution of the heat flow from the calorimeters can be viewed contin-
uously as a function of time. When a pressure sensor is connected, the ampoule pressure can also be dis-
played, see the Pressure Ampoule Operator’s Manual for details. A more detailed description of the of the
functionalities associated with the plot window is found earlier in this chapter.

Figure 36 Overview tab.

The Signals Tab

Click on the Signals tab (Figure 37). A similar view appears for the 3208 Multicalorimeter of TAM III or
the TAM III 48 Channel instrument.

Figure 37 Signals tab (minicalorimeter)

Each rectangle in the figure represents a minicalorimeter. In this case, the three indicators represent the cal-
orimeters of a 20-mL Multicalorimeter and the current signal is displayed for each channel.

TAM Assistant Software Getting Started Guide Page 35

A red rectangle indicates that the signal from the Minicalorimeter is not stable according to a specified sta-
bility criterion. When the signal becomes stable according to the given criterion the rectangle changes
color to green. The criterion can be defined in the drop-down menu named Indicate signal stability. The
signal stability conditions include Low, Moderate, and High. The default value is Moderate. This is a cri-
terion that should be fulfilled by all calorimeters in a TAM III system. The values for the different stability
criteria are given in the table below.
Table 7: Stability criteria for 20 mL minicalorimeters

Slopemin Slopemax Deviation Window

/nW h-1 /nW h-1 /nW /min

High 50 500 100 30

Moderate 250 3000 200 20

Low 1000 5000 500 15

For a detailed explanation and definition of the stability criteria see “The 4 mL Multicalorimeter Device”
in this chapter.

TAM Assistant Software Getting Started Guide Page 36

Analyze Peak Function
1 From the toolbar click on the Analyse peak icon. Move the cursor to the plot, select the curve, then click
and drag the cursor over the curve to make the fit. (Figure 41).

Figure 38 Make the fit by selecting the curve

2 A linear baseline will be used and the total integration of the curve with respect to this line will be
displayed in the window among other calculated peak parameters (e.g. onset and peak height). See also
the document titled "Method for TAM III Validation: Heat of Fusion - Biphenyl," which describes the
use of this function to validate the enthalpy of a TAM III calorimeter.
NOTE: Watch the sign for integrated values. Values for an exothermic integral will be displayed as posi-
tive values in TAM Assistant software; however, exothermic heat should be negative when used for calcu-
lation purposes. In this example the melt of Biphenyl is an endothermic transition, but the enthalpy or
integral reported is negative.

TAM Assistant Software Getting Started Guide Page 37

The 3811 Flow Control Device
The Flow Control device controls the mass flow controllers, which are used for gases. The system can be
configured for flow-through using one gas, or it can be used for flow-mix systems with which gases are
mixed. In addition to the software module, the system consists of mass flow controllers connected to a spe-
cially-designed electronic interface.
In the case of flow-mix, the mixing can take place either outside the calorimeter or in situ in the measuring
ampoule depending on the ampoule design. The controlled RH perfusion ampoule is a special case. This
type of ampoule controls two mass flow controllers to set a mixture of a dry flow line, and a flow line sat-
urated with a vapor, most commonly water.
Click the Flow Control Mini-view button to display a view that is used for various settings and controls.
To set the value for the mixture and mass flow, enter the preferred value in the text box in Set wanted mix-
ture.

Figure 39 Flow Control Mini-view.

The total mass flow should not be higher than 200 mL h-1.
Click the arrow to apply the new settings; it will be displayed in the Current wanted mixture section on the
right-hand side of the window.

Setting Up a Ramp
The easiest way to set up a RH controlled ramp or step experiment is to utilize the specific Flow Control
wizard available when starting a new experiment.
The most convenient way to control mass flow controllers is to do it within an experiment. Using this
method, you can coordinate different events with respect to baseline and main sections.

TAM Assistant Software Getting Started Guide Page 38

You can use a Generic experiment or an Ampoule experiment, for example, to capture data while control-
ling devices directly from the Devices manager. Select the General tab as shown in the figure below.

Figure 40 General tab.

Follow these steps to set up a ramp:

1 Use the text boxes in the Ramp section to set up a ramp from the Device control. You can program both
linear continuous ramps and stepwise ramps.
2 Enter the duration, in seconds, for the overall ramp in the Duration text box. This value is independent
of the Linear or Stepwise ramp selection.
Example: Set up a stepwise ramp consisting of 4 steps where each step is 5% and the initial value is
10%. Let's assume that the calorimeter signal needs 30 minutes to reach stability after each step change
and it is stabilized before the ramp is initiated.
a Enter 10.0% in the Start text box and 30.0% as the end value.
b Enter 1440 seconds (240 min) in the Duration text box. This time will dispersed among the different
mixture values as follows: 30 min (10%) - 60 min (15%) - 60 min (20%) - 60 min (25%) - 30 min
(30%).
3 Click Start ramp to initiate the programmed ramp.

TAM Assistant Software Getting Started Guide Page 39

Controlling the RH Perfusion Ampoule
As already mentioned, a special case appears when using the RH perfusion ampoule. Since the mass flow
of the wet flow line increases when the incoming dry gas picks up vapor from the humidifier cups, the mix-
ture between the wet and the dry flow line doesn't correspond exactly to the relative flow rates as set by the
mass flow controllers. The software compensates for this automatically if the check box Use RH compen-
sation has been selected (as shown in Figure 41 below).
Choose the RH compensation when running the RH perfusion ampoule with water as the vapor.

Figure 41 Use RH compensation.

Leave this option blank when running other types of flow mix experiments (e.g., liquid mixing). If you use
vapors other than water, the compensation will be erroneous since that liquid has a vapor pressure different
from that of water. In such cases, the correction must be made manually after the experiment.
The setting in Set wanted temperature section (Figure 40) applies only to RH perfusion experiments. This
refers to an electrical heater mounted at the top of the RH perfusion ampoule. The function of this heater is
to warm the outgoing wet gas to a temperature above the dew point to avoid condensation inside the
ampoule. Set the temperature of the heater to the recommended value of 20°C above the TAM thermostat
temperature. If you chose the Relative bath option, the heater temperature will automatically be set to the
chosen value above the calorimetric temperature.
It is strongly advised not to heat the RH perfusion heater to temperatures above 80°C as this may shorten
the heater lifetime.
The procedure for setting up a ramp for an RH perfusion experiment is the same as described in the previ-
ous section.

TAM Assistant Software Getting Started Guide Page 40

The Experiment Explorer
TAM Assistant provides customized, step-by-step wizards that can be used to guide you through the pr
cess of running an experiment. Experimental wizards, specific to the type of experiment to be run, are
available. For example, you can use a wizard to set up a static ampoule experiment in isothermal or non-
isothermal mode.
A wizard consists of a number of dialog boxes, instruction views, etc., which appear consecutively in the
view area of the TAM Assistant main window, and prompt you to enter information about the experiment
or perform specified tasks. The wizard divides the experiment into different parts of pauses, baselines, and
main sections that are identified by the various analysis programs for performing automatic calculations or
model fitting to data. Figure 42 is an example of a view appearing in the ampoule wizard where decisions
about the initial baseline are entered.

Figure 42 Experiment Wizard–Initial Baseline.

NOTE: Exothermic data is positive and curves in the upward direction.

When the experiment group is shown, the names of the experiments that are currently running on the TAM
III system are displayed. Click a Mini-view button for a desired experiment to display its current status.
The signal evolution can then be viewed as a function of time. For a fast assessment of the current status
for an ongoing experiment, the Mini-view buttons contain information such as signal evolution and current
experiment section (initializing, main, baseline etc.).
Detailed descriptions of the experimental wizards and how to run different types of experiments are given
in Chapter 3.

TAM Assistant Software Getting Started Guide Page 41

The Results Explorer
When an experiment is finalized and saved, the results file will automatically appear under the Results
group in TAM Assistant Embedded. The filenames of earlier finalized, saved, and open experiments are
also listed.
Click on a filename to open the view for the chosen experiment in the view area. All information associ-
ated with the experiment, e.g., Experiment information, devices, raw data etc., can be accessed from this
view.
This is a result file where the results from 48 channels have been collected and saved in a single file. You
can show the result from all 48 channels in the same plot, or from a selected number of calorimeters by the
check boxes above the plot window.

Figure 43 Results file.

NOTE: Experiments saved on the TAM III embedded computer should be relocated to an external com-
puter at regular intervals to prevent over-burdening the memory capacity on the instrument system. The
procedure for moving or copying files to an external computer is described in the section called
“Downloading Results Files,” found in Chapter 3.

TAM Assistant Software Getting Started Guide Page 42

The Report Explorer
TAM Assistant contains a flexible environment for creation of laboratory reports. As mentioned previ-
ously, the report function is included in the external version of the TAM Assistant, but not TAM Assistant
Embedded.
Reports can be created manually, or by use of templates associated with various analysis programs. You
can also view data from different sources and perform interactive calculations and data fitting.

Creating a Results File Report

The report function can be accessed under the Results file report... in the File menu. In order to access the
Results file report function the results file for which the report is to be written should be open and shown in
the view area.
When chosen, a wizard opens that lets you determine which information to be included in the report
(Figure 44).

Figure 44 Results Report wizard–select information.

Choose the information and click Next.

TAM Assistant Software Getting Started Guide Page 43

The next dialog lets you select the signals and the type of plots to be included in the report. Many different
plots can be defined by pressing the plus sign by the Graph text box (Figure 45).

Figure 45 Results Report wizard–select signals and type of plots.

When the choices have been made click Finish to create the report.

Figure 46 Example report.

TAM Assistant Software Getting Started Guide Page 44

Once the report has been created it can be saved under a name and location of choice with the Save report
name or Save report name as… under the File menu.

The Graph Group (TAM Assistant Embedded)

The Graph group exists only in TAM Assistant Embedded and can be regarded as a stripped down version
of the Reports function in TAM Assistant.
Graphs from various plots in the Device group, Experiment group, or the Results group can be copied to a
separate plot placed in the Graph group. This may be done in order to compare plots from different experi-
ments.

Figure 47

Use the arrow and click within the domain of the graph that is to be added to the plot. Broken lines are
shown on both sides of the marked graph. Use the Add to graph menu to add the marked graph to an
already existing plot or to a new plot. You must select the down arrow in order for the option to be active.

Figure 48 Add to graph menu.

TAM Assistant Software Getting Started Guide Page 45

The added graph is online when chosen from a Devices group or the Experiment group. This means that
the signal evolution, as a function of time, is displayed in the plot of the Graph group.
However, if a graph from the Results group is added, the whole graph will be added to the plot with the
time scale preserved
.For each new plot created, a Mini-view button appears under the Graphs group.

Figure 49 Mini-view button.

Creating a Results File

Results Report Wizard
The report function can be accessed from the File menu by selecting Results file report. In order to access
the Results file report function the results file for which the report is to be written should be open and
shown in the results view area.
1 When chosen, a wizard opens that allows the user to determine which information to be included in the
report. Choose the information and press Next.

Figure 50 Results Report wizard–select information.

TAM Assistant Software Getting Started Guide Page 46

2 The next dialog window displays the signals and the type of plots to be included in the report. Select the
signals to be included in the report. Multiple plots can be defined in a single report by pressing the plus
sign by the Graph text box. Again, be sure to select the signals for the appropriate plot.

Figure 51 Results Report wizard–select signals and type of plots.

3 When the choices have been made, click Finish to create the report. The report will be displayed under
the reports view area as shown in the example.

Figure 52 Example report.

4 Once the report has been created, it can be saved under a name and location of choice with the Save
report name or Save report name as… under the File menu. Report files will be saved with a file
extension (.lrpt) that can be opened by TAM Assistant.

TAM Assistant Software Getting Started Guide Page 47

Creating and Manipulating an Overlay Plot or Report
This section will show an example on how to create an overlay or report from multiple signal curves
whether from a single results file or from multiple files.
1 Choose the Enter Selection mode icon from the tool bar in order to have the ability to select the data
to add to a report. If the cursor is not an arrow when placed onto the plot area the incorrect option may
be selected.

Figure 53 Tool bar.

2 Click the arrow cursor on the curve to add to a report. If multiple curves from the same screen or results
file are desired just use the CRTL button and click on multiple curves. Each curve should be highlighted
as shown in Figure 54.

Figure 54 Select curves.

3 Click on the Add to Graph drop-down arrow and select New Report.

Figure 55 Select New Report.

TAM Assistant Software Getting Started Guide Page 48

4 The curves selected will now appear under the Reports device menu.

Figure 56 Reports device menu.

TAM Assistant Software Getting Started Guide Page 49

5 The overlay plot can be saved directly by using the File menu and Save Report As function. Before
saving the report it may be useful to perform some simple analyses and change the plot properties. Figure
57 shows an example of the Integrate two curves function.

Figure 57 Integrate two curves.

TAM Assistant Software Getting Started Guide Page 50

6 Once integrated, a text box displays on the plot with the enthalpy calculated. Use the Enter Selection
mode arrow to move the text box or double-click on the text box to change font properties.
Properties of the plot can also be changed at anytime using the Enter Selection mode arrow by double-
clicking any region inside the graph. The Graph Properties dialog box displays, which has multiple tabs
for each curve shown on the plot. Figure 59 shows how the integration shading, background, line colors,
and line thickness can be changed. Use the Enter Zoom mode icon to change the scaling of the plot in
a report.

Figure 58 Graph Properties.

Figure 59 Changing integration shading, background, line colors, and line thickness.

TAM Assistant Software Getting Started Guide Page 51

NOTE: Watch the sign for integrated values. Values for an exothermic integral will be displayed as posi-
tive values in TAM Assistant software; however, exothermic heat should be negative when used for calcu-
lation purposes.
If curves from multiple results files are to be overlaid the process is the same: select the curve, click the
Add to Graph drop-down arrow, but then select the report and graph to add the newly selected curve(s)
from the drop-down list that appears.

Figure 60 Select report and graph.

Figure 61 shows an example of a three curve overlay plot created from two separate TAM results files.

Figure 61 Three curve overlay plot.

TAM Assistant Software Getting Started Guide Page 52

TAM Assistant in Network
TAM Assistant Embedded on the TAM III system is mainly used for running experiments and visualiza-
tion of signals and experimental data. TAM Assistant installed on a desktop computer can, in principle, be
used for all of the same operations as the TAM Assistant Embedded software. In addition, TAM Assistant
also contains powerful packages for data analysis, data export, creation of reports, etc. For this reason,
results data has to be transferred from the TAM III system to an external computer loaded with TAM
Assistant.
Therefore, the external computer must be able to communicate with the TAM III system in order to down-
load data. This communication is normally made through a local area network (LAN).
An external computer can also be connected directly to the TAM III system by use of an external network
card and a cross-over cable. It should be noted that the communication status of the TAM III system in a
local area network is comparable to that of a printer, i.e., it will not negatively affect any other components
on the network or beyond.
Communication between client computers on the network and the servers on the TAM III device is made
with dynamic IP addresses generated with DHCP.

Connecting TAM Assistant to a TAM III System

The following is only relevant for the external version of TAM Assistant.
To add (or remove) TAM III systems to TAM Assistant, follow these directions:
1 Select the File menu and choose Manage Connections.

Figure 62 File > Manage Connections.

TAM Assistant Software Getting Started Guide Page 53

2 Add or remove a connected instrument system along with its devices.

Figure 63 Manage connected servers dialog box.

3 Removing a system: Select the name of the system that is to be removed and click Remove selected
server(s). The header corresponding to the selected TAM III system disappears from the Devices group.
The removed instrument system can be added again at any time.
4 Adding a system: Click Add new server… The Add a new server dialog box displays. TAM Assistant
seeks out TAM III systems that are connected to the Local Area Network and lists the identified
instruments. Select the desired system from the list displayed. If the system that is to be added is not
included in the list, click the Add explicitly specified server option button and enter the IP number.
When the information has been entered, click OK.

Figure 64 Add a new server dialog box.

5 Click Done on the Manage connected servers dialog to return to the basic user interface. Within a few
seconds the added devices can be seen under the Device group.

TAM Assistant Software Getting Started Guide Page 54

Chapter 2:
Calibrating the TAM III Calorimeter

Background
Calibration helps to assure that the calorimetric signal, as delivered by the software, corresponds to the
heat flow generated by an arbitrary process. The calibration process closely mimics any measured process.
This is achieved by electrical heaters mounted in the sample holder in close proximity to the sample
ampoule.
In the TAM III System, the calibration procedures are included in the TAM Assistant software.
The primary signal, as generated by the heat flow sensors (thermopiles), is an electromotive force directly
proportional to a temperature gradient over the sensor. The gradient is a direct consequence of the heat
flow generated by an arbitrary non-inert sample in the calorimeter. The magnitude of the electromotive
force is directly proportional to the size of the heat flow.
The signals, as generated on the sample and reference side of the calorimeter, enter an amplifier where they
are differentiated and amplified approximately 100 times. An RC filter reduces the noise generated by the
amplifier. The bandwidth of the filter is 30 seconds, which is approximately 10 times lower than the time
constant of a calorimeter.
After the amplification step the filtered analog signal is converted to a digital signal by a 24-bit A/D con-
verter. The dynamic range of the calorimetric signal is -20 to 20 mV. This results in a resolution of 7 nW
bit-1 (the sensitivity of the heat flow modules are approximately 3 W V-1).
The digital signal is received by a software filter function with one data point per 1/10 second. The window
size of the filter function is one second, meaning that filtered data is collected with one data point per sec-
ond.
The next step in data processing is the conversion of the signal from the A/D converter digits to heat flow
values. The first step is the multiplication with a temperature-dependent calibration function, determined at
four different temperatures. This procedure is done before you receive your instrument. A certified service
technician should make subsequent temperature-dependent calibrations. The main reason for the tempera-
ture dependence is that the “Seebeck coefficient of the heat flow” sensors change slightly with changing
temperature.
Relative deviation from the temperature-dependent calibration constant (which is, unity, by definition) is
called the Gain factor. This is a factor that you will determine through the TAM Assistant software. Proce-
dures for the determination of the gain factor are described in detail in this chapter.
NOTE: For detailed information on running a TAM III experiment, refer to Chapter 3.

TAM Assistant Software Getting Started Guide Page 55

The Gain Factor
The calculated calibration constant is called a Gain factor, as described in the previous section. This factor
is independent of temperature to within TA Instruments specifications. The gain constant is always calcu-
lated relative to a temperature-dependent calibration factor. After a temperature-dependent calibration has
been performed, the gain factor in TAM Assistant is automatically set to one. A subsequent gain calibra-
tion reveals any deviation of the recorded signal relative to the expected signal. The result is expressed the
fractional deviation from 1. For example, a gain constant of 0.992 indicates a deviation of -0.8% from the
signal obtained by the temperature-dependent factor alone.

Calibration with TAM Assistant

Calibration Procedures
Electrical calibration with the TAM Assistant can be made directly from the device interface under the
Devices group, or while collecting data with the Generic experiment type.
The procedures are very similar, and the calibration experiment consists of a 10-minute baseline recording
followed by a heat flow release with the internal heaters of one hour. After the power has been switched
off, the calorimeter is given one hour to return to a steady baseline. A final five-minute baseline is
recorded.

Calibration Directly from the Device Control

Follow these steps to calibrate from the Device Control:
1 Click on the calorimeter mini-view button in the Devices group mode.
2 Choose the channels for calibration from the multicalorimeter drop-down list. One or more channels
can be chosen for simultaneous calibration.
In Figure 65, Channel 33 from the TAM 48 was chosen.

Figure 65 Device control calibration results.

TAM Assistant Software Getting Started Guide Page 56

3 Click the Signals tab to show the current signals from the calorimeters as shown in the figure below.

Figure 66 Current signals.

4 Select the desired Signal stability condition from the drop-down list (moderate is the default).
When the square representing the channel that is to be calibrated has the color green, the signal is stable
in accordance with the chosen stability conditions.
5 Click the Control tab to access the information shown in Figure 67.

Figure 67 Control tab.

NOTE: It is possible to abort the calibration at any time and the calibration values (i.e. gain and offset val-
ues) will not change from the previous calibration.

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6 Start the calibration by clicking Perform gain calibration. The time taken for a calibration is
approximately one hour for the 3206 calorimeters. A heat pulse of 3 mW is released by the inbuilt
calibration heaters during a time period of 30 seconds giving a total heat of 90 mJ. The Abort gain
calibration text on the click button will change back to Perform gain calibration when the calibration is
ready.
The new calibration constants will replace the old values when ready. It is not possible to change these val-
ues manually.
The calculated calibration values will remain until the next calibration is performed.

Calculation of the Calibration Constants

TAM Assistant automatically calculates the calibration parameters when the calibration recording is ready.
The two parameters calculated are the gain constants, described above, and an Offset value describing the
deviation of the steady state signal from the instrument zero level, i.e., no thermal activity in the calorime-
ters.

Calibration in a Generic Experiment

To save the data for the calibration in a results file, make sure that you perform the calibration while col-
lecting data to a results file. The Generic experiment type allows you to do this. This section describes one
of several different ways to perform a gain calibration.
1 Start a Generic experiment as described in Chapter 3, “Running Generic Experiments.” Include all the
calorimeters that are to be calibrated in the experiment.
2 Make sure that the signal is stable, according to the stability criterion, before starting the calibration.
The signal is stable when the background color in the current signal text box is green.
3 Start the calibration on several calorimeters simultaneously by marking more than one in the device field
to the left of the experiment view (see Figure 68 below). Simply press down the Ctrl or Shift key, while
clicking on the calorimeters to be calibrated.

Figure 68 Select multiple calorimeters.

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4 When the stability criterion is met click Perform gain calibration in order to start the calibration.
The text on the Perform gain calibration button changes to Abort gain calibration once the electrical
calibration has been started.
When the calibration recording is ready, the software automatically calculates a new calibration constant
and signal offset that automatically replaces the old values. The change of the calibration values is not
unique for the Generic experiment. The change is global, meaning that the calibration values under the
device control are also changed. These values will remain until the next calibration is performed.
When the text on the calibration button has changed back to Perform gain calibration, the calibration is
finished.
5 End the generic experiment.

Manual Calibration
You can also use an alternative method to perform calibration with more flexibility regarding the heat flow.
In this approach the calibration heaters deliver a thermal power of choice.
Follow these steps to manually calibrate:
1 Access the Control tab for the multicalorimeter device under the Devices group.
2 Mark the calorimeters to calibrate. Calorimeters 17-23 have been marked in Figure 69.

Figure 69 Mark the calorimeters.

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3 Wait until the stability criterion has been met. When the images representing each chosen calorimeters
have turned green, as shown in the Figure 80, the stability is reached.

Figure 70 Stability reached.

4 Click the Overview tab to access the plot window.

The first step in the calibration procedure is to determine the zero offset of each calorimeter. This is the
signal deviation from zero when there is no thermal activity in the calorimeters.
5 Click Set Offset in the tool bar of the plot window. The Lab Assistant dialog box displays.

Figure 71 Set Offset (left); Lab Assistant (right).

6 Click OK.

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7 Mark an interval of the stable baseline by clicking and dragging in the plot. A 20- to 30-minute interval
on the stable graph (or graphs) is sufficient for the software to calculate an offset that is representative
for the real case. See the figure below for an example.

Figure 72 Mark an interval of the stable baseline.

After the section has been marked, the offset from the zero level is calculated and the curve is shifted
to zero.
8 Turn on the calibration heaters as follows:
a Select the Control tab.

Figure 73 Control tab.

b Make sure that the channels to be calibrated are chosen.

c Enter a thermal power of choice in the Power text box.
d Leave the Duration text box empty. The heaters will run indefinitely and must be turned off manually
when the calibration is finished.

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 e Choose Side A (default) and click Start heater pulse. It is now seen in the plot (Overview tab) that
the signals are increasing towards a steady state value close to the entered power value.
f Wait approximately 1.5 hours to reach a true steady state.
9 When the steady state has been reached, and there are 10 to 20 minutes with a constant signal, press the
Define signal gain button in the plot tool bar.

Figure 74 Define signal gain.

The Define Signal Gain dialog box displays, unless the check box labeled Don't show this message
again, always … has been marked previously. The Expected signal text box has already been filled in
with the current power value of the heaters.

Figure 75 Define Signal Gain dialog box.

10 Click OK and mark a region of 10-20 minutes of the graph were the signal is at steady state. See the
image below for an example.

Figure 76 Signal at a steady state.

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 After the section has been marked, the offset from the true power value is calculated, and the curves are
shifted to the true power value.
11 Click Stop heater pulse under the Control tab to turn of the heaters. If only one of the calibrated
calorimeters is chosen at a time, the Calibration results can be seen in the Gain calibration frame.

Figure 77 Click Stop heater pulse.

In the procedure described for the manual calibration, the heat flow data has not been stored in a results
file. In order to collect data from a manual calibration, a generic experiment should be started before the
manual calibration starts. See the section in this chapter called “Calibration in a Generic Experiment.”
NOTE: The date for the Last gain calibration doesn't change when performing a manual calibration. The
date from the last automatic gain calibration remains.

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Dynamic Calibration
The heat flow produced by a sample or disturbance will be measured across the heat detector. However,
due to the heat capacity and heat exchange coefficient the heat flow monitored by the heat detector may be
different from the rate of heat production from the sample. For slow processes this effect is insignificant,
but for rapid processes this effect must be considered. From knowledge of the time constant of the calorim-
eter it is possible to apply a correction procedure termed the Tian correction (below).

Figure 78 Tian correction.

In this equation, PR is the raw data signal monitored by the heat detector and PC is corrected data, which
closely represents the true rate of heat production by the sample. The time constant (τ) of the calorimeter
can be calculated by using the calibration heater to apply known calibration powers in two consecutive
steps. The response on the heat flow will exhibit exponential curvature. An error function, representing the
sum of the squares of the difference between the estimated Pc and the actual calibration power, is calcu-
lated and a minimization routine is utilized to reduce the error function and calculate the values of τ1 and
τ2. TAM Assistant uses two time constants, rather than one, to get a better precision in the correction (cf.
Taylor expansion). In this case the fitting parameters has no relevant physical interpretation.

Performing a Dynamic Calibration

For fast reaction, i.e., in titration experiments, it is necessary to take into account the thermal inertia of the
calorimeter, ampoule and sample. This is done by running the experiment in a dynamically corrected
mode.
The nanocalorimeter and the 20-mL Microcalorimeter can be run in a dynamically corrected mode, and to
do this a dynamic calibration should be performed.
To perform a dynamic calibration, load the calorimeter with the ampoule (i.e., titration ampoule) in mea-
suring position and with the sample loaded. The reason for this is that the thermal inertia, τ, depends on the
heat capacity and heat transfer from the sample to the surroundings.
1 Lower the sample and reference ampoules into the calorimeter.
2 Wait for a stable baseline.
3 Click on the calorimeter device and on the Control tab.

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4 Select the Dynamic correction option button in the Set Measuring Principle section. See Figure 90.

Figure 79 Select Dynamic correction.

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5 Press the arrow to execute the command. The following dialog box displays.

Figure 80 Dynamic calibration information displays.

6 There are two options on the dynamic calibration:

a Perform time-constant calibration (quicker):
With this option only the time constants of the system is calculated. This option can be used if a full
dynamic calibration is previously performed with the same experimental setup. This would be done if
the sample volume is changed, solvent is changed or the stirring rate is significantly changed.
b Perform full dynamic calibration:
With this option time constants as well as Gain and Offset is calculated. This option should be used
when a new ampoule type is used.

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7 Press the button of the preferred calibration option. [The button will change to Abort Calibration while
the calibration is in progress.] The calibration will be automatic and the signal will look like the blue
curve below.

Figure 81 Red curve - Power to calibration heater; Blue curve - Measured heat flow.

8 When the calibration is finished, the button will change back to Perform Calibration. The values for
the time constants as well as gain and offset is now displayed.

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Chapter 3:
Running Experiments

Experimental Practices
This chapter deals with some practical aspects of experimental design and methods used to run experi-
ments. Balancing between the reference and sample sides of a calorimeter, especially the 3206 and 3226
minicalorimeters, is an important step that must be performed before running experiments. The noise level
of the calorimetric signal and thus the quality of the measurements may be affected if this is not performed.

Sample Ampoules and Reference Inserts

Each minicalorimeter is equipped with a reference ampoule holder similar in design to the ampoule holder
on the sample side of the instrument. Each reference ampoule holder contains an inert Aluminum reference
body, which is intended to balance the sample side relative to the reference side, with respect to the heat
capacity. An important purpose of this design is to reduce the short-term noise and also the offset signal
during a temperature scan. The long-term stability of the calorimetric signal is not affected by an unbal-
anced system.

The Reference Inserts of the 3206 Minicalorimeter

Each 3206 Minicalorimeter is equipped with a fixed reference insert. There are a number of reference
inserts with different mass to create heat capacity balance for a number of different applications. The refer-
ence inserts consists of an aluminum plug screwed into the reference side of the calorimeter.

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The Sample Ampoules
Selecting a reference insert depends on the type of sample ampoules that are to be used with the minicalor-
imeters, as well as the type and amount of sample.
The table below shows the heat capacities of the ampoules (empty) that are used for static measurements.
Table 8: Sample Ampoules

Product No. Cp,a /J K-1 Description

2509-51 2.34 5-mL Heat Seal Glass Ampoule

95.53.1015 4.32 3-mL Disposable Glass Ampoule

24.20.0400 5.84 4-mL Disposable Glass Ampoule

2502-40 11.9 4-mL Stainless Steel Ampoule Circlip Cap

2277-301 11.5 4-mL Stainless Steel Ampoule Threaded

Cap

3320 10.8 4-mL Stainless Steel Ampoule Threaded

Cap

3440-1 34 20-mL Stainless Steel Ampoule with

Threaded Cap

3348-1 53 20 mL Stainless Steel Ampoule (thick

walled) with Threaded Cap

24.60.2001 15 20 mL Disposable Glass Ampoule with Cap

(86.33.2000)

Balancing the 3206 Minicalorimeter

An ideal twin heat conduction calorimeter should not have any noise produced by the calorimeters other
than that produced by the electronics. This is because the differential nature of the measurements should
cancel out all thermal fluctuations from the environment. However, in our practical world it is not possible
to create a perfectly balanced system.
The lowest heat capacity on the sample side is achieved with an empty ampoule holder. The percentage
difference in heat capacity, for example, becomes -48.2% for reference insert 1, without any ampoule in
the holder. The minus sign implies that the mass should be increased on the side of the sample ampoule
holder in order to improve the balance and thus the noise level.
NOTE: The heat capacities given include all details that constitute the ampoules, i.e., caps, gaskets, eye-
lets, etc.

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For a given ampoule and reference insert the heat capacity balance can be improved by optimizing the
amount of substance in the sample ampoule. The percentage difference in heat capacity, between the sam-
ple and reference sides of a minicalorimeter, D, can be calculated by the following formula:

Figure 82 Equation for calculating difference in heat capacity between sample and reference sides.

Where:
Cp,ri = Heat capacity of reference insert

Cp,a = Heat capacity of ampoule

Cp,c = Heat capacity of the compound used in the measurement
7.18 = Heat capacity of the ampoule holder on the reference side, reference insert excluded
0.24 = The difference in heat capacity of the ampoule holders on the sample and reference side respec-
tively).
m = The mass (m) of the substance used, which can be optimized so that the absolute value of D
approaches zero.
The maximum deviation specification for the signal is ±20%.
Values of larger than 20% may be accepted in many cases as the quality of the measurements are depen-
dent on the signal to noise ratio rather than the absolute value of the noise level. A large sample size may
be preferred instead of a close balance if this results in a larger signal-to-noise ratio. It is important to note
that the specifications regarding the short term noise applies only when the heat capacity difference is
within the specified limits.

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Common Heat Capacities
In the table a few compounds are listed with the heat capacity at ambient temperature
Table 9: Heat Capacity at Ambient Temperature

Compound Cp /J K-1 g-1

Liquids
Water 4.18
Ethanol 2.43
Propanol 2.40
Benzen 1.73
Toluene 1.71
Pentane 2.33
Heptane 2.24
DMSO 1.93

Solids

Inorganic
NaCl 0.86
Quartz (SiO2) 0.76
Organic
Lactose 1.22
Urea 1.55
Glucose 1.24
Salicylic acid 1.16
Common gun powders 1.28

An Example
For this example the following are the experimental paramters:
• Sample is a water solution.
• Minicalorimeter 3206 is equipped with reference insert 1.
• Ampoule is the 3-mL glass vial.
• To get a perfect balance (D = 0), a mass of 0.61 g of solution is required as calculated by the equation
on the previous page.

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This would give the lowest absolute value of the noise level. However, it might not give the best signal to
noise ratio. If more sample mass can be used (in this case 3 g), the quality of the measurements might
improve. It is recommended that you take into consideration the positive and negative factors that are
unique for each experimental setup when planning the experiment.

Balancing the 3226 Minicalorimeter

Choosing the Correct Reference for the 20 mL Minicalorimeter

An idea of the experimental setup and choice of ampoule must be known in order to choose the proper
minicalorimeter with built-in reference. For best calorimeter performance, it is recommended to balance
the heat capacity (Cp) of both the ampoule and sample to within 20% of total reference Cp value. This Cp
balance is dependent on both choice of ampoule and sample loaded (material and mass). An example on
how to calculate the reference Cp is given below. Please refer to Table 1 that lists the total Cp of all 8 mod-
els of the 20 mL minicalorimeter references. For aid in sample Cp calculations, utilize Table 2 for a list of
some common sample materials.
Table 10: Heat Capacity of 20 mL Minicalorimeters
20 mL ampoule 3440-1 3348-1 Glass

Ampoule Cp (J/K) 34 53 15

Reference Total Cp (J/K) Sample Cp (J/K)

Number

X=1 29 14 ± 5.8

X=2 37 3 ± 7.4 22 ± 7.4

X=3 46 12 ± 9.2 31 ± 9.2

X=4 53 19 ± 10.6 38 ± 10.6

X=5 57 23 ± 11.4 4 ± 11.4 42 ± 11.4

X=6 62 28 ± 12.4 9 ± 12.4 47 ± 12.4

X=7 66 32 ± 13.2 13 ± 13.2 51 ± 13.2

X=8 71 37 ± 14.2 17 ± 14.2 56 ± 14.2

An Example
Sample of gunpowder loaded into a minicalorimeter with reference number 6 (62 J/K):
Using a stainless steel threaded ampoule (3440) with Cp of 34 J/K the remaining heat capacity to balance
the calorimeter is 28 J/K. Knowing the sample is gun powder that has a Cp of 1.28 J/g K one can calculate
that approximately 22 g 9.6 g of gun powder must be loaded into the ampoule to best balance the calorim-
eter to within 20% of the total reference Cp.
NOTE: Operation of an unbalanced calorimeter may lead to increased short term noise in the heat flow
signal.

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Sealing a Glass Ampoule
1 Tare the ampoule with or without the cap and load the sample. Record the mass of the sample.
2 Use the crimping tool to crimp the cap in place. Be sure to press the crimping tool firmly onto the cap
and ampoule. Then squeeze the crimping tool handle until the crimp stop is reached (Figure 83). If an
adjustment to the crimping tool is necessary, please refer to instructions included with the crimping tool.

Figure 83 Crimp the ampoule cap.

NOTE: Test that the cap is sealed by twisting the cap. If there is any movement in the cap, try to crimp
again and/or adjustment to the crimp stop may be recommended.
3 Place the adjustment tool over the aluminum cap and squeeze the handles a couple of times while rotating
the ampoule so as to flatten the side surface of the cap (Figure 84). The cap adjustment tool could slightly
loosen the cap seal. It is suggested to again test the cap seal by attempting to rotate the cap.

Figure 84 Cap adjustment.

NOTE: Test for alignment - Without squeezing the adjustment tool move the tool up and down over the
ampoule and cap. If the tool moves freely than no further action is required. If the tool does not move
freely over the cap this indicates that the cap is distorted, and therefore will not load smoothly into the cal-
orimeter. Please attempt to reseal and adjust the cap and if not successful it would be best to discard that
ampoule.

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4 With the ampoule inside the centering tool, press the center pin downwards to mark the center of the
aluminum cap (Figure 85). Remove the centering tool and there should be a small indentation on the
ampoule cap. This indentation is used as a starter guide for threading the lifting eyelet in step 5.

Figure 85 Using the centering/tolerance tool (left) and the resulting indentation in the cap (right).

5 Push an ampoule lifting eyelet or loop into the center indentation or mark on the cap and screw to tighten
(Figure 86). Do not over-tighten the lifting eyelet as this will lead to striping the aluminum cap and the
eyelet will not hold in place. Check that the eyelet is squarely and securely fitted to the cap.

Figure 86 Attach the lifting eyelet or loop (3 mL - left, 4 mL - right).

NOTE: Do not to throw away the lifting eyelet. After an experiment is completed, remove the lifting eye-
let from the ampoule for reuse.
6 Wipe off any residual sample and finger prints from the ampoule using a clean and dry fiber-less cloth
before loading the ampoule into the calorimeter.

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Running Experiments
The remainder of this chapter describes how to run experiments with TAM Assistant, using the experimen-
tal wizards. Initiating, running, and finalizing experiments with TAM Assistant are described in detail. The
images used throughout this chapter are from TAM Assistant Embedded. Although the user interface of the
TAM Assistant is somewhat different than that of TAM Assistant Embedded, the procedures of designing
and running experiments are identical in the two versions.

Starting a New Experiment

When starting a new experiment, independent of what type, select Experiment from the New menu.
1 Choose the type of experiment from those shown in the New Experiment window.

Figure 87 New > Experiment.

There are six basic types of experiments included in TAM Assistant: Ampoule and Non-isothermal
ampoule experiments, Validation, Titration, Flow control, and Generic experiments.
Generic experiments are the simplest type. In Generic experiment, data is collected without any division
into pause, baseline and main sections. Actions such as a temperature jump or scan can be implemented
in a generic experiment, but it has to be made manually under the device group. See the next section for
more details on Generic experiments.

Figure 88 New Experiment.

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2 Enter Experiment name. The experiment name is the filename where the result and additional information
is stored. A default name, stating the type of experiment and date will automatically appear as the
experiment name. You can alter this name, if desired.
3 Enter the Operator’s name or initials.
4 Click OK.

Running Generic Experiments

The Generic experiment is the simplest type of experiment run by the TAM Assistant. It may be considered
as pure data collection and the collected data is not divided into baseline, pause, or main sections. This
means that there are no possibilities to perform baseline corrections on saved data or data analysis using
the special analysis functions in the TAM Assistant.
Actions such as a temperature jumps or scanning can be performed in a generic experiment, but the neces-
sary control actions has to be made manually from the thermostat device in the Devices group.

Setting Up a Generic Experiment

1 Choose the Generic type of experiment from those shown in the New Experiment dialog. The dialog
shown in the figure to the right is displayed.
2 Select the device(s) to be included in the experiment. Click Next. An Add Device dialog box displays
(Figure 89).

Figure 89 Add Device.

3 Click on the calorimetric channels that you want to use in the experiment. To choose several channels,
press and hold the Ctrl-key, while clicking the respective channel(s). (You can also click on one channel
and drag the cursor over the remaining channels that you wish to select).
4 Choose from a set of security options in the Add Device: Choose Calorimeter dialog box (Figure 90):

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NOTE: If channels are occupied by another experiment (Figure 90), they will be displayed red. The color
on top of the channel turns green as it is chosen.

Figure 90 Add Device: Choose Calorimeter dialog box–channels occupied.

If you select the option Write lock wanted, the minicalorimeters will not be available for different kinds of
control actions from other experiments, i.e., others cannot write to the devices.
• If you choose the option Read lock wanted, it is not possible for any other experiment (and, therefore,
other users) to collect data to another experiment.
• If you select No device lock wanted, full access to the chosen devices are possible from other experi-
ments and users.

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5 Click Next. The Add Device dialog box shown in Figure 91 displays.

Figure 91 Add Device.

6 Select the type of experimental information to include in the results file using the two drop-down menus
are provided.
If None is chosen in both drop down menus, no sample information can be included in the experimental
file.
NOTE: The choices made on experimental information cannot be changed after the experiment.
7 Click Finish to start the data collection. A mini-view button (Figure 92) appears in the Experiment group.
This can be used to check the progress of the experiment at any time.

Figure 92 Mini-view button.

NOTE: Experimental information can be entered while the experiment is running or after the experiment
has been saved in an experimental file.

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Adding Additional Devices
At this stage you can add more devices than were selected before the data collection was initiated. For
instance, the thermostat device or additional minicalorimeters can be added.
To add a new device follow these steps:

8 Click the Add Device button . The dialog shown on the next page appears.

9 Select the device to add and click Next. A dialog is displayed to allow you to decide on experimental
information, see the previous page for details.
10 Click Finish in order to start the data collection from the newly added device.

Setting the Experiment Start

After the collection of data has been initiated, you can set the time to begin data collection.

11 Click Set Experiment Start . The following dialog displays.

Figure 93 Set Experiment Start dialog box.

12 Move the cursor to the time marker labeled Experiment start. Drag the time marker to the start time of
choice. This can be done back or forward in time.

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Finalizing a Generic Experiment
You will need to manually finalize data collection in a Generic experiment in order to save the data in a
results file.
13 Click End Experiment in order to finalize the data collection. An End Experiment dialog box displays
to let you decide whether to end the experiment and, if so, discard the results or reduce the experimental
data. How data reduction is performed is described in the Ampoule experiment section below.

Figure 94 End Experiment.

Ampoule Experiments
An Ampoule experiment is a static form of calorimetric experiment. In other words, there is no control of
auxiliary devices such as the stirring motor, the mass flow controllers for perfusion, or the pumps for injec-
tion. The ampoules containing the sample are either metallic (stainless steel or hastelloy) or disposable
glass vials.
You can use the Ampoule experiment wizard to guide you through a number of steps where instructions on
operational details are given. You will need to enter information about the experiment throughout the wiz-
ard.
Ampoule experiments can be run in isothermal or non-isothermal mode. An experimental wizard exists for
each of them. In this section the ampoule wizard is described in detail. Additional features belonging to the
non-isothermal ampoule wizard are also described, e.g., how to define a temperature program etc.

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The Ampoule Wizard
Follow these steps to run the Ampoule wizard:
1 Select Ampoule experiment and click OK. The first dialog is displayed, together with an icon under
the Experiment Manager. The icon shows the experimental name and the current status of the experiment.

Figure 95 Welcome to the ampoule experiment wizard.

2 Click Next to continue.

3 Choose the calorimeter channels to use in the experiment by clicking on the channel in the figure. To
choose several channels, press and hold the Ctrl key, while clicking the respective channel(s). (You can
also click on one channel and drag the cursor over the remaining channels that you wish to select).

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NOTE: If channels are occupied by another experiment (Figure 96), they will be displayed as red. The
color on the top of the channel turns green as it is chosen.

Figure 96 Select calorimeter channels.

4 Click Next.
At this stage, the chosen channels are listed under the tab labeled Devices (see below). By marking a calo-
rimeter device on the left, a view appears that lets you control the actions of the device and/or examine the
status (e.g., signal evolution). A plot displays the signal from the chosen device.

Figure 97 Control the device.

It is possible, at this stage, to add additional devices such as an additional minicalorimeter.

5 Click Add Device at the top left of the main program window (Figure 98). This opens a window allowing
you to choose additional device(s) to add.

Figure 98 Add Device.

6 Return to the Experimental wizard and click Next.

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Ampoule Wizard Results Tab
At this point in the Ampoule wizard a new tab is displayed labeled Results (Figure 99).

Figure 99 Results tab.

7 Enter experiment information under the Results tab (sample size, concentration etc.).
a Select the Sample tab to enter experimental information such as the name of substance, lot/batch
number).
b Select the Administrative tab to enter information such as the project name, affiliation etc.
c Choose the General tab to view the Experiment Start, Stop and Temperature field, which will be
entered automatically during and after the experiment. Any text can be entered in the field labeled
Additional information.
8 Return to the Experiment wizard and click Next.

Normalization Criteria for the Signal

This window in the Experiment wizard lets you enter information on how the signal should be normalized.

Figure 100 Define normalized signal.

9 Determine how to normalize the signal. Choose the desired options from the available drop-down lists.
The information on sample size of the component(s) is optional.
10 Select the Experimental wizard tab, then click Next.

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Decide about Initial Baseline
The next window (Figure 101) lets you decide about initial baseline for the experiment. You can enter the
time for recording the baseline. The default value, as given by the software, is 30 minutes.

Figure 101 Decide about initial baseline.

The baseline can be started manually, when desired, or automatically, when the signal is stable according
to a specified baseline criterion. The default value for the stability criterion as entered by the software is
moderate signal stability condition. These values will vary depending on calorimeter type.
11 Select the duration and stability conditions for the initial baseline. If the check box Use baseline average
as signal offset is marked, TAM Assistant automatically uses the calculated mean value of the initial
baseline to correct the signal in the main part of the experiment.
12 Click Next to continue.
Usually the baselines are run without an ampoule in the measuring position in order to be sure that no off-
set due to any thermally activity is recorded.
When you are sure that the measuring position of the minicalorimeter is empty, you may start the experi-
ment.

Figure 102 About to start the experiment.

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13 Click Start. The following window appears. The green curve indicates the baseline and the grey part of
the curve indicate the pause section prior to the baseline. The baseline section starts as soon as the chosen
Signal stability condition is met.

Figure 103 Initial baseline.

14 Running initial baseline: The program counts down the time specified for the baseline duration, and the
remaining time is specified in the text box labeled Time left. When the baseline recording is finalized,
you are instructed to introduce the sample ampoule into the equilibration position. Proceed to the next
section.

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Thermal Equilibration of the Sample
The sample has to be thermally equilibrated to the calorimetric temperature before the actual measurement
can be started. Follow the instructions given.
15 Carefully and slowly lower the sample into the equilibration position of the calorimeter.

Figure 104 Lower sample into equilibration position.

When lowering the sample into the equilibration position a disturbance of the signal is seen. This
disturbance originates from temperature differences between the sample and the calorimeter.

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16 Click Mark when the ampoule is in position. The software starts to count down the time starting from
15 minutes. This is the normal time required for the sample to equilibrate, and reach the same temperature
as the bath. The following dialog displays.

Figure 105 Waiting for sample to equilibrate.

17 Wait for equilibration to be reached. If the sample has a large mass and there is a large difference in
ambient temperature and that of the TAM thermostat, more than 15 minutes may be necessary for sample
equilibration. Keep the sample in the equilibration position for as long as needed to bring both the
ampoule and sample to the thermostat temperature. Thus, determination of the length of appropriate
equilibration time may be necessary for each experimental condition.

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Insertion into the Calorimetric Measuring Position
After 15 minutes of equilibration you are prompted to lower the sample into measuring position.

Figure 106 Lower sample into measuring position.

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18 Click Mark, and lower the sample ampoule slowly into the measuring position. This introduces an initial
disturbance of the signal, mainly caused by the friction generated between the sample holder and the
walls of the ampoule, as the ampoule is introduced into the ampoule holder of the calorimeter.

Figure 107 Waiting for signal to be considered correct.

The software waits until the signal is considered correct, that is free from the disturbances generated
because of the introduction of the sample ampoule. The default time is 45 minutes.
You may want to click Skip wait and mark button in case the signal is known to be correct before the
default time. The graph appearing after the mark is red, indicating the main part of the experiment.

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Managing the Main Part of the Experiment
When the time taken to reach a stable signal has passed, a time marker will appear labeled Signal correct.
At this point the signal is considered correct from the instrument’s point of view. Unwanted effects in the
sample such as redistribution of solvent in a solid sample, or different types of sorption phenomena, etc.,
which might occur when the sample is exposed to sudden temperature changes, is not included. To avoid
such unwanted effects, the sample should be well conditioned before the experiment.
19 Click End main when the main part of the experiment is considered to be ready. A new dialog displays
so that you may decide about the final baseline.

Figure 108 Running main part of experiment.

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Decide about Final Baseline
1 If the Want final baseline check box is marked (Figure 109), the software will wait for the signal to
become stable according to the chosen signal stability conditions.

Figure 109 Want final baseline.

2 Select the duration and stability conditions for the final baseline and click Next.
You will be prompted to remove the sample ampoule (or ampoules) from the calorimeter.

Figure 110 Remove sample ampoule(s) from calorimeters.

3 Remove the ampoules. After removal, place the ampoule lifter back in position then insert the lifters
into the lowered position.
4 Click Next when the ampoules has been removed. The software now waits until the chosen stability
criterion is met before starting the final baseline.

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You can follow the current slope and standard deviation for any channel in the experiment by choosing the
channel in the drop-down menu above the plot window.

Figure 111 Select the channel; Manual baseline start.

To manually start the baseline before the stability criterion has been reached, click Manual baseline start
(Figure 111 above).

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When the signal is stable in accordance with the set stability criteria, the final baseline section will start.
The plots change color from gray to green when the baseline starts.

Figure 112 Plots change from gray to green.

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5 When the final baseline recording is finished, a new window in the wizard automatically appears to let
you adjust the time settings. This may be done if the previous time settings are considered to be incorrect,
e.g., the duration before the signal was considered correct.

Figure 113 Adjust times (if necessary).

6 Click and drag a section change time marker to the correct time. Then adjust the time settings, using the
drop-down list, if necessary. Click Next.

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Decide on Experimental Data Reduction
In all experiments, data points are collected approximately every second. When running either the
Ampoule or Non-isothermal Ampoule wizard you have the opportunity to choose how to save the data
after the experiment. The following form appears when the experiment has been finalized in which one can
decide one of two data reduction methods—Equidistant and Adaptive.

Figure 114 Decide on experiment data reduction.

The default is always Equidistant with 6000 data points independent on the length of the experiment. The
results of the reduction are previewed in the Results frame with the approximate delta-time (rounded to 1
second) and the approximate size of the results file.

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In Adaptive mode, the chosen number of data points is dispersed to give a higher data point density in
parts of the experiment with high rate of change in the measured property, i.e., during a phase transition
after a period of relative calm.

Figure 115

The upper part of Figure 115 shows results of equidistant data distribution (500 points over approximately
8 hours). The lower part shows how the data points have been smoothened by use of the adaptive mode for
the same total number of data points.
7 Click Next. A new form appears to let you finish the calorimetric experiment.
8 Mark the check box if the results file should not appear.
9 Click Finish.
The results have now been saved as a results file. To view the results file, click the mini-view button repre-
senting the file under the Results group.

Ampoule Experiment–STANAG 4582

This section describes the general procedure for measuring stability of propellants with the TAM III
equipped with a multicalorimeter (4 mL) using 3 or 4 mL disposable glass ampoules or vials as calorimet-
ric sample vessels. Emphasis has been put on measurement according to the STANAG 4582 procedure,
which was designed to standardize a stability test procedure for single base (SB), double base (DB), and
triple base (TB) propellants using isothermal heat flow calorimetry (HFC). Measuring temperatures for a
STANAG test should be between 60-90 °C, and the duration (tm) of the experiment for different tempera-
tures is given in Table 1. Please also refer to the “The Ampoule Wizard” section of this manual.
NOTE: The STANAG procedure does not imply that a propellant with a higher heat flow is less stable
than one with a lower heat flow. Comparison is only meaningful for propellants of similar composition.
CAUTION: Please read the STANAG safety issues from the Appendix below before continuing.

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1 When starting a new experiment, regardless of what type, click Experiment in the tool bar.

Figure 116 New > Experiment.

2 A New Experiment dialog box displays, allowing you to select a number of experiment types. Click
Ampoule and then select STANAG 4582.

Figure 117 Ampoule > STANAG 4582.

3 Enter the Experiment name and the Operator name. Click Next to continue.
NOTE: The experiment name is the file name where the result and additional information is stored. As the
new experiment type is being chosen a default name stating the type of experiment and date will automati-
cally appear as the experiment name. However, the operator can enter any name. The operator name or ini-
tials is obligatory.
4 Select the channels that are to be used in the experiment by clicking the calorimeter channels desired.
Click Next.
NOTE: Several minicalorimeters can be chosen by pressing the Ctrl-key while clicking on the channel(s)
or alternatively by clicking on one channel and drag the cursor over the other channels to be used.

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5 Enter the experiment and sample information (Figure 119) and click Next.

Figure 118 Enter experiment and sample information.

The information on sample size of the component(s) is optional, but cannot be entered after the experiment
has been initiated due to the STANAG analysis operation in TAM Assistant. Thus, if using the STANAG
analysis feature in TAM Assistant a mass of the material must be entered at this point.
6 In the Define normalized signal screen, select the sample mass to be normalized against and click Next.

Figure 119 Define normalized signal.

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7 Decide about initial baseline for the experiment.

Figure 120 Decide about initial baseline.

• The time for recording the baseline can be entered in the Baseline duration text box. The default value
is 30 minutes.
• Select the Automatically start baseline based on signal stability conditions option to start the base-
line manually or automatically when the signal is stable according to a specified baseline criterion.
• Select the signal stability conditions in the drop-down list. The four options available are High, Mod-
erate, Low, and Advanced. The Advanced option allows for manual selection of the stability condi-
tions and time period mentioned. The default value for the stability criterion is Moderate signal
stability condition.
• If the check box Use baseline average as signal offset is marked, TAM Assistant automatically uses
the calculated mean value of the initial baseline to correct the signal in the main part of the experiment.
After the experiment has been finalized you can use more advanced baseline correction with initial/
final baselines using linear slope corrections or polynomial correction.
8 When you sure that the measuring position of the minicalorimeter is empty, click Start.

Figure 121 About to start the experiment.

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9 The Initial baseline window displays..

Figure 122

The green curve indicates the baseline section and the grey part of the curve indicates the pause section
prior to the baseline. The baseline section starts as soon as the chosen signal stability conditions are met or
if manually initiated. The program counts down the time specified for the baseline duration and the
remaining time is specified in the text box labeled Time left. When the baseline recording is finalized the
user is instructed to introduce the sample ampoule into the equilibration position. As the baseline is being
collected it is a good time to load the propellant into the sample vessel.

Preparing the sample and filling the ampoule

Prepare the sample
If possible, the propellant should be measured in its original condition and representative of the batch or lot
to be tested. The sample should be filled to the top of the ampoule in order to minimize the amount of air in
the head space. The resulting loading density (mass / ampoule volume) should fall in the range 0.8-1.1 g/
mL.
Alternatively, the loading density of the ammunition defined for the propellant in test may be used for the
HFC measurements. Use approximately the same loading density for replicate measurements. Different
atmospheric conditions may affect the decomposition rate and give slightly different HFC results. For
safety reasons the sample size can be reduced. In this case, the free volume inside the ampoule should be
filled nearly completely with an inert material, such as a glass rod or fine glass beads.
NOTE: If the volume of the sample vessel is too small to fulfill the appropriate loading density the propel-
lant should be cut or ground to 1-2mm particles and the mass used should be taken from a well mixed frac-
tion.
A balance should be used that can measure 1–5 grams material with a precision of at least 4 significant fig-
ures.
Fill the ampoule
1 Place an empty ampoule or vial on the balance and note the mass or tare.
2 Fill up the ampoule with the sample to be measured.

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3 Record the exact mass.
4 Seal and align the ampoule cap and then insert the lifting eyelet in order to load the ampoule into the
TAM calorimeter.
For further details on sealing the ampoule see the section titled “Sealing a Glass Ampoule” .

Loading, equilibration, and measurement

After sample ampoule preparation, the ampoules should be loaded carefully so that there will be minimal
disturbance to the temperature equilibrium of the thermostat. The sample has to be thermally equilibrated
to the calorimetric temperature before the actual measurement can be started.
When the baseline section has been completed the next window of the STANAG wizard will ask to lower
the sample(s) into the equilibration (or magnet stopped midpoint) position as shown in Figure 123.
NOTE: It takes approximately 30–60 min from the time the sample is loaded into the equilibration posi-
tion until actual heat flow measurement can begin, i.e. the measured signal can be considered correct.

Figure 123 Lower sample into equilibration position.

1 Slowly remove one of the ampoule lifters from the calorimeter cylinder. Use a steady movement over
about 15 seconds to minimize frictional heating and air disturbances.
2 Without touching the ampoule with bare hands, immediately hook one of the ampoules onto the lifting
tool hook. Then carefully and slowly load the sample ampoule into the equilibration position (or magnetic
held midpoint) of the minicalorimeter.
3 Remove the lifting tool from another calorimeter tube and immediately load the second ampoule into
the equilibration position in exactly the same way.
4 Once all samples are introduced to the equilibration position click the Mark button. The software starts
to count down from 15 minutes.
NOTE: Equilibration time can be reduced if the sample and ampoules are brought to temperature in an
external heater block or water bath prior to loading into the calorimeter. This is especially true for the
STANAG experiments, which are performed between 60 and 90°C.

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If the ampoules have been equilibrated to the thermostat temperature prior to loading, only about 10 min-
utes should be required to reach equilibrium. If there is a significant difference in temperature between the
ampoule and sample compared to the thermostat than more than 20 minutes may be required for equilibra-
tion.
When lowering the sample into the equilibration position a disturbance of the heat flow signal can be
observed. This disturbance originates from the temperature differences between the sample ampoule and
the calorimeter or thermostat and the cold air introduced to the calorimeter.

Figure 124 Waiting for sample to equilibrate.

5 After 15 minutes equilibration, you are prompted to lower the sample into the measuring position. Lower
all samples slowly all the way down into the measuring position and then press Mark.
6 Again, lowering the ampoule will introduce an initial disturbance in the signal mainly caused by the
friction generated between the sample holder and the ampoule walls. Another countdown will be initiated
as the software waits until the heat flow signal is considered correct. The heat flow signal is considered
correct when free from the disturbances generated due to ampoule introduction. The default time is 45
minutes, but can be adjusted later in the experimental wizard.
7 Press the Skip wait and mark button in case the signal is known to be correct before the countdown is
finished. The graph appearing after the “Signal Correct” mark is red, indicating the main part of the
experiment. Leave the experiment wizard running until the time recommended by the STANAG 4582
(Refer to Table 14 in the Appendix).
8 Press the End main button when the main part of the experiment is considered to be complete.
The remaining of the wizard is identical to that described in “The Ampoule Wizard” and will only be
described in brief detail here. For further detail please refer to the respective section of this manual.
9 A new dialogue window appears about the final baseline. Select the necessary boxes, conditions and
then click Next.
10 If a final baseline is selected the software will prompt the user to remove all sample ampoules. Click
Next when all ampoules have been removed.

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11 The next window allows for time setting adjustments. This may be done if the previous time settings
are considered to be incorrect, e.g. the duration before the signal was considered correct. Click and drag
a section change time marker to the correct time as needed. Click Next.
12 The next window allows experimental data reduction. The default values of equidistant and 6000 data
points are sufficient for STANAG 4582 measurements. Click Next and then click Finish. The results
have now been saved as a results file (.rslt) that can be viewed under the Results devices group.
NOTE: The TAM III thermostat must remain ON at all times in order to be stable for measurements. If
further experiments are to be made at a different temperatures, set the new bath temperature and allow a
minimum of 12 hours for the TAM III thermostat to equilibrate to the new temperature before proceeding
with additional experiments.

Non-Isothermal Measurements
Most features of the Non-Isothermal Ampoule Wizard are similar to the Ampoule wizard described on the
previous pages. In the non-isothermal ampoule wizard a window for the definition of a temperature pro-
gram is included. The temperature program can be continuous, i.e., scanning or stepwise temperature
jumps.

Figure 125 Define reference experiment.

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Setting Up a Temperature Profile
The following is an example of how a continuous wizard is defined.

Figure 126 Define temperature profile.

In Figure 126, the settings for a scanning experiment are displayed. The initial temperature is set to 20°C,
and normally a stable signal is achieved before the scanning initiates. It is seen that the final temperature of
80°C should be reached after 30 hours, leading to a scanning rate of 2°C/h. The experiment is finalized
with a down scan to 20°C. The scanning periods are initiated manually as indicated in the example.

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The temperature profiles can also be defined as stepwise as shown below.

Figure 127 Define temperature profile.

In this example a stepwise temperature profile is defined. The initial temperature is 20°C, with duration of
2 hours, followed by a number of 6 hour steps with 10°C intervals up to 60°C. The experiment is finalized
by decreasing the temperature to 40°C. The duration of each step is chosen as the shortest corresponding to
the fastest temperature change rate. The fastest achievable temperature change varies in the interval 2-10
Kh-1, depending on the absolute temperature, and whether the change is cooling or heating.
NOTE: The maximum time to wait for stability conditions can be entered. The means that the temperature
change will take place, if the conditions have not been met within the specified time period.
1 Set up the desired temperature profile.
2 Click Next. A new window is displayed to allow you to define the initial and final baseline.

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Defining a Baseline
You can collect a baseline with the sample ampoule inserted by marking the check boxes as shown in the
figure below. When measuring phase transitions, e.g., melting of lipids etc., this is the preferred experi-
mental design. In cases where a baseline corresponding to zero activity is required, such as when measur-
ing compatibility, stability, etc., a baseline should be recorded with the ampoule holders empty. In cases
where the sample has zero activity at the start (and/or end) temperature, the sample can be inserted in the
calorimeter when recording the baseline.

Figure 128 Decide about baseline.

3 Enter the baseline criteria and click the Next button.

The next window (Figure 129) lets you define the Initial signal stability conditions to be met after the ini-
tial temperature has been reached, and before the temperature program starts.

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You will also need to define the Intermediate signal conditions. This is the stability condition that should
be met at each isothermal period between temperature jumps or scans, other than the Initial.

Figure 129 Define signal conditions.

4 Click Next when all necessary information has been entered.

Starting the Non-Isothermal Experiment

At this point it is possible to review the experimental information given by clicking Previous.
When all setting are considered to be correct click Start to begin the non-isothermal experiment.

Figure 130 About to start the experiment.

RH Perfusion Experiments
The RH perfusion ampoule can be used to measure interactions between a vapor and a solid material, e.g.,
a powder. An inert carrier gas, usually nitrogen, with a set vapor pressure, is passed over the sample and
any interaction, in terms of heat, is measured as a function of time.

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The vapor pressure is set by use of two computer controlled mass flow controllers and can be changed
stepwise or continuously in a ramp.

Initiating an RH Perfusion Experiment

Follow the instructions below to initiate an RH perfusion experiment:
1 Choose New Experiment in the TAM Assistant menu. The following dialog is displayed, which allows
you to choose from a number of different experiments. Choose the group named Flow Control to initiate
the Wizard.

Figure 131 New Experiment.

2 Click OK and click Next when the next view appears.

3 Choose the calorimeter to be used in the experiment by clicking on the picture that appears on the screen.
4 Click Next and the next view lets you choose the flow controller to be used in the experiment.

Figure 132 Choose Flow controller.

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5 Mark the controller, even if there is only one connected.
6 Click Next.
At this point you can choose a blank measurement as a reference measurement. It is important that the
main part of the experiment is run in exactly the same way for the blank reference to be a good representa-
tive If this is not relevant, or if no reference experiment exists, leave the text frame empty.

Figure 133 Define reference experiment.

NOTE: When choosing a previously run reference measurement, make sure that the subsequent measure-
ment is run in an identical way.
7 Click Next.

Setting Up the RH Ramp

You can program an RH program as continuous or stepwise. Below is an example of how a continuous
ramp is defined starting from 40% RH to 80% RH. The change rate is 10% RH units per hour.

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The ramp is followed by a 1-hour delay, which in turn is followed by a fast (step wise) return to the initial
value.

Figure 134 Define mixture profile.

1 Define the desired RH profile.

2 If a ramp is defined, the signal of interest could be when the RH is being changed. In this case uncheck
the Omit data collection box under the RH profile table.
3 Click Next when finished. A new window is displayed to allow you to define the initial and final baseline.
See next page.

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Baseline Definitions
You can collect a baseline, with the sample ampoule inserted, by marking the check boxes on the dialog
displayed in the figure below. When measuring phase transitions, e.g., a solvate formation at a critical
vapor activity, this is the preferred experimental design. In cases, when the sample has zero activity at the
initial (and/or final) vapor activity, the sample can be inserted in the calorimeter when recording the base-
line.

Figure 135 Decide about baselines.

1 Enter the baseline criteria.

2 Click Next. The next window, shown in Figure 136, lets you define the Initial signal stability conditions,
which is to be met after the initial vapor activity has been reached and before the program starts.

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NOTE: You can enter a maximum time to wait for stability conditions. This means that the temperature
change will take place, if the conditions have not been met within the specified time period.

Figure 136 Define signal conditions.

The Intermediate signal conditions should also be defined. This is the stability condition that should be met
at each period of constant vapor activity between step wise changes or scans others than the initial.
3 Click Next when all necessary information has been entered.

Start the RH Control Experiment

1 Click Previous to review and change the experimental information entered.
2 Set the Flow rate between 60 to 180 mL/h.

Figure 137 About to start the experiment.

3 When all of the settings are considered correct, click Start to begin the RH-perfusion experiment.

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Titration Experiments
Titration experiments generally consist of initiating a physical, chemical or biological process by injecting
a reactant liquid with a syringe into another liquid contained inside the calorimeter so as to initiate a chem-
ical or physical process in situ.
This technique can be used to study slow chemical reactions (reaction time > 1 h or higher) or various
physico-chemical interactions in solution. A widely used application is the investigation of complexation
phenomena for determination of binding affinities and enthalpy changes, e.g., ligand binding between in
biological or chemical systems.

The Titration Experiment Wizard

Follow the instructions in this section to use the Titration Wizard:
1 Choose New/Experiment… from the menu on the top left of the main view. The New Experiment dialog
displays.

Figure 138 New > Experiment...

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2 Choose the Titration wizard in the branch structure.

Figure 139 Select Titration.

3 Choose Titration or any saved predefined experiment controller.

4 Enter the desired Experiment name (i.e., file name) and Location. (It is only possible to choose location
if the experiment is started from the external computer.)
5 Enter an Operator name to continue.
6 Click OK. When the “Welcome” screen appears, click Next to continue.
7 Choose the calorimeter to be used in the experiment. In the Titration wizard only one calorimeter can
be chosen due to the fact that only one calorimeter can be associated per one injection pump. Calorimetric
channels already occupied by ongoing experiments are shown in red color.

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8 Click on the calorimetric channel to be used in the experiment. When chosen, the calorimeter will be
shown in green color.

Figure 140 Chosen calorimeters are green.

9 Click Next. You will be prompted to choose an injection pump (named the Lund Syringe Pump) as
shown in the figure to the right. If several pumps are connected to the TAM III instrument, chose the
one to be used in the experiment.

Figure 141 Choose pump.

10 Click Next after selecting a pump. The following dialog is displayed.

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11 Enter information about the sample. This can also be done at a later stage, either during the experiment,
or after. If the sample information will be added after the experiment has already been started, click the
Results tab to access the sample information sheet.

Figure 142 Enter sample information.

12 Click Next to continue. The Decide on injections dialog box displays..

Figure 143 Decide on injections.

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NOTE: Before deciding on the number of injections and volume when determination of binding affinities
is to be made, you may wish to conduct a ligand binding simulation. See “Ligand Binding” for details on
how to use the binding simulation feature in TAM Assistant.
13 Enter the Number of injections, Injection volume, and Injection duration and click the arrow to move
the information to the table.
14 Binding Analysis feature: In cases when the binding constant is known, or can be estimated within a
certain error range (e.g., within ½ order of magnitude), a feature called Calculate adaptive injection
volumes for binding analysis … can be used to optimize the precision in the determination of the binding
constant.
If you click the button, you will be prompted to make a binding simulation; see the NOTE above. When
TAM Assistant has all the necessary input data, it makes an optimization calculation of the number of
injections in the region where the measured heat changes rapidly with the injected amount of reactant.
This feature can be used to increase the precision in determinations of binding constants in a number of
successive repetitive measurements.
15 When finished, click Next. The Choose injection intervals and measurement type dialog box displays..

Figure 144 Choose injection intervals and measurement type.

16 Determine the injection interval, i.e., the time between injections, using the guidelines described here.
The time required between injections is naturally related to the response time of the calorimeter, as well
as the reaction time. Most complexation reactions are very fast compared to the calorimetric response
time. In such cases, approximately 7–8 minutes between injections should be chosen to ensure that the
signal has time to return to baseline and record a small baseline section. This is the case only when the
instrument is run in Feedback or Dynamic correction mode. If the experiment is run with the instrument
in Heat flow mode, at least 20 minutes is required between injections.
In the case of slow reactions, initiated by the injection of a reactant, the time between injections must
be judged in accordance with the reaction rate.
If the measurement is to be run in Dynamic correction mode, the dynamics of the system must be
calibrated with the ampoule and initial sample volume in the measuring position. This can be made from

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 the Devices control before the Titration wizard is started, or it can be chosen to be included in the
experiment. Just mark the box Perform new calibration, if a dynamic calibration with the current sample,
or equivalent, has not already been made.
17 Make your measurement principle selection and enter the desired values. Click Next to proceed. Review
the information displayed and go back through the wizard, if something needs to be changed.
18 Click Start to initiate the experiment according to the values defined in the wizard.
If the signal is not stable with respect to the chosen stability conditions, the dialog box shown below
displays.

Figure 145 About to start the experiment.

In Figure 146, the signal is considered stable whenever a linear fit over the last 20 minutes has a slope less
than 50 nW/h, and the residuals have a standard deviation below 50 nW. These conditions correspond to
the predetermined “Moderate.” When they are met the software starts the initial baseline.

Figure 146 Waiting for initial baseline.

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The initial baseline runs for 5 minutes.
After the initial baseline has been completed the first injection starts automatically.

Figure 147 Performing titration 1.

In Figure 147, the value of the current signal and the time left is shown in the upper left corner. A table
with the injection volumes is shown to the right. You can alter the injection volumes of individual injec-
tions, if they have not already been made as marked in the table.
When all the injections have been made, and the measurement has reached its end, click Finish to create
the results file. The information that previously could be accessed from the Results tab in the experiment
view, is now stored in the results file.
The results can now be analyzed with the ligand binding module in the analysis menu, see “Ligand
Binding” for details.

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Downloading Results Files
Results files that have been saved on the instrument embedded computer should be moved to an external
computer at regular intervals to over loading the memory resources.
Follow these instructions to download the results files:
1 Under the File menu, select Download Results Files...

Figure 148 Download Results Files...

2 A Download Experiment Results dialog box opens with a list of results files that currently exist on the
instrument embedded computer. Select the desired results file by highlighting or clicking on file. Use
either the Transfer to folder or Transfer to specified location functions and use the Browse button to
select a location to save the file to be transferred.

Figure 149 Download Experiment Results.

3 The results file will irreversibly be moved from the instrument system. We recommend that this operation
be performed regularly to unload the system and release computer memory.

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NOTE: A copy of the file can be kept on the embedded computer if the check box Leave a copy of the file
on the device is selected during the download process.
4 Click Download to complete the procedure. A Lab Assistant dialog box prompts you if the operation
was performed successfully. Click OK.

Figure 150 Files were moved successfully.

5 Choose another file to download or press the Cancel button to exit the download dialog.
NOTE: If the desired file does not show up in the list from the embedded computer try, select the Show
pending downloads box and see if the file name appears in the updated list. If an experimental wizard has
been initiated from the external computer and during the experiment communications were lost between
the computer and the TAM III the file may require this option in order to download.

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Run Sequences
NOTE: Examples given in this section are based on an Ampoule Experiment Wizard. If you use the other
wizards, some screens and options will be different.
The run sequences option is used to program different sequential conditioned events within an experiment.
This allows for higher flexibility and more automated and complex experimental setups. Use of the other
tabs of the Experimental wizards were described previously in this chapter.

Figure 151 Welcome to the ampoule experiment wizard.

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To use the run sequences function, follow these steps:
1 Click on the Run sequences tab. The window will appear as shown in the figure below. To the left there
is a square [Click here to add new entry] and on the bottom of the screen there are two tabs, Experiment
and Main section.

Figure 152 Run sequences.

If the entries are programmed using the Experiment tab, the programmed sequences can be executed
in any parts of the experiments, i.e., also baseline and pause sections.
If entries are programmed in the Main section tab, the events will only occur in the main section of the
experiment.
These two can be programmed independently of each other. The Main section tab is only available in
the Ampoule Experiment Wizard.
2 Click on [Click here to add new entry]. Four options are shown.

Figure 153 Click here to add new entry.

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3 Select one of the four options described briefly in the list below:
• Action - Some kind of function should occur. It could be a calibration, an injection or change in rela-
tive humidity.
• Wait for - The next action will not occur until the defined condition(s) has been met. For example, you
can set the next action to occur after a certain time period has elapsed or a stability condition has been
met.
• Repeat - This repeats the last action or sequence of actions.
• If - An action will only occur if a certain condition is met.

Using the “Action” Option

If Action is chosen, a new text box will be displayed to the right as shown in the figure below. This box
will have several options. The drop-down menu will look a little different depending on whether devices
have been added to experiment.

Figure 154 Action.

1 Add a device by clicking the [+]. An Add Run Sequence Device dialog box displays.

Figure 155 Add Run Sequence Device.

2 Select a Device type from the drop-down list: Thermostat, Calorimeter, Accessory, Pump, Stirrer, Flow
controller or Thermometer.
3 Type a name for the device in the Device description field.
4 For the other options refer to the section “Running Generic Experiments” .
5 Click OK.

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6 Click the arrow to open the Using drop-down list and choose one to use.

Figure 156 Select a device.

In the first case no calorimeters have yet been chosen in the wizard, but when this is done the action will be
on the chosen calorimeter(s).
In the second example, the calorimeter in Channel 1 has already been chosen using the experimental wiz-
ard.
7 Choose an Action from the drop-down list depending on the type of device that is used. For a Calorimeter
the following choices are available: Heater pulse, Dynamic calibration, Gain calibration.
If heater pulse is chosen, power, duration, and heater options display.
8 Select Click here to add new simultaneous action add a simultaneous action in the same or in a new
device.
9 Optional: Program additional events by selecting [Click here to add new entry].

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Using the “Wait For” Option
In the example below, Wait for is chosen and a stability condition for the calorimeter is defined.

Figure 157 Wait for option selected.

The left side of the dialog box lists the events; to the right the events are defined.
The following functions can be performed from this window:
• To change the order of any event, use the Move up and Move down buttons at the bottom.
• To repeat an event, click Repeat.
• To remove an event, mark that event and click Delete.
• To add more conditions, select Click here to add new condition.

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• To choose more than one condition, check the desired conditions in the Conditions settings box.

Figure 158 Condition settings.

The conditions can also be set by using the Experimental events, such as Equilibration position reached,
Measuring position reached, Baseline started or Baseline ended.

Using the “Repeat” Option

The Repeat function can be used when adding a new entry if, for example, several sequential heat pulses in
a calorimeter should be performed.

Figure 159 Repeat.

In the Repeat Settings section, the number of times to perform the action can be set.

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In the example below, calibration pulses are performed six times with a stability condition between each
one.

Figure 160 Stability conditions.

Using the “If” Option

The If entry can be used to choose whether or not an action should take place.

Figure 161 If entry.

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In the above example an injection should be performed if a baseline section is ended and the calorimeter is
stable.

Option Overview
The following tables provide an overview of the different options and their functions.

Actions
Table 11: Actions
Actions Description

Add comment: Used To add a comment that is

saved in the experimental file. This could be a
comment about the action in the experiment.

Heater Pulse, Dynamic Calibration, and Gain

Calibration: Used to program calibrations and
heater pulses. You can chose a specific calorime-
ter or any calorimeter connected to the experi-
ment.

Set Temperature, Step Temperature, Scan

Temperature, and Scan Temperature Rela-
tive: Used to program a change in temperature.

Start Injection: Used to program injections, vol-

ume and speed of injection of a syringe pump.

Set Stirrer Rate: Used to set the stirrer rate and

start or stop the stirrer via the pump control mod-
ule.

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 Set RH, Step RH, Scan RH, Scan RH Relative,
and Set Total Flow: Used to set or change the
relative humidity via the flow control module.

Start Injections, Set Stirrer Rate, Set RH, Step

RH, Scan RH, Scan RH Relative, and Set Total
Flow: Used to control an Accessory such as the
pump, stirrer, or the relative humidity during the
experiment.

Wait For/If Conditions

Table 12: Wait For/If Conditions
Wait For/If Conditions Description

Elapsed Time Over: If (none) is selected it is

possible to set a time delay.

Equilibration Position Reached, Measuring

Position Reached, Baseline Started, and Base-
line Ended: Uses the selected experimental
events as conditions to wait for to continue the
Experiment.

Signal Stability: Uses the calorimeter stability as

a condition to continue the experiment.

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Repeat
Table 13: Repeat
Repeat Description

Number of times to repeat: Used to set the num-

ber of times an action should be performed.

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Chapter 4:
Data Handling & Analysis

Data Handling
This section describes how experimental results files are downloaded from TAM III to an external com-
puter connected to the network. It also describes in detail how data from a results file is exported to a for-
mat that can be imported by software like Excel, etc.

Downloading Results Files

Results files that have been saved on the instrument system should be moved to an external computer at
regular intervals in order to avoid overloading the memory resources.
Follow these instructions to download the results files:
1 From the File menu, select Download Results Files… A Download Experiment Results dialog displays
the results files that currently exist on the instrument system listed.

Figure 162 Select Download Results Files...

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2 Select the desired results file by clicking on the target directory for the downloaded file.

Figure 163 Select file.

3 Select the method to use:

• Use the Transfer to Folder function to move the multiple results files to the chosen folder.
• Use the Transfer to specified location function to move one results file to the chosen location.
• If the Leave a copy of the file on the device option is left blank, the results file will irreversibly be
moved from the instrument system.
• We recommend that file transfer be performed regularly to unload the system and release computer
memory.

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4 Select the results file, target location, and the Move or Copy option, and then click Download to complete
the procedure. If the operation was performed successfully the following Lab Assistant dialog box
displays:.

Figure 164 Operation successful notification.

5 Click OK.
6 Choose another file to download or click Cancel to exit the download dialog.

Exporting Data
Data that has been saved in a results file can be exported for use with other software for data treatment,
visualization, etc.
Follow these steps to export results files:
1 From the File menu, select Open/Results File…
2 Select and open the desired results file. From the File menu, select Export…

Figure 165 Select Export...

A Save as… dialog box displays to allow you to choose the directory and filename.
3 Choose the export format. There are three formats to choose from: CSV (comma-separated value), txt
(text file), and as a Microsoft Excel file.

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4 Click Save. The window shown in Figure 166 displays, which allows you to choose the content of the
exported data.

Figure 166 Export Settings wizard.

5 Check the desired options, then click Next to proceed. Include experiment information, various data
series, raw data, and/or statistics, if desired.
In an ampoule experiment the baseline can be subtracted from the exported data. If baseline data before
and after the experiment exists, the baseline is an interpolated linear function, taking possible baseline
drift into account.
6 Choose the data series (types) for each channel to include in the export file by checking the desired items
under Select columns to include. The data types are:
• Time column
• Heat flow
• Heat
• Normalized heat flow
• Normalized heat

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 By default, all of the data types are marked so you will need to deselect the ones that should not be included.
If the signals from more than one device were collected in the results file, the dialog lets you choose the
signals to be exported.
7 Click Next again.
8 Select the desired raw data options shown in 167 below. The following guidelines should be considered:
NOTE: Scroll down to select the information for all channels.
• If the check box labeled Include header is marked when selecting raw data to include, the experi-
mental information and sample information fields entered previously will be included in the
among the exported data.
• Use the items in the Time column section to choose how the data should be dispersed in time.
• Select Use all source times to set up the exported data to include all collected data points as deter-
mined at the end of the experiment. All source time data collected does not need to be equidistant.
• Select Resample at equidistant intervals to set a constant time interval between the data points,
according to the time chosen in the text box. If the chosen interval is shorter than the interval
between the raw data points, an interpolation method is used. If the chosen interval is larger, data
will be removed by use of a filter function, and the time is adjusted to fit the time series starting
with time=0.

Figure 167 Export Settings wizard.

9 Click Next to continue.

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10 Check Include statistics, if desired, then check the information to include in the exported file. When
completed, click Finish.

Exporting Data During an Experiment

If you are going to be running a long experiment, it can be useful to export and present the data collected
during the initial part of the experiment. This is possible by following the instructions given in the previous
section.

Results Analysis
The results analysis in TAM Assistant is performed by use of analysis modules, with each module dedi-
cated to a certain application.
All analysis modules of TAM Assistant are accessed from the Analysis menu. In order to perform an anal-
ysis, the data files have to be downloaded from the TAM III system and analyzed by the external TAM
Assistant.

Gain Validation
The Gain validation analysis is only applicable to results files that have been generated by the Gain Valida-
tion wizard.
For evaluation of the data and creation of a report, select Gain Validation… under the Analysis menu.
Open and view the results file when making the analysis.

Figure 168 Select Gain Validation...

A report is created automatically containing a graph of the calorimetric signal and validation parameters as
calculated by TAM Assistant. Click on the icon shown in 169 below to open the report.

Figure 169 Click TAM III Validation report.

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The report contains the values of the input parameters as well the results.

Figure 170 Example report.

• Measurement: Provides the calculated mean value of the steady state signal, corrected for the baseline
offset.
• Results: Provides the difference between the gain factors as obtained by a standard calibration, and the
results given by the Validation procedure.
• The Gain error is calculated according to the equation below:
Where P is the measured steady state signal and Pin is the heat flow released by the calibration heater when
exposed to a known electrical current.

The Gain error is an estimation of the accuracy of the calorimeter and, as such, it should be within the
accuracy given by the specifications for the validated calorimeter type.

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General Performance
To run the General Performance analysis, follow these steps:
1 Open the GPT results file and select the file in the Results file manager.
2 Start the analysis by choosing General Performance … from the Analysis menu. The analysis report
is then automatically generated.

Figure 171 Select General Performance...

The General performance analysis is only possible with results files generated by the experimental wizard
called General performance.

Figure 172 General Performance analysis report.

The example in 172 above shows the result from a general performance test on one 3208 multicalorimeter
(a total of 6 minicalorimeters). The calculated parameters in the results table must have values consistent
with TA Instruments’ specifications. The parameters reflect the performance of a calorimeter and thermo-
stat.
The DGainA is the relative difference between the calibration heat supplied and the measured heat. The
DGainB is the relative difference between the gain factors obtained for the Sample side (A) relative, to
that of the reference side (B) of a calorimeter.

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Tau A and Tau B are the time constants obtained for the A and B sides respectively. For a calorimeter well
balanced with respect to the heat capacity, the difference between the two time constants should be small.
In the example given on the previous page, the General performance test was run with the insert on the ref-
erence side, but with the sample side empty. This is clearly reflected in the lower time constant for the A
side.
The parameters Drift, Deviation and Error reflect the long term stability of a calorimeter. The drift is sim-
ply the slope of a fitted line over 24 hours, and the deviation is twice the standard deviation over the resid-
uals with respect to the fitted line. The error is the quadratic mean value of the drift and the deviation.

Ligand Binding
The Ligand Binding analysis module is used to analyze the results from complexation (or binding) reac-
tions obtained by isothermal titration experiments (ITC). The analysis consists of a numerical non-linear
regression procedure where the fitting parameters generally are the binding (or affinity) constant and the
apparent enthalpy change for the process.
Follow these steps:
1 Choose Ligand Binding… from the Analysis menu to start the program. The Get Binding Analysis
Data dialog box displays.

Figure 173 Ligand Binding...(left); Get Binding Analysis Data (right).

2 Use the Browse button to find the file to be analyzed and click OK.

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 The Binding Analysis form displays with the tabulated injection volumes and the integrated titration
calorimetric data.

Figure 174 Binding Analysis form.

3 Add new sources by clicking Get titration data… then Browse for the results file to be included.
4 Select additional input for the analysis: reaction volume, initial concentration in the ampoule and in the
syringe.
If this data has been included in the results file, it is imported automatically into the Binding Analysis
dialog box. Otherwise, you will need to add it manually.
Another input is the binding model, which can be changed with the buttons below the data table. The
subscript M represents “Macromolecule,” or host molecule, and L represents “Ligand.”
The ligand is considered to be the substance that is injected. This is the common terminology used in
biophysics or biochemistry where the host molecule might be a protein and the ligand is a smaller
molecule, for instance a drug compound. In metallo-organic chemistry for instance, the host molecule
is considered to be a metal ion and the ligand(s) are larger organic molecules.
The default model chosen is the most common model used, namely the 1:1 model. See the next section,
“Choosing a Binding Model,” for details on how to choose models.
In many cases, correction for dilution effects of the injected substance should be made. The heat of
dilution can be determined in a separate measurement and the obtained heat subtracted from that of the
main result.

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5 Check the Use dilution experiment box to subtract dilution heat.

Figure 175 Use dilution experiment.

6 Click Get dilution data… to import the dilution heat in a separate column of the table.
If the dilution heat doesn't change significantly with the concentration interval used in the experiment,
a single heat of dilution can be used instead. Enter this constant dilution heat in the text box to the right
side of the table.
7 When all the settings have been made, click Calculate. The software will calculate the affinity constant
and the apparent enthalpy change for the binding reaction.
You can “lock” or “unlock” certain parameters in the form. The binding constant and enthalpy changes
are commonly used fitting parameters and are, therefore, unlocked by default.
However, if you have a good estimation of the binding constant, by other means of determination, you
can choose to use only the enthalpy change as the fitting parameter.
Alternatively, one of the initial concentrations might not be well known (e.g., a concentration of an
unstable protein). In this case you can unlock the protein concentration and this will be used as a fitting
parameter. Hopefully you will have a good physical argument for doing this as adding fitting parameters
to experimental data inevitably will give a better fit. Hence, adding a fitting parameter must be
substantiated by solid scientific arguments.

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8 Click Generate report when the calculation has been made, and a ligand-binding report is made with
the estimated fitting parameters, together with the calculated free energy and entropy changes for the
reaction.

Figure 176 Ligand Binding report.

The plots in the report are heat per amount of injected volume versus the ratio of the injected volume to
the initial volume. The lower graph shows the accumulative heat versus ratio of the injected volume to
the initial volume. To refine the analysis it is possible to return to the Ligand binding form by choosing
Refine Analysis under Report in the top menu.

Choosing a Binding Model

Use the model buttons to choose different types of models. Click a button to choose the right the model as
in the table. Single equilibrium steps with one affinity with different stoichiometry can be entered or, alter-
natively, two or several equilibrium steps as seen in 177.

Figure 177 Choose a binding model.

The reaction is added as for example: ML+L>ML2 and entered by clicking anywhere outside the button
area.

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Ligand Binding Simulation
The Ligand Binding Simulation module is very useful when determining concentrations for the experi-
ment. This simulation provides input to the use of adaptive injection volumes as determined in the experi-
mental setup wizard.
Follow these steps:
1 Select Ligand Binding Simulation… from the Analysis menu. The following simulation view appears,
in which the binding constant and concentrations is entered.
2 Choose the binding model as described in the previous section “Choosing a Binding Model.”

Figure 178 Choose a binding model.

3 Set the ampoule concentration in relation to the magnitude of the binding constant. This is important to
get a reasonably good estimation of the binding constant. For example, an acceptable estimation of the
binding constant for a 1:1 stoichiometric binding reaction can be obtained, if the concentration is chosen
in the following interval:
10 < (concentration*binding constant) < 1000.
This ensures that a sigmoidal shape of the binding curve as seen in the figure above can be obtained.

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Heat Capacity Analysis
The heat capacity analysis function is used to analyze experimental data generated with the non-isothermal
experimental wizard. The experiments can be run either in scanning mode or in step isothermal mode for
heat capacity determinations.
Follow these steps:
1 Select Heat Capacity... from the Analysis menu (179). The heat capacity form displays (180).

Figure 179 Heat Capacity... Figure 180 Heat Capacity dialog box.

2 Click Browse to find the source file with the non-isothermal heat flow data.
3 For files containing data from several channels, choose which signals to include in the analysis from the
Heat flow data drop-down list.
With each calorimetric heat flow signal there is a calculated associated temperature. This temperature
is calculated from the measured temperature of the thermostat liquid and the thermal inertia of the
calorimeter heat sinks to get a temperature that is close to the real temperature of the sample.
4 Choose the temperature to use in the analysis by clicking either Use associated temperature or Use
separate temperature data. The separate temperature data is generally referred to the measured bath
temperature.
If a blank experiment has been run in a separate experiment, you can subtract the blank signal from the
main. The best result is obtained if the blank has been run on the same calorimeter using the same
temperature profile.

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5 Check the Reference box and choose the results file and the corresponding signal (calorimeter).

Figure 181 Check Reference.

6 Choose the same temperature data for the reference and the sample data to obtain the best results.
7 Decide if you wish to subtract the heat flow data at the same time, or at the same temperature. For
scanning experiments, you normally subtract at the same temperature to make sure that temperature
dependent events are subtracted correctly.
When calculating the heat capacity, the heat flow vector is divided by the chosen temperature vector.
This is a mathematical operation that increases the noise level in the resulting heat capacity vector quite
substantially as compared to the original heat flow and temperature data. For this reason a filter function
has been added.
8 Click the Filter box before creating the report.
9 Click Generate report after all settings have been selected.
A plot of apparent heat capacity versus temperature displays, along with the sample information and
source of the data.

Figure 182 Heat capacity vs. temperature plot.

The example shows an irreversible polymorphic phase transition and subsequent melting of Tripalmitic
acid. Two pairs of up and down scans in the temperature interval 35 to 80°C are shown and distinguished
by the different colors.

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Compatibility
The compatibility program is used to analyze heat flow data of mixtures. The sections below show the pro-
cedures for making compatibility analysis with TAM Assistant.

Loading Compatibility Data

Follow these steps:
1 Select Compatibility… from the Analysis menu to start the compatibility program in TAM Assistant.

Figure 183 Select Compatibility...

2 The Compatibility Analysis dialog box displays. Click Add mixture to find the results file and load
compatibility data.

Figure 184 Compatibility Analysis dialog box.

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The Add Mixture dialog box displays to let you choose which binary mixtures to be used in the calculation.
If all component information has been entered in the results file, the program recognizes the signals (calo-
rimeters) that represent the mixtures.

Figure 185 Add Mixture dialog box.

In the example given here, the name of the results file is “Compatibility demo.rslt.” All measurements
(components and mixtures) are contained in a single results file. In this example, a total of 5 measurements
were made: 1) a drug component, 2) excipient A, 3) excipient B, 4) mixture of drug and excipient A and 5)
mixture of drug and excipient B.
3 Choose the mixture signals to include in the calculation.
4 Click OK to import the data to the compatibility analysis.

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 The Compatibility Analysis dialog box displays with the mixtures included in the experiment file and
the individual components. The software identifies the single component measurements with the mixture
measurement. This is done automatically if you check, Automatically match single component measure-
ments.

Figure 186 Compatibility Analysis dialog box.

If Automatically match single component measurements is not checked, you need to match the single
component measurements to the mixture measurements manually by choosing the correct data in the
Components column.

Figure 187 Manually match component measurements.

5 Use the tabs on top of the Compatibility Analysis dialog box to choose the mixture that will have
information displayed.
In the component table, information about the individual components, from the single measurements
and the mixture measurements, is shown.
The range over which the analysis shall be made can be determined from the heat flow plot for the
different mixtures and components.

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6 Click the ellipsis [...] button to the right of the Mixture measurement signal field to display a graph.

Figure 188 Click [...]

The default range is the measurement period from the point at which the signal is considered correct
after introducing the ampoule, to the time when the main experimental section was finalized and the
sample was removed from the calorimeter.
7 Change the range for the individual signals, if desired, by moving the range markers back and forth along
the time axis, or by using the drop-down menus above the graph.

Figure 189 Select measurement dialog box.

8 Repeat the procedure for all the signals related to the current mixture, before proceeding to the next
mixture.
9 Press OK when the settings for all mixtures have been completed.
10 Normalize the mixture signal, taking into consideration the following points:

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 • The signal is generally normalized with respect to the size of the sample (mass, molar mass or vol-
ume).

Figure 190 Normalize mixture signal.

• You can determine if the signal is to be divided by total sample size, size of an individual compo-
nent in the mixture or any chosen factor and unit.
11 Determine what to include in the Compatibility report. There is a predefined template that can be used
to assist you. This is done in the Report settings section where a number of boxes can be checked.

Figure 191 Report settings.

• The box labeled Include mixture graph refers to one graph for each mixture. Each mixture graph
contains three plots: Measured, Theoretical, and Interaction.
• If the boxes Include components graph and/or Include interaction graph are checked, separate
graphs will be created displaying the results from the respective individual components and the
individual interaction plots.

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12 Click Generate report to create the report when the settings are satisfactory. The figure to the right is
an example showing the measured signal from one of the mixtures, the theoretical curve and the
interaction curve. The three calculated parameters from the data are: 1) interaction integral, 2) interaction
average heat flow and 3) interaction error, i.e., the standard deviation for the interaction (high slope,
high interaction error).

Figure 192 Example report.

The different pages in the report can be accessed either with the triangular arrows or the page tabs at the
lower left side of the graph window.

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Kinetic Analysis
Since the heat production rate associated with chemical, physical and biological processes is related to the
conversion rate of such processes, heat flow data can, in some cases, be analyzed with various kinetic mod-
els. In TAM Assistant you can import signals from results files into the kinetic analysis program for analy-
sis with a variety of different models.
NOTE: You can try different models without changing the entered settings.
Follow these steps:
1 Select Kinetics... from the Analysis menu. When the Kinetic Analysis dialog box displays, click Add
measurement to find the results file to use for data extraction.

Figure 193 Add Measurement dialog box.

2 Browse the file system to find the results file, and mark which calorimeter signals should be included
in the analysis (there is only one signal in the example).
3 Click OK when the choice has been made. The data is now loaded into the Kinetic analysis form and is
seen in the graph window.

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4 Enter details about the reaction, such as stoichiometric information (a/c and/or b/c), volume and
concentration or amount. When all model input data has been entered the fitted constants are shown in
the Results frame to the left of the graph.

Figure 194 Kinetics Analysis dialog box.

5 Adjust the time interval over which the fitting is to be made, if desired, by using the ellipsis button [...]
on the Signal drop-down.
6 Click Generate report when all of the settings have been selected to create the report.

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Arrhenius Analysis
Since heat production rates are generally related to the rate of chemical, physical or biological processes,
temperature analysis by the Arrhenius model can be made on calorimetric data collected for a process at
different temperatures.
Follow these steps:
1 Select Arrhenius… from the Analysis menu.

Figure 195 Select Arrhenius...

2 Enter at least three representative experimental values for the heat production rate at a few different
temperature values. You can choose heat flow values at time zero or a time later than zero, if the extent
of the reaction is approximately the same for the different temperatures.
If you choose heat flow values at a time later than zero, it is important that the heat flow values are
chosen at a point where the extent of reaction is the same, i.e., the integrated heat, up to the point where
the heat flow data is taken, should be the same at the different temperatures.
3 Enter the temperatures in degrees Celsius. Heat production data is usually entered as normalized against
sample size.

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4 Select the unit from the Heat flow normalization unit drop-down list.

Figure 196 Arrhenius Analysis dialog box.

In the plot, the scale on the ordinate is given as logarithmic in terms of heat flow. The unit on the abscissa
gives the temperature in degrees Celsius. This scale is proportional to 1/T with the unit reciprocal Kelvin
(K-1).
In the example above, three temperature values and three values for the heat production rate were entered.
The plot is made automatically when three values in both columns have been entered, and the result of
the linear regression is shown in the Results section.

Figure 197 Results section.

If the analysis is made with the heat flow data only, the activation energy is gained from the slope and
the term DH*A from the ordinate intercept.
If the enthalpy change for the reaction, DH, is known, and can be assumed to be independent of
temperature, the pre exponential factor, A can be calculated. This enables the rate constants for the
reaction to be calculated at different temperatures by use of the conventional Arrhenius equation.
Naturally, the rate constant is only relevant if the mechanism of the reaction is known, e.g., first order
kinetics.
5 Click Generate report to generate the Arrhenius report.

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STANAG 4582 Analysis
Measuring temperatures for a STANAG test should be between 60-90 °C. Propellants stored at tempera-
tures equivalent to an isothermal storage at 25°C will remain chemically stable for a minimum of 10 years
if the following criterion are met: The maximum normalized heat flow in the experimental part between
the time corresponding to a heat release of 5 J/g and the time defined as tm must not exceed the calculated
heat flow limit (Pl). Both measuring times and heat flow limits depend on the test temperature chosen
(Table 1). The heat flow must be normalized to 1 g of sample. If the sample mass had been entered during
the STANAG experimental wizard then the normalized heat flow signal available in the results file will
suffice.
Triplicate results of a typical STANAG test are displayed in 198. The test was performed at 80°C and thus
allowed to run for 10.6 days. Approximately 3-3.5 g material was loaded into a 3 mL glass ampoule, which
calculates to a load density of 1-1.17 g/mL. In the first part of the measurement some propellants show an
initial high rate due to aerobic decomposition reaction until the supply of air which is sealed within the
sample vessel is consumed. In the plot the normalized heat (or integrated heat flow) is displayed in order to
determine the initial time point where the heat flow exceeds 5 J/g. From that point the normalized heat
flow signal of all three samples did not exceed the maximum heat flow limit of 114 µW/g (refer to
Table 14 in the Appendix). Thus, these samples pass the STANAG criteria.
STE Ch1 Integrated Ch1 STE Ch2 Integrated Ch2
STE Ch3 Integrated Ch3

25

60

20
50

15
40
)
)

g
/
g
/

W
J
(

10
(

30

5 20

0 10

0 2 4 6 8 10

Figure 198 Propellant measured in triplicate at 80°C - All pass STANAG 4582 criteria.

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TAM Assistant has a built in STANAG analysis function to create a report similar to that shown in 198 that
utilizes the information listed in Table 14.
1 To initiate STANAG analysis, from the Analysis menu select STANAG 4582

Figure 199 Analysis > STANAG 4582.

2 The main analysis screen displays with two options: Add propellant and Add results file.

Figure 200 Main analysis screen.

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3 If you have entered all relevant sample and experimental information previously during the wizard,
select Add results file. Click Browse and locate the respective results file.

Figure 201 Add Results.

If the calorimeter signals do not appear in the Measurements window, then deselect the Only include
properly attributed signals option and the selected calorimeter signals should appear.
To proceed with analysis report TAM Assistant will require you to enter the propellant information. If
this step is necessary, please also refer to the “Add propellant” section below on how to enter additional
sample information and associate to the respective results file.
4 If all signals appear, click Generate report(s).

Figure 202 Generate report(s).

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5 The generated report will have an overlay plot displaying all calorimeters selected and the maximum
heat flow signal for the test temperature. Additional pages of the report will have tabular information
regarding each sample analyzed.

Figure 203 Overlay plot (left); tabular information (right).

NOTE: When the propellant results file does not include the proper attributes, the STANAG feature will
not open or analyze. For example, if the Add Result file button is selected and there is no propellant infor-
mation entered in the results file, nothing will open in the analysis. The Add propellant button must be
used in this case to associate the propellant information with the relevant calorimeter results before a report
can be generated.

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Add propellant
If the Add propellant button is selected, much of the sample information and conditions must be entered
manually in the Info tab and results files can then be corresponded with the information entered.

Figure 204 Info tab.

1 Click the Measurements tab to insert the results file signals corresponding to the sample information
entered.

Figure 205 Measurements tab.

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2 Browse for the files and select Add Measurement. This will have to be performed for each signal
desired. At any point, it is possible to double click on a tabular value and make changes (e.g. sample mass).
3 The Select Measurement dialog box displays. Define the length of each experiment for each calorimeter
selected. This window can also be accessed at any time by selecting a measurement signal field and
pressing the button that appears on the right-hand side. Click OK.

Figure 206 Select Measurement.

4 Click Generate report to create a report as described above.

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Chapter 5:
TAM Assistant Security

Introduction
The TAM Assistant Security system provides user and permissions management for devices and experi-
ments controlled by TAM Assistant. It also provides audit trails for keeping track of all changes to devices
and all experiments.
The following functionality is provided:
• User and group management
The security system includes a built-in user database that can be used to define the users that have access
to the system, as well as define groups of users for easier permissions management. Additionally, the
security system can be integrated with Active Directory, allowing the standard Windows login to be used.
• User login
When accessing an instrument that is connected to the security system, the user needs to login to the
system. It is the responsibility of the security system to authenticate the user. The authentication can be
performed either against the built-in user database or, if Active Directory integration is enabled, using
the standard Windows login. If Active Directory integration is enabled, it is possible to automatically
login as soon as the TAM Assistant software is started, without providing any additional credentials.
• Permissions management
Permissions can be assigned to all parts of the security system. Securable objects (i.e., devices, instruments
or the security system itself) are arranged in a hierarchical structure. Permissions can be assigned for
the whole system, an instrument or even down to a specific calorimetric channel.
• Audit trails
Another part of the security system is the audit trails. The audit trails are used to keep track of all events
that happen on the system. The events can for instance be: setting new temperature on a thermostat,
performing a calibration, starting an experiment, or any system problem. Each entry in the audit trail
contains information like time, user, severity, and a description. The entries can be filtered based on
different criteria and exported to a file or sent to a printer.
• CFR Part 11 support
The above functionality provides the basis for implementing a system that is compliant with the CFR
Part 11 regulations.

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Setting up TAM Assistant Security
To use the security system, TAM Assistant Security has to be available. There are two options for setting
up the security system. Either the security system embedded on the TAM III instrument can be used, or it
can be installed on a standalone computer.

Using TAM Assistant Security on a TAM III Instrument

If the instrument setup consists of a single TAM III instrument, the easiest way to set up TAM Assistant
Security is to use the embedded security system on the TAM III instrument. The embedded security system
is identical to the security system that can be installed on an external computer, with the limitation that
Active Directory integration is not available.
To enable the embedded security system, perform the following steps:
1 From the Settings menu on the TAM III, select System

Figure 207 Select System.

2 Under the Security page, select “(local)” as the Security system.

Figure 208 System Settings dialog box, Security tab.

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3 Click OK. A prompt for the system password displays. The system password is used to protect the TAM
III system from unauthorized changes. However, the default password is empty, so unless a system
password has been previously set, no password needs to be entered.
4 The first time the embedded security server is used it needs to be initialized. The security server is
initialized by adding an Administrator account to the user database, as well as the default Administrators
and Users groups. Members of the Administrators group are assigned full permissions to the whole
security system. To be able to initialize the user database, the password for the Administrator needs to
be defined.

Figure 209 Administrative Password dialog box.

5 After entering the Administrator password, the system will restart. On the next startup, the system
overview and login screen will appear.

Figure 210 System login page.

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 The overview screen provides information about the thermostat and all calorimeters installed in the TAM
III, as well as information about currently logged in users and running experiments.
6 To log into the TAM III system, enter “Administrator” as the user name and specify the password defined
when initializing the embedded security system.
For information on how to setup additional users, see the sections “Users and Groups” and “Permissions
and Roles.”

Installing TAM Assistant Security on a Standalone Computer

If more than one TAM III instrument should be connected to the security system, or if Active Directory
integration is wanted, it is recommended that the TAM Assistant Security system is installed on a stand-
alone computer. The security system can be installed on the same computer as the TAM Assistant software,
but if possible it is recommended that it is installed on a server computer which is always running.
NOTE: If a previous version of TAM Assistant or TAM Assistant has been installed before, it is highly
recommended that it is uninstalled before installing the new version.
To install the TAM Assistant Security software, perform the following steps:
1 Insert the TAM Assistant CD into the computer. The installation start screen appears automatically.

Figure 211 Installation Start screen.

2 Click Install TAM Assistant Security.

If the installation start screen didn’t appear in step 1, select Run from the Windows Start menu, enter
“D:\ServerSetup.exe” (where D is the driver letter for the CD-drive) and click OK.
3 The TAM Assistant Security installation wizard begins. Follow the instructions provided by the wizard
until the Logon Information page is reached.

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4 On the Logon Information page, the account to use for the TAM Assistant Security service should be
selected. It is possible to select either the built-in local system account, or to select or create a normal
user account.

Figure 212 TAM Assistant Security Setup.

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5 If TAM Assistant Security has not been previously installed, the security settings window will appear
at the end of the installation.

Figure 213 TAM Assistant Security Server Settings.

Here, the folder where the security files should be stored is specified. The folder should either be a folder
containing TAM Assistant security files from a previous installation, or it should be an empty folder. For
security reasons, the selected folder should not be used for any other data. For more information, see
“Security Considerations and Backup of Security Data.” If the specified folder does not contain any secu-
rity files, a first time initialization must be performed.
The security system can be initialized to use either the built-in user database, or to enable Active Directory
integration.
• Use built-in user database
This option enables the built-in user database. The database will be initialized with a single Administrator
account, an Administrators group and a Users group. The Administrators group will be assigned full
administrative rights to all objects in the security system.
To initialize the Administrator account a password must be specified using the Define Administrator
password and Confirm Administrator password fields.
• Use Active Directory integration
This option enables the integration with standard Windows user accounts and groups using Active
Directory. All users and groups that are defined in Active Directory are available to the security system.

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• Default domain
Defines the domain that should be used when looking up users and accounts. If the standard domain
should be used (i.e., the domain on which the security server is installed), this field can be left empty.
• Define initial administrative user or group
Defines the user account or a group that should initially be assigned full administrative rights to the
security system.
6 Finish the installation.
• Use the TAM Assistant Security Manager to set up users and permissions. For more information, see
“TAM Assistant Security Manager.”
• Connect the TAM Assistant software and TAM III instruments to the security system. For more infor-
mation, see “Connecting a TAM III Instrument to a Standalone Security System” and “Connecting
External Computers Running TAM Assistant to the Security System” in this chapter.

Connecting a TAM III Instrument to a Standalone Security System

To enable the security system on a TAM III instrument, the security server to use must be defined. If the
embedded security server should be used, follow the instructions under the “Using TAM Assistant Security
on a TAM III Instrument.”
To enable the embedded security system, perform the following steps:
1 Select System from the Settings menu on the TAM III.

Figure 214 Settings menu.

2 Under the Security page, select the wanted Security system.

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3 Click OK. A prompt for the system password will appear. The system password is used to protect the
TAM III system from unauthorized changes. However, the default password is empty, so unless a system
password has been previously set, no password needs to be entered.

Figure 215 System Settings dialog box, Security tab

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4 After entering the system password, the system will restart. On the next startup, the system overview
and login screen will appear.

Figure 216 Login screen.

The overview screen provides information about the thermostat and all calorimeters installed in the TAM
III, as well as information about currently logged in users and running experiments.
5 Use the Login area to enter the user name and password to login to the TAM III system.

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Connecting External Computers Running TAM Assistant to the Secu-
rity System
To be able to use the TAM Assistant software to connect to an instrument connected to the TAM Assistant
Security system, the TAM Assistant software must be connected to the same security server. To select
security system server for TAM Assistant, perform the following steps:
1 Select Settings from the File > Security menu in TAM Assistant.

Figure 217 File > Security > Settings.

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2 In the Security Settings window, select the desired Security system.

Figure 218 Security Settings.

For information about the other options, see “Security Settings.”

3 Click OK. The selected security server will be used the next time TAM Assistant is started.
4 Exit TAM Assistant and restart it. If the Automatically login at startup option is enabled, a login screen
displays.

Figure 219 Login screen.

If the Automatically login at startup option is not enabled, it is necessary to use the Log in new user
command under the File/Security menu.
5 Use the Login User screen to enter the user name and password to login to the TAM Assistant Security
system and gain access to secured instruments.

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TAM Assistant Security Manager
The TAM Assistant Security Manager is used to make define security settings, work with users and groups,
and assign permissions. It is installed together with the TAM Assistant Security system. It can also be
installed by doing a custom install of TAM Assistant. For more information, see the TAM Assistant instal-
lation instructions.
The TAM Assistant Security Manager can be started from the Windows Start menu or it can be accessed
from a TAM III instrument, using the Security Manager command under the Security menu.

Connecting to a Security Server

If TAM Assistant Security Manager is started on a standalone computer, the security server to connect to
must be specified. To define the security server, the Connect command under File menu should be used.
This will bring up a window that provides the possibility to select one of the available security servers. The
selection window will present all available security system servers. If the security managed is running on
the computer where the TAM Assistant Security Server is running, one addition option will also be pres-
ent: <Direct>. This option will connect the security manager directly to security server files, bypassing the
login to the security system. Only users which have access to the security files can use this option. For
more information, see “Security Considerations and Backup of Security Data.”

The Security Manager Window

The security manager window contains two panes. The left pane presents all available security objects
(e.g., devices and the security server itself) in a tree hierarchy. This tree can be used to select the object that
should be viewed or edited.

Figure 220 TAM Assistant Security Manager.

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Depending on the selected object in the tree, the right pane shows the available security properties for the
object. The properties are divided into several pages. All items include the Security and Audit pages. The
top-level item (which represents the security system itself) includes additional pages: General and Users
and Groups.

Apply
This button is used to apply the changes made to the security settings or user permissions.

Cancel
This button is used to cancel any changes made to the security settings or user permissions.

Security Server Settings

The global settings for the security system can be accessed by selecting the top-level item in the navigation
tree, and then selecting the General tab. This page provides access to the settings:
• Name: This field is used to define the name of the security system. The default name is “Root” and it
can be changed to any suitable name.
• Allow automatic login: This field is used to indicate whether TAM Assistant is allowed to login auto-
matically using the current Windows credentials. Automatic login is only possible if Active Directory
integration is enabled.
• Suspend login after … minutes inactivity: This setting is used by the TAM Assistant Software and
the TAM III instrument. It defines the number of minutes of inactivity is allowed before suspending
the current login. After the login has been suspended, the user name and password needs to be reen-
tered to continue to use the TAM III instrument or TAM Assistant software.
• Lock out account after … failed login attempts: This field defines the number of failed logins that
are allowed before locking out a user account. For information about how to re-enable a locked out
account, see “Users and Groups.”
• Minimum password length: Defines the minimum allowed length of a user password. This setting is
only used if the integrated user database is active.
• Enable password aging: This field is used in conjunction with the Maximum password age field to
define the maximum age of a password. If this option is enabled and a user logs in with a password that
is older than the specified age, the user will be prompted to enter a new password. This setting is only
used if the integrated user database is active.
• Enable password history: This field is used in conjunction with the Passwords remembered field to
define the password history. If this option is enabled, then the Passwords remembered field is used to
define the number of passwords that are stored for each user. When assigning a new password, it is not
allowed to use a password that exists in the password history. This setting is only used if the integrated
user database is active.

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Users and Groups
In order for a user to login to the system, information about the user must be added to the system. The
TAM Assistant Security system keeps track of all users, either by using a built-in user database or by using
existing user accounts in Active Directory.
To simplify permissions management, it is also possible to combine users into user groups. The user
groups are either handled by the built-in user database, or by Active Directory, if Active Directory integra-
tion is enabled.
The Users and Groups page provides access to the users and groups that have been added to the security
system. This page can be used to add or edit users, add or edit groups and assign members of groups.

Figure 221 Users and Groups.

To change the settings on this page, the logged in user must have the “Change security settings” permission
on the root object. For more information, see “Permissions and Roles.”
The settings on the next pages are available on the Users and Groups page.

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Enable Active Directory Integration
This option indicates whether Active Directory integration is enabled. It can only be changed if the secu-
rity manager is connected directly to the security data.

Figure 222 Enable Active Directory integration.

Default Domain
This field is only available if Active Directory integration has been enabled. It can be used to define the
domain that should be used when looking up users and accounts. If the standard domain should be used
(i.e., the domain on which the security server is installed), this field can be left empty.

Use All Users and Groups from Active Directory

If this option is enabled, it is possible to log in to the system using any available Active Directory user
account. If the user has not previously logged in to the system, it will be automatically added to the list of
users.

Only Use Selected Users and Groups from Active Directory

If this option is enabled, only users whose account has been explicitly added to the user list can login to the
system. For more information on adding users, see “Editing Users.”

Users
This list contains all users that are registered with the security system. New users can be added using the
Add button below to list and user information can be viewed and edited by double-clicking a user entry.
For more information, see “Adding New Users.”

Hide Inactive Users

If this option is enabled, then only active users will be listed in the Users list.

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Groups
The Groups list contains all groups that are registered with the security system. A group can be used to
assign permissions to a group of users (and groups), thus simplifying permissions management. If Active
Directory integration is enabled, the group list is not available, however, all groups in Active Directory are
available when assigning permissions. For more information about groups, see “Working with User
Groups.”

Adding New Users

New users can be added to the security system by using the Add button under the Users list. To add new
users, the logged in user must have the “Modify users” permission on the root object. For more informa-
tion, see “Permissions and Roles.”
If Active Directory integration is enabled, a user selection screen will appear, allowing the selection of an
Active Directory user to add. For more information on selecting the user, see “User and Group Selection.”
If the built-in user database is enabled, the Add User dialog box displays.

Figure 223 Add User dialog box.

This screen is used to define the most important settings for the new user.

Logon Name
This is a mandatory field where the logon name of the user should be entered. The logon name is used to
identify the user when logging in to the system.

Full Name
Use this field to enter the full name of the user. The full name is used when presenting the name of the user,
for instance in audit trails entries.

E-mail
This field can be used to enter the e-mail address of the user.

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Password/Confirm Password
The password fields are used to define the initial password for the user.

User Must Change Password at the Next Logon

This option indicates that a new password should be requested the next the user logs in to the system. It is
recommended that this option is enabled when the password has been reset.

Password Never Expires

This option indicates that the password of the user never expires, even if password aging is enabled.

Editing Users
The settings for a user can be viewed and modified by double-clicking the user in the Users list. This will
bring up a window that provides access to all user properties. If Active Directory integration is enabled, the
properties are extracted from Active Directory and cannot be modified, except the Active and Locked out
options. To change the settings of an Active Directory user, the standard Active Directory interface should
be used.
The user properties window consists of two tabs. The General tab provides access to the standard user
properties and the Member of tab shows the groups that the user is a member of.

Figure 224 Properties for user.

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Logon Name
This is a mandatory field where the logon name of the user should be entered. The logon name is used to
identify the user when logging in to the system.

Full Name
Use this field to enter the full name of the user. The full name is used when presenting the name of the user,
for instance in audit trails entries.

E-mail/Company/Department/Title/Location/Street address/PO box/City/State/

Postal code/Country/Telephone Number
These fields can be used to enter optional contact information for the user.

Active
This field indicates whether the user is active. A user account cannot be removed from the security system,
but by clearing the Active option, the user will be prevented from logging in to the system.

Locked out
This option indicates that the user has been locked out. It is only available when the user has been locked
out by making too many failed login attempts. Clearing this option will allow the user to login to the sys-
tem again.

Password never expires

This option indicates that the password of the user never expires, even if password aging is enabled.

Reset Password
This button can be used to reset the password for the user. Clicking this button brings up a window prompt-
ing for a new password (and password confirmation). To reset the password, the logged in user must have
the “Reset passwords” permission on the root object. For more information, see “Permissions and Roles.”

User Must Change Password at Next Logon

This option indicates that a new password should be requested the next the user logs in to the system. It is
recommended that this option is enabled when the password has been reset.

Member of
The Member of page is only available when the built-in user database is enabled. It contains a list of all
groups that the user is a member of. To add the user as a member of a new group, click the Add button. To
remove the user as a member of a group, select the group and click Remove. For more information, see the
next section.

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Working with User Groups
A user group can be used to assign permissions to a group of users (and groups), thus simplifying permis-
sions management. Permissions assigned to a user group are automatically assigned to all members of the
group.
If Active Directory integration is enabled, the security groups in Active Directory are available when
assigning permissions, and group management is performed using the standard Active Directory adminis-
tration tools.
If the built-in user database is used, the available groups are managed using the Groups list on the Users
and Groups page.

Creating a New User Group

When the built-in user database is initialized, two user groups are automatically added; the Administrators
group and the Users group. The Administrators group initially contains the Administrator user account.
Additional user groups can be created to provide more specialized groups. For instance, all users that are
allowed to access a specific instrument might be added into a new group. To create a new user group, per-
form the following steps:
1 Click the Add button under the Users list.
2 In the screen that appears, enter a name for the group, and optionally a description.
3 Add members to the group, as described in the next section.

Adding Members to a Group

There are two ways of adding members to a group. Either by using the User properties screen, or the Group
properties screen.
To add a user to one or more groups using the User Properties screen:
1 Double-click the user in the User list. This will bring up the User properties screen.
2 Select the Member of tab.
3 Click Add. This will display the Select Groups screen.
4 Select the group or groups that the user should be a member of. For more information, see “User and
Group Selection.”
5 Click OK to accept the group selection.
6 Click OK again to close the User properties screen and save the changes.
To add members to a group using the Group properties screen:
1 Double-click the group in the Groups list. This will bring up the Group properties screen.
2 Click Add. This displays the Add Users and Groups screen.
3 Select the users (or groups) that should be added to the group. For more information, see “User and
Group Selection.”
4 Click OK to accept the group selection.
5 Click OK again to close the Group properties screen and save the changes.

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User and Group Selection
Users or groups need to be selected when assigning permissions, working with group memberships, or fil-
tering audit trails. This is done by using the users and groups selection screen.

Figure 225 Add Users and Groups.

The top part of this screen is used to search for users and groups. The bottom part is used to specify the
selected users/groups.

Searching for Users and Groups

The User/group name field is used to define the user or group to select. Clicking the Search button will
search for users and groups matching the text in the field and the matching items will be presented in the
list below. The list can be used to select the wanted users or groups by either clicking the Add button or by
double-clicking the name in the list. This will add the user or group to the Selected users and groups field.

Selected Users and Groups

This field contains a list of names (delimited using ‘;’) of the users or groups to select. This field can either
be filled in by typing the name of the user or group, or by using the search feature in the top of the screen.

Check Names
This button can be used to validate the names in the Selected users and groups field. If a name cannot be
found among the available users and groups, or if multiple users or groups match a name, a prompt will
appear.

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Permissions and Roles
Permissions and roles determine the actions that are allowed by a specific user or group on the selected
object.
For each selected item a set of permissions is available. The actual permissions available depend on the
type of the item. For each permission it is possible to define whether the selected user or group is allowed
to perform the related action (Allow), or if the user or group is explicitly denied to perform the action
(Deny). Permissions assigned to one item are normally inherited by child items (unless prevented by clear-
ing the Inherit permissions from parent option). For example, if a user has permission to change device
settings on an instrument, then, by default, the user has permission to change device settings on all devices
installed in the instrument.
It is also possible to define permissions by assigning roles to the user or group. A role is essentially a set of
predefined permissions. When a role is assigned to a user or group, all associated permissions will be
granted to the user or group.

Figure 226 Security tab.

The Security tab is used to define the permissions and roles. It is accessed by selecting the top-level item in
the navigation tree and contains two lists: the User/Group list, which lists all users and groups that have
any permission setting for the selected item, and the Permission list, which lists the permission settings for
the user or group that is selected in the User/Group list.

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Users and Groups List
The User/Group list includes all users and groups that have any permission setting for the selected item. It
has three columns:
• User/Group: This is a read-only column that shows the name of the user or group
• Role: This column shows the role that is explicitly assigned to the user or group for the selected item.
The role of the user and group can be modified by using the drop-down list in this column and select-
ing one of the predefined roles. If no permissions have been assigned to the user or group, the text
None will be presented in this column. If custom permissions have been set using the Permissions list
below, the text Custom will be presented.
• Actual role: This is a read-only column that presents the actual role of the user or group. The actual
role is derived from the permissions assigned to the selected item, and all permissions derived from
parent items.
To add a new user or group to the list, use the Add button. This will allow a user or group to be selected
using the User and group selection screen. When a new user or group is added to the list, it has no defined
permissions. Use the Role drop-down list to assign a role to the user or group, or use the Permissions list to
grant or revoke specific permissions.

Permissions List
The permissions list includes all available permissions for the selected item. It can be used to view or
define the specific permissions for a user or group. The list contains the following columns:
• Permission: This column presents the name of the permissions
• Allow: This column indicates whether the selected user or group has been explicitly granted the per-
mission for the selected object.
• Deny: This column indicates whether the permission has been explicitly revoked for the selected user
or group.
• Actual Allow: This is a read-only column that indicates whether the permission is actually allowed for
the selected user or group. This is derived from the permissions assigned to the selected object, and all
permissions derived from parent objects.
Inherit Permissions from Parent
This option indicates whether permissions set on parent objects should be inherited by the selected object.
Replace Permissions on Child Items with the Permissions from This Item
This option indicates that the permissions settings for this item should be assigned to all child items, when
the changes are applied. This will remove any specific permission settings on the child items.

Available Roles
Currently only two roles are defined:
Administrator
This role includes all permissions available. It is recommended that this role is assigned to the Administra-
tors group at the root item. It can also be assigned to other groups and users at lower level items. It can for
instance be assigned at instrument level to the user responsible for the instrument.

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User
This role includes the permissions needed to work with the instruments and run experiments. It does not
include permissions that allow the user to change advanced settings on devices, or to modify security set-
tings.

Available Permissions
In this section is a list of the default permissions that are available:
Device Rights
• Change device settings (own experiment)
Allows the user to make changes to a device, as long as it is not in use by an experiment run by another user.
• Change device settings (any experiment)
Allows the user to make changes to a device, even if it is in use by an experiment run by another user.
• View device
Allows the user the view the device, e.g., its signal histories and any settings.
• Change device settings
Allows the user to make changes to a device, as long as it is not in use by any experiment.
• Change advanced settings
Allows the user to make changes to the advanced settings of a device.
Experiment Rights
• View any experiment: Allows the user to view any running experiment, even if it is started by another
user.
• Create experiment: Allows the user to start new experiments
• Change any experiments: Allows the user to make changes and control any running experiment, even
if it is started by another user.
Generic Rights
• View permissions: Allows the user to view the security permissions of the selected item.
• Reset password: Allows the user to reset the password of other users. This permission is only avail-
able on the top-level item (the security system itself).
• Change permissions: Allows the user to make changes to the security permissions of the selected
item.
• Modify users: Allows the user to modify the user database, e.g., adding, editing or removing users and
groups. This permission is only available on the top-level item (the security system itself).
• Change security settings: Allows the user to make changes to the security settings of the system. This
permission is only available on the top-level item (the security system itself).
• Connect: Allows the user to connect to the Device and Experiment server (e.g., a TAM III instrument)

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Audit Trail
The audit trail is used to keep track of all events that happen on the system. The events can for instance be:
setting new temperature on a thermostat, performing a calibration, starting an experiment, or any system
problem. Each entry in the audit trail contains information like time, user, severity, and a description. An
audit trail is automatically collected by the security system. As soon as an instrument is connected to the
system, audit entries are collected from the instrument as well. The audit trail can be examined using the
Audit page, which is available for all securable items.
The Audit page consists of two parts. The top part is used for setting up a filter for the audit entries that
should be presented. The bottom part contains a list of all the filtered audit entries.

Audit Entries Filter

The following fields are used to define the audit trail filter.

Show Entries for User(s)

This option is used to filter audit entries based on the user that caused the event that was logged.

Figure 227 Audit tab.

• All users: The audit trail will include entries logged by any user.
• Selected users: The audit trail will only include entries logged by the selected users. The list of users
can be entered in the field below, or it can be defined using the Browse button.

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Show Entries Added During
This area is used to specify the time period for the filter. Events that occurred during the specified time
period will be included in the audit trail.
The time period can be specified using the following predefined intervals:
• Any time: No filtering of the time of the event is performed.
• Last month: Only events added during the last month are included.
• Last week: Only events added during the last week are included.
• Last day: Only events added during the last day are included.
• Custom: The time period is defined using the from and to fields below.

Show Entries in Categories

This drop-down list is used to specify the categories of the event entries that should be included. One ore
more categories can be included by selecting them in the drop-down list.

Minimum Audit Level

This field is used to specify the minimum audit level of the event entries that should be included. The audit
level indicates the severity of the event. The following levels are available:
• Info
• Warning
• Error
• Fatal

Show Entries for Children

This option indicates whether event entries that occurred in child items should also be included in the fil-
tered audit trail.

Show Most Recent Entries First

If this option is enabled, the entries will be presented in reverse chronological order, i.e., the most recent
entry will be presented at the top.

Show Oldest, Show Older, Show More Recent, Show Most Recent
If too many entries match the specified filter, these fields are used to navigate through the entries.

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Exporting Audit Trails
The filtered audit trail presented can be exported to a file by selecting Export Filtered Audit Trail from
the File menu. (If the audit trail is view inside TAM Assistant, the Export Filtered Audit Trail command is
found in the tool bar above the audit trail. For more information, see “Security in Property Windows.” This
will bring up a standard save file window, providing the possibility to specify the file to export to and the
file type.
The following export file types are available:
• Text File: If file type is selected, the audit trail will be exported as a plain human-readable text file.
• Comma Separated Value File: If file type is selected, the audit trail will be exported as a Comma
Separated Value file (CSV).
• Comma Separated Value File (compatible): If this file type is selected, the audit trail will be
exported as a Comma Separated Value file that is compatible with Microsoft Excel.
• XML File: If this file type is selected, the audit trail will be exported as an XML-file.

Printing Audit Trails

The filtered audit trail presented can be printed by selecting Print Filtered Audit Trail from the File
menu. (If the audit trail is viewed inside TAM Assistant, the Print Filtered Audit Trail command is found in
the tool bar above the audit trail. For more information, see “Security in Property Windows.”

Commands in TAM Assistant Security Manager

The following commands are available from the File menu in TAM Assistant Security Manager:
• Connect: Connects the TAM Assistant Security Manager to a security server. This command will
bring a window that allows a security server to be selected.
• Initialize Local Security Server: Initializes the local security server. This command is only available
if a security server is installed on the computer running.
• Export Filtered Audit Trail…: Exports the results of an audit trail search. This command is only
available when viewing audit trails. For more information, see “Audit Trail”
• Print Filtered Audit Trail…: Prints the results of an audit trail search. This command is only avail-
able when viewing audit trails. For more information, see “Audit Trail.”
• Exit: Exits TAM Assistant Security Manager.

Security System Access in TAM Assistant

The TAM Assistant software and the TAM III instrument provides access to most functionality if the secu-
rity system. It also provides functionality for specifying the security system to used, and other settings such
as how login should be performed. Audit trail and permissions management can be accessed using the
Properties for a securable object, such as a device or results file.

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Security Settings
The Security Settings screen is available in TAM Assistant by selecting the Settings command under the
File/Security menu.

Figure 228 Security Settings.

It provides the possibility to change the following security settings.

Automatically Login at Startup

This option indicates whether TAM Assistant should automatically bring up the login window when the
program is started. If this option is not selected, TAM Assistant will not login nor connect to any devices
until the user explicitly logs in using the Login command under the File/Security menu.

Use Current Windows Credentials When Logging In

This option is used to decide whether the current Windows credentials should be used when logging in to
the security system. If Active Directory integration is enabled and the security system settings allows auto-
matic login, then it is possible for TAM Assistant to login without prompting for a user name and pass-
word.

Automatically Connect to Devices at Login

Indicates whether TAM Assistant should automatically connect to all registered device servers when the
user has logged in. If this option is not enabled, the Connect to Device Servers command under the File
menu must be used to initiate the device connection manually.

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Security in Property Windows
When a device or results file window is being shown, it is possible to use the Properties command (on the
View menu) to view and edit the properties of the device or results file. If TAM Assistant is connected to a
security server, the properties window will include two additional pages: Security and Audit. These pages
are used to view and edit permissions for the object and to view the audit trail. They are equivalent to the
Security and Audit pages in the TAM Assistant Security manager, but they only act on the selected device
or results file.

Figure 229 Properties of the device.

Commands in TAM Assistant

The following commands are available from the Security submenu under the File menu in TAM Assistant:
• Log in new user: Logs in a new user.
• Log out current user: Logs out the currently logged on user. All open documents will be closed, but
any running experiments will not be affected.
• Suspend current user: Suspends the current user. The main windows will be closed and a login screen
will appear, allowing another user to login. However, the original login is still active. If the same user
logs in again, all open documents will be restored.
• Change password: Changes the password of the currently logged in user.
• Settings: Opens the security settings window. For more information, see “Security Settings.”

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Commands on the TAM III Instrument (TAM Assistant
Embedded)
On the TAM III instrument, the security related commands are found under the Security button in the top
menu. The following commands are available:
• Log out current user: Logs out the currently logged on user. All open documents will be closed, but
any running experiments will not be affected. The system overview and login screen will be shown.
• Suspend current user: Suspends the current user. The main windows will be closed and a login screen
will appear, allowing another user to login. However, the original login is still active. If the same user
logs in again, all open documents will be restored.
• Change password: Changes the password of the currently logged in user.
• Security Manager: Opens the Security Manager window. This window is equivalent to the TAM
Assistant Security Manager main window. This allows security settings and permissions to be edited
on the TAM III instrument.

Security Considerations and Backup of Security Data

NOTE: There is currently no way of backing up the security data files if the security system is running on
the TAM III instrument. If the audit trails and user database is important, it is recommended that the secu-
rity system is installed on a standalone computer which is properly backed up.
The security system server stores security data (user database and permissions) and audit trails in normal
files. When installing the software, a folder where these files should be stored must be specified. In order
to avoid tampering with the security files, this folder should only be used for the security files, and the
access to the folder should be limited. The account that runs the security system service must have read/
write access to the folder. To simplify file management and to allow direct access to the security system (as
described below) it might be a good idea to allow the LocalSystem account and the Windows Administra-
tors group to access the security files folder as well.
If a user (who should be an administrator) has access to the security files, it is possible to locally use TAM
Assistant Security Manager, without first logging in to the security system. This provides the possibility to
restore permissions and settings even if normal administrative access to the system is not possible, for
instance if the administrator password has been lost, or administrative permissions have mistakenly been
removed.

Backup
The security system service is designed to allow files to be backed up while the service is running. To pre-
vent loss of audit trails and other security data, it is recommended that the folder containing the security
files are backed up regularly, as part of the normal backup procedures.

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Appendix:
STANAG 4582

Measurement Duration and Heat Flow Limits

Measurement times (tm) and heat flow limits (Pl) for temperatures 60–90°C recommended in the STANAG
4582 procedure.
Table 14: Values taken from STANAG 4582

Tm [°C] tm [days] P1 [µW/g] Tm [°C] tm [days] P1 [µW/g]

60 123 9.8 76 16.9 71.1

61 108 11.1 77 15 80

62 95 12.6 78 13.4 90

63 83.6 14.4 79 11.9 101

64 73.6 16.3 80 10.6 114

65 64.9 18.5 81 9.43 127

66 57.2 21 82 8.41 143

67 50.5 23.8 83 7.5 160

68 44.6 27 84 6.7 179

69 39.4 30.5 85 5.98 201

70 34.8 34.5 86 5.35 225

71 30.8 39 87 4.78 251

72 27.3 44 88 4.28 281

73 24.2 49.7 89 3.83 314

74 21.5 56 90 3.43 350

75 19 63.1

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STANAG Safety Issues
There is always demand to be extra cautious when working with propellants. As the decomposition reac-
tion proceeds and the concentration of gases increases there will be a corresponding pressure increase
inside the sealed ampoule. Naturally there might be a risk for personal injury when handling the ampoules
after a measurement. The pressure inside the ampoule will decrease a little when bringing the temperature
down to ambient. However, this is merely a 10% decrease or less if the measurement was performed at
90°C. It is recommended to carefully penetrate the teflon/rubber gasket with a thin hollow needle (e.g. an
injection needle) in order to release the pressure in the ampoule. This should be done with the ampoule
positioned inside some kind of safety cabinet.
Another complication that might arise is the possibility that the aluminium cap swells due to the pressure
increase and the ampoule may get stuck inside the measuring position. This may make the ampoule impos-
sible to remove without severe damage to the lifting tool and possibly the calorimeter. If this occurs it is
strongly advised to lower the temperature of the TAM III to ambient temperature and wait to see if the
pressure decrease will allow for the ampoule to be removed. If no luck removing the ampoule please con-
tact TA Instruments service for assistance.
WARNING! Due to safety it is advisable to stop a measurement and remove the ampoule when the
total heat produced reaches 150 J.

References
For more in depth reading on the basis of the STANAG 4582 standard, please see reference [1] and [2].
1 U. Ticmanis, S. Wilker, G. Pantel, P. Guillaume, C. Balès, N. van der Meer. Principles of a STANAG
for the estimation of the chemical stability of propellants by Heat Flow Calorimetry", Proc. Int Annu.
Conf. ICT 31, 2 (2000).
2 P. Guillaume, M. Rat, S. Wilker, G. Pantel, "Microcalorimetric and Chemical Studies of Propellants",
Proc. Int Annu. Conf. ICT 29, 133 (1998).
3 STANAG 4582: Explosives, nitrocellulose based propellants, stability test procedure and requirements
using heat flow calorimetry.
4 TAM III Quickstart Presentation

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