VELP SER 158 Operating Manual
VELP SER 158 Operating Manual
Solvent AutoExtractor
Operating manual
Velp Scientifica thanks you for choosing the SER158 Solvent AutoExtractor for the extraction of
solid or semisolid materials using solvents according to Randall technique. The Velp extraction
apparatus uses a two-principal stage procedure (Immersion and Washing) and three accessory
stages (Removing, Recovery and Cooling) drastically reducing the extraction time and solvent
consumption.
Safety warnings:
Before using the unit, please read the operating manual supplied with the apparatus
carefully.
SAFETY PRECAUTIONS
In order to prevent the risk of electric shock, fire and personal injury when the unit is in use,
basic safety measures must always be taken including:
• It is the responsibility of the user, to properly decontaminate the unit in case of hazardous
substances remaining on the surface or interior of the device. Non-reactant
decontaminating substances are recommended for use when cleaning, to avoid chemical
reaction with the material(s) contained therein. If in doubt about the compatibility of a
cleaning or decontamination product, contact the manufacturer or distributor
• Keep all electrical cords, cables and wires away from liquids.
• Ensure that the power supply corresponds to the rating plate on the rear of the unit.
• Use only power cables provided with three terminals that is wired to ground.
• If unit is not operating properly do not use. In case of any malfunction, contact your
nearest service center
• All Personal Protective Equipment [PPE] used must be compatible with possible risks
posed by the operation of the unit (i.e. glass of the containers) and the
materials/substances being processed
• For additional information on the handling of the solvents used, see chapter
"Recommendations for the use of organic solvents."
• Follow the instructions of maintenance of the instrument as described in this manual.
• During operation not bringing any flame or electrical equipment that could ignite the
substances being processed.
• The heating plate can reach the temperature of 380°C, this occurs during the cycle phase
but also during the cooling phase. In case of need to use appropriate protections.
• Both the product and the containers used in processing, must be compatible with the
temperature set on the instrument
10006905/B2 1
• Use the table in this manual, which provides for all types of solvent heat level to be set.
• Do not use the instrument in locations that require explosion protection or overpressure
conditions.
• Do not use the instrument with solvents other than those specified in this manual or with
an amount more than is allowed (max. 200 ml).
• Do not use samples that combust, or become flammable as a result of shock friction,
heat, sparks etc.… explode
• Use only original Velp extraction glassware.
• To clean the instrument using a cloth dampened with water.
The safety of the instrument is no longer guaranteed in the case of improper use or if the
instructions in this manual are not followed.
RÈGLES DE SÉCURITÉ
Pour éviter tout risque de choc électrique, incendie ou blessure corporelle pendant l'utilisation
de l'appareil, toujours appliquer les mesures de sécurité de base, y compris les
recommandations suivantes :
10006905/B2
This unit has been designed and produced in compliance with the following standards:
Safety requirements for electrical apparatus for
measurement and control and for laboratory use IEC/EN 61010-1
IEC/EN 61010-2-010
IEC/EN 61010-2-081
UL Std. 61010-1 2nd Ed.
CAN/CSA 61010-1-04 2nd Ed.
CAN/CSA 61010-2-010-04
CAN/CSA 61010-2-081
The manufacturer is committed to constantly improving the quality of the products and reserves
the right to modify the characteristics without prior notice.
10006905/B2
CONTENTS
1. Introduction ....................................................................................... 7
1.1 Parts included .......................................................................... 8
1.2 Instrument description ............................................................ 10
2. Chemicals .................................................................................. 12
2.1 Recommendation for the use of organic solvent ................... 12
2.2 Emptying the solvent tank ...................................................... 12
2.3 Reuse of solvent .................................................................... 13
2.4 Change the solvent ................................................................ 13
3. Assembly and installation ............................................................... 13
3.1 Hydraulic connection .............................................................. 13
3.1.1 Tap water connection ......................................................... 13
3.1.2 Solvent tubes connection ................................................... 14
3.2 Connection to electric power supply ...................................... 15
3.3 ControlPad Connection .......................................................... 15
3.4 Connection to external devices .............................................. 15
3.4.1 USB Pen drive ................................................................... 15
3.4.2 Mouse ................................................................................ 15
3.4.3 PC ...................................................................................... 15
3.4.4 Balances ............................................................................ 17
3.4.5 Barcode scanner with USB socket .................................... 17
3.5 Connection to “Slave” Extractors ........................................... 17
3.6 VELP Ermes Configuration .................................................... 18
3.7 Choice the temperature level ................................................. 19
3.7.1 Solvent flash point .............................................................. 22
3.8 Choice of gaskets .................................................................. 22
3.9 Preliminary Operations .......................................................... 23
4. Using the menus ............................................................................. 24
4.1 Quick Guide ........................................................................... 24
4.2 Main menu ............................................................................. 25
4.3 Analysis .................................................................................. 26
4.3.1 Fill the analysis parameters ............................................... 26
4.3.2 Fill the weight with balance ................................................ 27
4.3.3 Use of the barcode reader ................................................. 28
4.3.4 Start the analysis ............................................................... 28
4.3.5 Loading solvent .................................................................. 29
4.4 Archive ................................................................................... 30
4.5 Methods ................................................................................. 31
4.5.1 Standard Methods (from 1 to 49) ....................................... 31
4.5.2 Custom methods (50 to 79) ............................................... 32
4.5.3 Favorites methods ............................................................. 35
4.6 Results ................................................................................... 35
4.7 Check up ................................................................................ 36
4.7.1 Lift ...................................................................................... 36
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4.7.2 LEDs .................................................................................. 36
4.7.3 Heating plates .................................................................... 37
4.7.4 Cooling water ..................................................................... 37
4.7.5 Safety guard ...................................................................... 37
4.7.6 Recovery tank .................................................................... 38
4.7.7 Fill solvent tubes ................................................................ 38
4.8 Set up .................................................................................... 38
4.9 Service ................................................................................... 39
4.10 Guide ..................................................................................... 39
5. Operating Controls ......................................................................... 40
5.1 Safety devices ....................................................................... 40
5.2 Warning signals and messages ............................................. 40
6. Working cycle ................................................................................. 41
6.1 Calculation of the results ....................................................... 42
6.2 Randall system ...................................................................... 43
7. End-of-work operations .................................................................. 44
8. Maintenance ................................................................................... 44
8.1 Routine maintenance ............................................................. 44
8.2 Extraordinary maintenance .................................................... 45
8.3 Expedients for transport ........................................................ 46
9. Disposing of the unit ....................................................................... 46
10. Accessories ............................................................................... 47
11. Spare parts ................................................................................ 48
12. Technical features ..................................................................... 49
13. Wiring diagram ........................................................................... 51
14. Hydraulic scheme ...................................................................... 54
15. Warranty .................................................................................... 58
16. Suggestions ............................................................................... 58
ANALYTICAL METHOD ........................................................................ 60
1 Determination of crude fat in meat and processed meat........... 60
2 Determination of total fat in meat and processed meat ............. 61
3 Determination of total fat in fish and derived products .............. 62
4 Determination of total fat in whole eggs .................................... 63
5 Determination of total fat in oily seeds and nuts ........................ 64
6 Determination of total fat in milk powder ................................... 65
7 Determination of total fat in condensed milk ............................. 66
8 Determination of total fat in cheese ........................................... 67
9 Determination of total fat in flour, bakery products and pasta ... 68
10 Determination of crude fat in fried potatoes .............................. 69
11 Determination of crude fat in animal feed .................................. 70
12 Determination of total fat in animal feed .................................... 71
13 Determination of crude fat in creams and sauces ..................... 72
14 Determination of crude fat in chocolate ..................................... 73
15 Extraction of oil and grease from wastewater ........................... 74
16 Extraction of oil and grease from sludges ................................. 76
17 Extraction of petroleum source rocks ........................................ 78
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18 Extraction of plasticizer mixture from vinyl chloride plastics ...... 80
19 Extraction of rosin from paper and paperboard ......................... 81
20 Extraction of oils from leather .................................................... 82
21 Determination of unsaponified and unsaponifiable fat in soaps 83
22 Extraction of ethanol soluble components from detergent
formulations ........................................................................................ 85
23 Extraction of finishing oils from textiles and synthetic or natural
fibers ................................................................................................... 87
24 Extraction of oil content in insulating material............................ 89
25 Extraction of organic micro-pollutants for GC-MS analysis ....... 90
26 Extraction of oil and grease from plastic .................................... 91
27 Extraction of crude fat in Standard (Cod. A00000318) .............. 92
Declaration of conformity ........................................................... 93
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1. Introduction
Extraction of an organic solvent in most cases, allows the quantitative separation of a
substance or group of substances (e.g. Fat) from a mixture of solids or semisolids.
The most widely used technique, all over the world, takes name from German
chemist Franz Soxhlet (1848-1927) professor of chemistry at the High School of
Agriculture of Munich (Bayern). This technique puts in contact a pure solvent, by
distillation, with the mixture to extract. In the case of solid or semi-solid mixtures, the
sample is contained in a porous cellulose or fiberglass extraction thimble that is
covered by the pure solvent dripping from a reflux condenser above. From time to
time the solvent with the extracted substances is reported in the extraction cup by
means of the trigger of an automatic siphon. The thimble holds the porous portion of
the mixture that is insoluble in the solvent. The extracted substance must not be
volatile at the boiling temperature of the solvent. The Soxhlet extraction apparatus
has been modified in different aspects, in some cases in an attempt to increase the
temperature of the solvent that comes into contact with the mixture to be extracted, in
order to reduce the extraction time. The Velp extraction apparatus uses a five-stage
procedure:
In the first step (Immersion), the thimble containing the sample to be extracted is
immersed directly into the boiling solvent contained in the extraction cup; after a set
time, a part of the solvent is automatically removed from the extraction cup
(Removing), and the remaining solvent will fall by condensing the refrigerant in the
overlying (Washing). At the end of the extraction all the residual solvent is
automatically removed from the extraction cup (Recovery). Subsequently, the
glasses of extraction are raised for the final cooling (Cooling).
This procedure named Randall, reduces the time required for a complete extraction
from 1/4 to 1/6 of that required by a classical Soxhlet analysis.
The fields of application include analysis of food, feed, detergents, rubber and plastic
formulations, pharmaceutical products, soils, etc. for the content of soluble products
such as fats, surfactants, plasticizers, pesticides.
The Velp apparatus allows the use of many different solvents, a large part of which is
recovered at the end of the extraction cycle, minimizing the contribution to air
pollution. Velp equipment is manufactured according to the safety standards IP41
which allows use without risk.
For most of the samples of food or feed for animals, before extraction with solvent, it
requires acid or base hydrolysis.
The preliminary hydrolysis may be carried out with the unit of hydrolysis HU 6 that
allows the simultaneous hydrolysis of up to 6 samples.
The purpose of hydrolysis, is preliminary to release the fat in the sample that could
be linked to other molecules or enclosed in cellular structures, making them fully
available to the subsequent extraction.
At the end of the hydrolysis with HU 6, the sample is located in a glass crucible which
can be directly inserted in the drive SER158 for the determination of total fat.
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1.1 Parts included
Check that the unit is complete after unpacking.
The table below shows the parts included:
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T shaped key 5 mm 10006916 1
* The gaskets and extraction thimbles are considered consumables and they must be
replaced when necessary according to the solvents used and the cumbersome work.
** In addition to the seals already installed
NOTE: The Control Pad, code A00000286 is not included into the packaging of the
instrument. It is delivered in a dedicated box.
NOTE: Keep the special shock-resistant packing material for future use.
10006905/B2 9
1.2 Instrument description
2
11
10
5
8
7 4
6
3
1 Control Pad
2 Extraction Unit
3 General switch
4 Extraction cup
5 Extraction thimbles
6 Display touch screen
7 Handle
8 Ceramic heating plate
9 Safety guard
10 Collection funnel solvent
11 Titanium condenser
10006905/B2 10
The extraction unit is equipped with innovative devices, materials and cutting-edge
technology:
• The stainless-steel structure and the particular surface treatment, which is fitted
to the extractor, guarantees a high chemical resistance to the solvents used
during the analysis and high durability.
• Glass ceramic heating plate, for easy and fast cleaning
• Independent 6 or 3 heating positions with automatic shut off at the end of
analysis.
• Titanium condenser to maximize efficiency and reduce consumption of solvent
and water.
• Ability to connect a dispenser for automatic dispense of the solvent within each
glass.
• In a world where the respect for the environment is increasingly important, the
Titanium condenser provides a significant contribution to this cause. The cooling
water supply is automatically stopped during pauses, thus cutting consumption
considerably.
The SER158 series guarantees unmatched savings whist ensuring an extremely high
level of reliability.
Energy: Cooling water consumption starting from only 1 l/min; excellent insulation of
internal parts.
Space: The extremely compact footprint saves useful laboratory bench space.
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2. Chemicals
WARNING!
The heating plate and the extraction cup for the collection of the extract may reach a
high temperature which can generate burns. Use pliers to remove the collecting
vessels at the end of the extraction and recovery of the solvent.
The stock of organic solvents in the laboratory should be kept to a minimum; solvents
not in use should be stored in metal cabinets provided with holes, outside of the
laboratory. Whenever possible, it is recommended to avoid the use of volatile
solvents. If they can be replaced by less volatile counterparts (i.e. toluene instead of
benzene, heptane instead of pentane). Remember that when handling ethers,
unsaturated hydrocarbons, aldehydes and ketones, form peroxides, these
substances may give rise to explosions, by distillation, friction and also energetic
agitation. Monitoring for the presence of peroxides can be performed with test kits
easy to use.
The destruction of peroxides is not always easy because in most cases will form two
phases with the aqueous solutions that do not allow contact between the polymeric
peroxides and reducing agents used.
The destruction of peroxides is not always easy because in most cases will form two
phases with the aqueous solutions that do not allow contact between the polymeric
peroxides and reducing agents used.
10006905/B2 12
2.3 Reuse of solvent
It’s possible to reuse the recovered solvent for gravimetric determinations (i.e. fat
quantification), but it’s suggested to use fresh solvent for qualitative analysis (i.e.
chromatography analyses).
NOTE: It is not recommended to reuse the solvent recovered from the first analysis,
after installation or when the solvent has to be changed, because of a possible
mixing.
NOTE: It is necessary to use the instrument under a fume hood Laboratory only in
presence of chloroform or diethyl ether that are used as solvents.
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The instrument requires a minimum tap water flow rate measured at the discharge of
the instrument (depending on the temperature of the tap water) of approximately:
NOTE: the inlet solvent connection has to be done when the extraction unit is
connected to a dispenser for adding the solvent directly in the beakers without
entering in contact with the solvent. It is possible to load the solvent in different ways
(see chap. 4.3.4)
NOTE: All dispenser types can be connected to the SER. The important feature is
the tube connected to the dispenser must have the features of one of the two fittings
in the table above.
NOTE: Connect the dispenser to the SER 158 before starting the procedure from the
ControlPad, in order to avoid drips.
10006905/B2 14
The maximum pressure insertion solvent is 0.05 MPa (0,5 bar)
NOTE: The switch allows to completely disconnect the device from the power supply
when not in use, in order to reduce energy consumption.
3.4.2 Mouse
A mouse with USB plug can be connected to one of the two USB ports on the
SER158 or on the ControlPad to navigate the menus.
3.4.3 PC
Connect the unit to the LAN port on the right of the SER158 in order to access the
instrument database from remote PC.
10006905/B2 15
- Go to the “Set up”/”Connectivity”/PC connection
NOTE: After the first configuration is advisable to restart the instrument after entering
the IP address and the Subnet Mask.
The database file is continually updated as data is saved in the instrument Archive.
To update the information on the PC, repeat the steps described above.
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3.4.4 Balances
The SER158 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.
The SER158 can be connected to the following balances with a resolution in grams
of 2 to 4 digits after the decimal point:
- Mettler
- Bel
- AND
- Sartorius
- Ohaus
- Precisa
- Gibertini
It is necessary to use the USB port of the instrument with the adaptor code
A00000195 (optional accessory) and enable the balance in "Set up" / "Connectivity" /
"Balance".
NOTE: The balance connected to the SER must be set with the default parameters
mentioned above. Read its operating manual to do this.
NOTE: Set the balance in “print” mode. Balance has to print only the weight, not the
other info. Please see its operating manual to do this.
NOTE: for each “Slave” unit, one connection cable (A00000287 – Slave connection
cable SER158) is required.
10006905/B2 17
After connecting the ControlPad to the “Master” unit, as descripted in the chapter 3.3,
connect the “Slave” extractors by inserting the connection cable in the dedicated
ports marked as “Extra units”, positioned on the back of the instruments.
Turn on all the available “Slave” units and then turn on the “Master” extractor.
NOTE: it is always necessary to turn on the “Slave” units before turning on the
“Master” extractor.
Furthermore, the software will enable the buttons that allow to control independently
all the connected extractors in the lower grey bar showed in each submenu.
10006905/B2 18
To be able to communicate, the laboratory LAN needs to have the possibility to
access on internet. In order to activate the communication between SER158
and ERMES platform, is necessary perform the following steps:
• Connect the LAN cable to the SER158, using the LAN port on unit.
• Configure the SER158 with laboratory LAN parameter (see chap.
3.4.3). If necessary contact your IT administrator.
• Select in connectivity the ERMES menu.
• Check the box “Enable SER158 to transmit on the ERMES platform;
• Keep open this menu (OTC) and Proceed with the product registration
from the ERMES platform. For more information, see FAQ on VELP
website.
NOTE: the boiling stones must be weighed in advance together with the glass
extraction cup for the determination of the initial tare.
The following table shows the levels of heating for each solvent, gaskets suggested
and in which cases use the boiling stones:
10006905/B2 19
You can use other types of solvents or mixtures, it is important to know the boiling
point or establish this in the case of mixtures; it is suggested to start from the info in
the table above to find the solvent with a boiling point more similar and to choose the
level of heating correctly.
NOTE: the instrument comes with butyl and Viton gaskets. The vaflon gaskets, code
A00000288, are optional accessories.
NOTE: Vaflon gaskets have an excellent chemical compatibility so they can be used
with all types of solvents or mixture.
10006905/B2 20
Commonly used solvents listed in order of increasing boiling point.
SPECIFIC HEAT OF
mm of Hg a 25°C
SPECIFIC HEAT
TEMPERATURE
TEMPERATURE
EVAPORATION
FLASH POINT °C
IGNITION °C
g/ml at 20°C
PRESSURE
BOILING °C
SOLVENT
DENSITY
VAPORE
gcal/g/°C
gcal/g
Petroleum ether 30 ÷ 80 -40 >200°C 0,662 >400 ~0,500 ~80
Diethyl ether 34,6 -45 180 ÷ 190 0,713 442 0,473 84
Pentane 36,1 -40 (C) 309 0,626 420 0,507 85
Methylene chloride 39,7 - (605) (*) 1,325 340 0,288 60
Acetone 56,5 -18 538 0,788 180 0,538 123
Chloroform 61 ÷ 62 - (*) 1,484 100 0,234 59
Methyl alcohol 64,7 +12 470 0,791 95 0,601 263
Tetrahydrofuran 66 -17 321 0,889 200 0,486 105
n - Hexane 69 -40 234 0,660 155 0,600 80
Carbon 76,7 - (*) 1,594 90 0,200 46
Tetrachloride
Ethyl acetate 77 +7 427 0,902 71 0,476 102
Ethyl alcohol 78,8 +13 423 0,789 42 0,680 204
Methyl ethyl 79,6 -6 516 0,805 71 0,549 106
ketone
Benzene (1) 80,1 -11 562 0,879 76 0,419 104
Cyclohexane 80,7 -18 259 0,778 81 0,520 94
Acetonitrile 81,6 +13 523 0,787 83 0,541 174
Isopropyl alcohol 82,5 +12 456 0,785 32 0,640 159
Trichloroethylene 86,7 - (*) 1,465 60 0,223 57
n Heptane 98,4 -1 215 0,684 38 0,518 76
Isooctane 99,3 -12 250 0,692 11 0,563 71
Dioxane 101,1 +5 379 1,034 4 0,420 99
Isobutyl alcohol 108 +28 343 0,802 3 0,716 138
Toluene 110,6 +4 536 0,867 24 0,440 87
n-butyl alcohol 117 +37 343 0,810 13 0,687 141
Acetic acid 118 +39 427 1,050 11 0,522 97
Octane 125,6 +22 210 0,703 12 0,578 73
Alcohol Cinnamyl 138,1 +38 (C) 300 0,817 2 0,711 120
Xylene 138,5 +29 464 0,86 5 0,400 83
(*) not inflammable
(C) into a closed container
(1) Finally determined as carcinogenic
10006905/B2 21
3.7.1 Solvent flash point
The flash point temperature is the temperature at which a liquid gives off a quantity of
vapors sufficient to form an ignitable mixture with air near the surface of the liquid or
within the extraction cup.
There are two groups of devices for flash point determination. For the purposes of
official standards on transport (IIC, OG IATA) the flash point is determined by the
method Tagliabue Open Cup (ASTM D-1310/63) commonly abbreviated TOC. IATA
also admits the Abel or the Abel-Pensky in open cup.
Other methods used, mostly for the higher flash points, are the Tag closed cup and
the Cleveland open cup. The methods with open vessel reproduce better conditions.
NOTE: The Viton gaskets are assembled on the instrument. The butyl gaskets come
with the accessories of the instrument.
In general terms the Viton is easily attacked by ketones and esters, and the butyl
rubber by hydrocarbons and halogenated.
Before starting with the extraction, please check the compatibility of the gasket to the
solvent. (see table at page 17).
To replace the seals, use the item 10006916 (“Key for gasket”). Remove seals,
supplied with the instrument, in order not to damage the connection funnel solvent.
Block the seal with the key tool, then by fingers remove the gasket from the support.
NOTE: Do not use the key as a lever, to remove seals. This operation can damage
connection funnel solvent and cause leakage of solvent.
10006905/B2 22
3.9 Preliminary Operations
At the end of installation proceed as follows:
• Open the safety guard;
• Position the extraction cup;
• Turn on the tap water;
Turn the instrument on by pressing the main POWER switch (LED on), on the right of
the instrument. The instrument automatically carries out the following steps
simultaneously:
With the solvent that will be used for the analyses, perform an extraction without
sample and without thimble using the method “Washing” (see chap.4.5) in order to
wash the internal circuits.
At the end of the analysis, empty the recovery tank following the instruction at the
display (see chap 4.7.6.)
NOTE: before beginning the analysis, if the automatic loading solvent is set (see
chap 4.7.7) enter the Check-up/Fill solvent tubes menu in order to fill the tubes
NOTE: It is suggested NOT to use the solvent recovered from the first wash down.
10006905/B2 23
4. Using the menus
4.1 Quick Guide
This page shows the heating block software. The purpose is to help the user identify
the different possibilities offered by the instrument and how to reach them easily.
Analysis
Archive Options Export Excel
Cancel Text
Select all Lims
Recalculate
Filters by sample name
by operator
Methods Standard by date
Customizable by ID
Favorites by type
by serial number
Results Calculate
Check-up Lift
Leds
Heating plates
Cooling water
Safety guard
Recovery tank
Fill solvent tubes
Set-up Date and time
Language
Connectivity PC Connection
Balance
Extractors
Barcode Scanner
Guide
10006905/B2 24
4.2 Main menu
When the instrument is switched on, the display shows the logo VELP SCIENTIFICA
for a few seconds.
The main menu then appears:
The main menu consists of 8 submenus that can be selected using the touch screen
or the pointer of the mouse (see chap. 3.4.2)
The blue bar at the top of the main screen shows information as:
- name of the instrument
- account
- date and time
and some setting if on, as (from the left to the right side):
- solvent loading
- end recovery step
- balance connected
Located under each sub-menu, the following grey bar becomes present, displaying
the two symbols below: In the bottom left corner, the “Home” symbol allows the
return to the main screen; the “Question Mark” symbol in the bottom right corner,
allows the opening the operating manual
10006905/B2 25
4.3 Analysis
Select "Analysis" from the main menu:
To return to the main menu press the symbol in the bottom left corner (home).
NOTE: All positions are selected as default. The correspondent LEDs are switched
on.
10006905/B2 26
NOTE: If SER 158/6 is used, start analysis selecting at least 4 positions. If SER
158/3 is used, start analysis selecting at least 1 position.
NOTE: If the balance is connected, please see chap 4.3.2
NOTE: If you want to enter the identification code of the extraction cup using the
barcode reader, refer to paragraph 4.3.3
NOTE: if more than one SER158 is connected to the ControlPad (slave units)
pressing SER2, SER3, SER4 it is possible to set the same parameters for each unit.
NOTE: Blank is a real analysis but without the sample, necessary to check the
cleaning of the instrument to avoid possible contaminations. This value is not used
for the final calculation of the extracted.
NOTE: Information in “Details” window is not mandatory, but they are necessary to
perform the final calculation. They are stored in the Archive and they can be
exported.
The weight is transferred in the same column sequentially, starting from the selected
position. To change the column, it is necessary press the “Continue” button.
10006905/B2 27
If it is necessary to modify the weight, the old weight will be displayed and it is
possible to overwrite it.
It is possible to scan the first extraction cup, weigh it and transfer the tare value from
the balance to SER158. This operation is repeated sequentially for the remaining
positions. In addition, the Velp barcode reader can also be used to fill in the field for
the Sample Name.
The barcode reader can also be used to calculate the results by selecting the
appropriate extraction cups in the results menu.
Press START to start the analysis. Press “Analysis set up” to come back to the
“Analysis set up” window.
10006905/B2 28
NOTE: if more than one SER158 is connected to the ControlPad, pressing SER2,
SER3, SER4 it is possible to start the analysis for each SER in different times.
NOTE: if automatic loading solvent is set, please see chap 4.3.4
The current step is highlighted/indicated in blue and underlined with the relative ETA
as a count down. Also, the total ETA changes. The instrument will automatically
perform all of the selected steps, until the end of the analysis.
During the first 4 step, press STOP to end the analysis. The display will ask
confirmation. Pressing YES, the instrument will perform the Cooling step (the green
bar will become orange) and after will ask if the analysis must to be saved in the
archive.
NOTE: It is possible to skip steps and go straight to the step require by keeping the
step required pressed for 2 seconds.
NOTE: With the slave unit, during analysis, it is possible to navigate in the menu of
the other software and start in different analysis. In this case the blue bar will become
green. To come back into the analysis in progress, press on the green bar.
10006905/B2 29
Follow the instructions reported in the window above to proceed with the solvent
loading.
It is possible to choose the position where the solvent is loaded, among the positions
selected in “Analysis setup”, also not in sequence.
NOTE: see chap. 3.2.2 to perform the connection with the dispenser.
There is also the possibility to add solvent when the analysis is running using the
little hole on the top white flange of the titanium condenser.
NOTE: in case of adding solvent using the hole on the top white flange of the
titanium condenser, use small tube wit OD 2.5mm.
NOTE: when this procedure is used to empty the tubes, please take note that in the
tubes of SER158/3 remains 10ml of solvent, in a SER158/6 13 ml about.
The solvent volume for the analysis depends on the type of the beaker. Below the
min and max volume for each beaker and the suggested for the analysis:
Becker type Min volume (ml) Suggested volume (ml) Max volume (ml)
Small 70 80 110
Standard (glass or
90 100 150
aluminum)**
Large 110 170 200
** for qualitative analyses, it is suggested to use the glass beaker.
4.4 Archive
Select “Archive” from the main menu. The display shows the list of the analyses
performed with the whole SER (master and slave) connected to the ControlPad.
To return to the main menu press the “Back” button.
Use the scroll bar at the right of the display to view the other rows and the bottom bar
to visualize the other columns.
In the bottom part of the screen, some buttons are shown:
- Options:
10006905/B2 30
It is possible to:
- Export the whole archive or selected rows in Excel, Lims or Text format to the USB
pen drive, by pressing Export
-apply some filters on the archive, pressing Filters:
NOTE: if Superuser password is set, “Cancel” function doesn’t work in User level
4.5 Methods
Select “Methods” from the main menu.
Press Down button (next page) or Up button (previous page) to scroll through
standard methods listed.
Use the touch-screen to select the method required. The following window appears:
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Method name: Name of the method selected.
Official reference: reference to the official method.
Sample: indication about the weight of the sample to be used
Extraction cup: type of the extraction cups in terms of dimensions to be used
Thimbles: type of thimbles in terms of dimensions to be used
Solvent type: solvent to be used
Solvent (ml): volume of the solvent to be used
Gasket: type of the gasket to be used
Immersion: the time and the temperature level for the immersion step
Removing: the time and the temperature level for the removing step
Washing: the time and the temperature level for the washing step
Recovery: the time and the temperature level for the recovery step
Cooling: the time for the cooling step
Press Confirm to confirm the method selected and go directly to the "Analysis" menu
(see chapter 4.3).
Press Favorites to save this method in the Favorites method menu. (see chap. 4.5.3)
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Press Down button (next page) or Up button (previous page) to scroll through the 30
custom methods listed.
Use the touch-screen to select the method required and to set the fields listed in the
chap. 4.5.1:
- Method name: Name of the method (free field)
- Official reference: reference to the official method (free field)
- Sample: indication about the weight of the sample to be used
- Extraction cup: type of the extraction cup in terms of dimensions to be used. It is
possible to choose among:
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or to create a new one, pressing on “Custom” button. In this case it is necessary to
set solvent name and temperature level and correct gasket material:
NOTE: to choose the heating level for the new solvent, please see chap.3.6
- Solvent volume: volume of the solvent to be used
NOTE: the maximum set solvent volume is 200ml (with large extractions cup). It’s
possible to set and introduce solvent volume less than the minimum suggested just
to create custom methods for wash down with custom solvents.
- Gasket: type of the gasket to be used. It is possible to choose among:
NOTE: the temperature level for the different steps is just shown because it is
connected to the type of solvent.
Press Confirm to save the method and go to the "Analysis" menu (see chapter 4.3).
Press Save to save the method and remain in the same window.
Press Favorites to save this method in the Favorites method menu (see chap. 4.5.3).
NOTE: it is possible to create, save and modify the custom methods only in
Superuser level if Superuser password is set.
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4.5.3 Favorites methods
This menu contains the list of standard or customer methods chosen as favorites. To
remove the method from the list, press the button “Favorites” off.
4.6 Results
Select the menu “Results”. The display shows the rows of the archive still with no
results yet.
It is possible to select maximum 24 rows and press “Calculate”. Information about
type and sample name are copied in the table below:
After filling the “TOTAL” column manually or using a balance (see chap. 4.3.2 “Fill
the weight with balance”) with the final weight (tare + extract), press “CALCULATE”
in order to obtain the results in terms of EXTRACT (g) and EXTRACT (%).
If more than one row is filled, pressing Calculate, the results automatically appear in
term of Average, SD (standard deviation) and RSD (relative standard deviation) in
(g) and (%).
Pressing SAVE, the results are saved in the archive.
NOTE: It is possible also to overwrite previous results.
By pressing REPORT, the instrument creates a report directly onto the pen drive, if
connected to the SER, after filling the file name.
NOTE: it is possible to move into this menu also from the “Archive” menu. It is
always possible to recalculate final results by selecting the corresponding row(s) and
pressing “RECALCULATE”.
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4.7 Check up
Select the menu “Check-up” from the main menu.
4.7.1 Lift
It is possible to check the functionality of the lift: Press “START” to launch the
automatic procedure. At the end of the procedure, the instrument shows whether the
movement is correct or incorrect. In case of failure, please contact the service dept.
of VELP SCIENTIFICA S.r.l.
Press and hold the “UP” or “DOWN” button to move the lift manually up or down. It is
possible to check the lift of other units connected to the ControlPad by pressing on
SER2, SER3, SER4 if connected.
4.7.2 LEDs
It is possible to check the operation of the LEDs.
Pressing START, sequentially after each position (1-3 or 1-6), the LEDs are
switched on and then off and the correspondent positions becomes blue. During
the procedure, the button reading “START”, changes to read “STOP”. Press it to
stop the procedure.
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4.7.3 Heating plates
It is possible to check the operation of the heating elements.
By pressing “START”, the heating elements are switched on for 1 minute. After 1
minute, they are then switched off. The corresponding icon(s) become blue with red
flame. During this procedure, the START button then displays as “STOP.” By
pressing the STOP button, it is possible to end the procedure. At the end of the
procedure, the instrument shows whether the procedure is correct or incorrect. In
case of failure, please contact service dept. of VELP SCIENTIFICA S.r.l.
Press START to begin the procedure. If the procedure fails, check and ensure the
tap water is open and the flow is more than 1l/min. If the tap water is open, but the
check persists to fail, please contact the service dept. of VELP SCIENTIFICA S.r.l.
10006905/B2 37
4.7.6 Recovery tank
It is possible to empty the recovery tank from the solvent recovered during the
analysis. It is necessary to perform this at the end of each analysis or before starting
a new one. (see chap. 2.1.1)
Press the START button to start the procedure, after following the instructions
reported.
4.8 Set up
Select the menu “Set up” from the main menu.
It is possible:
-to set date and time (Date and time menu)
-to set the language (Language menu)
-to connect some external devices (Connectivity menu, see chap. 3.4)
-to decide to load the solvent automatically or in manual way (Analysis
options/Solvent loading menu)
- to decide the end of recovery step (Analysis options/End recovery menu).
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-LFU: last finish up: the extraction ends when the last extraction cup is dried
NOTE: in case of LFU set, the heating elements of the positions that step by step
become dried are switched off. This avoids burning the extract.
NOTE: The presence of the solvent, in any single extraction cup, is only detectable
during the first three steps of analysis. If an extraction cup becomes dried during any
of the three analysis steps, the corresponding heating element is switched off and
the software advises with a message.
CREDENTIALS: The account “USER” is the default access credential for the
software use. Every time the instrument is switched off and on, User Level is set. In
this level, it is possible to create or delete methods and data only if the
“SUPERUSER LEVEL” has not been previously recorded. (Superuser password
differs from default password “0000”)
NOTE: The Service level is for technician who performs the maintenance of the
instrument
4.9 Service
Select the menu “Service” from the main menu it is possible:
- to see the number of the analyses performed by each instrument, the movements
of the lift and the operating hours of the heating element (Counter menu).
- to see information about the software version (software information menu)
- to update the software using a pen drive (Update software menu)
- to empty the archive (Empty archive menu, not possible in User level)
- to create a diagnostic file, if a pen drive is connected (Diagnostic menu)
- to come back in the standard configuration of the instrument (Reset menu).
NOTE: Resetting the unit does not delete serial numbers, archive and counter
information.
4.10 Guide
Select Guide from the “Main” menu. The Guide contains the full operating manual.
10006905/B2 39
5. Operating Controls
5.1 Safety devices
The instrument is equipped with various safety devices that can prevent start-up or
interrupt a work-cycle to protect the operator and the instrument itself.
Safety guard:
If the safety guard in front of the extraction cups is not closed, analysis will not start
when START is pressed. An acoustic signal warns the operator of an error and the
following warning message appears on the display: "Close safety guard”
If the safety guard is opened during a work cycle an acoustic signal warns of the
danger, till the safety guard is closed. The analysis is not interrupted.
Overfilling
The unit is fitted with a dedicated hydraulic circuit for the removal of solvent residue
which is conveyed to an internal cooled tank for recovering it.
If the volume of the solvent into the recovery tank is too high, at the beginning or
during the analysis, the display shows " Recovery tank full” and the analysis is
stopped. Empty the solvent tank to proceed.
- in the case of insufficient water supply during the work-cycle, an acoustic signal
warns the operator of an error and the display shows the above message whilst
continuing the work-cycle. If the minimum flow-rate is not restored within 20 seconds
the cycle is automatically interrupted;
- in the case of insufficient water supply when START is pressed in the "Checkup-
cooling water menu”, the display shows the above message
Empty tank
When the analysis finishes, or after switching on the instrument with the tank is filled
with the solvent, the display shows: ”Solvent detected in the recovery tank”.
10006905/B2 40
- When START is pressed in the "Analysis" menu, if one or more sensors of active
positions read temperature too high, the display shows "Wait, heating plate $
temperature too high" to remind the operator that it’s necessary to wait for the
cooling of the heating plate.
- When START is pressed in the "Check-up/Lift", “Check-up/Fill solvent tubes” and
FILL in the “Analysis/Automatic loading” menu, if one or more sensors read
temperature too high, the display shows "Wait, heating plates temperature too
high" to remind the operator that it’s necessary to wait for the cooling of all heating
plates.
6. Working cycle
After the installation of the new equipment it is suggested to perform a wash down
cycle with the solvent that will be used for the extraction. This is aimed to remove
traces of grease deriving from the assembling which could impair the results of first
extractions.
1. Turn on the unit by the general switch located on the right of the instrument.
2. Open cooling water tap.
3. Go into the Analysis menu and set the operating parameters or confirm the set
ones.
NOTE: As delivered the unit is equipped by Viton seals. If the used solvent
requires Butyl seals or Vaflon proceed to change them at described at chap.3.7.
10006905/B2 41
5. Weigh the extraction cup with boiling stones, if necessary.
6. Place extraction cups on the SER with solvent or empty if automatic loading
solvent is set
7. Press Confirm.
8. Load the solvent automatically if this way is selected, following the instruction.
9. Press Start, the instrument performs automatically the steps for Randall
analysis, that consist of
-Immersion
-Removing
- Washing
and the additional Recovery and Cooling steps. At the end of the analysis
automatically, the instrument lifts up the EXTRACTION CUP and switches the
heating elements off.
NOTE: The minimum time of the Removing step is calculated by instrument
depending on the quantity of solvent and extraction cup selected. This time can
only be increased by the user.
NOTE: The minimum time of the cooling step is calculated by instrument
depending on the selected solvent. This time can only be increased by the user. It
can be reduced automatically if the temperature of the heating plate decreases
under safety temperature within minimum time of cooling step.
NOTE: When the time of the cooling is gone by, the tap water flow is closed.
10. Open the protection guard and remove the extraction cups. Remove extraction
thimbles or the crucibles. Recover solvent with the recovery tank procedure.
11. Put the extraction cup in the oven and then into the desiccator before taking the
total weight
12. If the Details page is filled in before to start the analysis, fill this value into the
Results menu to obtain directly the results in terms of grams and percentage of
extract.
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6.2 Randall system
Below the steps of the SER158
4- RECOVERY 5- COOLING
More than 90% of the The heating elements are
solvent is recovered in switched off and the
the internal recovery tank. extraction cups containing
the extracts are
automatically lifted to
prevent extracted matter
burning.
10006905/B2 43
7. End-of-work operations
At the end of the day, perform the following operations:
NOTE: the instrument can automatically, at the end of the analysis, switch the
heating element off, lift up the beaker(s), and close the circulation of the cooling
water (Load and go)
8. Maintenance
The instrument is equipped with a stroke counter to alert the operator, via display
messages, when to the maintenance schedule.
The maintenance (ordinary 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's important to follow these guidelines.
When the warning about the extraordinary maintenance is visualized, please contact
the dealer VELP SCIENTIFICA S.r.l.
CAUTION
Always wear personal protective equipment (goggles, protective clothing and gloves)
during maintenance operations.
Before performing any maintenance, switch off the power supply and remove all
sources of flammable vapor.
Never use solvents or detergents, which could damage the instrument.
Pay attention in the disassembly and seals (Viton, EPDM and Vaflon). In order to not
damage the seals and the collection funnel, use the supplied wrench. Do not use or
touch the seals with sharp objects that could damage them.
Do not grease the seals under any circumstances because it could distort the results
of subsequent tests.
Make sure the heating plate is cold.
Maintenance work not mentioned in this manual including the response to internal
parts, must be performed by persons authorized by Velp Scientifica S.r.l.
• Wipe the visible parts of the machine using a damp cloth or sponge moistened
with water; in particular, the glass-ceramic heating plate.
• Clean the extraction cups and crucibles with hot water and detergent using a
brush to clean them thoroughly or wash them in a laboratory dishwasher, if
present. The glass parts can be dried in a drying oven at 100 °C for 30 minutes
or in a vacuum oven at 70 °C for 20 minutes. Allow to cool slowly after the glass
parts before reuse.
10006905/B2 44
8.2 Extraordinary maintenance
Cleaning of cooling tap water filter
Unplug the unit from electric supply and remove the connection to tap water.
Remove the cooling water tube from the unit and pull out the filter using small
pincers. Clean the filter under flowing water or by compressed air
Replacement of gaskets
Retaining gaskets between extraction cups and titanium condensers are to be
changed if required. This includes if they are worn or no longer elastic. See chap.
3.7.
Oxidizing procedure for cleaning glassware
Glassware can be washed normally using a solution prepared dissolving 30 g
of sodium hydroxide (NaOH, technical grade), 10 g of sodium tripolyphosphate
(Na5P3O10, technical grade) and 2 g of sodium lauryl sulfate (C12H25NaSO4,
commercial mixture) in 1 L of deionized water.
Glassware can be cleaned by chromic acid oxidation (dichromate and concentrated
sulfuric acid), sulfonitric acid oxidation (warm concentrated sulfuric acid with small
amounts of potassium or sodium nitrate or nitric acid), or by nitrous oxide oxidation
(sodium nitrite and concentrated sulfuric or hydrochloric acids). Chromic-sulfuric acid
mixture is prepared adding slowly 1 l of concentrated sulfuric acid (H 2SO4, d.1.84,
technical grade) to 35 ml of saturated sodium dichromate aqueous solution
(Na2Cr2O7, 73% w/w at 20°C, technical grade) while stirring.
The cold mixture must be left in contact with glassware for at least 15 minutes, better
if its left overnight. The freshly prepared solution is orange-red and becomes green
after repeated use due to the reduction of Cr VI to Cr III.
Exhausted chromic-sulfuric mixture must be disposed of in a proper manner due to
environmental toxicity of chromium.
Nitrous oxide oxidation of organic residues can be obtained washing the glassware
with hot concentrated sulfuric acid (H2SO4, 70%, d. 1.62 technical grade) to which a
few drops of saturated sodium nitrite aqueous solution (NaNO2, technical grade, 100
g into 150 ml of tap water) are added before use.
Another method is based on concentrated nitric acid oxidation: the addition of a few
drops of ethanol produces after minutes an exothermic reaction and the evolution of
oxidizing nitrous oxide.
Attention: all these treatments must be performed under a fume hood due to the
extreme toxicity of evolved nitric-nitrous fumes. After oxidizing treatment, the filters
must be thoroughly rinsed with tap water and finally with deionized water and then
10006905/B2 45
dried. Using nitric acid protect hands with PVC gloves and not rubber which is
attacked.
NOTE: It is important to empty the internal pipes of the machine, in order to prevent
any residues of solvent and water from the mains may damage the machine during
transport.
10006905/B2 46
10. Accessories
Description Code Image
Connection cable SER158 Slave A00000287
10006905/B2 47
Handling device extraction cups SER158/6 A00000304
10006905/B2 48
12. Technical features
PERFORMANCES
Recovery rate % 90
CONSUMPTION
Cooling water
(during analysis only) l/1’ > 1
10006905/B2 49
ANALYTICAL METHODS
Standard methods N° 34 pre-defined based on official methods
Customizable methods N° 30
ANALYSIS DATA
The following parameters can be set for each analysis:
Method
Operator name
Sample name
Sample quantity g
Results %extract, g extract
Average; SD, RSD in g or %
INTERFACES
N°2 USB for balance, USB pen drive, mouse
N°1 USB on the controlPad suggested for USB pen drive
LAN for network connection
10006905/B2 50
13. Wiring diagram
SER158/6
10006905/B2 51
SER158/3
10006905/B2 52
N° Description
1 Fuse 5x20 8A
2 General switch
3 Ceramic heating plate
4 Air pump
5 Vacuum pump
6 Tap water valve
7 3-way valve
8 Discharge solvent valve
9 Discharge solvent motor
10 Solvent inlet motor
11 Sensor lift electronic board
12 Microswitch lift motor
13 Fill sensor tank
14 Over fill sensor tank
15 Inlet solvent sensor motor
16 Discharge solvent sensor motor
17 Microswitch frontal protection
18 Flow meter tap water
19 Heating sensor Pt100
20 ControlPad
21 USB LAN electronic board
22 “Extra unit” connectors
23 LED electronic board
24 Power supply
25 Power board
26 Lift motor
27 Inlet power
10006905/B2 53
14. Hydraulic scheme
SER158/6
A-Tap water valve B-Tap water flow-meter C-IN solvent valve D-OUT solvent valve
E-Vacuum Pump F-Air Pump G-3-way valve H-Discharge solvent valve
10006905/B2 54
SER158/6
DIAMETER LENGTH
No. Qty MATERIAL
(mm) (cm)
1 1 LLDPE 6x8 67
2 2 LLDPE 6x8 21,5
3 2 LLDPE 6x8 34,5
4 2 LLDPE 6x8 32
5 4 LLDPE 6x8 18
6 1 LLDPE 6x8 45
7 1 LLDPE 6x8 40
8 1 PTFE 6,5x7,5 6
9 1 PTFE 4x6 52
10 1 PTFE 4x6 22
11 1 PTFE 4x6 71
12 1 PTFE 4x6 8
13 2 PTFE 4x6 9,2
14 1 PTFE 4x6 17,5
15 12 PTFE 1/16’’x1/8’’ 50
16 1 PTFE 4x6 150
17 1 PVC 7x10 200
PUR = Polyurethane
PTFE = Polytetrafluoroethylene
PVC = Polyvinyl chloride
10006905/B2 55
SER158/3
A-Tap water valve B-Tap water flow-meter C-IN solvent valve D-OUT solvent valve
E-Vacuum Pump F-Air Pump G-3-way valve H-Discharge solvent valve
10006905/B2 56
SER158/3
DIAMETER LENGTH
No. Qty MATERIAL
(mm) (cm)
1 1 LLDPE 6x8 96
2 6 PTFE 1/16’’x1/8’’ 50
3 2 LLDPE 6x8 18
4 1 LLDPE 6x8 71
5 1 LLDPE 6x8 40
6 1 PTFE 6,5x7,5 6
7 1 PTFE 4x6 52
8 1 PTFE 4x6 22
9 1 PTFE 4x6 71
10 1 PTFE 4x6 8
11 2 PTFE 4x6 9,2
12 1 PTFE 4x6 17,5
13 1 PTFE 4x6 150
14 1 PVC 7x10 200
PUR = Polyurethane
PTFE = Polytetrafluoroethylene
PVC = Polyvinyl chloride
10006905/B2 57
15. Warranty
The unit is guaranteed against production defects for 25 months from our invoice
date.
Warranty claims can be accepted only if the system has been installed and used as
specified on the manual and carried out by qualified service personnel as appointed
by VELP Scientifica.
Exclusions
The guarantee will be considered null and void for faults resulting from:
- inexperience and carelessness of the operator
- repairs, maintenance or replacement of parts carried out by personnel or
Companies not authorized by the manufacturer
- use of the instrument that does not comply to the instructions/recommendations
given in the present operating manual
- use of non-original spare parts.
16. Suggestions
We will be pleased to receive any comments and/or suggestions that will help us to
improve this operating manual.
e-mail: [email protected]
10006905/B2 58
Flow sheet for a typical extraction of soluble
matter by an organic solvent from solid
samples
A Grind and homogenize the sample
D Dry and weigh the extraction cup with some boiling stones (if they are
required).
G Start the analysis. The unit will perform automatically the 5 steps of the
analysis if set: Immersion, Removing, Washing, Recovery, Cooling.
Dry the extract collecting vessel with boiling stones (if used) in an oven
H during 60 minutes at a temperature high enough to evaporate
completely solvent residues.
10006905/B2 59
ANALYTICAL METHOD
1 Determination of crude fat in meat and processed meat
The solvent extraction is performed on dried samples.
1) Sample preparation:
A ground and homogenized sample is dried in a fan oven at 102-105 °C for
6 hours, mixing sometimes to help the drying. Record the weight of the
sample before and after the desiccation in order to calculate the loss of
humidity. If necessary, grind the dried sample in order to increase the
homogeneity of the sample.
Put 3 - 4 g of dry sample in each thimble (Msample). The sample weight can
be adjusted in accordance with the expected fat content.
2) Glass extraction cups preparation:
Dry the extraction cups in a drying oven at 102-105 °C for 1 hour. Cool them
in a desiccator until constant weight of the tare (Mtare) to the nearest of 0.1
mg.
3) Solvent:
Petroleum ether 40-60 °C
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Crude fat in meat
and processed meat” including the following parameters:
• Immersion Time: 25 minutes
• Removing Time: 10 minutes
• Washing Time: 55 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum Ether 40-60 °C, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) Calculation of the result:
See chap. 6.1.
6) References:
ISO1444:1996; AOAC 991.36; AOAC 960.39
10006905/B2 60
2 Determination of total fat in meat and processed meat
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in meat and
processed meat” including the following parameters:
• Immersion Time: 50 minutes
• Removing Time: 10 minutes
• Washing Time: 45 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum Ether 40-60 °C, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) References:
ISO 1443-1973
10006905/B2 61
3 Determination of total fat in fish and derived products
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in fish and
fish products” including the following parameters:
• Immersion Time: 50 minutes
• Removing Time: 10 minutes
• Washing Time: 45 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum ether, 100 ml
• O-ring: Butyl (grey) (Viton)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) References:
AOAC 948.15
10006905/B2 62
4 Determination of total fat in whole eggs
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in whole
egg” including the following parameters:
• Immersion Time: 60 minutes
• Removing Time: 10 minutes
• Washing Time: 50 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• Diethyl ether, 100 ml
• O-ring: Vaflon (white)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) References:
AOAC 925.32
10006905/B2 63
5 Determination of total fat in oily seeds and nuts
A preliminary acid hydrolysis is aimed to free occluded or bound lipids.
Follow accurately the “Hydrolysis procedure for oily seeds and nuts”,
detailed in the HU6 operating manual, in order to carry on the preliminary
hydrolysis in the best conditions to assure reliable and accurate final results.
1) Glass extraction cups preparation:
Dry the extraction cups in a drying oven at 102-105 °C for 1 hour. Cool them
in a desiccator until constant weight of the tare (Mtare) to the nearest of 0.1
mg.
2) Solvent:
n-Hexane
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in oily seeds
and nuts” including the following parameters:
• Immersion Time: 60 minutes
• Removing Time: 10 minutes
• Washing Time: 50 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• n-hexane, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) References:
AOAC 2003.06
10006905/B2 64
6 Determination of total fat in milk powder
On the control pad select “Analysis”, and then method “Total fat in milk
powder” including the following parameters:
• Immersion Time: 55 minutes
• Removing Time: 10 minutes
• Washing Time: 55 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum ether 40-60 °C, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
4) Calculation of the result:
See chap. 6.1
5) References:
AOAC 963.15
10006905/B2 65
7 Determination of total fat in condensed milk
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in
condensed milk” including the following parameters:
• Immersion Time: 60 minutes
• Removing Time: 10 minutes
• Washing Time: 50 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum ether 40-60 °C, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
10006905/B2 66
8 Determination of total fat in cheese
2) Solvent:
Petroleum ether 40-60 °C
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in cheese”
including the following parameters:
• Immersion Time: 60 minutes
• Removing Time: 10 minutes
• Washing Time: 50 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum ether 40-60 °C, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
4) Calculation of the result:
See chap. 6.1
5) References:
AOAC 933.05
10006905/B2 67
9 Determination of total fat in flour, bakery products and pasta
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in flour,
bakery products and pasta” including the following parameters:
• Immersion Time: 90 minutes
• Removing Time: 10 minutes
• Washing Time: 50 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• Diethyl ether, 100 ml
• O-ring: Vaflon (white)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
References:
AOAC 2003.05;
10006905/B2 68
10 Determination of crude fat in fried potatoes
1) Sample preparation:
Put 3 - 4 g of ground and homogenized sample in each thimble (Msample), and
add about 2 g of sodium sulfate anhydrous, in order to absorb humidity. Mix
using a glass rod and use defatted cotton in order to remove sample
residues from the glass rod and to plug the thimble.
The sample weight can be adjusted in accordance with the expected fat
content.
3) Solvent:
Petroleum ether 40-60 °C
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Crude fat in fried
potatoes” including the following parameters:
• Immersion Time: 20 minutes
• Removing Time: 10 minutes
• Washing Time: 15 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum Ether 40-60 °C, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
6) References:
AOAC 963.15
10006905/B2 69
11 Determination of crude fat in animal feed
1) Sample preparation:
Put 5 - 7 g of grounded and homogenized sample in each thimble (Msample).
The sample weight can be adjusted in accordance with the expected fat
content.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Crude fat in feed”
including the following parameters:
• Immersion Time: 25 minutes
• Removing Time: 10 minutes
• Washing Time: 55 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• Diethyl ether, 100 ml
• O-ring: Vaflon (white)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
6) References:
AOAC 920.39
10006905/B2 70
12 Determination of total fat in animal feed
3) Solvent extraction:
If dried test portions will not be immediately extracted, put them in a
desiccator, or let the crucibles cool to room temperature and then, mix the
layer of hydrolyzed sample and Celite with a spatula to obtain a powdery
hydrolysis. Take care to not damage the bottom layer of glass sand.
At this point, before starting the extraction, add a new layer of glass sand (20
g) to avoid the Celite buoyancy.
The extraction cups containing the glass crucibles can now be placed on the
ultra-fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Total fat in feed”
including the following parameters:
• Immersion Time: 55 minutes
• Removing Time: 10 minutes
• Washing Time: 55 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• Diethyl ether, 100 ml
• O-ring: Vaflon (white)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the crucibles. Allow the solvent
to filter through the crucible before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
10006905/B2 71
13 Determination of crude fat in creams and sauces
1) Sample preparation:
Put 1 g of homogeneous sample in each thimble (Msample) and add about 1 g
of sodium sulfate anhydrous, in order to absorb humidity. Mix using a glass
rod and use defatted cotton in order to remove sample residues from the
glass rod and to plug the thimble.
The sample weight can be adjusted in accordance with the expected fat
content.
6) References:
AOAC 920.172
10006905/B2 72
14 Determination of crude fat in chocolate
1) Sample preparation:
Put some chocolate blocks in a beaker and melt it at 45 °C for 1 hour in a
fan oven. Mix thoroughly using a spatula in order to homogenize it.
Put 2 g of melted sample in each thimble (Msample) containing about 15 g of
sodium sulfate anhydrous. Mix thoroughly using a glass rod and use
defatted cotton in order to remove sample residues from the glass rod and to
plug the thimble.
The sample weight can be adjusted in accordance with the expected fat
content.
6) References:
AOAC 963.15
10006905/B2 73
15 Extraction of oil and grease from wastewater
The method is empirical and reproducible results are obtained only following
exactly all details.
1) Sample preparation:
1 l of wastewater collected in a wide mouth glass bottle and immediately
acidified to pH 2 or lower with hydrochloric acid (HCl) to hydrolyze soluble
soaps.
Prepare a 12 cm Buchner funnel with a disk of muslin cloth overlaid with a
filter paper disk. Filter under vacuum 100 ml (Msample) of filter aid suspension
on the Buchner and wash with 1 l of distilled water. Filter acidified sample
until no more water passes the filter. Transfer paper filter to a watch glass
using forceps. Wipe walls and bottom of collecting bottle and Buchner funnel
with pieces of filter paper soaked in solvent and add them to paper filter on
watch glass. Roll the paper filter and introduce it into extraction thimble.
Dry thimble in an oven at 103°C for half an hour.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Oil and grease from
wastewater” including the following parameters:
• Immersion Time: 60 minutes
• Removing Time: 10 minutes
• Washing Time: 50 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• n-Hexane, 100 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (15 minutes at 80 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
10006905/B2 74
5) Calculation of the result:
See chap. 6.1
6) References:
10006905/B2 75
16 Extraction of oil and grease from sludges
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Oil and grease from
sludges” including the following parameters:
• Immersion Time: 30 minutes
• Removing Time: 25 minutes
• Washing Time: 15 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• n-Hexane, 160 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 160
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (15 minutes at 80 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
10006905/B2 76
5) Calculation of the result:
See chap. 6.1
6) References:
10006905/B2 77
17 Extraction of petroleum source rocks
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Extraction of
petroleum source rocks” including the following parameters:
• Immersion Time: 40 minutes
• Removing Time: 25 minutes
• Washing Time: 50 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• n-Hexane: Acetone 50:50, 160 ml
10006905/B2 78
• O-ring: Vaflon (white)
Close the safety guard and, using the automatic or manual mode, dose 160
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
6) References:
US EPA 3541,
DIN ISO 16703 EN 14039
10006905/B2 79
18 Extraction of plasticizer mixture from vinyl chloride
plastics
1) Sample preparation:
Crush the sample and grind it (particles dimension from 0.6 to 2 mm). Weigh
20 g of sample (Msample) into an extraction thimble.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Plasticizer mixtures
from vinyl chloride plastic” including the following parameters:
• Immersion Time: 50 minutes
• Removing Time: 40 minutes
• Washing Time: 20 minutes
• Recovery Time: 30 minutes
• Cooling Time: 4 minutes
• n-Hexane, 200 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 200
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) Calculation of the result:
See chap. 6.1
6) References:
ASTM Standard Practices
10006905/B2 80
19 Extraction of rosin from paper and paperboard
The extracted matter is really colophony but in paper manufacture the term
“rosin” is commonly used.
1) Sample preparation:
Cut the sample into 6x40 mm strips. If the paper contains carbonates the
sample must be immersed 5 minutes into 1 N hydrochloric acid (HCl),
washed with water and dried at room temperature.
Weigh 5 g of sample (Msample) into an extraction thimble.
6) References:
TAPPI T408
10006905/B2 81
20 Extraction of oils from leather
During tanning of hides to make leather, vegetable, animal and mineral oils
are used to give waterproofness and flexibility.
1) Sample preparation:
Cut the sample into 6x10 mm strips. Weigh 10 g of sample (Msample) into an
extraction thimble.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Oils from leather”
including the following parameters:
• Immersion Time: 30 minutes
• Removing Time: 30 minutes
• Washing Time: 20 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum ether 40-60 °C, 180 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 180
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
6) References:
ISO 4048:2008
10006905/B2 82
21 Determination of unsaponified and unsaponifiable fat in
soaps
1) Sample preparation:
Weigh 10 g of sample (Msample) into an extraction thimble and keep overnight
in an oven at 105°C. In the thimble add 2 g of celite.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Unsaponified and
unsaponifiable fat in soaps” including the following parameters:
• Immersion Time: 30 minutes
• Removing Time: 25 minutes
• Washing Time: 20 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum ether 40-60 °C, 160 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 160
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
The weight is due to neutral fat and unsaponifiable fat and is to be referred
to the weight of sample before drying.
Determination of unsaponifiable fat: The extract of preceding
determination is saponified directly in the extract vessel by boiling one
10006905/B2 83
hour with 20 ml of ethanol KOH 1 N solution. At the end the residue is
dissolved with three 20 ml volumes of petroleum ether which removes
the unsaponifiable fat and whose weight can be determined by
evaporation in a weighed vessel.
6) References:
ISO 1067:1974
10006905/B2 84
22 Extraction of ethanol soluble components from detergent
formulations
1) Sample preparation:
Weigh 5 g of sample (Msample) into an extraction thimble which was
previously tared in a weighing bottle together with a cotton plug. Keep the
samples overnight in an oven at 105 °C and plug the thimble with the
defatted cotton.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Ethanol soluble
components from detergents” including the following parameters:
• Immersion Time: 30 minutes
• Removing Time: 10 minutes
• Washing Time: 50 minutes
• Recovery Time: 45 minutes
• Cooling Time: 2 minutes
• Ethanol, 100 ml
• O-ring: Butyl (grey)
Close the safety guard and, using the automatic or manual mode, dose 100
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Msoluble) to the nearest of 0.1
mg.
Drying of insoluble residue: Introduce the thimble with insoluble
residues in the same weighing bottle used before. Dry in an oven at 105
10006905/B2 85
± 2 °C during 3 hours. Cool them in a desiccator to room temperature
and record the accurate weight (Minsoluble) to the nearest of 0.1 mg.
Where:
Msample = sample weight (g)
Mtare = weight of the empty extraction cup (g)
Msoluble = weight of the extraction cup + extract (g)
Minsoluble = weight of the thimble after the extraction (g)
6) References:
10006905/B2 86
23 Extraction of finishing oils from textiles and synthetic or
natural fibers
The finishing oils used for natural and synthetic fibers provide a better
crease resistance, water repellence and permanent press. They also act as
lubricants for synthetic thread. Without them, high-speed commercial sewing
machines could overheat. Finishing oil enhances the processability of fibers.
Reasons for sample extraction:
- gravimetric analysis
- sample preparation for GC, HPLC, etc.
1) Sample preparation:
Cut the sample into 6x40 mm strips. Weigh 10 g of sample (Msample) into an
extraction thimble.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Finishing oils from
textiles and synthetic fibers” including the following parameters:
• Immersion Time: 20 minutes
• Removing Time: 25 minutes
• Washing Time: 0 minutes
• Recovery Time: 30 minutes
• Cooling Time: 3 minutes
• Petroleum ether 40-60 °C, 140 ml
• O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 180
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
10006905/B2 87
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) References:
ASTM D2257
10006905/B2 88
24 Extraction of oil content in insulating material
1) Sample preparation:
Grind the sample and weigh 8 g of sample (Msample) into an extraction
thimble.
4) Solvent extraction:
The extraction cups containing the thimbles can now be placed on the ultra-
fast heating plate of SER 158.
On the control pad select “Analysis”, and then method “Oil content in
insulating material” including the following parameters:
Immersion Time: 20 minutes
Removing Time: 30 minutes
Washing Time: 10 minutes
Recovery Time: 30 minutes
Cooling Time: 3 minutes
Petroleum ether 40-60 °C, 170 ml
O-ring: Viton (green)
Close the safety guard and, using the automatic or manual mode, dose 170
ml of solvent into the glass cups containing the thimbles. Allow the solvent to
filter through the thimble before adding more solvent.
Open the cooling water and press START to begin the extraction process.
At the end of analysis, position the extraction cups containing the extract in a
drying oven (1 hour at 105 °C), cooled them in a desiccator to room
temperature and record the accurate weight (Mtot) to the nearest of 0.1 mg.
5) References:
BS 2972:1989
10006905/B2 89
25 Extraction of organic micro-pollutants for GC-MS analysis
1) Sample preparation:
Weigh 0.5 g of sample in each thimble.
5) References:
EPA 3541
10006905/B2 90
26 Extraction of oil and grease from plastic
1) Sample preparation:
Dry the sample in a desiccator for about 6 hours (1 night).
Weigh 10 g of dried sample in each thimble (Msample),
10006905/B2 91
27 Extraction of crude fat in Standard (Cod. A00000318)
1) Sample preparation:
Weigh 5 g of standard in each thimble (Msample).
6) References:
AOAC 2003.05
10006905/B2 92
Declaration of conformity
We the manufacturer VELP SCIENTIFICA S.r.l.
Address Via Stazione, 16
20865 USMATE (MB)
Italy
EN 61010-1/2010
EN 61010-2-010/2014
EN 61010-2-081/2015
EN 61326-1/2013
2006/42/EC
2006/95/EC
2004/108/EC
2011/65/UE (RoHS)
2012/19/UE (RAEE)
plus, modifications and that the documents listed in annex I are available at
Velp's offices as foreseen by the machinery directive.
10006905/B2 93
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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
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18001 Quality System Certification.
Our instruments are manufactured in Italy according to the IEC 1010-1 and CE
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