OXITEST Operating Manual Velp
OXITEST Operating Manual Velp
www.velp.com
10003023/C7
OXITEST
Oxidation Test Reactor
Operating manual
Thank you for choosing the Oxidation Test Reactor.
OXITEST allows to investigate quickly the oxidative stability of foods and feed
containing lipids.
Safety instructions:
Before using the instrument please read carefully the operating manual
provided with the equipment.
In order to reduce possible risks of electric shocks, fire or personal injuries when the
instrument is used, the basic safety precautions must always be followed. These
include:
• Ensure that no liquids come into contact with the power cable or with the
electrical parts inside the unit.
• Check that the power cable is connected to a power point in accordance with
the information stated on the equipment registration plate.
• Only use power cables provided with three terminals, namely those with an
earth cable.
• Do not use the instrument if malfunctions have been detected. In this case,
contact the nearest technical assistance center.
• The personal protection devices, containers and products used in
manufacture must be compatible with the temperature set on the instrument.
• Follow the instructions for cleaning the instrument, as described in this
manual.
This instrument must be used only for laboratory applications
The manufacturer is not liable for use of the instruments that is not in accordance with
the instructions.
SAFETY REGULATIONS
1) The reactors may reach the temperature of 120°C. This occurs both during the test
and in the cooling period. Use the appropriate cover-locking key provided to open the
reactors. Use the knob of discharge valve to move the covers and the threaded key to
remove the sample-holder containers and the spacers from the reactors themselves at
the end of the test.
2) The containers and the products used in the various tests must be compatible with
the temperature reached by the instrument (approx. 120°C).
3) Always leave the transparent protective shield in place when the instrument is in
operation.
The instrument has been designed and built in accordance with the following
standards:
Safety stipulations for electrical equipment
for measuring and control and for use in a laboratory EN 61010-1/2001
Stipulations of electromagnetic compatibility EN 61326-1/2000
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CONTENTS
1. Introduction .................................................................................................. 4
1.1 Parts included .............................................................................................. 5
1.2 Instrument description .................................................................................. 5
1.3 Keys and functions....................................................................................... 8
2. Assembly and installation ............................................................................. 9
2.1 Pneumatic connection .................................................................................. 9
2.2 Mains power supply connection ................................................................... 9
2.3 PC Connection ........................................................................................... 10
2.4 Balance connection .................................................................................... 11
3. Use of the software .................................................................................... 12
3.1 Database and test conditions ..................................................................... 13
3.1.1 Laboratory information......................................................................... 13
3.1.2 Database ............................................................................................. 14
3.1.3 Test conditions .................................................................................... 16
3.1.4 Heating and pressurizing step ............................................................. 18
3.1.5 Test execution ..................................................................................... 20
3.2 Evaluating data .......................................................................................... 21
3.2.1 Configuring the data base ................................................................... 22
3.2.2 Filtering the database .......................................................................... 23
3.2.3 Working with several databases .......................................................... 24
3.2.4 Modifying the graph ............................................................................. 25
3.2.5 Creating some procedures with their archives ..................................... 26
3.2.6 Recalculating analysis ......................................................................... 26
3.2.7 Exporting data ..................................................................................... 27
3.3 Procedures ................................................................................................ 29
3.3.1 Repeatability test ................................................................................. 29
3.3.2 Freshness test ..................................................................................... 32
3.3.3 Formulas comparison .......................................................................... 35
3.3.4 Packaging comparison ........................................................................ 36
3.3.5 IP during ageing .................................................................................. 37
3.3.6 Estimated shelf life .............................................................................. 38
3.4 Test reports................................................................................................ 40
3.4.1 Test report for single analysis .............................................................. 40
3.4.2 Test report for multiple analysis ........................................................... 41
4. Quick Guide ............................................................................................... 42
5. Indicators, warnings and blackouts............................................................. 44
5.1 Indicators ................................................................................................... 44
5.1.1 – Heating LED ..................................................................................... 44
5.1.2 – Pressurized oxidation chambers ....................................................... 44
5.1.3 –Induction period not found ................................................................. 44
5.1.4 – Removal of record ............................................................................ 44
5.2 Warnings.................................................................................................... 45
5.2.1 - Warnings relating to correct operation of the instrument: .................. 45
5.2.2 - Warnings relating to correct record selection ..................................... 47
6. End-of-task operation ................................................................................. 47
7. Maintenance............................................................................................... 48
7.1 Routine maintenance ................................................................................. 48
7.2 Extraordinary maintenance ........................................................................ 50
7.3 Preparing instrument for transport.............................................................. 50
8. Uninstalling the software ............................................................................ 51
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9. Disposing of the unit ................................................................................... 51
10. Spare parts .................................................................................................... 51
11.Technical features .......................................................................................... 52
12. Wiring diagram ........................................................................................... 53
13. Pneumatic diagram .................................................................................... 54
14. Suggestions ............................................................................................... 55
15. The oxidation test – analytical aspects ....................................................... 56
15.1 The sample .............................................................................................. 56
15.2 The temperature ...................................................................................... 57
15.3 Oxygen pressure...................................................................................... 57
15.4 End of a test ............................................................................................. 57
15.5 Calculation of the Induction Period (IP) .................................................... 58
16. Analytical procedure ................................................................................... 59
Methods .............................................................................................................. 60
Oxidative stability test on pasta sauces (Genoa-style pesto, Bolognese ragout,
Amatrice-style sauce) ...................................................................................... 60
Oxidation stability test on salami ...................................................................... 61
Oxidation stability test on nuts (walnuts, hazelnuts, almonds, pine-seeds,
pistachios, Macadamia nuts)............................................................................ 62
Oxidation stability test on sauces (mayonnaise, cocktail sauce) ...................... 63
Oxidation stability test on chips ........................................................................ 64
Oxidation stability test on milk powder ............................................................. 65
Oxidation stability test on cheese ..................................................................... 66
Oxidation stability test on cereals flour ............................................................. 67
Oxidation stability test on the substitutes of bread (crackers, Italian bread sticks)
........................................................................................................................ 68
Oxidation stability test on vegetable oils (olive, seeds, palm) ........................... 69
Oxidation stability test on fat (margarine, butter, lard) ...................................... 70
Oxidation stability test on dry feed (animals food as pellets) ............................ 71
Oxidation stability test on bio-diesel (FAME, Fatty Acids Methyl Esters) .......... 72
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1. Introduction
The auto-oxidation of the lipids contained in food and animal feed is recognized
as one of the most important factors to the negative impact on the shelf-life
(commercial duration of foods and feeds).
The Velp Scientifica Oxidation Test Reactor, OXITEST, allows the sample to be
submitted to highly oxidative conditions (high temperature and pure oxygen over-
pressure) in order to know, within a short time, the product stability against the
oxidation of the lipids (rancidity).
During the sample oxidation, the instrument records the oxygen pressure drop
inside the oxidation chambers (called “Reactor” in the software), due to the
chemical reactions. OXITEST has two separate oxidation chambers to compare
the oxidative stability of different formulations of the same food or to test two
different samples at the same time.
The software allows the user to connect four OXITESTs to the same PC; in this
way it is possible to perform eight oxidation tests at the same time.
In case of black out or power failure, when the power comes back, it is possible to
continue the cycle, after connecting manually the OXITEST.
The analysis time depends on the sample type, sample quantity, and operating
conditions (temperature and oxygen pressure).
The instrument working temperature range is room-120°C, the maximum oxygen
pressure is 8 bar. In the present manual are detailed VELP analytical methods to
carry on the oxidation tests, optimized for the different kinds of samples.
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1.1 Parts included
Check that the instrument is complete when you receive it.
The table below describes the parts contained in the pack:
NOTE
Keep the shockproof instrument pack intact as it may be necessary to use it for
possible future transport.
3 3
1 2
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4
10
9 8 8 7 6
12
14
11
13
15
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List of OXITEST components:
Test customization
Using sample-holder containers and spacers is possible to vary the quantity and/or the
distribution of the sample inside the oxidation chambers.
Connectivity:
The software can be connected by serial mode to an external balance to transfer
the weight of the sample automatically into the OXISoft, in order to avoid mistakes
in transcription of the data and to speed up operations.
GENERAL SWITCH
The general switch makes it possible to turn the
instrument on and off. When the button is pressed, a
green light indicates that the instrument is on.
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2. Assembly and installation
After unpacking the instrument, place it correctly on a laboratory bench if possible next
to an oxygen supply point that is needed for oxidation. Keep well away from sources of
heat.
The instrument requires to be connected constantly to a PC during the test, when the
data of pressure is recorded.
In case of black out or power failure, when the power comes back, it is possible to
continue the cycle, after connecting manually the OXITEST (see chap.3). The PC
will lose the data during the period of the black out; it will start to record from the
last point before the black out. It is possible to decide to continue with the analysis
(in case of short black-out, for example) or to abort the analysis.
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2.3 PC Connection
The necessary PC requirements are:
* If the drivers automatically installed by Windows are not correct, the instrument
can’t communicate with the PC. In this case, overwrite the current drivers with
those in the USB-pen drive folder thanks to the “Device manager” in the PC
“Control Panel”.
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2.4 Balance connection
The OXISoft can be connected to the most common models of analytical
balances in order to enter the correct sample weights without any possibility of
transcription errors.
Connect the balance to the RS232 or USB port of the PC and set the relative
serial port in Service/Balances menu.
The OXISoft can be connected to the following balances:
Read the operating manual of the balance carefully to ensure correct use. The
software parameters of the balance should be the same as the default parameters
of the OXISoft see above (select Service/Balances).
NOTE: use the Custom section for connecting balances not listed above.
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3. Use of the software
After start-up, the software shows the welcome page and then ask for the logon
information. The User level password is “velp”.
NOTE: the software automatically searches for OXITEST units. If the automatic
search fails, manual connection can be carried out in Service/Find OXITEST.
NOTE: It is possible to connect four OXITEST independently. Use the manual
connection to connect one or more units while other OXITEST are already connected
and analyses are running.
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3.1 Database and test conditions
3.1.1 Laboratory information
In File/Laboratory information it is possible to compile the laboratory-related
fields.
These information are automatically saved and they will be included in the test
report. (see paragraph 3.4)
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3.1.2 Database
The database is the list of the analyses already performed or to be run with the
OXITESTs (maximum four instruments) connected to the OXISoft.
Before starting analyses, some of the columns in the database must be filled.
Several databases can be created and stored in the PC. Each database can
memorize max. 1000 analyses.
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Comments: Non-compulsory field where it is possible to enter some
comments about the analysis.
NOTE: once analysis has been carried out, the content of the database columns
cannot be modified.
NOTE: if mandatory information is missing, when “START” is pressed the
software will highlight the related columns.
The information can be entered once and copied using Copy/Add (select the
row and press the right button of the mouse) to add new rows. The new rows will
be added in sequence; the only information that is not copied is the sample
weight.
Each row of the database corresponds to an .oxi file, automatically saved in the
path indicated in the column “File name”.
In order to move the files to a different PC, it’s necessary to save the .oxi files in
the same folder.
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3.1.3 Test conditions
- Set Point P: Starting pressure for the analysis. This pressure may be
different for the two oxidation chambers (that can be set from 0 to 8 bar)
- Sampling time: Time interval that elapsed between recording the data
(pressure and temperature if set) and the subsequent ones
- Max analysis time: When the maximum analysis time is exceed, the
analysis is interrupted. The default value is 200 hours
NOTE: if the estimated analysis time is long, in order to avoid the creation of a big
file, it is suggested to use 1 minute (or more) as sampling time.
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In System/Work conditions:
If “enable graph temperature” is switched on, also the graph of the temperature
will be visualized on the graph in the main window.
To choose the test conditions, the menu Method could be useful (in
Analytics/Method):
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3.1.4 Heating and pressurizing step
To heat the OXITEST it is necessary:
- to fill the database with the analysis information (see chap.3.1.2);
- select one of the two filled rows for each OXITEST using the left key of the
mouse (the row will become blue);
- use the right key of the mouse to open the following menu:
and select “Set START”. Automatically, the numbers of the selected row and of
the row connected to the other chamber of the same OXITEST will be written on
the top part of the main window, in the correct OXITEST field:
- Press “Work OXITEST” button: it will become green and the LED on the
instrument will flash until the temperature set in Work Conditions has been
reached (constantly lit heating LED and green value on the right part of the main
window). The visualized status of the instrument will be WORK.
The rows selected will turn from blue to grey and a lock will appear in the first
column of each rows.
NOTE: During the heating step, the OXITEST chambers can already be filled with
the sample, but the discharge valves must be open (as in the picture at chap.
1.2).
NOTE: It is suggested to fill the Oxitest chambers with the sample before putting
the Oxitest in work condition.
NOTE: after filling the chambers with the sample, place the black upper insulating
panel.
NOTE: If it is necessary to stop the heating, it is enough to press again the WORK
button. The button will become grey and the OXITEST will stop heating. The rows
previously selected will be unlocked.
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To pressurize the chambers of the OXITEST, press of the corresponding
OXITEST. If the OXITEST is already at set temperature, after about 10 minutes
the following warning message will be displayed and the software will give an
acoustic signal:
Attention!
Close the discharge valve before pressurizing.
Close the discharge valves by placing the knobs at 90° in relation to the valve
bodies, lower the transparent protective shield and press the “Continue” button.
The system starts filing the chambers with oxygen till the pressure reaches the set
point value (the current pressure values are showed on the right part of the main
window).
The OXITEST will be in “In progress” status.
The software starts recording the file and, according to the selected sampling
time, to show the correct graph for each row selected.
NOTE: It is possible to press the Work button then right away the START button.
In this case, automatically the OXITEST will reach the set temperature, will wait
for the stabilizing time and then will give the message above.
NOTE: If Work and START buttons have been pressed, to stop the analysis is
necessary to press the STOP button, even if the analysis is not started. In this
case, a red “X” will appear in the first column of each rows.
NOTE: After pressurizing the OXITEST, the oxygen inlet can be closed.
If there are four OXITESTs connected to a single PC, the software manages them
independently giving the possibility to heat up the instruments and to run analyses
in different moments.
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3.1.5 Test execution
Selecting one row of an ongoing analysis, it is possible to monitor the trend of the
oxygen pressure inside the oxidation chamber and, if the analysis is completed, to
stop the data recording by pressing the “STOP” button. In this case, both of the
analyses of the OXITEST selected will be interrupted.
NOTE: On the main window, below the database, it is possible to show the
oxidation curve of the selected row.
With ongoing analyses, the operator can:
- switch ON the “enable graph temperature” option to see also the temperature
graph on the main window.
- use the procedures (see chap 3.3);
- recalculate already analyzed rows (see chap.3.2.6)
- create report of already analyzed rows (see chap. 3.4)
- connect other OXITEST units (if less than 4 OXITEST are
connected to the PC).
After fixing the issue, it is possible to reconnect manually the instruments (use
Service/Find OXITEST). In this case, the user can decide to continue the test (for
example, in case of a short blackout) or to abort it.
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If necessary, use the “Forced remove” function (select one row and mouse right
click) to remove completely the rows from the database and to put OXITEST in
“Waiting” status.
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3.2.1 Configuring the data base
The database consists of a set of data entered by the operator as well as data
calculated by the software after analysis. Select “Modify” to modify the
configuration of the data base:
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3.2.2 Filtering the database
The data viewed can be filtered using the filter function.
Select Modify/filters. The following window appears:
The possible filters criteria for OP1 (option 1) and OP2 (option 2) are displayed in
the picture below:
4- Press “Save”, insert the file name and a path to save the filter
5- To use previously created filters, press “Load” and select the filter required.
6- To activate the filter selected (Filter ON), press “Filter OFF” and exit the
window.
NOTE: to disactivate filter/s, select the filter/s as described above and press
“Filter ON”.
The filter status (“Filter ON” or “Filter OFF”) is shown at the bottom of the main
window.
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3.2.3 Working with several databases
Select File/Open to load a previous database for evaluation, to perform similar
analyses, or to modify the contents of the “laboratory information” file.
To modify the laboratory information, load the previous data base, select
File/laboratory information and make the necessary modifications. The
laboratory information will be included in the test reports (see chap. 3.4 “Test
reports”).
The number of databases that can be created or uploaded is unlimited. The
maximum number of analyses that can be recorded in each data base is 1000.
Each database is saved in C:\OXITEST\database. The path of the database is
displayed at the bottom of the main window.
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3.2.4 Modifying the graph
The graph of the analysis selected is shown at the bottom of the main window
whether the analysis is in progress or already completed.
1 2
The green line indicates the induction period (IP). The blue line indicates the
pressure curve. The red line, if enabled, indicates the temperature.
The pressure (vertical axis on the left) and the temperature (vertical axis on the
right) are fixed, the Time (horizontal axis) is in auto-scale mode.
The following graph tools are available:
1- Graph palette
2- Scale palette
Graph Palette
Activates the drag function on the cursors
Pointer and it is useful for positioning the straight
lines for induction period calculation.
Press to activate the zoom pop-up:
3 types of zoom in the window
Zoom Automatic detailed display zoom
Dynamic zoom in video extension
Dynamic zoom in video compression.
Scale Palette
Closed: locks the axis scale.
Padlock
Open: the axis scale can be modified.
Permits to visualize the details of the
Zoom
graph increasing the axes scales.
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3.2.5 Creating some procedures with their archives
In “Analytics” menu, there is the possibility to work with different procedures:
NOTE: this menu can also be reached by highlighting a row, pressing the right
key of the mouse and selecting Recalculate.
Selecting the GM as IP calculation method, it is possible to compare the result
given by the OXISoft using the graphical method (GM) (in the New column) with
the default result calculated by the Least square method (LSM) (in the old
column).
Alternatively, it is possible to choose GM method and then move the 2 tangent
curves pressing on the points of the curves.
If the new results are accepted, press OK to confirm. The value will be updated in
the relative row of the database. The indicator in the first column will switch to
“attention” (see chap.3.1.5) and the “Error” column will indicate “recalculated”.
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3.2.7 Exporting data
Information can be exported from the database in Excel, Text or Lims format by
selecting Report/Export Data EXCEL or Report/Export Data TEXT or
Report/Export data LIMS.
Below is an example of the file exported in Excel
NOTE: it is possible to export only one row. If more than one row is selected, the
software will show:
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Below is an example of the file exported in text format.
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3.3 Procedures
Select one or more rows from the database and press Analytics/Repeatability test.
The window below will be visualized:
If no rows have been selected from the database, the Repeatability Test window
will be empty.
Using the “Add” button, it is possible to select analyses from the current database
or from a different one (thanks to the “Open Database” button)
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In the Repeatability Test window:
- press “Confirm” to save the “.rpt” file
select a folder on your PC, insert the file name and press “Save”
NOTE: the repeatability test files are necessary to use the other
procedures.
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- press “Report” to create a dedicated report, as Excel file, with all the
information about the selected rows
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3.3.2 Freshness test
This procedure allows to determine the product freshness by analyzing different
lot numbers of the same samples (or raw materials) and comparing their IP with
the reference lot number IP.
This procedure permits to evaluate if the sample (i.e. raw material or good) is
conformed to the reference material.
Press the “Load” button to import the previously created “.rpt” files.
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In the table, information about the file name, IP value, date, and operating
conditions are reported.
It is necessary to decide which row will be the reference:
The graph shows the IP +/- SD of the reference material and where the IP of the
other materials fall.
In the table on the left, it is possible to see if the value of the material is in the
range of the reference or not.
The functioning of the “Confirm”, “Open”, “Report”, “Guide” buttons is the same as
that descripted above.
The “Add” button allows to import other information; the software will guide the
user creating the repeatability test file.
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It is also possible to edit (hide, remove) the lines of the table in the same way as
descripted in the chapter 3.3.1
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3.3.3 Formulas comparison
This procedure allows to determine the best formula (normally the one with the
highest IP) for the sample by analyzing the same sample with different formulas
and comparing their IP with the reference sample formula IP.
The graph shows the average IP of the reported rows in the table with their
standard deviation (SD).
The table on the left shows results in terms of “Delta IP [h:m]” and “Delta IP [%]”
compared to the reference value.
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3.3.4 Packaging comparison
This procedure allows to determine the best packaging (normally the one with the
highest IP) for the sample by analyzing the same sample differently packaged and
stored for the same time and comparing their IP with the reference sample
packaging IP.
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3.3.5 IP during ageing
This procedure allows to obtain a prediction of the oxidation stability during a shelf
life study by measuring the product at defined time intervals. From IP decreasing,
a curve is built. The same sample is analyzed at different times and at the end,
the software calculates the linear regression equation.
The software shows the straight tendency line and the correlation square (R2).
The blue lines show the IP value of the selected analysis and its standard
deviation at the time recorded as “Start time”.
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3.3.6 Estimated shelf life
This procedure, by analyzing the same sample at different temperatures, allows to
extrapolate and estimate the sample oxidation stability at room temperature (in
case of linear dependence with the temperature).
By inserting the desired temperature in the dedicated box, the software will give
the results in terms of “Estimated IP [d:h:m]”
The software shows the straight tendency line and the correlation square (R2).
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Example of the test report:
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3.4 Test reports
Information can also be exported from the data base to a predefined Excel file
called Test report.
It is possible to create:
- test report for single analysis
- test report for multiple analyses (comparison)
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3.4.2 Test report for multiple analysis
Highlight the rows and select Report/Create Comparison
The test report shows the following information:
- laboratory information (including company logo);
- software version;
- operator name
- serial number of the instrument;
- the results of the selected rows;
- the Average and SD for IP;
- the curves of the rows selected on the same graph.
- the IP of the different analyses.
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4. Quick Guide
These pages summaries the OXISoftTM dropdown menus. The aim is to guide the
user quickly in searching for the functions he/she needs and how to access them.
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5. Indicators, warnings and blackouts
5.1 Indicators
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5.2 Warnings
The instrument can display various types of warnings.
Check that the USB cable and the power cable are connected and that the
general switch is on (“I” position). Press the “Find OXITEST” button.
Different situations can cause the interruption of the PC-OXITEST
communication:
- the USB cable connector is accidentally removed from the instrument or from the
PC (OXITEST remains ON)
- the power supply is cut suddenly also for short time (OXITEST and/or the PC
is/are turned OFF)
If the OXITEST remains ON and the analysis is running, press Service/Find
OXITEST. When the communication is ok, the software gives a warning message
to communicate that the analysis is in progress. It is possible to continue the test
or to interrupt it.
The table below shows some examples:
PC
OXI status Operations
status
The software warns with an acoustic signal.
Connect manually the OXITESTs: the
OFF when analysis is instruments proceed with the analyses in
ON
in progress running.
In the graph an irregularity in the line can
appear, if the shutdown has been long.
The software warns with an acoustic signal.
Connect manually the OXITESTs: the
heating element of the instruments are
OFF when instrument
switched off and the OXITESTs are in
ON is in work but not in
waiting status even if the WORK button
temperature
remains pressed.
Press WORK button to turn it off: the rows
selected will be unlocked.
The software warns with an acoustic signal.
Connect manually the OXITESTs: the
heating element of the instruments are
OFF when instrument switched off and the OXITESTs are in
ON is in work and in waiting status even if the WORK button
temperature. remains pressed.
Press WORK button to turn it off: the rows
selected will be stopped with the red sign. To
start new analyses filling news rows.
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The software warns with an acoustic signal.
Connect manually the OXITESTS (in
Service/Find): the heating element of the
OFF when instrument instruments are switched off and the
is in work, temperature OXITESTS are in waiting status even if the
ON
and START button has WORK button remains turned on.
been already pressed. Press WORK button to turn it off: the rows
selected will be stopped with the red sign. To
start new analyses filling news rows is
necessary.
The message indicates that you can proceed to the oxygen loading stage after
manually closing the discharge valves.
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5.2.2 - Warnings relating to correct record selection
If you try to create a single report with no rows selected or with more than one
rows selected, the software shows the following message:
If you try to create a comparison report with no rows selected or with more than
20 rows selected, the software shows the following message:
6. End-of-task operation
At the end of the test:
1. lift the transparent protective shield;
2. discharge the gases contained in the oxidation chambers by gently
opening the discharge valves (knobs in line with the valve bodies).
In this way, traces of oxidized sample cannot be deposited in the
gas outlet tubes;
3. Remove the upper insulating panel
4. loosen the cover-locking screws using the appropriate locking key,
5. remove the covers of the two oxidation chambers,
6. remove the 4 filters (2 for each oxidation chamber) using the
dedicated spanner supplied with the instrument and check them
(see chap. 7.1)
7. wash the sample-holder containers and the spacers using hot water
with a non-corrosive degreasing detergent (eg. washing-up liquid).
Then use acetone so as to remove all sample traces and to prevent
the subsequent test being contaminated by possible residue;
8. in the same way as above descripted, clean the oxidation
chambers and the covers.
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7. Maintenance
The maintenance (routine and extraordinary) is the basic requirement to extend
the life of the instrument and to ensure that it will always find the best working
conditions. It is therefore important to follow the instructions described below.
To run a Blank test, fill the database selecting “Blank” as Test Type and follow the
previously mentioned procedure; use cleaned and empty oxidation chambers to
check just the reactors or put inside the chambers also spacers and/or sample-
holder containers to check them too.
The system will run a 24 hours test (temperature and pressure setpoint as
inserted in the Work and Analysis Conditions menu) checking the pressure trend.
Blank test is successful if the pressure drop is less than 2% from the starting
point.
Performing a Leak test is possible to check if there are leaks in the system.
To run a Leak test, fill the database selecting “Leak Test” as Test Type and follow
the previously mentioned procedure; perform the test in the same conditions of
the blank test (temperature and pressure set point; just cleaned and empty
oxidation chambers or with spacers and/or sample-holder containers inside them)
but using compressed air or Nitrogen (purity degree above 99%) to pressurize the
chambers.
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The system will run a 24 hours test (temperature and pressure setpoint as
inserted in the Work and Analysis Conditions menu) checking the pressure trend.
Using compressed air or Nitrogen instead of oxygen allow to exclude the
oxidation process.
Leak test is successful if the pressure drop is less than 4% from the starting point.
The software is able to check the status of the maintenance activities for each
OXITEST connected to the PC (in Service/Maintenance):
Replace periodically the filters to prevent the next test being contaminated by
possible residue.
Press the respective “Refresh” button in the Service/Maintenance menu when the
filters are cleaned or replaced.
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7.2 Extraordinary maintenance
Replacement of fuses
The fuses are replaced only when necessary. If one of the two fuses blows, the
instrument does not switch on.
After disconnecting the mains power cable, open the window on the black rear
socket to access the two fuses.
The instrument has two 5x20 mm delayed fuses (one for each phases). According
to the OXITEST version the fuses rating is different: 5 A for the 230 V version and
10 A for the 115 V version.
Cleaning procedure for the discharge valves
Discharging oxygen from the oxidation chambers through the valves, some
sample residues may deposit inside the valve exhaust channel.
If necessary, inject or spray acetone inside the valves channel. Be careful to avoid
contact between solvent and the external part of the valves.
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8. Uninstalling the software
Removing the software does not involve cancelling the *.oxi files present, even if
saved in the directory C:\OXITEST\record.
Remove the software following the normal program deletion procedure.
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11.Technical features
GENERAL Measurement
unit
Power supply V/Hz Code F30900248: 230~(+/- 10%)/50-60
Code F30910248: 115~(+/- 10%)/60
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12. Wiring diagram
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13. Pneumatic diagram
A O2 inlet
B Needle valve
C Solenoid valve
D Pressure transducer
E Reactor outlet valve
F Safety valve
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14. Suggestions
We would be pleased to receive your criticism and suggestions aimed to improve
this manual.
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15. The oxidation test – analytical aspects
15.1 The sample
The sample quantity for the analysis depends both on the lipids content and the
intrinsic characteristics (i.e. unsaturated fatty acids content).
Generally, the more lipids has the sample, the less sample has to be used.
For example, few grams of pure oils and fats will be sufficient; thus, to analyze foods
with high fat content (like mayonnaise sauce, 50-60% of lipids) the oxidation test can
be performed using only 10g.
Increase the test portion, up to 50-90 g for each chamber, for sample with low
percentage of lipids or when it is difficult to visualize the sample oxidation flex.
The following table contains some examples of sample amount related to total fat
and unsaturated fatty acids.
Sample
Unsaturated
Total fat amount in
fatty acids Example
% each reaction
%
chamber
Feed, face cream, pasta, flavored
2-4 2-4 30-40 g
drinks
< 10 < 10 30-40 g Bread substitutes, cakes, béchamel
Dressing salad, face cream, chocolate
10-30 <20 30 g
and nuts cream, biscuits
10-30 20-30 20 g Wurstel, pet food
40-100 < 30 20 g Sausage, noodles
Oils, chips, nuts, pasta sauce,
40-100 30-100 5- 10 g mayonnaise, vinegar, cold wax, ham,
cheese, seeds
In the present manual different analytical methods are provided, to carry on the
oxidative stability test on different kinds of samples.
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The VELP Analytical Department has developed and tested these methods to allow
the user to work under the best operative conditions in order to visualize a good
oxidation flex, getting reliable and reproducible results within a reasonable short
time.
NOTE: increasing the work temperature, the Induction Period will decrease.
The best and the most commonly used pressure for the oxidation test with the OXITEST
is 6 bar. This pressure allows to obtain the sample Induction Period within a reasonable
short time.
NOTE: to obtain reliable and reproducible results use 5.0 (or higher) degree pure
oxygen.
The curve flex corresponds to the end of the intrinsic resistance of the product
against the oxidation of the lipids and to the beginning of the accelerated absorption
of oxygen (appearance of olfactory rancidity).
When the test ends (automatically or manually as descripted in chapter 3.1.5), if
“Sample” was selected as Test Type, the software shows the Induction Period on
the graph as a vertical line.
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15.5 Calculation of the Induction Period (IP)
At the end of the test, the software automatically calculates the Induction Period using
the Least Squares Method (LSM). Thanks to the Recalculate function (accessible in
Service menu or with a mouse right click), it is possible to use the Graphical Method
(GM).
The Induction Period is the intersection point of the two tangent lines (before and after
the flex) of the pressure curve.
With the graphical method, it is possible to position manually these two lines.
By confirming the modification, the IP value will be overwritten on the database.
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16. Analytical procedure
Clean the titanium chambers, sample holders and spacers with a tissue
A
paper and acetone
Insert the spacers if required and place the filters (2 for each oxidation
B
chamber)
C Prepare the sample and weigh it directly in the sample holders
D Load the sample holders with the sample into the OXITEST chambers
Grease the O-rings with High temperature sealing grease and place them
E
in the dedicated grooves (top part of the oxidation chambers)
G Leave the discharge valves open (knobs in line with valve bodies)
Fill the data base with the necessary information: sample name, weight,
I
test type, s/n OXITEST, reactor.
L Set the analysis temperature in System/Work Conditions
When the system is stable, it shows the message “Attention! Close the
Q
discharge valves before pressurizing.” and gives an acoustic signal
Close the discharge valves (knobs at 90° in relation to valve bodies) and
R
open the oxygen line
Press ok. Automatically, oxygen is loaded into the oxidation chambers
S
and the software starts recording
T Close the oxygen line
NOTE: the analytical procedure descripted above allows to work under the best operative
conditions in order to visualize a good oxidation flex, getting reliable and reproducible
results within a reasonable short time.
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Methods
Oxidative stability test on pasta sauces (Genoa-style pesto,
Bolognese ragout, Amatrice-style sauce)
Sample preparation
Mix accurately the pack content.
Analysis setup
Load the sample-holder containers into the chamber.
If just one sample-holder container is in use, place 2 spacers on the chamber base
before loading it.
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Oxidation stability test on salami
Sample preparation
Grind by a suitable device the pack content. Mix accurately the ground
sample.
Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder
container on the top.
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Oxidation stability test on nuts (walnuts, hazelnuts,
almonds, pine-seeds, pistachios, Macadamia nuts)
Sample preparation
Grind by a suitable device the pack content. Mix accurately the ground sample.
In the case of complete nuts (having the shell), eliminate previously the shell.
Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container on
the top.
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Oxidation stability test on sauces (mayonnaise, cocktail
sauce)
Sample preparation
Mix accurately the pack content.
Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder
container on the top.
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Oxidation stability test on chips
Sample preparation
Grind by a suitable device the pack content. Mix accurately the ground sample.
Analysis setup
Load the sample-holder containers into the chamber.
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Oxidation stability test on milk powder
Sample preparation
Mix accurately the pack content.
Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container
on the top.
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Oxidation stability test on cheese
Sample preparation
- Spreadable soft cheese: mix accurately the pack content
- Grated cheese: mix accurately the pack content
- Hard and semi-hard cheese: grind by a suitable device the pack content; then,
mix accurately the ground sample
Analysis setup
Load the sample-holder containers into the chamber.
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Oxidation stability test on cereals flour
NOTE: In order to obtain a visible oxidation flex, the tested sample should
contain at least 4-5% of fat.
The following samples can be tested by OXITEST: whole cereals flour, cereals-
legumes mixed flour, cereals flour enriched with oil –seeds (sesame, sunflower).
Sample preparation
If the sample is whole grain, grind it by a suitable device; then mix accurately the
ground sample.
If the sample is as flour, just mix accurately the pack content.
Analysis setup
Load the sample-holder containers into the chamber.
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Oxidation stability test on the substitutes of bread
(crackers, Italian bread sticks)
Sample preparation
Grind by a suitable device the pack content. Mix accurately the ground
sample.
Analysis setup
Load the sample-holder containers into the chamber.
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Oxidation stability test on vegetable oils (olive, seeds,
palm)
Sample preparation
Mix accurately the pack content, avoiding as much as possible the contact
between the sample and the atmospheric oxygen.
Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container
on the top.
Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder
container on the top.
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Oxidation stability test on dry feed (animals food as
pellets)
Sample preparation
Mix accurately the pack content.
NOTE: The oxidation stability test can be performed on the whole pellets, without
preliminary grinding.
Analysis setup
Place 1 spacer on the chamber base and then load the sample-holder containers
on the top.
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Oxidation stability test on bio-diesel (FAME, Fatty Acids Methyl
Esters)
Sample preparation
Mix accurately the pack content.
Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container
on the top.
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Declaration of conformity
We the manufacturer Velp Scientifica srl
address Via Stazione, 16
20865 USMATE (MB)
Italy
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Declaration of conformity
We the manufacturer Velp Scientifica srl
address Via Stazione, 16
20865 USMATE (MB)
Italy
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Thank you for choosing a VELP product!
Established in 1983, VELP is today one of the world’s leading manufacturer of
analytical instruments and laboratory equipment that has made an impact on
the world-wide market with Italian products renowned for innovation, design
and premium connectivity. VELP works according to ISO 9001, ISO 14001
and OHSAS 18001 Quality System Certification.
Our instruments are manufactured in Italy according to the IEC 1010-1 and
CE regulation.
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