Primacs Mcs Operat

PRIMACSMCS TOC
ANALYSER
CHAPTER 3: OPERATING THE ANALYSER
Preface:
This chapter gives routine and detailed operating instructions.

PrimacsMCS TOC Analyser Chapter 3 Operating 3-1
3 OPERATING
3.1 Standards and sample pretreatment
3.1.1 Preparation of standards
Introduction:
Only pure chemicals are to be used as standards for organic and inorganic
carbon. The chemicals require no further preparation, as they are pure.
Required Chemicals:
Calcium carbonate p.a., CaCO3 (Merck, cat. no 102066)
Oxalic acid, (COOH)2 .2H2O (Merck, cat. no. 100594)
Standards for the calibration curve of solid samples:
Only weigh different quantities of the standard for the calibration curve. The
amount depends on the required measuring range and the measuring
range of the IR detector (see chapter 6.1 for possible ranges). For TC
measurement Oxalic acid is advised and for IC measurement Calcium
carbonate.
3.1.2 Preparation of reaction solutions
Preparation of the 20% Phosphoric acid solution for the IC reactor
Dilute 235 ml 85% phosphoric acid to 1000 ml with carbon-free water and
mix.
3.1.3 Sampling and general pre-treatment
Solid samples:
Taking a sample one must pay attention that the sample is representative.
Therefore the sample must be completely homogeneous. Collection of the
sample should be done in a clean glass bottle and then treated according
to ISO 11464 and 11465. A representative sub-sample of the laboratory
sample has to be milled until it passes a 250 m aperture sieve. Standards
need no pretreatment and can be analyzed directly.
Use an analytical balance with accuracy of 0.1 (recommended) or 1 mg
(depending on the weight) to weigh the amount of sample directly into the
crucible (TC, cat.no 2CS22003) or into the test tube (IC, cat.no.
2CA50002). The sample in the crucible should be analyzed directly after
weighing.
For an IC analysis the sample must be wet with approx. 0.2 ml (5 10
drops) of carbon free water. The water has to wet all present sample in the
test tube before measurement for better acid/sample contact.
Sludge samples:
Taking a sample one must pay attention that the sample is homogeneous.
Mix before taking a sample. We advise to homogenize the samples by
means of an Ultra Turrax device or good alternative.
3.1.4 Quality Control

To make sure the obtained results are reliable one has to analyze quality
control samples daily. Prepare quality samples from standards as
mentioned at Preparation of standards at the top of this page.
Depending on the concentration of the test samples the following
tolerances are allowed:
1 to 10 mg C /g. 5%
>10 mg C /g. 3%
When the tolerances are not kept, also after several analyses, follow these
troubleshooting procedures to solve the problem:
Clean the analyser components that are in direct contact with the
sample.
Check the system on liquid and/or gas leakage.
Check the system on temperature accuracy.
To examine the oxidation degree one has to select a concentration of
quality control samples, which are in the concentration range of the
samples.
To report a correct TOC value if IC concentration is approx. < 5% of the TC
value, we advise to re-analyze the sample for IC in a more sensitive mode
and calculate the final TOC concentration offline.
3.2 Operating the hardware

3.2.1 Routine start up and shut down procedure
Short operator reference instructions
Start up Procedure in combination with Formacs:
Turn on the gas supply for the Formacs and the PrimacsMCS.
Switch on the Formacs (mains switch at the rear and also the
button on the display at the front) and PrimacsMCS (mains switch at
the rear), the computer and the printer.
Switch on the balance.
Start the software program for the Formacs, connect the analyser
and select Send settings to Analyzer.
Put the Formacs in Standby mode.
Open the Control panel and select Enable MCS.
Close the software program.
Start the software program for the PrimacsMCS, set the TC temp on
250C, connect the analyser and select Reset all or Send settings
to analyser.
Wait till the oven reaches temperature (1100C) and the analyser is
stabilised ( hour).
Run the baseline in the software on the computer screen.
If stable (1000 counts) the system is ready to run an analysis.
Shut down Procedure.
Close the Primacs software program.
Turn off the gas flows.
Close the windows software program.
Switch off the Formacs, the PrimacsMCS, the computer and the
printer.
Switch off the balance.
Remove samples from the analyser and empty waste vessels.
3.2.2 Extended operating instructions

A. Turn on the gas supply at the gas bottle
The pressure valve indicates the proper gas flow. The gas supply must be
2 bar (0.2 MPa) on the gas pressure gauge on the bottle, correct if
necessary by adjusting the valve on the gas bottle. The gas flow enters the
analyser where the flow is stabilized and divided. (The manometer on the
front panel of the PrimacsMCS shows the actual inlet pressure (0.2 MPa)
(which is adjusted to140 ml/min. by flow regulator).
Note: The gas flow for the Formacs analyser has to be put on as well.
Refer to the manual for the Formacs analyser.
B. Switching on the instrument
1. Switch on the mains supply of the PrimacsMCS TOC Analyser and the
Formacs analyser, which can be found at the rear of the instruments
above the power supply connection. Then switch on the FormacsHT by
the button on the display.
2. Switch on the PC and the printer.
3. Switch on the balance.
4. Select the software for the Formacs analyser and select Autoconnect
from the Connection menu. Select Send Settings to Analyser. Wait
until analyser is initialized.
5. Put the Formacs analyser in Standby mode.
If connected to a FormacsHT analyser: Standby with the oven
temperature on 250C and flow off.
6. Open the Control panel, select Enable MCS and then close the
Formacs software program.
7. Select TOC4WinMCS from the desktop to start the software program
for the PrimacsMCS.
8. Select Autoconnect from the Connection menu.
9. Select Analyser Settings and set the TC temp on 250C (= Standby
temp of FormacsHT oven).
10. Select Reset All. You can check the IR detector, the Peltier
temperature and the Read and Write pointer in the Info window.
11. Wait until the display on the PrimacsMCS analyser shows that the oven
has reached the required temperature.
12. Run the baseline in the Peaks window. Press the Reset button of the
IR detector on left side the FormacsHT (see chapter 3.2.1 of the
Formacs user manual). When the baseline is stable the system is
ready to start an analysis.
3.2.3 Shut down procedure
1. Close the software program.
2. Turn off the gas flows at the gas bottles.
3. Close the windows software program.
4. Switch off the main power switch on the PrimacsMCS and Formacs
analyser.
5. Switch off the computer, the printer and the balance.
6. Remove samples and empty the waste vessels.
3.2.4 Sampling on PrimacsMCS
Note: For measurement on the PrimacsMCS, set range in template on high.
1. Prepare a template with standards and/or samples (see chapter
3.3.7.1). It is advised to place a blank TC on the first position.
2. Prepare a new analysis file (see chapter 3.3.8.1).
3. Check the baseline and adjust if necessary by pressing the Auto Zero
button.
4. Check your settings (see chapter 3.3.4.2).
5. Press Start Analysis. The Status Panel is displayed (see Figure
3.47). Press Continue. The analysis is started. Depending on the
sample in the template the program asks for a sample in the TC or IC
port.
Note: Quartz TC crucibles which are used to analyze acidified
samples cannot be used to analyze neutral or alkaline (pH >2)
samples.
3.2.4.1 TC sampling procedure
Remark: Make sure that an IC sampling tube is sealed in the IC port.
1. Release the hand lever by pushing it down and pull the TC crucible
holder out of the TC sampling port by its handgrip.
2. Carefully place the required TC sample of the template into the crucible
holder.
3. Push the handgrip with the crucible holder (see Figure 3.1) completely
into the TC sampling port and pull up the hand lever to seal the port.
Figure 3.1 TC port, place sample Figure 3.2 TC port, lift sample
4. Wait until the zero level is stabilized. Then push the crucible up into the
reactor by means of the slider (see Figure 3.2). Fixate the slider at its
highest position.
5. Click OK to start the analysis of the sample. After finishing the peak (a
message is displayed that a sample has to be inserted), pull the slider
down. Release the sealing hand lever and pull the handgrip with
crucible holder from the TC sampling port.
6. Place a new sample and repeat step 3-5 until the last sample of the
template is measured. When the last sample is measured a message
is displayed that the analysis is ready.
Warning!!!
The crucible is extremely hot after the analysis!
DO NOT TOUCH!!
The crucible holder is heated by the crucible
DO NOT TOUCH by fingers!!
3.2.4.2 IC sampling procedure
Remark: Make sure that the TC port is closed and sealed with the hand
lever.
1. Turn the screw head of the IC one turn until the tube can be pulled out.
2. Place the required sample tube (see Figure 3.3) carefully into the
screw head (through the sealing ring) as far as possible and turn the
screw head until fixed.
Figure 3.3 IC sampling Figure 3.4 Place IC oven
3. Turn the heating unit under the IC tube (see Figure 3.4) and push it up
as far as possible. Fixate it with the hand bolt (see white arrow in
Figure 3.4).
4. Add the required amount (3-4 ml) of 20% phosphoric acid by means of
a dispenser and press OK.
5. After the analysis (when the software asks for a new sample) release
the hand bolt and slide the heating unit down and aside. Remove the
tube from the screw head and place a new test tube. When all samples
of the template are done a message is displayed that the analysis is
finished.
Warning!!
After the analysis the test tube is hot and contains strong acid!
Use Gloves!!
3.2.4.3 TOC sampling procedure

When TOC has to be measured, a template is created with TC and IC
samples.
1. Follow the same procedure as for the TC or IC to create a template,
but weigh of each sample a duplicate, one in a crucible and one in a
glass tube and enter their respective weights into the template on the
same position.
2. Start the analysis with the measurement of the TC sample. When the
analysis is finished the message that is shown on the screen, indicates
that a sample is to be inserted in the IC port.
3. Place the IC sample with the same identity as the TC sample just
measured, in the IC port and click OK to start the measurement.
4. Proceed with the analysis (check each time in which port the next
sample is to be placed) until the last sample of the template is
measured. A message will be displayed that the analysis is finished.
3.2.4.4 Short procedure
Make a template with at least three samples as described above and start
the analysis.
During the analysis add the rest of the samples (positions) to be measured
to the template in the Results screen (see chapter 3.3.8).
Warning: Be aware of the fact only positions can be added or inserted
at least two positions after the position that is being
measured.
3.3 Software
3.3.1 Introduction
Note: Please take some time to look through the manual and become
acquainted with the features of this software program.
Remember that this is a windows program and several windows can cover
each other so you cannot see them. The program follows the usual
Windows conventions. The windows in which parameters are set and
where specific information is entered for the program to be continued, must
be closed before proceeding. These windows are called dialog boxes. The
program can be easily operated by keyboard or (preferably) by mouse.
The text between quotes refers to text within the window.
Note: It is highly recommended not to open other programs during an
analysis run.
3.3.1.1 Keyboard
Hot keys These are the underlined letters that in combination with
the Alt. key provides a short cut to that item in the main
menu.
Tab Go to next selectable item.
Cursor Cursor movement keys, to toggle up, down, left and right
through menu's, lists etc.
Enter To go into edit mode, also used to confirm edited script.
3.3.1.2 Mouse
Operating the program with a mouse is fast and direct. Although a
combination of both keyboard and mouse is recommended for normal day
to day usage.
Mouse pointer The little I-beam pointer (or arrow in the graphic section)
that moves around the window as you move the mouse
on a flat surface.
Click Means pressing either left or right mouse button.
Double click Means pressing the mouse button for the second time
directly after the first click.
Drag Means holding the mouse button down while dragging the
mouse over the area required.
3.3.1.3 Regional Settings
The program can be run in English, French and German. To open the
program in the required language the Regional Settings have to be set
according the used language.
For Windows NT:
Select Settings, Control Panel, Regional Options from the Start menu.
The settings for the French language have to be set only on French
(Standard) and for the German language only on German (Standard).
Select the button Set Default. Set the language to the required language in
the Select System Locale screen.
For Windows 2000:
Select Settings, Control Panel, Regional Options from the Start menu.
(France) (see Figure 3.5) and for the German language only on German
(Germany).
Select the button Set Default. Set the language to the required language in
the Select System Locale screen.
Figure 3.5 Windows 2000 Figure 3.6 Windows XP
For Windows XP:

Select Control Panel, Regional settings and Languages from the Start
menu.
Select the Advanced tab.
(France) and for the German language only on German (Germany) (see
Figure 3.6).
3.3.2 The main window

Note: The program can be run in English, French and German. To run the
program in the required language the Regional Settings have to be
set according the used language (in Settings, Control Panel,
Regional Options) before opening the program. For Windows 2000
and Windows XP the settings for the French language have to be
set only on French (France) and for the German language on
German (Germany); for Windows NT the settings for the French
language have to be set only on French (Standard) and for the
German language on German (Standard). Any other regional setting
will start up the program in English.
The program is installed in the Program Files directory and automatically
placed in the Start menu. Also a shortcut icon is placed on the desktop.
Select Start/Programs/TOC4Win MCS to start the program or double click
on the shortcut icon on the desktop.
The following window is opened. (see Figure 3.7).
Figure 3.7 Main window

The window shows an information (=) menu and eight main menus:
Settings, View, Connection, Template, Analysis, Method, Logon and
Language. Also an information box with information about the status of the
connection is displayed (see Figure 3.31).
The program is password protected. The program has to be started in the
highest level of access in order to be able to change the password settings
and to add the users with the required level of access to the program.
Press Esc to begin. A Password entry form is displayed (see Figure 3.8).
Enter Administrator for the user name and Administrator (look for the
exact match) for the password to access all levels of the program. (The
password settings have to be changed later by a level 3-user in the
Password Settings option, see chapter 3.3.4.10).
The program can be closed by selecting the close box in the upper right
corner or by selecting the Exit button. A message will be displayed whether
you really want to leave the program or not.
Figure 3.8
Note: When an analysis file is still open the Exit button shows Analysis.
Click the button to display the Analysis window. Close the Analysis
window by clicking the Exit button. The main window will then be
displayed with the Exit button.
The main menus of the main window are explained in the following
chapters. In the explanation full access to the program is assumed.
The program is used by different types of combustion analysers. See
chapter 3.3.4.1 to change the analyser type if the type was set on another
type than PrimacsSC. Changing the type also leads to changes in the layout
of the Options window and the info box.
Note: Once the analyser has been set online, the analyser type and
settings are automatically set on PrimacsSC.
3.3.3 The Information menu

The Information menu displays the following option: About (see Figure
3.9).
Figure 3.9 The information and general tool menu
3.3.3.1 About
Select about and the following information window appears:
Version PC Software:
Number of the used
software version. If you
have any questions about
the software be sure to
quote the version number
given in this menu.
Version firmware:
Version of the used
firmware in the
instrument. This
information is only visible
when the instrument is set
on-line. If you have any
questions about the
firmware be sure to quote
the version number given
in this menu.
Figure 3.10
3.3.4 The Settings menu

The Settings menu displays the following
options: Alarm Settings, Analyser type,
Miscellaneous settings, Analyser
settings, Detection, Curve order, Stand-
by, Options, Balance Settings,
Password Settings, Default Calibration
Curves, Print Layout, Export layout and
Print Setup (see Figure 3.11).
3.3.4.1 Analyser type
Select Analyser type and the Options
window is opened with seven tabs:
Analyser Settings, Detection Settings,
Alarm Settings, Curve order, Analyser
Type, Miscellaneous and Stand-by (see
Figure 3.12). The tab Analyser type is
always displayed in front. All tabs in this
screen (except Miscellaneous) are also
available from the Settings menu.
The analyzer type is PrimacsSLC. The Figure 3.11
analysis type is inaccessible as only carbon
can be measured with the PrimacsMCS. Click Apply to save the settings.
Click OK to accept the settings and to close the screen.
Figure 3.12 Analyser type

3.3.4.2 Analyser Settings

Select Analyser Settings from the menu or select the tab in the Options
window.
The screen is displayed with two tabs: General and PrimacsSLC.
The General tab (see Figure 3.13) displays several general options that
count for all analysers controlled by the program.
Figure 3.13 General Analyser Settings

1. The IR range. The range has to be set on high for the PrimacsMCS.
(This must also be done in the template for each separate sample).
2. The Automatic start option cannot be used for the PrimacsMCS as the
oven is not regulated by the software.
The buttons on the lower part of the screen are also available when the
PrimacsSLC tab is displayed.
Send Settings to Analyser: Sends changes in the settings to the
analyser (to be done each time a setting is
changed). The settings are not saved after
closing the program, unless they are saved
under Save Settings.
Reset all: Puts the IR detector to zero, starts the
Peltier cooler and sends settings.
Restore Defaults: Resets the factory set Default settings.
Save Settings: Saves the settings in the application
database.
The PrimacsSLC tab displays the specific settings for the PrimacsSLC
(see Figure 3.14).
Figure 3.14 Specific Analyser Settings

Default Integration time: The time the peak is integrated
Default Sample Time TC: The time the sample stays in the TC
oven.
Default Sample Time IC: The time the sample stays in the IC
oven.
Default Conc. St.TC: Depending on the used standard. It is
the percentage C in the standard. For
e.g. Oxalic acid this is 19.04%.
Default Conc. St.IC: Depending on the used standard. It is
the percentage C in the used standard.
For e.g. Calcium carbonate this is
11.99%.
TC temp: Is not used for the PrimacsMCS, but is
the set TC temperature of the
FormacsHT (= standby temp or the
required TC temp for later analysis).
IC temp: Is not used for the PrimacsMCS.
TC sampling time: Is not used for the PrimacsMCS.
IC sampling time: Is not used for the PrimacsMCS.
Acid to Cup: Is not used for the PrimacsMCS.
3.3.4.3 Detection Settings

Select Detection Settings from the menu or select the tab in the Options
window.
The screen is displayed with one tab (see Figure 3.15).
The default settings are displayed.
Figure 3.15 Detection Settings
Delta Up: 300 Digital units

Delta down: 50 Digital units
Delta detected: 4/3 Seconds
If during Delta Detected (4 sec.) the signal was always increasing and the
difference between the first and the last value is larger than Delta Up
(300), the start of the peak is detected.
If during Delta Detected (3 sec.) the signal was always decreasing and the
difference between the first and the last value is smaller than Delta Down
(50), the end of the peak is detected.
Choose whether you want to use Auto zero or not (activated in the Show
Graph window before the analysis. See chapter 3.3.8.1). Auto zero sets
the baseline at 10000 digital units before the analysis, when activated.
3.3.4.4 Alarm Settings

Select Alarm Settings from the menu or select the tab in the Options
window.
The Alarm Settings screen is displayed with two tabs: General and
PrimacsSLC.
The General tab (see Figure 3.16) displays several possible actions that
count for all analysers controlled by the program.
A Restore Defaults button is visible in both tabs to restore the default
settings after a change by the operator.
Figure 3.16 General Alarm Settings

Message The following message is displayed when the analyser
exceeds the pre-set limits of the FormacsSLC tab:
Values are out of alarm limits. The message is
repeated every 15 seconds, when OK is clicked, until
the analysis is ready. When the setting is changed into
the Continue option, the message is stopped.
Continue: No action is taken when the analyser exceeds the pre-
set limits. This option is selected by default.
Shutdown: When the values are out of the alarm limits the
analysis stops and the following message is displayed:
Values are out of alarm limits. Analyser will be shut
down. Click OK to exit the analysis. You are returned
to the main window.
Interruption: When the values are out of the alarm limits, the
analysis stops and the following message is displayed:
Values are out of the alarm limits, Continue? Select
Yes to continue the analysis. (In this case it is best to
change the setting into Continue, other wise the
software will ask the same question every 30 seconds).
When No is clicked you are returned to the main
window.
SLC
The Primacs tab (see Figure 3.19) displays the limits for the Alarm
Settings for the flow, the temperature of the TC oven and the temperature
of the Peltier cooler.
Figure 3.17 Alarm Settings

TC Temp: Temp is the temp for the FormacsHT. To prevent an
alarm, insert a temperature lower than the temperature
set in the Analyzer Settings. The upper limit should be
the same as in the HTAccess software.
IC Temp: Is not used for the PrimacsMCS. To prevent an alarm,
insert 0C for the lower temperature limit.
Peltier Temp: The default settings for the lower and upper limit of the
Peltier cooler temperature are respectively: 1C and
7C.
3.3.4.5 Curve Order

Select Curve order from the menu or select the tab in the Options window
(see Figure 3.18).
Figure 3.18 Curve order

Select the calculation order for the calibration curve. This depends on the
used IR detector and the used range. Default is 1st order.
3.3.4.6 Stand-By
Select Stand-by from the menu or select the tab in the Options window
(see Figure 3.19).
This tab is not relevant for the PrimacsMCS.
Figure 3.19 Stand-by
3.3.4.7 Miscellaneous
Select Miscellaneous from the Settings menu or select the tab in the
Options window.
The Miscellaneous screen (see Figure 3.20) displays some extended
settings about the detection. Only some of these settings are relevant for
the PrimacsMCS.
The option Dont send commands to analyser during analysis is not
checked. This should not be changed.
Before the start of the analysis the choice can be made to use raw data
or filtered data for the calculation. For filtered data a selectable filter
constant is available (0-7).
The detector range is selectable for the PrimacsMCS but not as dual
detector. The detector can be set on a certain range for an analysis (low
or high). However, for each separate sample position in the template
the range can be changed.
Figure 3.20 Miscellaneous

For display of the calculated results that are negative three options are
available: The text ZERO, the display of 0.00 and display of negative
results.
Linearize IR Raw Signal: This is not relevant for the IR detector type
that is used in the PrimacsMCS.
The constants and the Restore Default Constants option are not
relevant for the PrimacsMCS.
Use special TOC calculation is not relevant for the PrimacsMCS and is
not selectable.
The units for the PrimacsMCS can be set on %, mg/kg or g/kg, mg/l and
ppm.
The graphic Y Offset is set by default on 10000 units; this can be
changed.
The settings for the delay after changing the IR range, the maximum
concentration for the low range and minimal concentration for the high
range are not relevant for the PrimacsMCS as the sample cannot
automatically be re-analysed in the other range during a run.
3.3.4.8 Options
Select Options from the Settings menu to open the same window as the
previous ones. The window is displayed with the tab in front that was open
when the Options window was closed the last time. When the window is
opened the first time after starting up the program, always the tab Analyser
type is displayed in front.
3.3.4.9 Balance settings

This option is only available for a user with the highest level of access to
the program.
Select Balance settings from the menu; the following screen is displayed
(see Figure 3.21). In this window the properties of the balance that is
connected to the system are defined.
Figure 3.21 Balance settings

1. Select the used type of balance. The balance parameters for the
Mettler-Toledo and the Sartorius are already entered. If another type of
balance is used, enter the required parameters.
2. Check the Comport parameters of the balance and change if required.
Click Init ComPort to set these parameters.
3. If required, the settings can be checked. Weigh an amount on the
balance and click on Test get Weight. The weight should be displayed
in the field.
4. Click Apply to accept the settings.
5. Use the Close box in the right upper corner to close the screen.
3.3.4.10 Password Settings

This option is only available for users with the highest level of access to the
program.
Select Password settings from the menu; the following screen is
displayed (see Figure 3.22).
Figure 3.22 Password settings

In this screen the different levels of access to the program can be defined
as desired by the user(s).
In the screen the highest level is set by default with Administrator as user
name. Replace the password by your own password and add new users
with their level of access to the list. (Administrator as user cannot be
deleted).
Note: Remember that only level 3 users can change any settings in this
screen.
A level 1 user is not able to
change any settings except
Analyser settings and cannot
access the Control Panel, the
Log and the Method menu.
A level 2 user cannot access
the Miscellaneous and
Password Settings and the
Log.
A level 3 user has full access
to the system.
To change the password settings
of the administrator: Figure 3.23 Set Password
1. Click Set Password. The
following box is displayed (see Figure 3.23):
2. Enter the old password (Administrator).
3. Enter a new password.
4. Confirm the new password.
5. Click OK. A message is displayed that the password has changed.
6. Click OK to close the message.
To define a new user:

1. Click Add. A new line is added to the list.
2. Click in the field for the user name and type a name for the user.
3. Click in the field for the password (or use Tab) and type a level for the
user.
4. Click Set Password. The box as Figure 3.23 is displayed with the old
password entry box grayed out.
5. Enter a new password.
6. Confirm the new password.
7. Click OK. A message is displayed that the password has changed.
8. Click OK to close the message.
To delete a user:
1. Click in a field of the user to be deleted.
2. Click Delete. The line is deleted.
3. Click OK to close the screen.
3.3.4.11 Default Calibration curves
Select Default Calibration curves and the following screen is displayed
(see Figure 3.24). By selecting the TC or IC button the default calibration
curve(s) for the selected parameter will be shown.
Figure 3.24 Calibration curves
Each analysis needs a calibration curve to calculate the results. The

software will check to see if there is more then one standard in the
template, if so it will perform a calibration according to the standards used.
All samples will then be calculated using this calibration curve. When the
program finds no standards or only one standard in the template the
software will check the list of default calibration curves in the Default
Calibration Curves window and use the most appropriate one. (If no curves
are available, add curves by the option Add Curve, see later in this
chapter). Curves can be added or removed from the list and selected or de-
selected. Make a selection of curves you wish to use (only selected curves
will be used). When you start the analysis the list of default (selected)
curves will be copied to the analysis file. Even during the analysis itself it is
possible to modify the list. The program will automatically select the most
appropriate curve. A curve to be used for calculating results must be of the
same type as the sample (TC, IC). Then the program will select the best
curve by looking at a number of parameters.
1. Range selection Low-High

2. It will take the curve(s)with the smallest maximum area in which the
sample fits (high priority).
3. It will take the curve with the best correlation (lower priority).
If the program cannot find such a curve, it will keep trying, dropping
parameters one by one (lowest priority first) until it finds a curve.
Here follows an explanation of the items in the headings.
Selected: A checkmark denotes that the curve is selected to be
possibly included in the calculation of the results. Click to
select or de-select.
Type: The type of analysis performed for calibration.
Curve No.: The curve is automatically given the next available number
(this number is also displayed in the final results screen).
File name: The name of the analysis file the calibration curve came
from.
Date Time: The date and the time the curve was created.
Max. Area: The area of the highest standard used in the calibration
curve.
Max. Cont.: The highest weight of a standard in the calibration curve.
Order: Order of the calibration curve.
R-squared: The second order correlation between the scattered points
and the calibration line.
Correlation: The first order correlation between the scattered points in the
calibration window.
Range: Only high for the PrimacsMCS.
At the bottom of the box are the following selection buttons:
Show graph
Add curve
Remove curve
Exit
Exit
Select this button to close this window.
Show graph
Select this item to view the calibration graph of the selected calibration
curve; an example is shown in Figure 3.25.
At the right side of the graph in the Calibration curves window information
about the calculation of the calibration curve, the concentrations and
measured values are displayed. The values used for the calibration are
checked; the ignored concentrations are not checked. It is not possible to
change this in this window.
Move the mouse anywhere on the graph and the mouse changes into a
cross hair; the concentration and the measured value of the position where
the cross hair is situated will appear in the upper right corner when the
mouse is clicked. The blue (selected) values are used in the calibration; the
red (deselected) values are ignored.
Figure 3.25 Calibration curve

The Confidence intervals and the Detection and Determination limit can be
displayed for 95 or 99% in the curve, if the option is checked. With the
arrow buttons one can be switch to the next or previous calibration curve in
the Default Calibration Curves window. The curve can be printed.
To print the curve:
1. Click the Print button. The Print setup dialog box is displayed (see
chapter 3.3.7.1).
2. Change the settings if required. Click OK to accept the settings. The
curve is printed.
Add curve
Select this item and the window in Figure 3.26 appears with a list of data
files.
Figure 3.26 Data file list

To add a curve to the Default Calibration curves list:

1. Select the file from which you wish to add a calibration curve.
2. Press the Open button or double click on the file name. The Add
Curve window will be displayed with the calibration curves present in
the selected file (see Figure 3.27), which is dependent on the
measured parameters.
Figure 3.27 The Add Curve window
3. Select the curve you wish to add to the Default Calibration curves list.
4. Select the Add to Default Curves button. The curve is added to the
list in the Default Calibration Curves window (see Figure 3.28).
Remove curve
To remove a curve from the Default Calibration curves list select the curve
you wish to remove and press the Remove curve button. A warning box
appears (see Figure 3.28), if the selection is correct press Yes. The curve
is only removed from the Default curves list.
Figure 3.28 The Remove curve window

Print Layout
Select Print Layout: the following window is displayed (see Figure 3.29).
Figure 3.29 Print Layout

In this window the layout for the printed report is set. Click to select the
items to be printed in the report. The report is printed from the Analysis
window (see chapter 3.3.8.1).
General info (cannot be deselected)
In general this info is the information as displayed in the Analysis window.
Analysis name = The name given to the analysis. Cannot be
deselected.
Template name = The name of the used template. Cannot be
deselected.
Operator = Operator name.
Date/time = The date and time the analysis was started.
Cannot be deselected.
Start Oven Temp = The oven temperature at the start of the
analysis (not for PrimacsMCS).
Start Cooler Temp = The Peltier temperature at the start of the
analysis (not for PrimacsMCS).
Version = The software version used for the analysis.
Info = The info displayed text box for the Analysis
info in the Analysis window.
Method = The name of the method used for the
analysis (not relevant for PrimacsMCS)
Template info
In general this info is the information about the elements as displayed in the
Template and Analysis, Results window.
If Template Info is deselected, no information about the template will be

displayed in the report.
Element = The measured element with the information
about the sampling performance of the
element.
Integration time = The minimum integration time of the peak
area in seconds.
Samples = The number of times each sample is
analyzed (not for PrimacsMCS)
Extra Samples = The number of extra Samples, when the CV
is not obtained (only for FormacsHT).
Max. CV = The maximum value allowed for the
coefficient of variation between samples
from the same position(not for PrimacsMCS).
Sample time = The time period between sample
measurements.
Wash time = The time the tubing is rinsed (grayed out,
only for FormacsLT).
Start Ignore time = The time period the program waits until data
is collected (grayed out, only for FormacsLT).
Sample Values
These items show the information about each sample as set in the
Template window. Information about the samples is only displayed when
Sample Values is selected.
Injection order = Sequence number for the measurement of
the samples.
Position = Position of the sample in the sample table.
Type = Sample type (Standard, Unknown or Quality
sample).
Identification = Identification code for the sample.
Dilution factor = The number of times the sample was diluted
before analysis (final result will be
multiplied)(grayed out, not for PrimacsMCS).
Range = High or low measuring range.
Result TOC = Calculated result of TOC.
Result TC = Average result TC analysis.
Result IC = Average result IC analysis.
Result TKN = Calculated result TKN (grayed out, only for
FormacsTN).
Result TN = Average result TN analysis (grayed out, only
for FormacsTN).
Result NN = Average result NN analysis (grayed out,
only for FormacsTN).
Result POC = Calculated Result POC (grayed out, not for
PrimacsMCS).
Result NPOC = Average result NPOC analysis. (grayed out,
not for PrimacsMCS)
Average area = The average of the raw values of the
Samples (not for PrimacsMCS).
CV = Calculated variation of the raw values
(grayed out, not for PrimacsMCS).
Sample weight = Weight of the measured sample.

Concentration = The result of a measurement.
Area = The raw value of a measurement.
Link to curve = The number of the calibration curve used for
the calculation of a result.
Oven Temp = Temperature of the TC oven during the
measurement (not for PrimacsMCS.
Cooler Temp = Temperature of the Peltier cooler during the
measurement.
Edited = Raw value is original or edited (shows -, E,
O, S, W, see for explanation page 3-26).
Selected = Value is selected for the calculation.
Calibration
When selected general information about the available calibration curves
(as displayed in Analysis, Results, Calibration Curves window) is
displayed in the report.
Type of Samples
Here the type of samples that you want to be displayed in the report can be
selected.
3.3.4.12 Export Layout
Select Export Layout and the next window is displayed (see Figure 3.30).
Figure 3.30 Export Layout

In this window only the identification and the results cannot be deselected.
3.3.4.13 Print setup
Select this option to display the Print setup dialog box (see Figure 3.40) in
chapter 3.3.7.1.
3.3.5 The View menu

The View menu displays the following options:
Control Panel, Info, Log and Live Signal
Monitor (see Figure 3.31).
3.3.5.1 Control Panel
Select Control Panel and the following window
is displayed (see Figure 3.32).
Figure 3.31
Figure 3.32 The Control Panel window
Warning 1: Do not use these commands during analysis.

For General the following commands can be executed:
Auto zero C: Sets baseline at 10000 digital units before the analysis for
C.
IR Range Low: Sets the detector on low range. Range 0.02-1 mg C (not
for PrimacsMCS).
IR Range High: Sets the detector on high range. Range 1-40 mg C
absolute.
Standby On/Off: Sets the Analyser in Standby or operational mode (not for
PrimacsMCS).
No.: Number of cycle counts.
The next three items are for Skalar Service engineers only.
Cycle Once: Initiates one cycle count.
Cycle Start: Starts the cycle count.
Cycle Stop: Stops the cycle count.
For PrimacsSLC the commands cannot be executed for the PrimacsMCS.
3.3.5.2 Info
The Info window (see Figure 3.33) is
opened by default in the upper left
corner when the program is started.
The window displays information about
the performance of the analyser.
The following parameters are
displayed:
IR Raw Signal: Direct value from IR
detector
IR Signal: Filtered value (7-
points mean value) Figure 3.33 Info
TC Temp: Temperature of the
TC oven (not available for PrimacsMCS
IC Temp: Temperature of the IC oven (not available for
PrimacsMCS
Peltier Temp: Temperature of the Peltier Cooler
Write Pointer: Displays information about the communication. The
Write Pointer should always be 1 higher than the Read
Pointer, when the communication runs properly.
Read Pointer: Displays information about the communication. The
Read Pointer should always be 1 lower than the Write
Pointer, when the communication runs properly.
To close the Info window click the close box in the upper right corner or
select the View menu. The option Info shows a checkmark. Select Info.
The option is unchecked and the window disappears from the screen. To
display the window again, select Info from the View menu. Info is
displayed and gets a checkmark.
3.3.5.3 Log
The Log window is not visible by default. It is only intended for service
purposes.
3.3.5.4 Live Signal Monitor
The Live Signal Monitor window is intended for
service purposes.
3.3.6 The Connection menu
The connection menu displays the following
options: Auto Connect, Disconnect and
Connect (see Figure 3.34).
Figure 3.34
Click Auto Connect to connect the
PrimacsMCS to the computer. Auto Connect searches for the COM
port to provide the communication with the analyser. The display will
show Searching. Once the COM port is located the display shows
Online.
Click Disconnect to disconnect the software to the PrimacsMCS.
Select Connect if the PrimacsMCS is connected to another COM port.
Click Connect. A dialog box is opened where the COM port can be
selected for the connection with the PrimacsMCS. Select the required COM
port and click OK.
3.3.7 The Template menu

The template is used to set the performance of an
analysis. A template can be used for different analyses,
when the same sampling performance is required.
Templates can consist of only standards, only unknowns
or standards, QCs and unknowns. Each analysis needs
a template to set the sampling volume and the other
sampling settings as sampling time, integration time, the
Figure 3.35
number of samples and the number of extra samples.
The template can be edited during the analysis as long as the analyser has
not yet reached the position that is edited. The Template menu displays
the following options: New and Edit.
3.3.7.1 New
Select New and the following dialog box (see Figure 3.36) is displayed:
Figure 3.36 Save Template as

Give the template you will prepare a name in the box for Filename. Select
Save to save the name. The file is saved by default in the Template
subfolder.
Saving the file closes the dialog box and opens a Template window with the
file name just saved. The window has two main menus: File and View (see
Figure 3.37).
In this window all relevant information for the performance of the analysis
run is entered.
Figure 3.37 The Template window

The File menu has seven options: New, Open, Save as, Close, Save on
Exit, Print, Print Setup and Exit.
New has the same function as the New command from the Template
menu and displays the Save as dialog box as shown in Figure 3.36.
Type a name in the file name box for the new template and select Save.
A new template is displayed with the given name.
Open has the same function as the Edit command from the Template
menu and displays the Open dialog box (see Figure 3.38). Select the
required template and select Open. The selected template is displayed.
Figure 3.38 Edit template

Save as opens the Save as dialog box as shown in Figure 3.36. Type
a new name in the file name box for the template and select Save. The
current template will be closed. The template is displayed with the new
name.
Close closes the selected template, but leaves the template window
open.
Save on Exit (checked by default) saves any changes made in the
template when the window is closed by means of the OK button.
Figure 3.39 Print window

Print displays the Print window with the template work list (see Figure
3.39).
To print the work list:
1. Select if required Print Setup to display the Print Setup dialog box
(see Figure 3.40) to set the print options.
Figure 3.40 Print setup

2. Select Properties to change the settings to your demands and then
select OK. Again select OK to close the dialog box.
3. Select the Print button in the Print window. The work list is printed.
4. Select the Exit button to close the Print window.
Print Setup displays the Print Setup dialog box (see Figure 3.40) to
set the print options.
1. Select OK to accept the default settings or select Properties.
Change the settings to your demands and select OK. Select OK to
close the dialog box.
2. Select the Print button in the window to open the Print window to
print the work list.
Exit closes the template window.
The Edit menu has three options: Add Position, Del Position and
Renumber.
Add Position is used to add a new sample to the template. Usually the
last position is selected, when a new position is entered. Only when a
sample line has to be inserted, select the sample position above the
position where the sample is to be inserted. Renumber the positions
after finishing the template. This option has the same function as the
button in the window.
Del position is used to delete a sample line from the template. Select
the position to be deleted from the template. This option has the same
function as the button in the window.
Renumber is used to renumber the positions in the template when a
sample has been inserted. This option has the same function as the
button in the window.
The View menu has one option: Refresh.
Refresh. When this option is clicked, the curser position returns to the
first position in the template and the first five positions of the template
are displayed.
Items in the template window (see Figure 3.41):
Position: The position of the sample in the sample tray. (The
injection order is set by the sequence in the template).
Type: Standard or sample code. The following types are
available: Standard, Unknown and Quality sample.
Identification: Identification code for standards, samples and quality
samples.
Range: Selection between high/low range (for PrimacsMCS only
high).
Injections: The parameter to be measured. If TOC is selected
automatically TC and IC are selected too.
Sample weight: The sample weight in mg. If TOC is measured the
weight for TC as well as IC has to be filled in.
Element: The parameter for which the sampling information is
set.
Integration Time: The time starting from the injection till the end of the
peak. The software looks for the end of the peak. If the
peak is very wide and flat the integration time possibly
has to be longer as the program might consider the flat
top as the end of the peak. The default time is 60 sec.
Recommended time for PrimacsMCS is 120 sec.
Sample time TC: Here the sample time as set in the Analyser Settings
window for TC is set. The sample time is the time
between two displays of the pop-up window with the
message to insert a sample.
Sample time TC: Here the sample time as set in the Analyser Settings
window for TC is set. The sample time is the time
between two displays of the pop-up window with the
message to insert a sample.
Stand. conc. TC The concentration of C in the TC standard (by default
the concentrations from the Analyser settings window
are filled in).
Stand. conc. IC The concentration of C in the IC standard (by default
the concentrations from the Analyser settings window
are filled in).
The figure displays the default settings.
No. of Positions: The total number of positions entered in the template.
Add Pos: Adds a new position under the selected position.
Automatically the next position number is added.
Del Pos: Deletes the selected position.
Get Weight TC: Inserts the weight of the sample on the connected
balance directly in the field of the TC sample weight.
Get Weight IC: Inserts the weight of the sample on the connected
balance directly in the field of the IC sample weight.
Renumber: Renumbers the positions starting from 1 if editing has
led to an incorrect position range.
Print: Displays the template as it will be printed in the Print
window (see Figure 3.39).
Cancel: Closes the template without saving any changes.
OK: Closes the template window (and saves any changes
in the template, when Save on Exit is checked).
Procedure to create a template:
Note: If only samples are entered skip step 1 - 6.
1. Select Add Pos. A position is entered in the template with the type
Unknown.
2. For the standard curve the type has to be changed to Standard.
3. Enter the identification for the standard and the required measuring
range.
4. For Injection enter the required parameter (TC or IC) to be measured.
5. Weigh a suitable amount of standard on the connected balance (for TC
samples in the low range enter a weight of 100 and weigh the samples
just before analysis in a pre-heated crucible, see also chapter 3.2.4).
6. Enter the weight for the selected parameter by means of the Get
weight TC or the Get Weight IC button or type the weight in the
sample weight box.
7. Repeat step 1 to 6 for each standard in the template.
8. When all Standards are entered select the Add Pos button. A new
position is added to the list with the type Unknown.
9. If desired change the type to Quality sample.
10. Enter the identification for the sample.
11. For Injection enter the required parameter(s) to be measured.
12. Weigh a suitable amount of sample on the connected balance (for a
TC measurement in a quartz crucible and for an IC measurement in a
glass tube).Enter the weight for the selected sample by means of the
Get Weight TC or Get Weight IC button.In the case of a TOC
measurement weigh two amounts of the same sample (one for TC and
one for IC) and enter the weight by means of the respective Get
Weight button.
Figure 3.41 A created Template

13. Select Add Pos for each sample to be entered. By default the settings
of the previous position are entered.
14. Repeat step 9 14 until the last sample is entered.
15. Check that your work list is numbered properly. This is easy to do by
selecting the Print button. The work list is displayed. Renumber the
work list if necessary.
16. Check if the settings for integration time and concentration of the TC
and IC standard are OK. If not: make the required changes.
17. If everything is set according to your wishes, select Exit. The template
window closes and you are returned to the main window.
3.3.7.2 Edit
Select Edit and the following window is displayed (Figure 3.42):
Figure 3.42 Edit template

1. Select the Template you wish to edit and select Open. The template is
opened.
2. If required save the template under a new name. The template will be
displayed with its new name.
3. Edit the template according to your wishes.
4. If everything is set according to your wishes, select Exit. The template
window closes and you are returned to the main window.
3.3.8 The Analysis Menu

Once one or more templates are saved, it is not
necessary to make a new template for every analysis,
if the same kind of calibration is used. An existing
template can be used. The analysis to be performed
gets a name, a template is attached to the analysis
and the weights of the samples can be adapted in the
Results window. Make sure that the samples for at
least the first three positions are weighed before the
analysis is started. Figure 3.43
The Analysis menu shows the following options: New,
Edit, Restore and Version (see Figure 3.43).
3.3.8.1 New
Select New and the following window is displayed (Figure 3.44):
Figure 3.44 New Analysis

1. Type a file name for the analysis. By default the data are stored in the
Analysis subdirectory as a database file. If the name is already in use a
warning box appears to confirm or use another name. A date will
automatically be given.
Figure 3.45 Attach template

2. Press Save and the Template: Open window is displayed. The

Template Open window (Figure 3.45) shows the available templates.
3. Select a template to attach to your analysis.
4. When a template is selected, press Open or double click on the
selection and the Analysis window is displayed (Figure 3.46):
Figure 3.46 Analysis window

The window shows the name given to the analysis, the name of the method
to be used (if applicable), the name of the attached template, the date and
time this screen was created, whether Re-analysis will be performed (not
possible for PrimacsMCS) and the state of the analyser.
If required a method can be used for the analysis. This method contains
special settings (different from the settings in Analyser Settings) for the
temperature of the ovens and/or the sample time. For creation of a method
see chapter 3.3.9.
The method is not a relevant option for the PrimacsMCS as the oven
temperatures are software controlled and the sample is manually
introduced.
To use a method:
1. Click Load. A dialog box is displayed with the created method(s).
2. Selected the required method and click Open. The selected method is
displayed in the field for the method name.
3. Check the Use Method option (if not checked the method will not be
used).
The state of the analyser is Monitoring before the analysis is started,
Analyzing during analysis, Done when the run is finished and Editing
when a finished analysis is opened.
As soon as the analysis has started the date and time the analysis has
started and the temperature of the oven and Peltier cooler at the start of the
analysis are displayed. Special information about the analysis can be typed
in the Analysis info field.
The option Go to Stand-by after Analysis can be checked (to put the
analyser in the Stand-by mode with the corresponding settings).
Nine selection buttons are visible: Start Analysis, Pause Analysis,
Results, Graph Peaks, Print Results, Export Results, QC chart,
Sample Report and Exit. Pause Analysis is only selectable after the start
of an analysis (but is irrelevant for the PrimacsMCS), while QC chart and
Sample Report are only selectable after the analysis.
Current Sample Time, Injection order, Position and Injection display
information about the analysis during the Analyzing state.
Before an analysis is started the baseline can be checked in the Peaks
window. If necessary select Auto zero in this window to adjust the baseline
(available when Use Auto zero is selected in the Detection Settings
screen). In the Results window the template is displayed (see Figure
3.48).
Start Analysis
To start the analysis:
1. Select the Start Analysis button. The Status panel is displayed. This
panel checks if the state of the parameters is according the settings as
set in the Alarm Settings.
Note: The TC Temp in this panel is the TC temp of the FormacsHT. The TC
temperature of the PrimacsMCS is displayed on the instrument.
2. If the settings are OK (not relevant for the IC temp, see Figure 3.47)
press Continue to start the analysis or Cancel to return to the
Analysis window.
3. The text on the button turns gray and the state changes to Analyzing.
The date and the time the analysis was started will be displayed.
Figure 3.47
Another button is available when temperature of the Peltier is also outside

the limits: Wait and a field for the waiting time. Enter a waiting time and
click Wait. If this button is pressed the analysis waits until the waiting time
has passed and then automatically starts the analysis.
Results
Select Results to open the Results window (see Figure 3.48).
Figure 3.48 Results screen before analysis

The template list and the sampling information as set in the template are
displayed on the left side of the window. The right side of the window
shows the fields where the raw values and the calculated concentration of
the highlighted sample for the selected parameter will be placed.
Samples can be added, deleted or edited in the displayed template. This
can be done before, during or after the analysis.
To insert a sample in the template:
1. Select the position after which a sample has to be inserted.
2. Click the right mouse button in the template and select Insert from the
displayed menu. A dialog box is displayed (see Figure 3.49).
3. Here the new sample can be defined. When a sample is inserted after
an unknown, by default the identification and the parameters of the
selected sample position are visible.
4. Insert the identification, type, range, the parameter(s) to be measured
and the weight(s).
5. Click OK to insert the sample and to close the dialog box.
Figure 3.49 Inserting a sample

To edit a sample in the template:

1. Select the position that is to be edited.
2. Click the right mouse button in the template. A menu with three
options: Insert, Delete and Edit is displayed.
3. Select Edit. A dialog box is displayed (see Figure 3.50).
Figure 3.50 Edit sample

4. Edit the sample as required.
5. When changing the type into a standard the content of the parameter
has to be entered and also the curve number where the standard is to
be used.
6. Select OK to accept the changes. The dialog box is closed.
Note:The dialog box is also used to enter the weight of TC samples in the
low range.
To delete a sample from the template:
1. Select the sample to be deleted from the template.
2. Click the right mouse button in the template and select Delete from the
displayed menu. A dialog box is displayed whether you are sure to
delete the sample.
3. Click Yes to confirm the deletion.
The window shows four selection buttons: Calibration Curves, Calculate
Results, Peaks and Exit.
Selecting Calibration Curves displays the Calibration Curves window,
where curves can be added or deleted and selected or deselected for the
calculation of the samples (see chapter 3.3.4.1)
Selecting Calculate Results calculates the results with the most
appropriate curve of the curves selected in the Calibration window. The
used curve no. is displayed.
Selecting Peaks displays the Peaks window.
Selecting Exit closes the Results window.
After the measurement of a sample a information box is displayed in front
of the displayed window (see Figure 3.51).
Figure 3.51
TC port will be IC port if the next sample in the template is an IC sample.

Remove the measured sample from the port and place a new sample. The
measurement is started when OK is clicked.
During the analysis the fields are being filled with information about the
measurements (see Figure 3.52). The sample being measured is
highlighted.
Figure 3.52 Results window
Make sure to have a calibration curve available for the measured range
otherwise the results in the measured range cannot be calculated.
The Selection checkbox displays whether the result is used for calculation
or not.
D If the dilution factor was changed after the injection of the
sample.
S For changes of the (de)selection of the individual sample. This
is the case if the software originally selected the sample, but the
user deselected it afterwards and re-selected it afterwards.
E For changes in start or end point of the integration of the peak.
O For peaks that were edited, but where the original peak was
selected for the calculation.
- If no editing was performed on the peak.
When all samples of the template are measured also a message is
displayed (see Figure 3.53).
Figure 3.53
Graph peaks
Select Graph peaks from the Analysis window or Peaks from the
Results window to open the Peaks window (see Figure 3.54) to view the
peaks either during the analysis run or after the analysis is finished.
Figure 3.54 Peaks window

The window has seven selection buttons and two check boxes.
The Auto Zero button is used to set the baseline at 10000 digital units and
is only available before the analysis.
The Results button is used to switch to the Results window.
The Analysis button is used to switch to the Analysis window.
The Print button is used to print the displayed peaks.
The Exit button is used to return to the previous screen.
The Use Original Peak and Use Edited Peak buttons are used when a
peak is edited to select whether the original or the edited peak is used for
the calculation.
Automatic scrolling is checked by default. This means that the screen
follows the analysis and displays the last measured peak. It can be
unchecked to scroll by hand to view previous measured peaks. As soon as
the option is checked again, the view returns to the last peak.
Show theoretical peak is not relevant for the PrimacsMCS.
The window has five zoom buttons.
Zoom in Y. Each time the button is clicked the peaks are zoomed in
vertically.
Zoom out Y. Each time the button is clicked the peaks are zoomed out
vertically.
Zoom in X. Each time the button is clicked the peaks are zoomed in
horizontally.
Zoom out X. Each time the button is clicked the peaks are zoomed out
horizontally.
Default setting. Click this button to restore the default setting.
By default the peaks are displayed 100%.
For information on a particular peak, click in the peak. The information

about the peak is displayed in the box on the right.
The peaks can be edited after the analysis. The view shows the original as
well as the edited values in the box on the right (see Figure 3.55). Also
information is given whether the original peak or the edited peak is
displayed.
Figure 3.55 Edit peaks

To edit the beginning of a peak:
1. Double click on the left mouse button at the beginning of the peak, just
above the green marker.
2. Drag the mouse to the new starting point and release the mouse
button.
3. Select the Use edited peak button first and then the software will
calculate the area from this point to the end of the peak. The edited
peak is displayed.
To edit the end of a peak:
1. Double click on the left mouse button at the end of the peak, just above
the red marker.
2. Drag the mouse to the new end point and release the mouse button.
3. Select the Use edited peak button first and then the software will
calculate the area from this point to the beginning of the peak. The
edited peak is displayed.
Select the Use Original Peak button if the original peak is to be used for
calculation (and display) and the Use Edited Peak button if the edited peak
has to be used for calculation (and display). In the case that edited peaks
are used, recalculate the results in the Results window (in this case the
original box is not checked).
Print Results
Click the Print Results button in the Analysis window to display the Print:
Analysis window (see Figure 3.56).
Figure 3.56 Print results
The window displays the results of the analysis as set in the Print Layout
window.
Click the Print button to print the results (if desired first click Print setup to
set the print options).
Click the Exit button to return to the Analysis window.
Export Results
Click the Export Results button in the Analysis window to display the
Analysis: Export Results window (see Figure 3.57). The name of the
analysis is displayed.
Figure 3.57 Export Results

To export the analysis file:
Accept the name in the file box or type a new name for the analysis and
click Save. The file will be exported in text format with the information as
set in the Export layout window. This exported file can be opened in
Notepad or Wordpad (see Figure 3.58).
Figure 3.58 Exported file in text format

This exported file can be imported in an Excel file, if Excel is installed. If
Excel is not installed it is also possible to copy the file to another computer
(which must have the same operating system!) that has Excel installed and
then import in Excel.
To import the file in Excel:
1. Open a new Excel file.
2. Select Open from the File menu. A dialog box is displayed where the
directory can be selected where the file to be imported is saved.
3. Select for Files of Type: All Files to display the filename.
4. Select the filename and click Open. The Text Import Wizard will be
displayed.
5. Check if the correct format of the file is selected and click Next.
6. Select Comma as the delimiter and click Next.
7. Set the format for each column in the Excel file and click Finish. The
file will be displayed in the Excel file (see Figure 3.59). Save the file in
Excel format.
Figure 3.59 File imported in Excel

For working in Excel refer to your Excel manual.
QC chart
If QC samples are measured, the performance of these QC samples can
be viewed in the QC chart (see Figure 3.60).
Figure 3.60 QC chart
This screen displays if the values of the measured QC samples are within
the control limits of the given control value.
The screen has four selection buttons to easily switch to the Graph Peaks
window, the Analysis window, the Results window and the Sample
Report window.
Sample Report
The values of the samples and their performance are displayed in the
Sample report (see Figure 3.61).
Figure 3.61 Sample Report

3.3.8.2 Edit
Select Edit from the Analysis menu and the following window appears
(Figure 3.62):
Figure 3.62 Edit Analysis

Select the file to be edited from the list and click Open. The Analysis
window is opened. The only difference with a new analysis is that the Start
Analysis button is gray, so no analysis can be started.
3.3.8.3 Restore
Select Restore from the Analysis menu and the following window is
displayed (see Figure 3.63):
Figure 3.63 Restore original results

When a category is selected in this window, all edited peaks for that
category are restored to their original Raw data peaks in the Peaks
window. In the Results window the original values are restored and
flagged. The results will have to be recalculated.
To restore all peaks of an analysis category:
1. Select the category for which all peaks have to be restored.
2. Click Restore. A warning is displayed with the question if you want to
continue the operation. Click Yes to continue.
3. Go back to the Results window and notice that the values are flagged
as originals.
4. Click Calculate Results to recalculate the results with the original

values.
3.3.8.4 Version
Version is used to check with which version of the software the analysis
was done.
1. Select Version to open the Analysis: Check Version dialog box. All
performed runs are displayed.
2. Double click on an analysis name or select the analysis and click
Open.
3. An information screen displays with which software version the
analysis was done.
3.3.9 Method
The Method menu has two options: New and Edit. (see
Figure 3.64). This option is used to define a special
combination of settings for a certain group of samples or
a certain type of analysis.
3.3.9.1 New Figure 3.64
Select New and the following window is displayed: (see
Figure 3.65).
Figure 3.65 New Method
1. Double click on Method to open the Method subdirectory.

2. Type a name for the method. The method file gets automatically the
extension .mtd.
3. Click Save to save the name of the method.
4. Now the Method Settings window is displayed with its possible
settings (see Figure 3.66).
5. Here special settings for the temperatures of the ovens (not for
PrimacsMCS) and the sample time can be selected.
6. Click OK to save the settings and to close the window.
7. The method can now be loaded into the analysis file.
Figure 3.66 Method settings window
3.3.9.2 Edit
Select Edit and the Method settings window is opened (see Figure 3.67).
Figure 3.67 Edit Method

Now the settings of the method can be changed.
Click OK to save the changes and to close the window. The method can
now be used in an analysis.
3.3.10 Logon
The Logon menu has two options: Log On and Log Off. This menu is meant
to log on and log off the users with their different
levels of access to the program, when the program is
open.
A logon is required to start the program, but it may be
possible that a level 1 user started the program, while
some settings have to be changed. In this case the
Logon option is used to change the user and the Figure 3.68
access to the program without closing the program.
By using Log off all users are logged off and the Password entry form is
displayed to enter a new user.
By using Log On the Password entry form is displayed to enter a new
user.
3.3.11 Language
This menu has three options: English, German and
French and is used to select the required language.
When a language is changed by means of this menu,
the program has to be closed to set the proper
regional settings (see also chapter 3.3.1.3) to be able
to reach all functions of the program. The program
opens in the language as set in the regional settings of
the computer. Figure 3.69
3.3.12 Short operator software reference instructions.

Note: The decimal symbol of the TOC4Windows program must be a period
(.). This can be checked and/or changed in Control Panel, Regional
Settings on the Numbers tab.
1. Start the analyser according the instructions in chapter 3.2.2.
2. Create a Sampling Template: Open the Template menu and select
New. Give the template a name and select Save. Create the
template as indicated in chapter 3.3.7.1. Exit the template.
3. Name analysis: Open the Analysis menu and select New. Give the
analysis a name. Select Save and you will automatically go to the next
(= Select a template) window.
4. Select a Template: Select the Template you have just created or an
existing template. Exit the window with Open and you will
automatically go to the Analysis window.
5. Check baseline: Select Graph peaks and check if the base line is
good. Adjust if necessary with Autozero. Exit to return to the Analysis
window.
6. Start run: Select Start Analysis to start the analysis run.
7. Confirm analysis: Place the first sample in the port according the
message in the information box and click OK. The analysis starts. If
you didnt fill in the weight of your sample a window will appear to fill in
the weight of the sample (only when no balance is connected to the
analyser).
8. Follow progress: Select Graph peaks again to follow the progress of
the analysis. Exit and you will return to the Analysis window.
9. After the analysis has finished: Click OK in the displayed box to
confirm the end of the analysis. From the Analysis window select
Results. Press Calculate results; the results are then calculated.
Select Print results from the Analysis window and press Print to
print the results.
3.3.13 Extended software instructions to start an analysis

These instructions cover an analysis as an initial start up. Example
windows are shown on the right. Follow the instructions in the sequence
given. In the case of a routine start-up with an existing template, skip
instruction 2-3.
1. Start the analyser
Start up according the instructions in chapter 3.2.2.
2. Create a Sampling Template
Select the Template menu and select New. The Template: New dialog
box is opened. Type a name for the template (see Figure 3.70) and select
Save.
Figure 3.70
The template is saved by default in the Template directory. The Sampling
template as shown in Figure 3.71 is displayed. Select Add Pos. A position
is entered in the template with the type Unknown. For the standard curve
the type has to be changed to Standard. Enter the identification for the
standard. For Injection enter the required parameter (TC or IC) to be
measured. If a balance is connected, weigh the standard and press Get
weight TC (or IC, dependent on the type of standard). If no balance is
connected, type a weight for the standard to be measured. This may be the
intended weight. The real weight may be entered later in the Results
screen.
Figure 3.71
Follow this procedure for all standards and also for the samples
(unknowns). Check if the settings for integration time, sample time and
concentration of the TC and IC standard are OK. If not: make the required
changes. If everything is set according to your wishes, select Exit. The
template window closes and you are returned to the main window.
3. Name analysis
Select the Analysis menu and select New. Type a name for the analysis
in the Analysis: New dialog box Figure 3.72). Select Save. The dialog box
is closed and the Template Open dialog box is displayed.
Figure 3.72
4. Select a template
Select the template you just created or another existing template (see
Figure 3.73). Exit the dialog box by selecting Open. This will open the
Analysis window (see Figure 3.76). This window is described in chapter
3.3.8.1.
Figure 3.73
5. Check baseline
Select Graph peaks and check if the base line is good (see Figure 3.74); if
not there may be a hardware problem (see for solving Chapter 5
Troubleshooting). When the baseline is too high or too low, adjust with the
Auto Zero.
Figure 3.74
6. Start run
Select Start Analysis (see Figure 3.75) to start the analysis run. An
information box will be displayed.
Figure 3.75
7. Confirm analysis
Place a sample in the port (TC or IC) according to the first sample in the
template and click OK in the displayed box. The first sample will be
analysed.
8. Follow progress
Go back to Graph peaks where you can watch the peaks as they appear
or select Results and watch the Raw values appear.
9. After analysis has finished
Select Results from the Analysis window (see Figure 3.75). Select
Calculate results so that the results can be calculated. If necessary select
Calibration curves to calculate the results with another calibration curve.
Exit the window to return to the Analysis window. Select Print results. If
the displayed print layout (Figure 3.76) is according your wishes, press
Print.
Note: Do not print unless a printer is on-line, only print after an analysis.
Figure 3.76

Primacs Mcs Operat

Uploaded by

Document Information

Original Description:

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Primacs Mcs Operat

Uploaded by

Copyright:

Available Formats

PRIMACSMCS TOC

This chapter gives routine and detailed operating instructions.

3.1.4 Quality Control

3.2 Operating the hardware

3.2.2 Extended operating instructions

Figure 3.3 IC sampling Figure 3.4 Place IC oven

3.2.4.3 TOC sampling procedure

Figure 3.5 Windows 2000 Figure 3.6 Windows XP

For Windows XP:

3.3.2 The main window

Figure 3.7 Main window

3.3.3 The Information menu

Figure 3.9 The information and general tool menu

3.3.4 The Settings menu

Figure 3.12 Analyser type

3.3.4.2 Analyser Settings

Figure 3.13 General Analyser Settings

Figure 3.14 Specific Analyser Settings

3.3.4.3 Detection Settings

Figure 3.15 Detection Settings

Delta Up: 300 Digital units

3.3.4.4 Alarm Settings

Figure 3.16 General Alarm Settings

Figure 3.17 Alarm Settings

3.3.4.5 Curve Order

Figure 3.18 Curve order

Figure 3.19 Stand-by

Figure 3.20 Miscellaneous

3.3.4.9 Balance settings

Figure 3.21 Balance settings

3.3.4.10 Password Settings

Figure 3.22 Password settings

To define a new user:

Figure 3.24 Calibration curves

Each analysis needs a calibration curve to calculate the results. The

1. Range selection Low-High

Figure 3.25 Calibration curve

Figure 3.26 Data file list

To add a curve to the Default Calibration curves list:

Figure 3.27 The Add Curve window

Figure 3.28 The Remove curve window

Figure 3.29 Print Layout

If Template Info is deselected, no information about the template will be

Sample weight = Weight of the measured sample.

Figure 3.30 Export Layout

3.3.5 The View menu

Figure 3.32 The Control Panel window

Warning 1: Do not use these commands during analysis.

3.3.7 The Template menu

Figure 3.36 Save Template as

Figure 3.37 The Template window

Figure 3.38 Edit template

Figure 3.39 Print window

Figure 3.40 Print setup

Figure 3.41 A created Template

Figure 3.42 Edit template

3.3.8 The Analysis Menu

Figure 3.44 New Analysis

Figure 3.45 Attach template

2. Press Save and the Template: Open window is displayed. The

Figure 3.46 Analysis window

Another button is available when temperature of the Peltier is also outside

Figure 3.48 Results screen before analysis