4. Turn on both the cooling and heater devices. Set the begin
temperature using the controller unit (heater device) and wait
until the sample holder reaches this temperature and remains
stable. Note that the thermometer with the thermocouple
touching the sample provides the actual sample temperature,
which generally differs (several degrees) from the value indicated by the controller unit.
In case a Linkam stage is used for cooling with LN 2, turn
on the manual pumping mode and use mode 1 for temperatures ranging from 0 to 20
C, mode 3 for temperatures from
0 to À20
C, and mode 5 for temperatures below À20
C
down to À60
C.
5. Enter the temperature ramp settings using the controller unit.
Most sample holders for spectral data acquisition are not suited
for high cooling or warming rates. A ramp rate of 1
C/min is
suitable for most studies.
When a Harrick controller unit is used for heating, settings
should be as follows: thermocouple type (input/set, Ln1), H;
control type (9LbL/set, CntL), nor; settings units (9LbL/set,
C_F),
C; low temperature limit in
C (input/set, rL1), À200;
high temperature limit in
C (input/set, rH1), 750; low power
limit in % (9LbL/set, LoP), 0; high power limit in % (9LbL/
set, HiP), 35; autotune set point (9LbL/set, AtSP), 90; ramp
setting (9LbL/set, Rp), i.e., StPt as mode for entering a set
point temperature to be reached; and ramp rate in
C/min
(9LbL/set, Rp), i.e., 1 for a cooling/heating rate of 1
C/min.
6. In the program for acquisition of spectra at timed intervals,
enter the settings for spectra acquisition: (1) enter data collection mode (timed interval, e.g., 30 s) and duration of the run
(dependent on the temperature ramp and range); (2) supply a
name for saving of spectra (folder, yymmdd-n; spectra, nNN#);
(3) add scan settings (8 co-added interferograms,
4000–900 cm
À1 wave number range); and (4) select view
during spectra acquisition.
7. Start acquisition of spectra during the temperature scan:
(1) start the program for spectra acquisition at timed intervals,
(2) start the temperature ramp by entering the end temperature
(set point) on the controller unit, (3) start de data logger
attached to the thermocouple monitoring the actual sample
temperature, and (4) start a stopwatch. Make sure that the
heater and cooling devices are in correct modes, dependent
on the temperature scan that is performed (adjust during the
run when needed). Check spectra quality and sample temperature during the course of the run. As an alternative for using
the data logger attached to the thermocouple, the sample
temperature can be noted manually as a function of time
(every 2–10 min) during the run. When the end temperature
is reached, return the sample holder temperature to 20
C.
In situ Infrared Spectroscopy
339
temperature using the controller unit (heater device) and wait
until the sample holder reaches this temperature and remains
stable. Note that the thermometer with the thermocouple
touching the sample provides the actual sample temperature,
which generally differs (several degrees) from the value indicated by the controller unit.
In case a Linkam stage is used for cooling with LN 2, turn
on the manual pumping mode and use mode 1 for temperatures ranging from 0 to 20
C, mode 3 for temperatures from
0 to À20
C, and mode 5 for temperatures below À20
C
down to À60
C.
5. Enter the temperature ramp settings using the controller unit.
Most sample holders for spectral data acquisition are not suited
for high cooling or warming rates. A ramp rate of 1
C/min is
suitable for most studies.
When a Harrick controller unit is used for heating, settings
should be as follows: thermocouple type (input/set, Ln1), H;
control type (9LbL/set, CntL), nor; settings units (9LbL/set,
C_F),
C; low temperature limit in
C (input/set, rL1), À200;
high temperature limit in
C (input/set, rH1), 750; low power
limit in % (9LbL/set, LoP), 0; high power limit in % (9LbL/
set, HiP), 35; autotune set point (9LbL/set, AtSP), 90; ramp
setting (9LbL/set, Rp), i.e., StPt as mode for entering a set
point temperature to be reached; and ramp rate in
C/min
(9LbL/set, Rp), i.e., 1 for a cooling/heating rate of 1
C/min.
6. In the program for acquisition of spectra at timed intervals,
enter the settings for spectra acquisition: (1) enter data collection mode (timed interval, e.g., 30 s) and duration of the run
(dependent on the temperature ramp and range); (2) supply a
name for saving of spectra (folder, yymmdd-n; spectra, nNN#);
(3) add scan settings (8 co-added interferograms,
4000–900 cm
À1 wave number range); and (4) select view
during spectra acquisition.
7. Start acquisition of spectra during the temperature scan:
(1) start the program for spectra acquisition at timed intervals,
(2) start the temperature ramp by entering the end temperature
(set point) on the controller unit, (3) start de data logger
attached to the thermocouple monitoring the actual sample
temperature, and (4) start a stopwatch. Make sure that the
heater and cooling devices are in correct modes, dependent
on the temperature scan that is performed (adjust during the
run when needed). Check spectra quality and sample temperature during the course of the run. As an alternative for using
the data logger attached to the thermocouple, the sample
temperature can be noted manually as a function of time
(every 2–10 min) during the run. When the end temperature
is reached, return the sample holder temperature to 20
C.
In situ Infrared Spectroscopy
339