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OXITEST Operating Manual Velp

The document provides operating instructions for an Oxidation Test Reactor instrument. It describes safety procedures, assembly, software use, maintenance, and analytical aspects of using the instrument to investigate oxidative stability of foods and feeds containing lipids through oxidation tests.

Uploaded by

albermola
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
100% found this document useful (1 vote)
208 views

OXITEST Operating Manual Velp

The document provides operating instructions for an Oxidation Test Reactor instrument. It describes safety procedures, assembly, software use, maintenance, and analytical aspects of using the instrument to investigate oxidative stability of foods and feeds containing lipids through oxidation tests.

Uploaded by

albermola
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 78

1

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.

Do not dispose of the equipment with domestic waste

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

The manufacturer, committed to the constant improvement in the quality of his


own products, reserves the right to vary their features without prior notice

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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

Declaration of conformity ....................................................................... 73

Declaration of conformity ............................................................................. 74

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10003023/C7
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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10003023/C7
1.1 Parts included
Check that the instrument is complete when you receive it.
The table below describes the parts contained in the pack:

Description Qty Code


Oxitest – Oxidation test reactor 1 Pc F30900248/F30910248
Spacers 4 Pc 10001984
35 ml sample-holder containers 6 Pc 10001985
Threaded key 1 Pc 10003266
4x6 mm tube for loading oxygen 3m 10002866
Power cable 1 Pc 10007180/10007181
USB cable x PC connection 1 Pc 40002309
OXISoft Software 1 Pc 40001907
Cover-locking key 1 Pc 10003304
Spanner for filters 1 Pc 10003826
Instruction manual 1 Pc 10003023
O-Ring 4 Pc 10002033
High temperature sealing grease 1 Pc A00000236

NOTE
Keep the shockproof instrument pack intact as it may be necessary to use it for
possible future transport.

1.2 Instrument description


OXITEST is made with state-of-the-art technologies and a special software that
enables the operator to monitor and record the oxidative process inside the two
oxidation chambers, calculate the induction period and easily compare the various
tests performed.
The operator can easily print the report with the conditions used for the test and
the induction period (IP) calculated for each individual oxidation chamber. The
induction period can be calculated by means of two different methods:
• graph method (GM), based on the positioning of straight lines tangent to
the graph
• least squares method (LSM), based on the principle of the limits chosen
for the graph.

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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:

1 35ml sample-holder container


2 Spacer
3 Threaded key
4 Transparent protective shield
5 Accessory-holder compartment
6 General switch
7 Discharge valve
8 Oxidation chamber cover
9 Heating LED
10 Cover-locking key
11 Spanner for filters
12 Filter for oxidation chamber
13 Oxidation chamber
14 O-Ring
15 Upper insulating panel

OXITEST is fitted with state-of-the-art devices and cutting-edge technology:


 The frame, made of metal, is treated with special resins and varnishes
that make the instrument resistant to mechanical agents and chemical
reagents found in the laboratory.
 The use of titanium for manufacturing the oxidation chambers, sample-
holder containers, spacers and covers in direct contact or likely to
come into contact with the sample guarantees excellent chemical
resistance and good thermal uniformity.
 The instrument is controlled by a PC through special software that
manages all the operations of test startup, monitoring and interpreting the
end results.
 The USB cable enables OXITEST to be connected to the PC. Up to 4
OXITESTs can be connected independently.

Other product features:


Accessory-holder compartment
The rubber accessory-holder compartment makes it possible to replace and
protect the sample-holder containers and/or the spacers, the threaded key, as
well as the cover-locking key, the spanner for filters, that are not used during the
test.

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.

Software customization and flexibility


The software makes it possible to save the laboratory information and the analysis
parameters, presenting them each time in order to speed up the test startup
phase.
It automatically calculates the induction period using the least square method.
The operator is able to recalculate the induction period using the graphical
method.
The export of the data collected in a text file or an Excel file makes it possible to
perform further processing of the oxidation curve.
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10003023/C7
Customization of the database and the possibility of using various search filters
contained therein help compare the results of the tests and their interpretation.
The possibility to super impose more curves allows to easily value the
repeatability of the test (control Repeatability test).
The procedures shown by the software help in using and interpreting the IP data
received from the OXITEST and create different archives for statistic evaluations.
It is possible:
- To compare different lot numbers of the same product, using the
freshness test procedure (see chap. 3.3.2)
- To compare different formula or packaging of the same product, using
formula or packaging comparison procedure (see chap. 3.3.3 and 3.3.4)
- To visualize the behavior of the decrease of the sample IP during the
ageing of the product, using the IP during ageing procedure (see chap.
3.3.5)
- To estimate the shelf life of the product at a precise temperature, using
the Estimated shelf life procedure (see chap. 3.3.6)

It is possible to connect four OXITESTs independently, helping to improve the


productivity.

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.

Ergonomics and safety:


The delicate stage of loading the oxidation chambers with the food to be analyzed
is helped by the threaded key that makes it possible to insert the sample-holder
containers easily into the chambers, limiting the risk of the sample spilling over.

1.3 Keys and functions

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.

LED When the heating LED is lit, it indicates that the


temperature of the two oxidation chambers is the same
as the one set.
When the heating LED flashes intermittently, it
indicates that the instrument has not reached the set
point temperature.
When the heating LED is off, it indicates that the
heating is no longer activated.

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10003023/C7
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.

2.1 Pneumatic connection


In order to perform analyses, OXITEST needs an oxygen supply point (use grade
5.0 or higher oxygen).
Use the kit 4x6mm tube, of suitable length, to connect the gas supply point to the
quick connector at the rear of the instrument.
Open the oxygen supply point tap in order to be able to load the circuit with
oxygen.
NOTE
• Ensure that the maximum pressure of the oxygen regulator is 8 bar.
• The desired pressure value for the analysis is set by the PC. If the
pressure set is not reached, check that the pressure at the oxygen
supply point is greater than that set by the PC.
• The instrument is fitted with a safety valve to protect the internal circuit if
the pressure exceeds 14 bar.

2.2 Mains power supply connection


Before connecting the instrument to the mains power supply, ensure that the
general switch is on the “0” (OFF) position and check that the details on the
instrument identification plate are the same as those available at the power point.
Depending on the code version, the instrument operates with power voltage of
230V 50/60Hz or 115V 60Hz. Connect the instrument to the mains power supply
by means of the appropriate cable with a plug.

NOTE: The general switch makes it possible to disconnect the instrument


completely from the mains power when the instrument is not being used, so as to
use less electricity.

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10003023/C7
2.3 PC Connection
The necessary PC requirements are:

• Operating system: Windows 7 (SP1), Windows 8 or Windows 10


Hardware: Pentium IV processor 2 GHz or more
RAM 4 GB
Available space on disk 70 MB
• Recommended graphic resolution: 1024x768 pixels

1. Boot up the PC with the machine administrator privileges, after having


checked that all the above-mentioned requirements are met.
2. Insert the USB-pen drive in the PC and follow the procedure to install
the OXISoft. To start the installation run “setup.exe” from the USB-pen
drive
When requested, restart the PC to complete the installation.
3. Connect one OXITEST to the PC using the USB cable supplied with the
instrument.
4. Turn ON the OXITEST using the general switch.
5. After few seconds the PC acknowledges the presence of a new
hardware and will automatically start up the drivers installation
procedure. If requested, specify the path of the USB-pen drive as source
directory for the drivers and proceed with the installation following the
instructions on the video. *
6. Launch the software from the PC (double-click on the appropriate icon
on the desktop or select the item OXISoft from the “Velp Scientifica”
section in Start/Programs).
See chap. 3 for the logon information.

* 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:

Brand Baud Data bit Stop bit Parity Flow control


Mettler 9600 8 1 none Xon/Xoff
A&D 2400 7 1 even none
Sartorius 1200 7 1 odd RTS/CTS
Precisa 9600 8 1 none none
Gibertini Crystal 9600 7 1 even none
Custom

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.

On the right, information related to each OXITEST are visualized:

- Serial number of the OXITEST if it is connected


NOTE: The OXISoft will perform the automatic connection between the serial number
of the instrument and the progressive number (from 1 to 4).
- Status of the unit: - Waiting: no analysis running
- Work: if the heating element is switched on
- In progress: when the analysis is running
- Current conditions in terms of temperature and pressure in the oxidation chambers
- Number of the analyses that is possible to run before the first maintenance event
(see chap. 7: Service/Maintenance menu).
In System/Language, it is possible to set different languages.

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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)

NOTE: The “Laboratory information” file can be modified as many times as


necessary. The information in this file are not mandatory.

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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.

Select File/New to create a new database


Select File/Open to load an already existing database
Each database is connected to a “Laboratory Information” file (see chap. 3.1.1)

The columns necessary to start the analyses are listed below:


Sample Name: Non-compulsory field where it is possible to enter the name of
the sample inserted into the chamber. It is an alphanumeric field.
Weight [g]: Non-compulsory field where it is possible to enter manually (or
automatically if the balance is connected to the PC) the weight in grams of the
sample inserted into the chamber.
Test Type: Compulsory field where it is necessary to select which kind of
analysis has to be performed: sample, blank or leak test.
S/N Oxitest: Compulsory field where it is necessary to set the serial number
of the OXITEST among the OXITEST connected.
Reactor: Compulsory field where it is necessary to select which chamber has to
be analyzed.
Operator Name: Non-compulsory field where it is possible to enter the
name of the operator who is performing the test
Notes: Non-compulsory field where it is possible to enter some notes relating to
the analysis (maximum 90 characters).

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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.

The other columns are filled automatically by the software:

IP calculation method: LSM (least squares method) is the default method


used by the software to calculate the IP. If the analysis is recalculated, the
method will be GM (graphical method).
Induction period: Result given automatically by the software in hh:mm
Curve 1 and 2: Equations of the curves found automatically by the software to
calculate the IP with graphical method.
Analysis time: Analysis time included between Start operation (pressing )
and STOP (pressing or automatic).

Date and time: Time when the analysis started.


Data recorded: When the analysis is recalculated.
Error: If some alarms or error occur during the analysis
File: The name and the path of the file that automatically the software
creates.

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

The content of the columns:

- 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

are set in the System/Analysis conditions for each OXITEST:

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.

NOTE: the maximum analysis time is the estimated analysis time.


The software will automatically stop the test if the end analysis conditions are
reached or if the maximum analysis time is reached.

If the time of the analysis is unknown, it is suggested to set a big value as


maximum analysis time and if it is necessary to stop the analysis manually when
the induction period is visualized.

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10003023/C7
In System/Work conditions:

it is possible to set at what temperature the analysis has to be performed (Set


point T [°C]). This temperature is the same for both the oxidation chambers of the
same OXITEST and it can be set from 10°C to 120°C.

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):

In this menu, there is an abstract of the analytical method reported on the


operating manual.
The following parameters are suggested for several samples families:
- test temperature
- test pressure
- sample weight for each chamber
- number of sample holders and spacer.
- sample preparation

It is possible to create a new method (New) or delete one or more (Delete).


To confirm the modifications, it is necessary to press OK.

NOTE: this menu is only to be consulted. In order to set pressure and


temperature, it is necessary to go in Analysis and Work conditions.

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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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10003023/C7
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.

NOTE: If necessary, it is possible to modify the temperature condition until the


OXITEST is in “Work” status. It isn’t possible to do this when the unit is in “In
progress” status. Attention: in this case, the information on the database will not
update.

NOTE: if necessary, it is possible to modify the pressure conditions until the


OXITEST is pressurizing the chambers (in “In progress” status before starting the
data recording). Attention: in this case, the information on the database will not
update.

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).

With ongoing analyses, the operator cannot:


- change the database or create a new one (see chap. 3.1.2)
-close OXISoft.

The stop of the analysis could happen:


- manually, by pressing the button;
- automatically, if the pressure drops under 1.5 bar or if the maximum analysis
time set in Analysis condition is reached, when “Sample” is selected as test type
in the dedicated column;
- automatically, after 24 hours or if the system detects a pressure drop, when
“Blank” or “Leak Test” is selected as test type in the dedicated column. The
maximum admitted pressure drop is 2% during a Blank Test and 4% during a
Leak Test
The OXITEST will stop the heating and the software will show the result in terms
of IP (hh:mm) and equation of the curves.
The several statuses of the instrument are shown by indicators that appear in the
first column of the database:
Indicator Meaning
OXITEST is reaching the Work conditions
The systems is recording analysis data
Analysis ended correctly (automatically or manually)
Analysis terminated incorrectly: no IP found.
Analysis ended correctly but there are some notes in the “Error”
column.
- Recalculated: the result was recalculated using a different IP
calculation method. (see chap. 3.2 “Evaluating data”)

NOTE: if the PC-OXITEST communication is interrupted or if the power supply of


the units is cut for a period when analyses are running, the software advises with
an acoustic signal.

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.

3.2 Evaluating data


In order to evaluate the obtained data, the software offers the following
possibilities:

- Configuring the database


- Filtering the database
- Working with several databases
- Modifying the graph
- Creating some procedures with their archives
- Recalculating analysis
- Exporting data

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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:

Filter Filter data (see chap. 3.2.2).


Order View data in ascending or descending order.
Alternative press the right key of the mouse and select Order.
Adapt Adapt the width of the column selected to its content.
Alternative press the right key of the mouse and select to
adapt width.
Standard column View columns in standard configuration.
Configure Change the order of columns (up and down arrows) or hide
columns (left and right arrows).
Alternatively, press the right key of the mouse and select
Configure.

Remove Delete one or more rows from the database.


Alternatively, press the right key of the mouse and select
Remove.
Select all Select all the rows in the database

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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:

Select filters as follows:


1- choose the fields to be filtered and press ;
2- select the field in “Selected Fields”: the name of the field selected is displayed
on the right in the “Field” box
3- select the OP1 and/or OP2 option and press SEARCH: the filter is displayed in
the the lower right part of the window.

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.

Drag Press to move the whole group of traces


function present on the diagram.

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.

Customize the format, precision, type


Drag
and color of the axis as well as making
function
the scale or scale label visible or not.

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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:

Each procedure has its archive, if used (in C\OXISoft\Procedures)


See chap 3.3 for further details.

3.2.6 Recalculating analysis


The Recalculate option can be used to calculate the induction period (IP) of one
analysis with the automatic graphical method (GM) calculated by the OXISoft or
with the graphical method obtained modifying manually the curves visualized.
Highlight the row and select Analytics/Recalculate. The following window
appears:

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.

By accessing the drop-down menu File/Export Data LIMS it is possible to export a


file containing test conditions and the results corresponding to the selected tests
in a format (*.csv) which can be easily read by the main laboratory management
systems (LIMS). This control allows to export in a unique file one or more record
(using the multiple selection).
When the control Export Data LIMS is selected, select the value/unit to be
exported (see below).
Select the configuration of the exported data from the options available. It is
possible to attribute the comma, semicolon or tab as delimiting character and the
comma or decimal point as the decimal indicator depending on the type of the
Lims. Press OK to confirm.

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3.3 Procedures

3.3.1 Repeatability test


This procedure allows to compare the IP of the same sample analyzed several
times, at the same analysis conditions.
Automatically, the OXISoft calculates the IP average, standard deviation (SD) and
relative standard deviation (RSD) of the selected analyses and shows these
values on a graph.

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.

- press “Open” to load a previously created repeatability test file


- press “Add” to add other following replicates
- it is possible to hide one or more rows by clicking with the left mouse
button on the relative points in the graph.
Otherwise, press and keep pressed the “Ctrl” button on the keyboard
and deselect one or more rows from the table with the left mouse button

- it is possible to delete one or more rows by selecting them and press


the right mouse button; then click “Remove”.

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- press “Report” to create a dedicated report, as Excel file, with all the
information about the selected rows

NOTE: the file is an open file that can be modified.

- press “Guide” to visualize a step by step procedure about how to work


correctly with the procedure.
It is also possible to flag with a tick the steps already done

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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.

To run this procedure repeatability test files are necessary.


So, proceed to create the repeatability test files of the reference lot number and of
the other lot numbers analyzed (see chap. 3.3.1).

Select Analytics/Freshness test.

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:

NOTE: it is possible to fix only one reference material.

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

Below an example of the report:

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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.

Select Analytics/Formulas comparison.


Proceed in the same way as descripted in the chapter 3.3.2

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.

Below an example of the report:

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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.

Select Analytics/ Packaging comparison.


Proceed in the same way as descripted in the chapter 3.3.2 and 3.3.3

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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.

Select Analytics/IP during ageing.

Press “Load” and import the interested “.rpt” files.

The file below is obtained:

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”.

Example of the test report:

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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).

Select Analytics/Estimated shelf life.

Press “Load” and import the interested “.rpt” files.

The file below is obtained:

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).

NOTE: it is possible to estimate the IP at the storage temperature if the R2 is ≥


0.9.

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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)

3.4.1 Test report for single analysis


Highlight a row and select Report/Create single
The test report shows the following information:
- laboratory information (including the company logo);
- software version;
- operator name
- serial number of the instrument;
- the results of the selected row;
- the graph.

NOTE: the test report is an open file and can be modified.

A single test report example below:

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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.

NOTE: the test report is an open file and can be modified.


NOTE: It is possible to create a comparison test report with maximum 20
analyses.

A test report for multiple analyses example below:

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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.

Menu Submenu Description

File New Create a new database and “Laboratory information” file


Open Load an already existing database.
Save Save changes made to an analysis database (including
“Laboratory information” file). If the file name does not exist
it can be entered.
Save as Save an analysis database (including “Laboratory
information” file) assigning a file name. If the file name
already exists, it can be overwritten.
Laboratory Enter the details of the laboratory concerned. These
information information will be included in the test report
Exit Exit from the program and return to the desktop.
Report Create Single Create a single report with the graph of the selected row.
Create Create a test report with the data and the curve of the
comparison selected rows in the same graph and perform automatically
the calculation of the IP average and standard deviation.
Minimum 2 rows must be selected.
Export data Excel Export data of the selected rows to an .xls file
Export dataExport data of the selected rows to a .txt file
TEXT
Export data LIMS Export data of the selected rows to a .csv file
Modify Filter Create database filters and apply them on the current
database
Order View the columns selected in decreasing or increasing
order
Adapt Adapt the width of the column/s selected
Standard column Reset the order of the database columns to the default
setting
Configure Configure the sequence of the database columns,
show/hide columns
Remove Remove one or more rows from the database definitively
Select all Select all the rows of the database containing a value
System Work conditions View and set the working temperature of the OXITEST
connected. Enable/Disable the graph of the temperature
during the analysis.
Analysis View and set the pressure of the single chamber of the
conditions OXITEST connected, the sampling time and the maximum
analysis time.
PT100 Alignment For VELP or authorized technical staff only.
Temperature For VELP or authorized technical staff only.
Adjustment
Temperature For VELP or authorized technical staff only.
Calibration
Offset pressure Set the current pressure as 0 bar (relative pressure)
Language View and set the language. Standard language is English.
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Analytics Methods Display, modify, create or delete analytical methods.
Repeatability test Create an archive of repeatability tests. The created files
format is .rpt
Freshness test Create an archive of freshness test comparison. Different
lot numbers of the same sample are compared with the
reference lot number to determine the product freshness.
The created files format is .frs.
Formulas Create an archive of same samples produced with different
comparison formulas to identify the best formula. The created files
format is .fcm.
Packaging Create an archive of same samples storage in different
comparison packaging to identify the best packaging. The created files
format is .pcm.
IP during ageing Same samples are analyzed at different times to fix the
linear equation and the decreasing of the Induction period
with the going by of the time. The created files format is
.ida.
Estimated shelfSame samples are analyzed at different temperature to fix
life the linear equation and estimate the shelf life at low
temperatures. The created files format is .shl.
Recalculate Recalculate the IP of the selected analysis with the
graphical method.
Service Find OXITEST Manual search for OXITEST to PC connection
Maintenance Shows the list of maintenance operations, the theoretical
life of the consumables and their consumption in terms of
number of analyses performed
Balances Shows the setting parameters for several brands of
balances and the connection port available
Acoustic signals Select which operations have to activate an acoustic signal
Logon Modify the software password and entry level
Control panel For VELP or authorized technical staff only.
Help Why to use Highlight on the advantages offered by the OXITEST
OXITEST
When to useSome analytical aspects for the analyses
OXITEST
How to use Explain the procedures in Analytics menu.
OXITEST
About OXITEST OXISoft information and VELP Scientifica contacts
Manual Instrument leaflet with general information
Routine Show the suggested daily operations
operations

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5. Indicators, warnings and blackouts
5.1 Indicators

5.1.1 – Heating LED


OXITEST is fitted with a heating LED on the front of the instrument that has the
following operating conditions:
- Intermittent, to indicate that the instrument is heating up to reach the
setpoint temperature;
- constantly lit, to indicate that the instrument reached the setpoint
temperature and is keeping it constant;
- off, to indicate that the heating is not enable.

NOTE: Keep the transparent shield closed during the analysis.


If the shield is raised during the work cycle, the test continues, but this may cause
temperature variation that could compromise the results.

5.1.2 – Pressurized oxidation chambers


If the “Work OXITEST” button is pressed, and the pressure inside the oxidation
chambers is above 0.5 bar, the following message appears on the screen:

In order to be able to proceed, it is necessary to discharge the oxidation


chambers by gently opening the discharge valves (knobs in line with the valve
bodies) and press the “Continue” button.

5.1.3 –Induction period not found


When the analysis is stopped for one of the reasons listed at chap. 3.1.5, the IP
column will show “NaN” and in the first column the red sign will appear. In this
case to obtain the data, it is possible to try to use the GM thanks to the recalculate
function.

5.1.4 – Removal of record


When “Remove” is pressed from the Modify menu or by using the mouse right
button, the software asks for the confirmation.

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5.2 Warnings
The instrument can display various types of warnings.

5.2.1 - Warnings relating to correct operation of the instrument:


A – PC - Oxitest connection status
If there is no PC-OXITEST connection, the parameters on the right part of the
main window become NC or NA. In this case, when the OXISoft is opened or
when the “Find OXITEST” function is used, the software will show:

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.

PC status OXI status Operations


ON when Open the OXISoft: it automatically searches the OXITESTs.
analysis is The software advises that some analyses are running. It is
OFF
in possible to decide if stop or continue them.
progress The OXITESTs remain in temperature.
ON when Open the OXISoft: it automatically searches the OXITESTs.
instrument The heating element of the OXITESTs are switched off and
is in work the units are in waiting status even if the WORK button
OFF
but not in remains pressed.
temperatu Press WORK button to turn it off: the rows selected will be
re unlocked.
Open the OXISoft: it automatically searches the OXITESTs.
ON when
The heating element of the OXITESTs are switched off and
instrument
the units are in waiting status even if the WORK button
is in work
OFF remains pressed.
and in
Press WORK button to turn it off: the rows selected will be
temperatu
stopped with the red sign. To start new analyses filling news
re.
rows is necessary.
ON when Open the OXISoft: it automatically searches the OXITESTs.
instrument The heating element of the OXITESTs are switched off and
is in work, the units are in waiting status even if the WORK button
temperatu remains pressed.
re and Press WORK button to turn it off: the rows selected will be
OFF
START stopped with the red sign. To start new analyses filling news
button has rows is necessary.
been
already
pressed.

B – Set temperature reached


At the end of a correct heating stage, if “START” button is pressed, the software
advises with an acoustic signal and the following message appears:

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.

7.1 Routine maintenance


Routine maintenance consists of the following operations.
Before each test
• Check that the sealing O-Ring between the oxidation chamber and the
cover always has a fine film of high temperature sealing grease
guaranteeing tightness and resistance over time.
• Check that the filters do not have traces of fat so as to avoid
contaminating the next test. In order to clean the filters, put them in
acetone for 24-48h.
• Check that the oxidation chambers, including the holes for filters
holders, have been thoroughly cleaned.
• Check that the covers, spacers and sample-holder containers do not
have any traces of sample.
Blank and leak test (after 10 analyses)

Analysis by analysis, some sample residues may remain on the OXITEST


elements (chambers, filters, spacers and sample-holder containers). This could
contaminate the following tests.

Performing a Blank test it is possible to check if the system is cleaned.

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.

The main reasons why a Blank test is not ok are:


- oxidation process caused by sample residues on the OXITEST elements
- leaks in the system

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):

Replacement of O-Rings (after 50 analyses)


The estimated life time of the O-Rings is 50 analyses. Once reached this value (or
if they are worn, damaged, no longer elastic) replace them.
Then, press the respective “Refresh” button in the Service/Maintenance menu.

Cleaning of filters (after 20 analyses)


Each reactor is fitted with 2 filters that are used to intercept any traces of sample.
It is suggested to clean the filters every 20 analyses or if, at the end of a test, they
are dirty or wet.
Clean them putting in acetone for 24 – 48 hours.

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

• Extraordinary maintenance operations not mentioned in this manual,


including operations on internal parts, must be carried out by personnel
expressly authorized by VELP Scientifica.
• All extraordinary maintenance operations must be carried out after
disconnecting the instrument from the power socket and from the gases.
• Given the risks resulting from high temperatures, let the oxidation
chambers cool down or use personal protection devices suitable for the
test temperature (normally 90°C).
• Below is a list of the extraordinary maintenance operations to be carried
out when necessary:

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.

7.3 Preparing instrument for transport


The transport of the instrument by shipping agents, couriers or other means must
be carried out using the original shockproof pack supplied with the instrument.
NOTE: It is important to empty the gases contained in the oxidation chambers
and clean the machine thoroughly, in order to prevent any sample residue being
deposited, during transport, in areas that are difficult to access.

NOTE: Remove the transparent covers to prevent damages.

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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.

9. Disposing of the unit


The instrument is classified as electrical/electronic apparatus and
must be disposed of accordingly. The unit is subject to waste
separation and cannot be disposed of as urban waste under EEC
directive 2002/96/CE. For more information please contact the relative
division of your local town council.

10. Spare parts


Description (see paragraph 1.2): Code
Sample-holder container 10001985
Spacer 10001984
O-Ring 10002033
Filter for oxidation chamber 10003631
The above-mentioned spares may easily be replaced by the operator.
For other spares (and the full list), please contact the nearest Velp technical
assistance center.

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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

Overall electrical power W 900


Dimensions (W x H x D) mm 365 x 190 x 485
Weight kg 16.5
Degree of pollution CEI Safety class 2
EN61010-1
Max. permitted moisture % Max 85
Storage temperature °C -10 ….+60
°F +14 …+140
Laboratory temperature °C +5 ..…+40
°F +41 …+104
Fuses A Code F30900248: 5
Code F30910248: 10
PC interface USB
PERFORMANCE
Stability of block °C ± 0,2
temperatures
Uniformity of block temp °C ±1
Precision of block temp °C ± 0,5
Precision of transducers bar ± 0,05
FUNCTIONS
Settable temperatures °C T amb.÷120
Settable pressures bar 0÷8 (relative)
Resolution of settable °C 1
temperature
Resolution of settable bar 1
pressure
Resolution of real °C 0.1
temperature
Resolution of real pressure Bar 0.01
Sampling time sec 1÷600
Set temp. reached Visual indicator
Test time calculation Visual indicator
Type of temperature probe Pt100 class A
Temperature probe range °C 10-145
Pressure transducer range bar 0,5÷10 relative
SAFETY DEVICES
Probe in short-circuit Visual indicator
Probe cut off Visual indicator
Outside temperature range Visual indicator
Reactors pressurized Visual indicator
PC connection off Visual indicator
Overtemperature On block with thermostat at 130°C with
automatic reset
Overpressure Safety valve with operation at 14bar +10%

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12. Wiring diagram

1 Inlet power supply


2 Lighted switch 22x30
3 Electronic board
4 Heating element
5 Safety thermostat 135°C
6 Reactor B solenoid valve
7 Reactor A solenoid valve
8 Pt100 probe
9 Heating LED
10 Reactor B pressure transducer
11 Reactor A pressure transducer

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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

N° Qty Material Diametro (mm) Lunghezza (cm)


1 1 PTFE 4x6 5,2
2 1 PTFE 4x6 47
3 1 PTFE 4x6 16
4 1 STAINLESS STEEL 1/8’’ 26
5 1 STAINLESS STEEL 1/8’’ 26

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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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10003023/C7
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

Follow the suggestions below for sample preparation:


- homogenize accurately the sample using a suitable device;
- solid samples often require a preliminary grinding procedure (example: grain);
sometimes the oxidation flex is visible also performing the test on the whole product
(example: dry animal feed as pellets);
- For liquid or doughy samples, an accurately mixing it is enough;
- distribute homogeneously the sample test portion on the entire sample-holder
containers surface;
- split the sample test portion in equal parts among the sample-holder containers in
use
- when necessary (see chapter “Methods”), place the required spacers on the
chamber base. Then, place the sample-holder containers with the sample test
portion.

6 sample-holder containers and 4 spacers are supplied with the instrument.

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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10003023/C7
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: samples have to be stored in a dark environment at low temperature, until


tested. They have to be also protected from air and stored in inert materials (glass or
plastic material, perfectly clean), without head space or extremely reduced one.
The tools used to take the sample test portion don’t have to be exposed to conditions
able to promote its oxidation, such as high temperature, oxygen, light, metals, before its
storage.

15.2 The temperature


The best and the most commonly used temperature for the oxidation test with the
OXITEST is 90 °C. This temperature allows to obtain the sample Induction Period within
a reasonable short time avoiding collateral phenomena or reactions which could
negatively interfere on the results.

NOTE: increasing the work temperature, the Induction Period will decrease.

Anyway in bibliography it is generally suggested not to exceed 90°C to carry on the


accelerated oxidation tests.
As mentioned before, for the most common food samples, 90 °C is the best temperature
for this purpose too. To analyze some kind of products (like meat-based pasta sauces,
with an high sugar content) it is suggested to work at a lower temperature (80 °C).

15.3 Oxygen pressure

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.

15.4 End of a test


When a test is running, the pressure trend is displayed on the graph.
Analyzing samples, the pressure trend should be similar to the one in the following
picture.

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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10003023/C7
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)

F Place the covers and tighten the screws thoroughly

G Leave the discharge valves open (knobs in line with valve bodies)

H Place the upper insulating panel to cover the chambers

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

Set the pressure, sampling time, and max analysis time in


M
System/Analysis Conditions

N Select the database rows to be analyzed

O Press “Work OXITEST n” to heat-up the chambers

P Press the green key to start the analysis

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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10003023/C7
Methods
Oxidative stability test on pasta sauces (Genoa-style pesto,
Bolognese ragout, Amatrice-style sauce)

Sample preparation
Mix accurately the pack content.

Sample test portion


Take 90 g of product and distribute it homogeneously on 3 sample-holder containers
(30 g each).
For meat-based sauces (eg. Bolognese ragout) or those with very high fat content
(eg. Genoa-style pesto), take 30 g and distribute it homogeneously on 1 sample-
holder container.

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.

Set 90 °C (or 80 °C in case of meat-based sauces in order to avoid burning the


sample) as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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10003023/C7
Oxidation stability test on salami

Sample preparation
Grind by a suitable device the pack content. Mix accurately the ground
sample.

Sample test portion


Take 30 g of product and distribute it homogeneously on 1 sample-holder
container.

Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder
container on the top.

Set 90 °C (or 80 °C in case of meat-based sauces in order to avoid burning


the sample) as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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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.

Sample test portion


Take 10 g (5 g for Macadamia nuts) of product and distribute it homogeneously on 1
sample-holder container.

Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container on
the top.

Set 90 °C (or 80 °C in case of meat-based sauces in order to avoid burning the


sample) as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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10003023/C7
Oxidation stability test on sauces (mayonnaise, cocktail
sauce)

Sample preparation
Mix accurately the pack content.

Sample test portion


Take 10 g of product and distribute it homogeneously on 1 sample-holder
container.

Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder
container on the top.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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Oxidation stability test on chips
Sample preparation
Grind by a suitable device the pack content. Mix accurately the ground sample.

Sample test portion


Take 30 g of product and distribute it homogeneously on 3 sample-holder containers
(10 g each).

Analysis setup
Load the sample-holder containers into the chamber.

Set 90 °C (or 80 °C in case of meat-based sauces in order to avoid burning the


sample) as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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10003023/C7
Oxidation stability test on milk powder
Sample preparation
Mix accurately the pack content.

Sample test portion


Take 20 g of product and distribute it homogeneously on 1 sample-holder
container.

Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container
on the top.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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10003023/C7
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

Sample test portion


- Spreadable soft cheese: take 60 g of product and distribute it homogeneously on
3 sample-holder containers (20 g each).
- Grated cheese: take 45 g of product and distribute it homogeneously on 3
sample-holder containers (15 g each).
- Hard and semi-hard cheese: 45 g of product and distribute it homogeneously on
3 sample-holder containers (15 g each).

Analysis setup
Load the sample-holder containers into the chamber.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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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.

Sample test portion


Take 45-60 g of product (depending on its density, in order to fill up completely
the sample-holder containers) and distribute it homogeneously on 3 sample-
holder containers (10 g each).

Analysis setup
Load the sample-holder containers into the chamber.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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10003023/C7
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.

Sample test portion


Take 30 g of product and distribute it homogeneously on 3 sample-holder
containers (10 g each).
Increase the sample portion if 30 g aren’t enough to fill up the sample-holder
containers.

Analysis setup
Load the sample-holder containers into the chamber.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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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.

Sample test portion


Take 5-10 g of product and distribute it homogeneously on 1 sample-holder
container.

NOTE: After drawing the sample amount to be analyzed it’s recommended to


reduce as much as possible, or completely eliminate, the head space created
inside the oil packing (if the oil is contained in a bottle some marbles can be
introduced).

Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container
on the top.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report


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Oxidation stability test on fat (margarine, butter, lard)
Sample preparation
The oxidation stability test can be performed on the whole fat, without
preliminary operations.

Sample test portion


Take 10 g of product and distribute it homogeneously on 1 sample-holder
container, 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.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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10003023/C7
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.

Sample test portion


Take 50g (if sample contains about 6% fat) of product and distribute it
homogeneously on 2 sample-holder containers (25 g each).

Analysis setup
Place 1 spacer on the chamber base and then load the sample-holder containers
on the top.

Set 90 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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10003023/C7
Oxidation stability test on bio-diesel (FAME, Fatty Acids Methyl
Esters)
Sample preparation
Mix accurately the pack content.

Sample test portion


Take 5 g of product and distribute it homogeneously on 1 sample-holder
container.

Analysis setup
Place 2 spacers on the chamber base and then load the sample-holder container
on the top.

Set 110 °C as analysis temperature in System/Work Conditions.

Set 6 bar as analysis pressure in System/Analysis Conditions.

Example of Test Report

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Declaration of conformity
We the manufacturer Velp Scientifica srl
address Via Stazione, 16
20865 USMATE (MB)
Italy

under our responsibility declare that the product is manufactured in conformity


with the following standards:

EN 61010-1 Safety requirements for electrical equipment for


measurement, control, and laboratory use
Part 1: General requirements
EN 61010-2-010 Particular requirements for laboratory equipment for
the heating of material
EN 61326-1 Electrical equipment for measurement, control and
laboratory use - EMC requirements -
Part 1: General requirements

and satisfies the essential requirements of the following directives:

2006/42/EC Machinery directive


2014/30/EU Electromagnetic compatibility directive
2015/863/EU (RoHS III) Restriction of the use of certain hazardous substances
2012/19/EU (WEEE) Waste of electric and electronic equipment

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10003023/C7
Declaration of conformity
We the manufacturer Velp Scientifica srl
address Via Stazione, 16
20865 USMATE (MB)
Italy

under our responsibility declare that the product is manufactured in conformity


with the following regulations:

S.I. 2016/1101 Electrical Equipment (Safety) Regulations 2016


S.I. 2016/1091 Electromagnetic Compatibility Regulations 2016

according to the relevant designated standards:

EN 61010-1 Safety requirements for electrical equipment for


measurement, control, and laboratory use
Part 1: General requirements
EN 61010-2-010 Particular requirements for laboratory equipment for the
heating of material
EN 61326-1 Electrical equipment for measurement, control and
laboratory use - EMC requirements -
Part 1: General requirements

and satisfies the essential requirements of regulations:

S.I. 2008/1597 Supply of Machinery (Safety) Regulations 2008


S.I. 2012/3032 Restriction of the Use of Certain Hazardous Substances
in Electrical and Electronic Equipment Regulations 2012
S.I. 2013/3113 Waste Electrical and Electronic Equipment Regulations
2013

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10003023/C7
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.

Our product Lines:

Analytical instruments
Elemental Analyzers
Digestion Units
Distillation Units
Solvent Extractors
Fiber Analyzers
Dietary Fiber Analyzers
Oxidation Stability Reactor
Consumables

Laboratory Equipment
Magnetic Stirrers
Heating Magnetic Stirrers
Heating Plates
Overhead stirrers
Vortex mixers
Homogenizers
COD Thermoreactors
BOD and Respirometers
Cooled Incubators
Flocculators
Overhead Shakers
Turbidimeter
Radiation Detector
Open Circulating Baths
Pumps

www.velp.com
VELP Scientifica Srl
20865 Usmate (MB) ITALY
Via Stazione, 16
Tel. +39 039 62 88 11
Fax. +39 039 62 88 120

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