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Frequently Asked Questions
How
long does an extraction take with an automated
SPE system?

How
much solvent is used during an extraction
process?

My laboratory is concerned with
solvent exposure.

What solvents are compatible
with the automated extractors?

How are solvent volumes determined?

Does
the Controller come pre-programmed with EPA
methods?

Can I create my own methods in
the 4700 Controller?

What are the differences between
the SPE-DEX 4790 Extractors, the Spe-Dex 4770,
and the Spe-Dex 4750 Extractors?

What are typical Background values
for the extractors?

I have difficulties with sample
flow rates when using 3M Empore™ Oil &
Grease disks. Is there anything that I can
do?
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Q:
How long does an extraction take with an automated
SPE (Solid Phase Extraction) system?
A:
On average, an extraction can take anywhere
from 15 - 20 minutes, with dirtier samples
taking longer. The total run time will
also be a function of the number of Pre-wet
and Rinse steps that have been programmed
into the method.
Q:
How much solvent is used during an extraction
process?
A: Horizon Technology’s Automated
Extractors use approximately 1/3 less solvent
than with conventional LLE (liquid-liquid
extractions). For a typical method, using
a 47 mm disk, the total amount of solvent
would be approximately 10 - 20 mLs for Prewetting
and 15 - 20 mLs for final Rinsing. A
typical method using a 90 mm disk will use
about twice that volume.
Q:
My laboratory is concerned with solvent exposure.
A: The 1000XL and 3000XL Oil & Grease
Machines come standard with an internal fan
and hose ducting. This permits the systems
to be operated directly on the lab bench.
The Sep-Dex 4790 system has an internal fan,
but the Vent Hose Kit is an option. If you
plan to operate Spe-Dex 4790's on the bench,
we recommend ordering the optional Vent Hose
Kit at the time of purchase.
The
fan pulls solvent fumes away from the technician
and can be vented into a fume hood. This minimizes
exposure to solvent fumes. Because the extraction
process is automated, all of the solvents
are contained in 2.5 Liter solvent bottles.
Therefore, there is minimal handling of the
solvents by the technician. Exposure levels
have been tested and fall below the OSHA limits.
Q:
What solvents are compatible with the automated
extractors?
A: Because the Spe-Dex® 1000XL
& 3000XL Oil & Grease Machines are
designed specifically for Method 1664A they
can only be used with hexane and methanol.
The use of other solvents will damage the
extractors. Since the Spe-Dex 4790 was designed
to perform all EPA approved SPE methods, it
can handle all solvents. Some customers even
use the Spe-Dex 4790 system for other internal
R&D applications.
Q:
How are solvent volumes determined?
A:
The
volume of solvent delivered to the system
is a function of the solvent bottle pressure;
the length of time the internal solvent delivery
valve (solenoid) stays open; the diameter
of the solenoid valve opening; the diameter
of the rinse tube and the number of Pre-wet
and Rinse steps programmed. On the Spe-Dex®
4790 Extractors, an IR sensor regulates dispense
time (or time the solenoid valve stays open)
depending on whether a 47 mm or 90 mm disk
is being used. For the 1000/3000XL Systems
the dispense time is programmed into the Controller
method.
Q:
Does
the Controller come pre-programmed with EPA
methods?
A: Yes. All of the currently approved
EPA methods are pre-programmed into the Controller. These
methods are simply called up by the operator,
(EXAMPLE 525.2) and downloaded to the individual
extractors.
Q:
Can I create my own methods in the 4700 Controller?
A: Yes. The 4700 Controller allows
you to modify the pre-programmed EPA methods
to create your own methods. The Controller
simply asks which solvents will be used and
the various times for soaking, air drying
and rinsing the disk. The Controller
can safely store about 200 individual methods
in its non-volatile memory.
Q:
What
are the differences between the SPE-DEX®
4790 Extractors, the Spe-Dex® 4770,
and the Spe-Dex® 4750 Extractors?
A:
1) Water Bottle Holder:
Unlike the 4770 & 4750 Extractors in which
the sample bottle sat loosely in the
bottle holder, the 4790 requires a tight seal
between the bottle holder and the sample bottle
cap adapter. This is required, as the
Water Inlet Valve now remains open during
the entire water sample. In
comparison, the 4770 & 4750 Water Inlet
Valves opened and closed to introduce the
water sample.
Therefore, since the Water Inlet Valve remains
open until all of the water has been filtered, the
sample bottle and cap adapter need to
be firmly attached together to prevent
air leaks. If you look into the bottle
holder, you will notice a black o-ring. This
o-ring provides the seal between the cap adapter
and the bottle holder. As long as a
good seal is maintained between the sample
bottle/cap adapter and the bottle holder,
the water sample can only flow out, as air
is introduced into the bottle.
2)
Loading the Sample Bottle: 4790
- Once the aluminum foil and cap adapter are
in place, follow the procedures in the manual
to load the sample bottle. Once the
bottle is loaded into position, it is important
to use a "clockwise" rotation to
open the foil. If the bottle is rotated
"counterclockwise" the cap adapter
could be loosened from the bottle and allow
an air leak to develop. This would cause
an overflow of the water sample. Also,
to prevent the aluminum foil from covering
the solvent rinse opening, only rotate the
bottle 3/4 of the way. Again, practice
with the unit first - use an empty bottle
with foil and observe how the foil opens.
4770 & 4750 – The rinse cone breaks the
aluminum foil when loading the sample bottle.
3)
Liquid Level Sensors: Unlike
the 4770 & 4750 Extractors, which had
fixed sensors, the 4790 sensors can be adjusted.
This design was used in order to handle dirty
samples that contain great amounts of particulate
matter. Being able to move the sensors
up (or down) is very useful.
Before running a water sample, inspect
and adjust the height of the sensors.
It is recommended to run a Purge method and
visually inspecting the volume of Prewet solvent
dispensed. Also, based on the vacuum
setting, inspect the disk to ensure sufficient
volume is left on the disk during the soaking
cycle. The sensor assembly can
be moved up or down until the desired Prewet
volume is obtained. Once this sensor
height is adjusted, it does not need to be
changed, unless the operator elects to.
4)
Water Inlet Valve: The 4790 Water
Inlet Valve uses air pressure to open the
valve. It is designed similar to a stopcock
on a separatory funnel. The opening of the
Water Inlet Valve is ½ “ in diameter. This
is ideal for processing dirty samples that
may not only be high in suspended solids but
may have larger particles or chunks. The Water
Inlet Valve opens during the sample-processing
step and remains open until the entire extraction
is complete. The Water Inlet Valve on the
4770 & 4750 Extractors operate on vacuum
and have a diaphragm assembly that opens when
vacuum is supplied to the valve. In this system,
the Water Inlet Valve alternates between the
open and closed positions during the sample-processing
step to prevent the Disk Assembly from over
filling. The diameter of the water path opening
on this valve is 0.24 “. Therefore, the extraction
of dirty samples with particulate material
could be a problem causing the diaphragm to
not seal properly and result in sample overflows.
The 4770 Extractors were designed for the
extraction of clean drinking water samples.
The 4750 Extractors are similar in design
to the 4770 Extractors. Although the 4750
Extractors were designed for Oil & Grease
extractions, samples that are very dirty will
be problematic. The 4790 Extractors were design
to overcome this limitation.
5)
Disk Holder Assemblies: The 4770
& 4750 Extractors have Disk Assemblies
that can only accommodate 47 mm disks. The
4790 Extractors can accommodate two different
size Disk Holder Assemblies. When running
clean samples, the 47 mm Disk Holder Assembly
is loaded onto the extractor platform and
is used with 47 mm disks. For running dirty
samples, the 90 mm Disk Holder Assembly is
mounted on the platform and used with 90 mm
disks. The Bakerbond Speedisks®
can be used on all three extractors.
These
are the main changes to the 4790. Internally,
the main circuit board is now located in a
higher position - not on the bottom.
Also, the keypad is a membrane design so as
to be impervious to liquids, plus, it is mounted
higher up on the chassis. Two of the
check valves have also been removed, which
will make daily operation more reliable and
user friendly.
Q:
What are typical Background values for the
extractors?
A: First, let's discuss the background
values typically found with method 1664A.
A clean extractor system with clean solvents
(and no disk), should give a background value
of 0.5 - 0.75 mg. Based on the particular
disk used, and the size of the disk (47 or
90 mm), the background value could range from
0.75 - 1.5 mg. Most of the higher backgrounds
are a result of the SPE disk. Various steps
can be taken to reduce these higher values.
With
regards to background values for organic contaminates,
the Spe-Dex 4790 model uses all PTFE, PEEK,
and Kalrez components. Again, as long
as the solvents are clean and no contaminating
materials are used in the extractor, such as
O-Rings, the background values are well below
standard EPA method requirements.
Q:
I have difficulties with sample flow rates
when using 3M Empore™ Oil & Grease disks.
Is there anything that I can do?
A: Yes. There has been three generations
of Disk Holder Assemblies. The old style snap
fit assembly required one o-ring on the groove
of the Insert that would hold the disk in
place and form a tight seal. The second generation
of Disk Holder Assemblies came in three parts,
the Base Cup, the Riser and the Aluminum Locking
Ring. No o-ring is needed when using a flat
disk. However, when using the 3M Empore™ Oil
& Grease disks the two o-rings are needed
to provide a tight seal for optimal flow rates.
The larger diameter, thicker o-ring is placed
in the bottom outer groove of the Cup and
the smaller diameter, thinner, o-ring is placed
in the groove of the Riser, which is inserted
into the Base Cup to hold the disk in place.
The orientation of the Riser is such that
the groove with the o-ring is face up and
the flat edge is face down on the disk. The
Aluminum Locking Ring is then screwed tightly
onto this assembly. If the assembly
is not tight, when vacuum is pulling, air
will flow through the parts and slow the flow
rates. A high amount of residual water
may also be left on the disk after the Air
Dry Time which can adversely effect recoveries.
The latest style of Disk Holder Assemblies
also come in three parts but have been redesigned
such that the o-rings are no longer used with
the 3M disks. Instead, a red gasket is used
to provide a better seal. The support screen
is placed in the center of the Base Cup. The
gasket is then placed into the Cup with the
flat even side face down. The 3M Oil &
Grease disk is placed into the center recess
of the gasket. For the 90 mm assemblies, the
Riser is inserted into the Cup with the grooved
side face down on the disk. For the 47 mm
assemblies, the side with the thin lip is
inserted face down on the disk and the flat
edge face up. Finally, tightly screw on the
Aluminum Locking Ring. This design provides
a better seal when using the 3M disks. For
the flat disks, the gasket is eliminated and
the orientation of the Riser in the Cup is
reversed (flip over). Refer to the Operator
Manual for detailed instructions and photos.
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