USER COM

1
Information for users of May 1995
METTLER TOLEDO thermal analysis systems

Dear customer
The aim of this customer maga-
Different
zine is to provide direct contact
between ourselves and you. After
several approaches from you
temperatures
regarding the subject of commu- TA TIP
nication, we have now brought
this customer forum into being. It We are constantly asked what temperature is shown, when and where it is
will provide you with an opportu- shown, in what relation and what this means. Several temperatures are im-
nity to communicate with us and portant in thermal analysis.
other TA users regarding an appli-
cation, a question, a wish or a
suggestion for improvement. We TS: effective sample temperature
shall attempt to provide answers TR: effective reference temperature
to questions in the edition follow- TP: set value of the temperature program
ing their receipt. Wishes and sug-
gestions for improvement will be The following temperatures are, however, measured:
collected by us and if possible
implemented in one of the follow- TC: furnace temperature
ing versions. TSM: measured sample temperature
Should you or one of your col- TRM: measured reference temperature
leagues find this magazine inter- ∆T: temperature difference between sample and reference
esting, may we ask you to inform
us by FAX or letter.
The measured temperatures are converted to the effective temperatures us-
We plan to publish the magazine
ing a mathematical model determined by the calibration. The effective
biannually.
sample temperature can be determined very accurately by this means with-
out direct measurement in the sample. As neither the sample temperature
nor the temperature difference are measured with the TG50 and the
Contents TMA40, the sample temperature and the program temperature are identical
here.
TA TiP:
Different temperatures
NEW in sales program:
New TGA850 cell
Software TSW870 V3:
SW option X-terminal
SW option Model-free kinetics
Expansions/Improvements
Trade fairs, symposia
Fax Back

USER COM May 95 1

When the different temperatures are plot-
ted as a function of time, the following pic-
ture results for a calibrated cell:
With our software (TSW870 Vx), a
curve can be shown as a function of
time, as a function of time/reference
temperature, as a function of the
reference temperature or the sample
temperature.
In the simple time representation, no
temperature information is given.
In the time/reference representation,
the curve is also shown as a function
of time except here the program
temperature is plotted above the
time axis. The program temperature
is taken from the curve which is first
opened in the evaluation window.
A curve and its four possible representations
2 USER COM May 95
If several curves with different tem-
perature programs are opened, this
representation is meaningless.
In the reference temperature repre-
sentation, the measured values are
plotted as a function of the reference
temperature.
In the sample temperature represen-
tation, on the other hand, the curve
is plotted as a function of the sample
temperature. Here, the temperature
remains practically constant during
the melting process and this is
shown by the vertical part of the
curve.
Irrespective of the type of represen-
tation, with our software (TSW870)
it is always possible to have the
numerical results calculated in terms
of the sample temperature or as a
function of the abscissa.
On the other hand, the following
temperatures are shown on the
module:
DSC820: TC
TGA850: TC
TC15: TP (before and after the measurement TC)
The module control window always
shows the furnace temperature.
The new TGA850 thermogravimetric
module is here!
The TGA850 module is available
from May and expands the thermo-
gravimetric product range in the top-
of-the-line performance segment. As
with the DSC820, a modular concept
has been selected here. This allows
you to assemble the instrument con-
figuration optimum for your needs.
An expansion (e.g. with sample ro-
bot) can also be implemented at a
later date.
The measuring cell incorporates
state of the art METTLER TOLEDO
weighing technology in the form of
the ultramicro balance. You can thus
rely on the results. With the SDTA
operating possibility, you can gener-
ate the DTA curve following the The features of the TGA850 module at a glance:
measurement. The SDTA (Single • large measurement range 2g
Differential Thermal Analysis) sig-
• high resolution 0.1 µg
nal is calculated from the measured
• minimal noise (RMS) < 1 µg
sample temperature and is a standard
• parallel guided balance no positioning error
feature. This allows the analysis of
• temperature range room temperature –1100 °C
effects which do not cause mass
• high temperature accuracy +/– 0.25 °C
changes. It can be seen simply and
• horizontal furnace minimum disturbing influence of
quickly whether the reaction is exo-
the purge gas
thermic or endothermic.
• gas-tight measuring cell definable measurement environment
• SDTA measurement physical transformations are visible
With the optional sample robot, you
• coupling possibility (TG-MS) analysis of decomposition products
can increase your productivity enor-
• modular expansion open for the future
mously. At the highest level of auto-
• computer control simple operation using the latest
mation, sample feed, performance of
computer software
the measurement, evaluation and
result assessment up to the color
printout are all undertaken automati-
cally. As with the DSC820, the sam-
ple robot can be loaded with 34 sam-
ples. Each sample can be assigned
not only a different method but also
a different evaluation.
If need be, the crucible can be fitted
with a lid and positioned on the sam-
ple turntable. Depending on the
method, the lid can be removed by
the sample robot immediately before
the measurement. As a result, the
sample exchanges virtually no mois-
ture with the surroundings between
weighing in and performance of the
experiment.
Measured TGA Curie and SDTA melting temperatures

USER COM May 95 3

 Further improvements
The TSW870
TA software – TA basic version
As a result of various suggestions Calibration of the heat flow has been
yet another step from our circle of customers, we have
made many improvements. The vari-
extended so that it can be performed
analogous to the temperature cali-
forward ous windows can now be started in
the following languages:
bration with several different sub-
stances.
English Further, a total calibration has been
The latest version V3 is available German implemented which in the case of
from May. In addition to two further French DSC and TGA determines all param-
options, X-terminal and model-free In addition to the US keyboard, eters by means of a single measure-
kinetics, the basic version and the Swiss, French and German keyboards ment. This allows simple and rapid
other options have been expanded are supported. To facilitate manual calibration of the modules. For the
by new possibilities. calculations, you can now power up greatest accuracy, you can naturally
an on-screen calculator. still use the single calibrations.
1st option: X-terminal operation
On an X-terminal (data input station
with mouse, keyboard and screen),
a UNIX PC (e.g. TAS810) or an
MS-Windows PC with X-terminal
emulation, additional evaluation
windows can be opened. For the first
time ever, this allows several per-
sons to work simultaneously with
one and the same software (and also
with the same database!). Only such
a feature allows genuine multiuser
operation.

2nd option: Model-free kinetics

The new way to calculate kinetics is
based on the theory of the Russian
scientist Dr. Vyazovkin and makes it
is possible for the first time to per-
form kinetic evaluations and draw
corresponding conclusions without
previous selection of a physico-
chemical model. Until today, the Here, three TG stages are evaluated collectively
model, usually nth order, had first to
be chosen and then the measurements
used to calculate the parameters.
At the very best, the results were only
as good as the degree to which the
chosen model reflected reality.
With the model-free kinetics, the
step which is associated with errors,
namely the model selection, has
been dropped. In addition, for the
first time complex reactions can also
be investigated very simply. These
kinetics are suitable for both DSC
and TG measurements.

Epoxy resin curing not nth order

USER COM May 95 4

New printing possibilities allow the
printout of a window or the entire
screen contents in black and white
on the HP DeskJet.
Calculated curves still retain the in-
formation of the original experiment
in V3.0. Consequently, the database
relations also exist for such curves
and search operations (e.g. by meth-
od or user) are possible.
A new feature is the deletion of entire
«trees» in the database. In other
words, you can not only delete sin-
gle objects as before, but entire,
related data structures (e.g. every-
thing that user X has generated)
→ methods → experiments
→ (curves) → evaluations
Whether curves should be deleted or
not can be decided for each individ-
ual case.
The evaluation window has been
expanded by many minor but useful
possibilities. With a double-click on
the ordinate you can switch between
the relative and absolute representa-
tion. You can now also use the nu-
meric key block. The peak tangents
and the hatching can be switched off
in the integration via the settings.
With horizontal step, the inflection
point is also calculated.
5 USER COM May 95
SW option
Automatic evaluation
Following feedback from a cus-
tomer, the Eval macro now contains
information on whether limits within
a definable range should set auto-
matically or fixed. If a reaction does
not always appear at the same place,
the expansion still allows fully auto-
matic evaluation. A wide range with-
in which the evaluation should be
automatically sought is simply
defined in the Eval macro. As the
effects which appear are not always
of the same magnitude, the plot is
automatically scaled on the ordinate
and plotted exactly in the aspect
ratio which the evaluate window had
on generation of the Eval macro.
SW option DOS Data import
The DOS data import has been ex-
panded. In addition to the TA72 files, We hope that these expansions and
mass spectrometer files from Balzers improvements will facilitate your
(MS Cube) can be imported.
SW option Mathematics
The Mathematics option has been
expanded by the Fourier analysis
evaluation. This can be used for an
even simpler analysis of periodic
curves (DLTMA or ADSC – alter-
nating DSC). The envelope curve
algorithm has been accelerated many
times so that with curves based on
many measured points the envelope
curve can be plotted within a few
seconds.
The manual plotting of lines (or base-
lines) has been made more user
friendly. You can now draw the
baseline in the manner of a rubber
band and correct it by moving back
the pointer.
SW option TGA
With the TGA option, the content
calculations have been expanded by
the drying loss. As a result, the dry-
ing loss, which appears between
weighing in and performance of the
experiment, is included in the first
mass stage and, depending on the
settings, reported as such.
work with the software.
For further questions, please contact
your local METTLER TOLEDO
company.