Hydro Series Wet Dispersion Units (MAN0479-05-En-00)
Hydro Series Wet Dispersion Units (MAN0479-05-En-00)
Hydro Series Wet Dispersion Units (MAN0479-05-En-00)
www.malvern.com
PARTICLE SIZE
MASTERSIZER 3000
HYDRO SERIES
WET DISPERSION UNITS
MAN0479
MRK1955-01
Head office:
Mastersizer, Malvern and the 'hills' logo are registered trademarks in the UK and/or other countries,
and are owned by Malvern Instruments Ltd.
Windows is a registered trademark of Microsoft Corporation.
Maintenance
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Warnings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Maintenance schedule . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Maintenance procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
Consumable kits. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-25
Appendix
Specification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Chemical compatibility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
Introduction
and Hardware
Introduction
This manual details the important features of the Mastersizer 3000 Hydro series
wet sampling dispersion units.
Note
The Hydro MV/LV (MAZ3210/3310) dispersion units are fitted with an
analogue level sensor and a manual drain button. These additions to the
Hydro MV/LV (MAZ3200/3300) dispersion units are identified in the rele-
vant manual sections.
Warning!
The dispersion units or the samples to be measured may be hazardous if
misused. Users must read the Health and Safety information in the
Basic guide before operating the system.
This manual focuses on specific issues of the Hydro series wet dispersion units that
are not covered by the above manuals. Within the following chapters the manual
will detail:
Maintenance
This chapter covers all the user maintenance procedures for the dispersion units.
This includes a maintenance schedule and associated maintenance procedures for
inspecting and cleaning each dispersion unit and its respective components. Spe-
cific procedures for inspecting and cleaning the flow cell windows are described.
Appendices
This chapter details the useful specifications of each dispersion unit and identifies
the chemical compatibility of the dispersion unit components that may come into
contact with the sample. Additionally it provides the important regulatory informa-
tion to which the dispersion units are compliant.
ill 8760
The materials used in the manufacture of the dispersion units maximise the range
of materials that can subsequently be handled. Variable pump/stirrer speeds allow a
wide range of particle sizes and densities to be suspended and circulated enabling
Hydro SV
The Hydro SV enables the Mastersizer to be used for particle-in-liquid particle siz-
ing, where the amount of sample available limits the amount of dispersant that can
be used to dilute it, or where just a small volume of dispersant is available. This is
ideal when the sample or dispersant is toxic or expensive.
The Hydro SV manual dispersion unit is designed for the measurement of small
amounts of a sample with a particle size typically less than 200μm.
The dispersion unit comprises a sampling cuvette that holds the sample and disper-
sant liquid together, the Hydro SV can contain a maximum volume of 7ml.
1 2
ill 8696
The dispersion unit comprises a tank that holds the sample and dispersant liq-
uid; up to 120ml for a Hydro MV, 600ml for a Hydro LV.
Aqueous or non-aqueous dispersant is added to the tank via either the standard
lower internally regulated inlet port (commonly used for aqueous samples) or the
upper externally regulated inlet port (commonly used for non-aqueous samples).
Alternatively the dispersant can be manually added directly into the tank.
A light positioned in the dispersion unit body above the tank will flash briefly
when the tank is filled to the correct level.
With the tank filled, a pump within the tank, controlled using the Mastersizer soft-
ware, circulates the dispersant from the ‘to cell’ port of the dispersion unit to the
wet cell located in the optical unit, via the sample tubing. The dispersant is
pumped through the wet cell and then returns to the tank via the sample tubing
and the ‘from cell’ port.
Sample is added to the tank and dispersant as required. A stirrer within the tank
agitates the sample to stop it from settling or separating out; the pump then circu-
lates it through the system and wet cell to be measured using the optical unit and
software. Refer to the Mastersizer 3000 User Manual for advice on adding sam-
ple.
An ultrasonic transducer is provided to aid sample dispersion and can also be
used to remove bubbles from the flow path.
Note
The lower ‘to cell’ sample tubing has yellow identifier markings, whilst
the upper ‘from cell’ sample tubing has blue identifier markings.
Once the sample has been measured using the Mastersizer optical unit, it can be
disposed of using the drain outlet. The drain outlet is compatible with most aque-
ous and non-aqueous dispersants.
The Hydro MV and LV dispersion units contain two fluid handling valves con-
trolled from the application software:
A internally regulated dispersant valve that opens to allow clean aqueous dis-
persant into the tank.
A motor-driven drain valve that allows the tank to be drained.
4
8
9
1
7
3 6
11
5 10 12
ill 8668
Sampling tank
The tank holds the sample and dispersant. The tank can hold up to 120ml (Hydro
MV) or 600ml (Hydro LV) of sample and dispersant prior for circulation through
the wet cell situated in the measurement area of the optical bench.
The sampling tank is normally filled using the dispersant inlet ports, though sam-
ple and dispersant can be poured directly into the tank if required. A light posi-
tioned in the dispersion unit body above the tank will flash briefly when the tank is
filled to the correct level.
Additionally the tank contains the pump and stirrer assembly, described in the
next section, whilst an ultrasonic transducer attached to the tank also helps to dis-
perse the sample.
Once a measurement has finished, the tank can be emptied automatically using a
drain valve in the base of the tank. The sampling fluid is emptied through the drain
pipe out to a sink or other waste container.
All functions of the tank area are controlled by the Mastersizer application software.
Sampling Tank features
The tank assembly incorporates these important additional features.
B D A C
may lead to particles being lost via the over-flow system, leading to an incorrect
particle size distribution being reported.
Caution!
If manually filling the tank, ensure that the tank does not overflow by fill-
ing it too quickly. Never overfill the tank as spillage may occur once the
pump starts. Clean any spillage off the covers immediately to prevent dam-
age.
Breather hole
A breather hole is incorporated into the metal shield on the top of the sampling
tank. This is used to enable a sufficient draining rate for the tank when empty-
ing. Note that under filling of the tank may lead to air being entrained into
the liquid, again leading to an incorrect particle size being reported.
Baffles
The tank incorporates additional baffles; these help interrupt the sample flow
and aid mixing.
Note
The level sensor in the dispersion unit stops the tank being overfilled
above a certain level. This level, when the dispersant is detected and the
tank light flashes, depends upon the liquid that has been used in the tank. A
threshold value needs to be applied to the level sensor for all liquids other
than water, so if the tank fails to fill properly then this threshold, for the
dispersant being used, may need adjusting. Refer to the Sample - Disper-
sant and accessory controls sections in the software chapter.
Warning!
Never put fingers into the tank when the pump/stirrer shaft is rotating.
Caution!
Never operate the pump/stirrer at more than half speed with the tank
empty.
Ultrasonic transducer
The ultrasonic transducer (not shown) is used to help disperse samples. The power
of the transducer is controlled through the Mastersizer application software.
Warning!
Due to the possible risk of sonication of the blood and its unknown effects,
never put fingers in the tank when the ultrasonic transducer is in opera-
tion.
Note
The Ultrasonics will switch off automatically after 20 minutes continuous
use.
Tank cover
The tank cover is there to protect the operator from splashes from the tank. Always
replace the cover after adding sample to the tank.
The tank cover is removed and replaced by holding on to the raised portions of the
cover.
Status indicator
A status indicator illuminates to indicate the operating condition when the disper-
sion unit is powered up:
Blue - full intensity
The dispersion unit is functioning correctly and the cell has been loaded into
the optical bench, (i.e. the dispersion unit is “active”).
Blue - pulsing
The dispersion unit is functioning correctly but its cell has not been loaded
into the optical bench, (i.e. the dispersion unit is at “standby”).
If communication has failed with the optical unit the status indicator will also
be on standby, but the optical unit indicator will be off.
Drain port
The drain port is the exit point where sample/dispersant leaves the dispersion unit.
A warning triangle warns that the contents of the tank are drained from this pipe.
The risk depends on the hazardous nature of the dispersants/samples being meas-
ured.
Refer to the connecting the dispersion units section, and the site requirements
section in the Basic guide, for advice on the drain/waste positioning.
Connecting the drain pipe
To connect the drain pipe:
1. Insert the pipe into the drain port fitting.
2. Tighten the collar nut until fully secure.
Removal is the reverse of the procedure.
A 90 degree support bracket can be fitted to the drain tube to direct the waste fluid
into the drain. Replacement drain pipes are available direct from Malvern Instru-
ments.
Note
It is important that the draining end of the drain pipe is above the level of
the waste liquid at all times. It must not be under the surface of the liquid
otherwise the dispersion unit will not drain efficiently.
Note
Using the Accessory controls in the SOP, the inlet ports can be used for
both tank filling, and cleaning. Refer to the Sample Dispersion-Acces-
sory SOP description.
Note
The upper dispersant inlet has no internal regulator controlling the disper-
sant input. It is therefore recommended that the supply to this inlet is ena-
bled and controlled through the use of an external pump and cable.
Note
Using the Accessory controls in the SOP, the inlet ports can be used for
both tank filling, and cleaning. Refer to the Sample Dispersion -Accessory
SOP description.
CAN connection
The CAN connection provides both the communications and power to operate the
dispersion unit.
The CAN cable is connected from the CAN connection to one of the CAN con-
nections on the side of the optical unit.
Auxiliary connector
When required, the auxiliary connector (AUX) is used for connecting any acces-
sory that can be used with the dispersion unit.
Note
The drain operation will not function when the dispersion unit is per-
forming a measurement. The function will only work when in standby
mode.
1
2
ill 8763
The Hydro EV dispersion unit uses a standard laboratory beaker to hold the
sample and dispersant liquid. Standard beaker sizes recommended are 600ml and
1000ml.
The pump head is tilted back, and a beaker containing an aqueous or non-aqueous
dispersant is then placed onto the beaker holder at the front of the unit. The pump
head is then tilted forward, lowering the pump arm into the beaker, and allowing
the sample to be pumped. Raising the pump head at any time will automatically
stop the pumping action.
The pump , controlled using the Mastersizer application software, circulates the
dispersant from the ‘to cell’ port of the dispersion unit to the wet cell located in
the optical bench, via the sample tubing. The dispersant is pumped through the
wet cell and then returns to the tank via the sample tubing and the ‘from cell’
port.
Sample is then added manually to the beaker by the user, as required. The stirrer
then agitates the sample, to stop it from settling or separating out, and then cir-
culates it through the system and wet cell to be measured using the optical unit and
software. Refer to the Mastersizer 3000 User Manual for advice on adding sam-
ple.
An ultrasonic transducer is provided to aid sample dispersion and can also be used
to remove bubbles from the flow path.
Once the sample has been measured using the Mastersizer optical unit, the pump
arm can be raised and the sampling beaker withdrawn, and the sample disposed of.
Caution!
Do not overfill the beaker as spillage may occur once the pump starts.
Clean any spillage off the covers immediately to prevent damage.
The tank contains the pump and stirrer assembly, described below, whilst an ultra-
sonic transducer (not shown) within the sample flow path also helps to disperse the
sample.
All functions of the tank area are controlled by the Mastersizer application software.
Once a measurement has finished, the pump head can be raised and the beaker
removed and emptied in to a sink or other waste container.
3 7
6 8 9
ill 8761
Pump head
By holding the pump head by the indent and front face, the pump head can be
raised and lowered into the beaker of sample. When the pump head is lifted, the
pumping action automatically stops and the cell and sample pipes are drained of the
sample and dispersant.
A light, positioned in the base of the pump head above the tank, is used to illumi-
nate both the beaker and the sampling fluid within.
The sampling pump and stirrer (described below) is attached to the bottom of the
pump head, whilst an ultrasonic transducer (not shown) within the sample flow
path also helps to disperse the sample.
ill 8762
The stirrer, located at the base the sampling pump, agitates the sample/dispersant
mixture ensuring it is adequately dispersed prior to a measurement. The central
sampling pump (in the middle of the assembly) circulates the sample through the
wet cell located in the measurement area of the optical bench.
The pump and stirrer speed is controlled by the Mastersizer application software.
Warning!
Never run the pump/stirrer without the beaker in place.
Warning!
Never put fingers into the beaker when the pump/stirrer shaft is rotating.
Caution!
Never operate the pump/stirrer at more than half speed with the tank
empty.
Ultrasonic transducer
The ultrasonic transducer (not shown) within the pump head is used to help dis-
perse samples. The power of the transducer and the ultrasonic timer are controlled
sing the Mastersizer Application software.
Warning!
Due to the possible risk of sonication of the blood and its unknown effects,
never place fingers in the beaker when the ultrasonic transducer is in oper-
ation.
Note
The Ultrasonics will switch off automatically after 20 minutes continuous
use.
Status indicator
A status indicator illuminates to indicate the operating condition when the disper-
sion unit is powered up:
Blue - full intensity
The dispersion unit is functioning correctly and the cell has been loaded into
the optical bench, (i.e. the dispersion unit is “active”).
Blue - pulsing
The dispersion unit is functioning correctly but its cell has not been loaded
into the optical bench, (i.e. the dispersion unit is at “standby”).
If communication has failed with the optical unit the status indicator will also
be on standby, but the optical unit indicator will be off.
ill 8898
To cell connection
The bottom connection is for connecting the wet cell sample outward tubing;
where the sample leaves the dispersion unit for the bottom connection of the wet
cell (yellow collar) in the optical unit.
The ‘to cell’ connection has yellow identifier markings.
From cell connection
The top connection is for connecting the wet cell sample return tubing; where the
sample returns to the dispersion unit from the top connection of the wet cell (blue
collar) in the optical unit.
The ‘from cell’ connection has blue identifier markings.
Connecting the wet cell sample tubing
To connect the wet cell tubing:
1. Push the wet cell tubing onto the connection. Ensure it is pushed on fully to
prevent any leaking risk.
2. Place a retaining clip over the connected tubing and compress using pliers to
provide a secure connection.
3. Follow the Hydro MV/LV wet cell connection procedure for connection to the
wet cell.
Removal is the reverse of the procedure. Ensure the cell is empty before
removing.
The retaining clips are removed by twisting apart using pliers - this will sepa-
rate the teeth allowing the clip to be removed.
Suitable aqueous and non-aqueous wet cell tubing is available direct from Malvern
Instruments.
CAN connection
The CAN connection provides both the communications and power to operate the
dispersion unit.
The CAN cable is connected from the CAN connection to one of the CAN con-
nections on the side of the optical unit.
Auxiliary connector
When required, the auxiliary connector (AUX) is used for connecting any acces-
sory that can be used with the dispersion unit.
1 3 2
ill 8764
The dispersion unit comprises a tank that holds the sample and dispersant liq-
uid; depending on the length of tubing used, the Hydro SM will require a maxi-
mum volume of 120ml.
Aqueous or non-aqueous dispersant is manually added into the tank. A pump
within the tank, its speed controlled using the dispersion unit controller , circu-
lates the dispersant from the ‘to cell’ port of the dispersion unit to the wet cell
located in the optical unit, via the sample tubing. The dispersant is pumped
through the wet cell and then returns to the tank via the sample tubing and the
‘from cell’ port.
Using a pipette or spatula, sample is added to the tank and dispersant as required. A
stirrer within the tank then agitates the sample, to stop it from settling or separat-
ing out, and then circulates it through the system and wet cell to be measured using
the optical unit and software. Refer to the Mastersizer 3000 User Manual for
advice on adding sample
Once the sample has been measured using the Mastersizer optical unit, it can be
disposed of using the drain outlet. The drain outlet is compatible with most aque-
ous and non-aqueous dispersants.
1
5
2
4
ill 8765
Caution!
Do not overfill the beaker as spillage may occur once the pump starts.
Clean any spillage off the covers immediately to prevent damage.
The tank contains the pump and stirrer assembly, described below.
Once a measurement has finished, the tank can be emptied using the drain valve
lever in the base of the dispersion unit. The sampling fluid is emptied through the
drain pipe out to a sink or other waste container.
Warning!
Never put fingers into the tank when the pump/stirrer shaft is rotating.
Caution!
Never operate the pump/stirrer at more than half speed with the tank
empty.
Tank cover
The tank cover is used to protect the operator from splashes from the tank and pre-
vent any ingress of dust when the system is left for extended periods. It also pre-
vents evaporation or the release of fumes when the system is in use (e.g. when
using a noxious solvent or sample).
Always replace the cover after adding sample to the tank.
B A C D E
ill 8766
2 1
ill 8855
The dispersion unit comprises a sampling cuvette that holds the sample and disper-
sant liquid together, the Hydro SV can contain a maximum volume of 7ml.
Aqueous or non-aqueous dispersant is manually added into the sampling cuvette. A
stirrer bar is added into the cuvette, and the cuvette then inserted into the cuvette
holder within the Hydro SV cell.
The complete cell is inserted into the cell bay of the optical unit. With the cell in
position, a motor within the cell rotates the stirrer bar continually circulating the
dispersant around the cuvette ensuring it is adequately dispersed prior to a meas-
urement. The stirrer speed is controlled using the Mastersizer software or front
panel dial. Refer to the Mastersizer 3000 User Manual for advice on adding sample.
Once the sample has been measured using the Mastersizer optical unit, it can be
disposed of by first removing the SV cell, and then removing the cuvette.
Note
As the Hydro SV incorporates a magnetic stirrer for dispersing the sample,
it is recommended that the Mastersizer 3000 is not used anywhere near
external magnetic fields, or used where stationary magnets may impact.
These may affect the effectiveness of the stirrer bar sample dispersion.
10
5 7 3
ill 8856
Note
The Hydro SV dispersion unit will generally be referred to as the "Hydro
SV" or "SV cell" or just "cell".
Cell shroud
The cell shroud prevents stray light entering the measurement area that may affect
a measurement. More importantly, the cell shroud stops human access to laser
radiation.
The cell shroud incorporates an arm that will open a mechanical shutter when
inserted into the cell bay of the optical unit. With the shutter open laser light is
allowed into the sample area. When the SV cell is withdrawn the shutter will move
back into position to prevent the emission of any laser light.
The system should never be used if the cell shroud or shutter arm is damaged.
Max. (7ml)
Min. (6ml)
ill 8857
Warning!
Never attempt to lift the optical unit by the locking handle of the cell. Read
the Health and Safety section in the Mastersizer 3000 Basic Guide for
details of correct moving techniques.
Drip tray
Any overspills will be captured within the drip tray and drained through a drain
port at the front of the cell and optical unit. If any liquid is noticed in the drip tray,
remove the cell and tip the contents away.
Pipette entry
Note
The pipette must be inserted fully before injecting the sample. Do not
drip sample into the top of the pipette entry hole.
The pipette entry is used for adding the sample into the cuvette once the SV cell has
been inserted into the cell bay of the optical unit. This enables sample addition to
be performed within the required obscuration range. The cuvette lid must be
removed first to allow this.
Sample is added by inserting the pipette until it stops. A guide within the pipette
entry ensures the pipette is positioned above the cuvette opening. Sample is then
injected as required. Take care not to overfill the cuvette.
Note
The internal pipette guide is curved to prevent any laser light escaping dur-
ing the sample addition.
The pipette must be removed once the sample is added. Refer to the Filling the
cuvette section.
Note
The software stirrer slider bar, and the SV front panel manual control dial
are synchronized. Altering the slider bar will alter the front panel display;
and vice-versa
Note
The cuvette and stirrer bar must be cleaned thoroughly before first use
and before performing any subsequent measurements. Refer to the main-
tenance chapter for details.
The technique for filling the cuvette used with the Hydro SV is the same as for any
cuvette, ensuing that the dispersant is carefully injected into the cuvette with the
minimum of bubbles produced.
The cuvette is filled and inserted into the SV cell while the cell is out of the optical
unit.
Note
It is recommend to not use dispersants with too high a viscosity. The
greater the viscosity of the dispersant, the less effective the stirrer bar sam-
ple dispersion will be.
Note
Any aqueous dispersant must be degassed fully before use. For aqueous
use only correctly degassed DI water (negligible dissolved C02), or signifi-
cant bubbles will form on the windows and stirrer and will affect the qual-
ity of the measurement.
Note
The maximum volume of the cuvette is 7ml. This corresponding to a min-
imum volume of 6ml dispersant + 1ml maximum of sample. If more than
7ml of sample/dispersant is inserted the cuvette will overflow.
ill 8858
To fill the cuvette:
Hold the cuvette at an angle, and with the syringe tip placed along an inner side of
cuvette, carefully inject the sample. The sample will flow along the side of the
cuvette slowly filling it up.
Rotate the cuvette while it is being filled, to prevent any spillage when as the maxi-
mum fill level is reached.
Continue filling until the minimum volume fill mark is reached (minimum 6ml).
ill 8859
Note
The stirrer bar must first be washed in the dispersant being used in the
measurement before inserted into the cuvette.
ill 8860
Place the cuvette lid on to the cuvette and place into the SV cell. Datum/position-
ing points in the corners of the cuvette holder aid correct insertion. The spout on
the top of the cuvette must be facing the front of the cell once inserted.
Secure with the cuvette clamps – ensure both clamps are fully in place after loading
the cuvette into the SV cell. Failure to secure the clamps may cause alignment and
measurement problems
You will note that the stirrer bar, will attach to the stirrer motor.
Press the speed dial to turn the SV cell on and test the SV operates correctly; the
stirrer bar should spin.
ill 8861
Place the SV cell into the Cell bay of the optical unit and Start the measurement.
Adding sample:
Take a pipette and draw the sample into it; filling until the maximum fill mark is
reached (maximum 1ml).
Note
The cuvette can hold a maximum total volume of 7ml of sample and dis-
persant. If the amount of dispersant in the cuvette is more than 6ml then
the amount of sample used must be less than 1ml, otherwise the cuvette
will overflow.
ill 8862
When in optical unit:
Note
To perform this action the cuvette lid must not be fitted.
Specific pipettes are required for use in the optical unit. When the measurement
requests the sample to be added, take the pipette and insert into the pipette access
until it stops and cannot be inserted anymore. While monitoring the live display,
add sample until the obscuration is in range.
Remove the pipette once the sample has been added.
ill 8863
Press Start to continue and complete the measurement.
When not in optical unit:
When the measurement requests the sample to be added, press the unlock button
on the cell handle and remove the cell.
Unlock the cuvette locks and place the cuvette alongside the SV cell. Ensure the
cuvette is kept vertical at all times.
Take a pipette and draw the sample into it; filling until the maximum fill mark is
reached (maximum 1ml), then insert the sample into the top of the cuvette.
ill 8864
Take the cuvette and place into the SV cell. Secure with the cuvette locks.
You will note that the stirrer bar, will attach to the stirrer motor.
Press the speed dial to turn the Hydro SV on and test the SV operates correctly; the
stirrer bar should spin
Insert the SV cell into the optical bench. The instrument will again align, and the
obscuration should then be checked.
If ok, continue with the measurement; if obscuration is not ok, repeat the sample
insertion.
Caution!
The flow cell is an optical device. Scratches to the surfaces of the cell may
affect performance.
Each Hydro dispersion unit will be connected to a matching Hydro series wet cell.
Two wet cells are available, for use with aqueous or non-aqueous based samples.
The dispersion unit continually circulates the sample/dispersant from the disper-
sion unit to the wet cell and through the analyser beam of the optical unit so that a
measurement can be performed.
The cell windows in the wet cell are critical parts of the measurement optical path
of the system and should be kept clean and free from scratches at all times. Refer to
the Maintenance chapter for details on cleaning/maintaining the cell.
Note
If the cell is not used for short periods (up to 24 hours), leave the cell and
beaker full of clean dispersant so that the cell windows do not dry out,
leaving smears or water marks on the window surface. If the cell is not to
be used for longer periods, remove and dry the cell windows.
The system should never be used if the cell shroud or shutter arm is damaged.
3 5
ill 8672
The cell windows can be removed to allow cleaning; the cell lock handle is
rotated and the front plate of the cell, containing a cell window and seal pair,
removed. The cell windows are delicate and should be treated with caution; refer to
the Maintenance chapter for details on removing the front plate and cleaning the
cell windows.
The cell window seals prevent the windows from leaking. Inspect them regularly,
especially if aggressive solvents are used as a dispersant. Details on changing the
seals can be found in the Maintenance chapter.
For the standard aqueous wet cell (blue badge) Fluoroelastomer (FKM)
seals are fitted.
For the chemically compatible cell (red badge) Perfluoroelastomer (FFKM)
seals are fitted.
Warning!
Never attempt to lift the optical unit by the locking handle of the cell. Read
the Health and Safety section in the Mastersizer 3000 Basic Guide for
details of correct moving techniques.
Drip tray
Any small leaks will be captured within the drip tray and drained through a drain
port at the front of the wet cell and optical unit. If any liquid is noticed in the drip
tray, remove the cell and tip the contents away. Locate and fix any leaks.
Warning!
Fully drain the cell and sample tube before attempting to disconnect the
cell.
ill 8673
The Heat exchanger consists of a 'jacket’ that is wrapped around the flow cell input
and output pipes. Into this jacket cooling/heating liquid is fed to cool/heat the sam-
ple. The heat exchanger can be used for two functions:
To heat or cool the sample so that sample measurements can be performed at
different temperatures.
To eliminate temperature fluctuations after any sonication of the sample. This
can be important when working with some organic solvents, where tempera-
ture fluctuations can cause a slight misalignment of the system. This misalign-
ment is caused by the changes in refractive index that are observed in solvents
as the temperature changes. This may cause the presence of large particles to be
reported and thus affect the particle size distribution measured by the Master-
sizer system.
The water cooling would normally be provided by an external heater/chiller circu-
lator unit. This will be connected to the inlet and outlet ports on the front
of the wet cell.
Always fill from the bottom inlet connection . This is to prevent any air bub-
bles being caught in the heat exchanger arrangement.
HYDRO
3
2
4
5
8
2m max
ill 8674
Note
The drain/waste must be within 2m of the dispersion unit and lower than
the bench surface, with the drain tube sloping gently downhill and have no
loops or kinks, so any liquid drains efficiently due to gravity. It can be a
normal sink, provided the sample and dispersant are non-hazardous.
It is important that the draining end of the drain pipe is above the level of
the waste liquid at all times. It must not be under the surface of the liquid
otherwise the dispersion unit will not drain efficiently.
Hydro SV connections
3
2
ill 8854
Hydro SM connections
HYDRO
3
2
4 5
ill 8767
Note
The drain/waste must be within 2m of the dispersion unit and lower than
the bench surface, with the drain tube sloping gently downhill and have no
loops or kinks, so any liquid drains efficiently due to gravity. It can be a
normal sink, provided the sample and dispersant are non-hazardous.
It is important that the draining end of the drain pipe is above the level of
the waste liquid at all times. It must not be under the surface of the liquid
otherwise the dispersion unit will not drain efficiently.
Hydro EV connections
HYDRO
3
2
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ill 8675
Note
The External dispersant pump and external triggering control is only com-
patible with later versions of software, please contact Malvern for details.
Supplied Pump
components Auxiliary Control cable
Tubing. For chemical compatibility of the tubing, refer to the
appendix.
Connection
The below illustration and paragraphs describe how to use the peristaltic pump
when connected into the Mastersizer 3000 system.
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2
3
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ill 8893
Refer to the Connecting the Dispersion units section for connection of the
Hydro LV and MV to the Optical unit.
Pump setup
The information below on setting the pump is taken from the pump user manual.
Refer to this manual for complete information regarding the operation of the
pump.
1. The pump must be set for the voltage specific to the country it is installed into.
Set the mains voltage selector at the back of unit to the correct voltage for
the country you are in. Refer to the Peristaltic pump user manual.
2. Connect the power cable into the back of the pump.
3. Connect the auxiliary control cable from the dispersant unit into the
back of the pump.
4. The pump must be set for Analogue-Automatic operation mode using the
control cable and Malvern software (Auto restart mode). In this mode the
pump will automatically start in automatic mode when turned on. To do this:
Turn pump off using mains switch on back of unit.
Hold down the Start button on the front of the pump, and turn the mains
switch on. An exclamation mark ( ! ) will appear on the screen.
Put pump into Analogue-Automatic mode.
Press Mode until ANA is displayed on screen, with the word Auto appearing
in the corner to indicate that the pump is in analogue and automatic mode.
The pump is now set.
It will now always restart in Analogue-Automatic mode whenever the power is
connected.
Note
With the auxiliary control cable connected and the pump set to auto mode,
manual mode will not be available.
Warning!
If the auxiliary cable is disconnected when the power is still supplied the
pump will briefly rotate. This may deposit any dispersant present in the
tubing.
Tubing Connection
The pumphead is uni-directional and travels anti-clockwise. The tubing must
be connected so that the flow travels from the right (the dispersant source) to the
left (the dispersant inlet).
Also refer to the pump manual for complete information on installing the tubing
into the pumphead.
1. Connect the tubing from the dispersant source to the upper externally
regulated dispersant inlet . Tubing lengths upto 15m can be used.
2. Place a retaining clip over the connected tubing at the dispersant inlet and
compress using pliers to provide a secure connection.
3. Open the top of the pumphead.
4. Set the tube clamps to the correct tube size.
Using the adjustment knobs on either side of the pumphead set the tube
clamps to 4.8mm as indicated on the pumphead scale (4.8mm is the inner
diameter of the supplied Tygon tubing).
5. Slide the tube into the open pumphead over the rollers. Ensure the tube is not
twisted or stretched.
6. The head can be loosened or tightened around tubing using the 2 adjustment
knobs on the sides of the pumphead. Ensure that the head height is tight
enough so that tubing cannot move forward or backward but loose enough that
flow is not restricted.
7. Close the top of the pumphead.
Control
Once setup the pump will always start in Automatic mode, with the Mastersizer
system automatically detecting the pump. Commands to activate the pump are pro-
vided using either the Sample dispersion - Accessory SOP window or the
Accessory control panel. Refer to the Software chapter for details.
Note
If the distance between the system and the liquid container is large, the
system may first need priming by performing a number of fills using the
accessory controls
Switching Box
A Switching box is available to allow a customers external pump to be controlled
from the Hydro LV and Hydro MV dispersion units. This allow dispersant to be
supplied from an unpressurised tank or flask.
Contact Malvern Instruments for more details
Making a measurement
Making a measurement using the Hydro LV, MV, EV, SV and SM dispersion units
is fully documented in the Mastersizer User Manual. Refer to that manual for
details.
The dispersion units can be controlled in several ways;
Manually or automatically by running an SOP. The system automatically
detects which dispersion unit and cell is connected. If more than one disper-
sion unit is connected, the system detects all dispersion units connected, but
only the dispersion unit that has its cell installed on the optical unit will be
“active”.
Alternatively the dispersion unit can be controlled by a separate manual acces-
sory control dialogue. This will enable simple control of the dispersion unit,
allowing individual selection and operation of the unit’s functionality.
If a fully manual accessory is connected to the optical unit, this will not have an
automated or manual software control, but will be controlled directly.
These are described in the following pages.
2. Select an SOP template from the list in the New SOP window or click the
From existing SOP... button to locate an SOP in the file system that fulfils
(or is close to) your required criteria.
3. The SOP Editor window is now displayed. This will be configured to apply to
the dispersion unit selected.
4. Complete the SOP Editor as described in the Mastersizer User Manual.
Sample - Dispersant
- Hydro MV/LV (MAZ3210/3310) units only
Please also refer to the Sample - Dispersion description in the Making
measurements chapter of the main Mastersizer user manual.
The Sample - Dispersion SOP window contains a level sensor threshold field
where a value can be inputted that is suitable for the level sensor to detect the
dispersant level when filled. The value will be different depending upon the
dispersant used.
The level sensor in the dispersion unit automatically stops the tank being overfilled
above a certain level. If the tank fails to fill properly then the level sensor threshold,
for the dispersant being used, may need adjusting. This value can be changed either
manually (for the current measurement only) or by using the dispersants
database, to store the new values for future use.
Configuring this threshold value will be done using the accessory controls
window described later in this chapter.
Section Description
Stirrer speed This Hydro dispersion units have a variable-rate stirrer allow-
ing flexible control of sample flow and agitation. The stirrer
speed may be controlled manually using the Wet Accessory
dialogue or by a predefined SOP for automatic operation.
Manual control would typically be used to determine the
optimum measurement setting prior to using an SOP proce-
dure or when doing one-off manual measurements.
To control the stirrer from an SOP, determine the optimum
stirrer speeds initially using manual control, ensuring that the
lowest setting to give satisfactory dispersion is obtained.
Section Description
Stirrer speed Make a note of the settings and enter these into the SOP
(continued) Accessory control settings. Click and drag the slider bar to
set the speed.
It is also possible to control the accessory manually by using
the Accessory Controls panel (from the manual measure-
ment window) or the from the Tools-Accessories option at
any other time.
Hydro SV only. The speed on the Hydro SV is also con-
trolled using the dial on the front panel of the SV accessory.
Note that the software stirrer slider bar, and the SV front
panel dial are synchronized. Altering the slider bar will alter
the front panel display; and vice-versa
Tank fill The tank can be filled with dispersant manually or automati-
behaviour cally. When set to Automatic the dispersant is plumbed into
(Hydro LV/MV) the lower dispersant inlet port at the rear of the accessory
and an internal regulator valve controls the flow of dispersant
into the tank.
However, if an organic dispersant is to be used, it is unlikely
that this dispersant will be plumbed into the accessory. In
these situations the filling of the tank can be set to Manual.
Under manual filling the solenoid valve is switched off (this
will mean that the dispersant inlet does not have to be dis-
connected during a manual fill) and the tank can be filled by
hand. The software will tell the operator when to fill the tank
during an SOP measurement.
The tank filling can be done by carefully pouring the disper-
sant directly into the tank, or by using the upper dispersant
inlet port. In this case the supply to this inlet is enabled either
through the use of an external pump and cable, or other reg-
ulation method.
Dispersant Source
This option enables the dispersant inlet to be switched
between the lower internally regulated inlet port (commonly
used for aqueous samples) and the upper externally regu-
lated inlet port (commonly used for non-aqueous samples) –
refer to the Features of the Hydro MV/LV dispersion units
section in the user manuals.
This is useful for instances after a measurement has been
performed using an expensive organic dispersant - supplied
via the upper externally regulated non-aqueous inlet. It may
be undesirable to then use this expensive dispersant for
cleaning, so the tank and cell can then be cleaned with a
cheaper comparable alternative - supplied via the lower
internally regulated aqueous inlet.
Section Description
Tank fill The Dispersant source options are:
behaviour Auto - Both inlets activated and can be used. This is the
(continued) default selection, and is the setting used for SOPs that were
(Hydro LV/MV) set up in previous software versions where this option did
not exist. This will activate both the lower regulated and
upper externally regulated inlets when required.
Note: If using this option, It is advised that only one supply is
connected to the accessory to prevent the two dispersant
supplies mixing inadvertently.
Internal - Will control and activate the lower internally regu-
lated dispersant inlet port (There is an internal regulated
valve rated to handle mains pressure).
External - Will control and activate the upper externally reg-
ulated dispersant inlet port (The upper dispersant inlet is
externally regulated.
There is no internal regulator controlling the dispersant. It is
therefore recommended that the supply to this inlet is ena-
bled through the use of an external pump and cable). Refer
to the Introduction and hardware chapter for details on
using an external pump.
Note: both valves will be in a closed state when in standby
or when power is supplied to the accessory.
Filling the tank manually:
Fill the tank slowly until the tank light flashes - this will indi-
cate the correct fluid level for adding sample and running
measurements. If the tank is filled higher than this, sample
and particles may be lost via the over-flow system (drain),
leading to an incorrect particle size distribution being
reported.
Degassing
If dispersant is stored under pressure or at low temperature,
consider de-gassing before use. The pressure release or
temperature rise reduces the solubility of gases, resulting in
possible bubble formation in the pipes and tank.
Select the Degas after fill check box to remove bubbles and
dissolved gases from the dispersant before use. Once the
tank is filled, this runs the stirrer briefly to dislodge any bub-
bles off the cell walls and out of cell, then stops the stirrer to
allow the bubbles to be released.
Note: It is preferable that all dispersants are degassed
before being added to the system. Degas by storing the dis-
persant at room temperature and pressure for before use.
Section Description
Ultrasonics This sample dispersion unit has an ultrasonic transducer
(Hydro LV/MV/EV) which can assist the dispersion of cohesive samples. The
level and duration of ultrasound may be set manually using
the Wet Accessory dialogue or may be set by a predefined
SOP for automatic operation.
To determine the correct ultrasonic level for an SOP, initially
determine the optimum ultrasound level and duration using
manual control, ensuring that the lowest setting giving satis-
factory dispersion is obtained. Record the settings and
transfer these to the SOP in the Sampler Settings page using
the slider controls. Click and drag the slider bar to set the
ultrasonics power level.
Set the Ultrasound mode to one of the following:
None - No ultrasound is applied.
Pre-Measurement - ultrasound is activated for a set time
prior to measurement. For pre-measurement mode, enter
the required duration in seconds in the Duration box.
Continuous (from Sample Addition) - ultrasound is acti-
vated after sample is added and will run continuously.
Continuous (from Measurement Start) - ultrasound is
active throughout the measurement. Ultrasound will start
after the electrical background is complete. The stabilising
period will add a delay between the electrical background
and the optical alignment - during this delay ultrasound will
be on allowing bubbles to be driven from the dispersant.
To manually control the ultrasonic level from the Wet Acces-
sory dialogue, either select and drag the Ultrasound slider
bar to set the level, or select the bar and use the keyboard
control up/down/left/right arrows; this will step the ultrasonic
level up or down in 10% divisions.
Alternatively, for an exact setting, double click on the dis-
played ultrasonic value and type in the required level.
Degas after ultrasound - select this check box to remove
any bubbles that may have occurred during ultrasound.
Align after ultrasound - select this check box to align the
cell once the ultrasound has completed.
Pulsed Enable pulsed ultrasonication - in this mode, ultrasonica-
Ultrasonics tion is applied in pulses (with fixed duration on and off
(Hydro LV/MV/EV) pulses). This option can be used in combination with both
continuous or timed ultrasonication mode. Specify the dura-
tion of on and off pulses by entering the required values
(seconds) into the corresponding boxes.
Note
The Ultrasonics will switch off automatically after 20 minutes continuous
use.
Section/option Description
Clean Sequence Each Clean type specifies a set number of cycles (nothing
further is changed in the cleaning method). Select a Clean
type of either Quick, Normal, Extensive or Custom. If Cus-
tom is selected the user must also manually specify the
number of Clean cycles.
If measuring the same sample type in succession a Quick
clean may be sufficient.
If making the last measurement of the session, it is prudent
to perform an Extensive clean to ensure that the system is as
free as possible from contamination in readiness for the next
measurement session.
Tank fill Refer to the Sample dispersion - Accessory section above
behavior for a description of the Tank fill behavior, including filling
(Hydro LV/MV) the tank manually; and the Dispersant source and Degas-
sing options.
Level sensor threshold
The level sensor threshold value is only required for Hydro
units that are fitted with an analogue sensor (MAZ3210/
3310). Refer to the Sample - dispersants (SOP) and the
Accessory Panel: Hydro LV/MV topics.
Ultrasonication Ultrasound can reduce agglomeration, which may help fur-
ther with cleaning. Select whether to Use ultrasound during
the clean sequence or No ultrasound during clean.
Tip
The same controls are also available from the Active accessory control
feature (choose Accessories from the Tools command ribbon).
The options available on this panel depend on the active accessory as follows:
Hydro LV/MV
The accessory controls panel for the Hydro LV/MV is shown as follows:
Section/option Description
Dispersant The Sample - Dispersion SOP window contains a level sen-
- Sensor sor threshold field where a value can be inputted that is suit-
Threshold able for the level sensor to detect the dispersant level when
(Only for Hydro filled. The value will be different depending upon the disper-
MV/LV units that sant used.
are fitted with an Refer to the description in the Sample - Dispersant (Hydro
analogue sensor - MV/LV (MAZ3210/3310 units only) SOP topic earlier in this
MAZ3210/3310) chapter.
Section/option Description
Dispersant Select Fill to fill the Hydro unit with dispersant.
- Fill The manner of filling depends upon the fill options selected.
Automatic fill
Automatic fill.
Manual fill
This is the default selection and allows back-compatibility
Automatic fill
with previously created SOPs. In this mode, the function
(Internal)
opens the internal dispersant valve (and external valve if con-
Automatic fill
figured) and then pumps dispersant into the unit until the
(External)
correct level is reached (detected by a sensor) and then
closes the dispersant valve.
Note: If using this option, It is advised that only one supply is
connected to the accessory to prevent the two dispersant
supplies mixing inadvertently.
To prevent overfilling, the Fill button command is disabled
when the Automatic fill option is selected if the chosen dis-
persant has a level sensor threshold of 0 (zero). The thresh-
old value has to be set for the Fill button to become enabled.
As with the tank light, this indicator can be used when filling
the tank manually.
Manual fill.
Manually fill the tank slowly until the indicator shows full -
this will indicate the correct level for adding sample and run-
ning measurements. If the tank is filled higher than this, sam-
ple and particles may be lost via the over-flow system
(drain), leading to an incorrect particle size distribution being
reported.
Automatic fill (Internal).
This fill mode uses the Lower internally regulated dispersant
inlet port to fill the tank. This is normally used for aqueous
dispersants. As with Automatic fill above, this mode opens
the dispersant valve, pumps dispersant into the unit until the
correct level is reached and then closes the dispersant valve.
Automatic fill (External).
This fill mode uses the Upper externally regulated dispersant
inlet port to fill the tank. This is normally used for non-aque-
ous dispersants.
There is no internal regulator controlling the upper disper-
sant inlet. It is therefore recommended that the supply to this
inlet is enabled and controlled through the use of an external
pump and cable. Refer to the Introduction and hardware
chapter for details on using an external pump.
Section/option Description
Dispersant This mode will work like Automatic fill above, except an
- Fill external pump or regulator is used to control the flow of dis-
(continued) persant into the unit. When the correct level is reached, the
external pump (or regulator) will be stopped.
Dispersant Select Degas after fill to remove any bubbles and dissolved
- Degas after fill gases from the fresh dispersant before use. Once the tank is
filled, this runs the stirrer briefly to dislodge any bubbles off
the cell walls and out of cell, then stops the stirrer to allow
the bubbles to be released.
Refer to the Hydro LV/MV/EV Accessory control settings
(SOP) section for more information on degassing.
Dispersant Empties all dispersant (and sample) from the Hydro unit.
- Empty This function opens the drain valve and initiates a pumping
sequence - the process stops when the unit is empty and
then closes the drain valve.
Stirrer Use the slider bar to set the RPM of the stirrer. In Manual
Measurement mode it is necessary to start the stirrer manu-
ally before making the measurement. To initiate the stirrer
once the speed has been set, click the Start button. To stop
the stirrer click the Stop button.
The sliders change to show the difference between the
requested and actual speeds.
The grey bar shows the requested speed:
The actual speed is less the requested speed. This will nor-
mally be seen during a fill operation:
Section/option Description
Stirrer The actual speed is more the requested speed. This will nor-
(continued) mally be seen during a fill or clean operation:
Section/option Description
Valves Opens/closes the dispersant inlet valves.
- Dispersant valve Controlling the valve in this way allows a manual fill to be
done using the dispersant inlets.
This might be required to only add a certain amount of dis-
persant, without using the level sensor, or if the system had
been partially drained (using the Drain valve option) and
then needs to be manually topped up.
Three valve options are available:
Auto
This is the default selection and allows back-compatibility. In
this mode, the function opens the internal dispersant valve
(and external valve if configured).
Note: If using this option, It is advised that only one supply is
connected to the accessory to prevent the two dispersant
supplies mixing inadvertently.
Internal
This fill mode uses the Lower dispersant inlet: (Internally reg-
ulated inlet) to fill the tank.
External
This fill mode uses the Upper dispersant inlet (Externally reg-
ulated inlet) to fill the tank.
ton .
Note: In the Active accessory control window (Tools-
Accessories) pressing Clean will start the cleaning
sequence
Refer to the Dispersant section above - Fill and Degas
options - for a description of the Tank fill behavior and
Degassing function.
Hydro EV
The accessory controls panel for the Hydro EV is shown as follows. Each section
can be collapsed to save space on the Measurement window.
Section/option Description
Stirrer Use the slider bar to set the RPM of the stirrer. In Manual
Measurement mode it is necessary to start the stirrer manu-
ally before making the measurement. To initiate the stirrer
once the speed has been set, click the Start button. To stop
the stirrer click the Stop button.
Ultrasound Select the Manual option if you wish to start and stop the
- Manual / Timed ultrasound manually for a period of time.
Select the Timed option to perform a precisely timed period
of ultrasound application. When Timed is selected, the timer
controls become available - click +/- to increase/decrease
the time period for which ultrasound will be applied.
Section/option Description
Ultrasound This option can be used in combination with both continuous
- Continuous / or timed sonication mode. Specify the duration of on and off
Pulsed pulses by entering the required values (seconds) into the
(continued) corresponding boxes.
Hydro SV
The accessory controls panel for the Hydro SV is shown as follows:
Section/option Description
Stirrer Use the slider bar to set the RPM of the stirrer. In Manual
Measurement mode it is necessary to start the stirrer manu-
ally before making the measurement. To initiate the stirrer
once the speed has been set, click the Start button. To stop
the stirrer click the Stop button (or alternatively push on the
speed control dial on the unit).
Stirrer The sliders change to show the difference between the
(continued) requested and actual speeds
The grey bar shows the requested speed:
Note: The software stirrer slider bar, and the SV front panel
manual control dial are synchronized. Altering the slider bar
will alter the front panel display; and vice-versa
The Stirrer speed can be controlled from the software when
the instrument is not installed into the instrument cell bay;
but only when the dispersion unit is 'active', as indicated on
the status bar.
Hydro SM
The Hydro SM is controlled via the speed control on the front of the controller
unit.
Depending upon the sample being measured and the SOP routine being followed
the speed of the pump can be varied between 350 and 3500rpm. The monitored
speed is shown on the front panel display.
Maintenance
Introduction
This chapter covers all the user maintenance procedures for the dispersion unit. Do
not attempt any maintenance procedure not specified here. This chapter covers:
Maintenance schedule
This section suggests a maintenance schedule for inspecting and cleaning the dis-
persion unit and its respective components.
Maintenance procedures
This section describes how to perform various maintenance procedures and actions
identified in the schedule to help ensure the dispersion unit is kept working opti-
mally. Maintenance procedures described are:
Cell window inspection and cleaning procedures
This section includes topics on:
How to inspect the cell windows, in case of poor background results.
Cell windows removal and inspection.
How to inspect the quality and cleanliness of the windows.
Appropriate cleaning techniques.
Warnings
General
Warning!
The dispersion unit contains no internal serviceable parts. Never attempt
to remove the covers of the optical bench or dispersion unit. Removal of
the covers invalidates the warranty and may expose the user to dangerous
laser radiation.
Warning!
Failure to follow these guidelines could result in the emission of laser radi-
ation or exposure to hazardous voltages. Laser radiation can be harmful to
the body and can cause permanent eye damage.
The Hydro dispersion units do not contain a laser but are connected to the
optical unit that does.
Warning!
Before carrying out any maintenance operation, read and observe the safety
warnings listed in the Mastersizer Basic Guide.
Warning!
Before cleaning, always disconnect the unit from the power supply and
computer and disconnect all electrical cables.
Ensure the unit is completely dry before re-applying power.
Maintenance schedule
Follow the maintenance schedule below to keep the dispersion unit working well.
This list is only a guide; the exact frequency at which to perform tasks depends on
many factors, including:
The samples being measured.
The dispersant being used.
The environmental conditions.
The number of measurements made (frequency of use).
The procedures indicated below for each Hydro dispersion unit are described in
the following pages of this chapter.
Hydro MV / Hydro LV
Procedure Period/situation
Inspect cell windows The cell windows should be checked for general
for dirt and scratches cleanliness every day, or if during a background
measurement either of these is seen:
One of the first few detectors displays a value
above 100 light energy units.
Background signal over 20 light energy units
recorded by one of the detectors above detector
20 (see below).
Either of these situations would indicate a poor
background; this will effect the quality of any meas-
urements.
Check the window At least once a month. Always watch for signs of
seals for damage leaks and rectify immediately.
Clean the covers Once a month.
Clean the sample flow Contamination by coarse particles or bubbles in the
path dispersant may cause fluctuations in the background.
Clean the path using the cleaning options.
Clean the sample tank If changing dispersant types, or if sample is seen to
adhere to the sample tank and the normal flush rou-
tine fails to remove it.
Replace the dispersant If the tubing leaks or becomes discoloured. This may
tubing allow bubbles to enter, causing rapid fluctuations in
the background (see below).
Perform a Quality Audit At least once a week or as internal quality procedures
Standard measurement specify.
Hydro EV
Procedure Period/situation
Inspect cell windows The cell windows should be checked for general
for dirt and scratches cleanliness every day, or if during a background
measurement either of these is seen:
One of the first few detectors displays a value
above 100 light energy units.
Background signal over 20 light energy units
recorded by one of the detectors above detector
20 (see below).
Either of these situations would indicate a poor
background; this will effect the quality of any meas-
urements.
Check the window At least once a month. Always watch for signs of
seals for damage leaks and rectify immediately.
Clean the covers Once a month.
Clean the sample flow Contamination by coarse particles or bubbles in the
path dispersant may cause fluctuations in the background.
Clean the path using the cleaning options.
Inspect and clean the If changing dispersant types, or if sample is seen to
sampling pump head adhere to the sampling head and the normal clean
routines fails to remove it.
Replace the dispersant If the tubing leaks or becomes discoloured. This may
tubing allow bubbles to enter, causing rapid fluctuations in
the background (see below).
Perform a Quality Audit At least once a week or as internal quality procedures
Standard measurement specify.
Hydro SM
Procedure Period/situation
Inspect cell windows The cell windows should be checked for general
for dirt and scratches cleanliness every day, or if during a background
measurement either of these is seen:
One of the first few detectors displays a value
above 100 light energy units.
Background signal over 20 light energy units
recorded by one of the detectors above detector
20 (see below).
Either of these situations would indicate a poor
background; this will effect the quality of any meas-
urements.
Check the window At least once a month. Always watch for signs of
seals for damage leaks and rectify immediately.
Clean the covers Once a month.
Clean the sample flow Contamination by coarse particles or bubbles in the
path dispersant may cause fluctuations in the background.
Inspect and clean the If changing dispersant types, or if sample is seen to
tank adhere to the top of the tank and the normal clean
routines fail to remove it.
Replace the dispersant If the tubing leaks or becomes discoloured. This may
tubing allow bubbles to enter, causing rapid fluctuations in
the background (see below).
Perform a Quality Audit At least once a week or as internal quality procedures
Standard measurement specify.
Hydro SV
Procedure Period/situation
Inspect cell windows The cell windows should be checked for general
for dirt and scratches cleanliness every day, or if during a background
measurement either of these is seen:
One of the first few detectors displays a value
above 100 light energy units.
Background signal over 20 light energy units
recorded by one of the detectors above detector
20 (see below).
Either of these situations would indicate a poor
background; this will effect the quality of any meas-
urements.
Check cuvette body for Periodically check for leaks from cuvette body. if any
leaks and damage leaking occurs or damage is visible contact Malvern
instruments
Clean the covers Once a month
Pipette guide tube Clean as required depending upon usage. Also check
for damage ensuring guide tube alignment for adding
sample into cell is correct.
Inspect cell holder Clean the area where the cuvette is positioned.
Check condition of cuvette locks - do they work cor-
rectly.
Inspect stirrer bar Inspect the stirrer bar before use. A worn, damaged
or dirty stirrer bar may not rotate correctly and will
therefore not disperse the sample sufficiently.
Maintenance procedures
Inspection of cell windows - Poor background
The cell windows should be inspected for cleanliness every day and after each
measurement session. Problems which indicate the need for cleaning or mainte-
nance are the following. These expand on the situations in the first row of the
maintenance schedule table.
ill 8830
If your system displays high detector channels, refer to the Cleaning the cell
windows section as described later in this chapter and remove and clean the
cell windows.
ill 8829
Bubbles may enter the system because of high pump or stirrer speeds with viscous
dispersants or those containing surfactants, or due to leaking tubing or seals. Check
and replace any damaged tubing or seals as described later in this chapter.
Note
The cell window faces must not be touched directly during the removal
and replacement procedure. Lens tissues should be placed over the win-
dow faces where necessary.
Standard laboratory gloves should also be used when handling the wet cell
seals. Malvern recommends disposable, powder free, nitrile (NBR)
gloves.
ill 8676
Whilst holding the cover plate slightly above a clean lens tissue, place another lens
tissue over the cell window area and using light pressure push the cell window and
seal out from the cover plate onto the bottom lens tissue.
ill 8677
Holding onto the ends of the seal turn the cell seal and window assembly over, on
the lens tissue, so the seal is uppermost.
ill 8678
While holding the centre of the cell window down with another lens tissue, take
hold of the longest end of the seal, and lift the seal clear of the window.
Repeat the procedure for removing the remaining cell window and seal from the
main body of the cell. This time though place the cell holder on its side again with
a clean lens tissue positioned under the rear cell window, then remove the cell win-
dow and seal as described above.
ill 8679
Caution!
The outer faces of the cell window are optically coated; treat them with the
same care as a camera lens.
Caution!
Do not wipe the windows with an ordinary dry cloth as this will cause
scratches. Always use the procedure below to clean the surfaces.
Note
The cell windows are part of the optical system and removing them for
cleaning will change their position. Remember to add an Align stage to the
next measurement sequence or click the Align button.
Note
Ensure that the face with the larger diameter is facing down when
inserted in to the cell seal.
ill 8727
Place the wet cell cover plate on to a flat surface with the seal cavity facing upward.
Holding by the ends of the seal, pick up the cell seal and window assembly and turn
it over so that the circular section is facing downward. Place over the seal cavity of
the cover plate and line up the lugs on the seal with the corresponding cut-outs in
the circular measurement area of the cover plate, then place it carefully to rest on
top of the plate - do not insert the assembly yet.
Without touching the exposed window face, push the circular section of the seal
into place in the measurement area of the cover plate by rocking the seal and win-
dow down.
Push the seal/window down at one end in the places indicated, then repeat
at the other end . Repeat these steps until the window is fully inserted out in
the measurement area.
A
B
ill 8681
Once finished the circular section of the seal must be flush with the flat surface of
the measurement area of the cover plate. There must be no bulges in the seal. The
section of the seal with the flat sealing face must be located fully into the seal cavity,
edge to edge.
The seal in its fitted position.
ill 8682
Repeat the above procedure when replacing the cell seal/window assembly into the
main body of the cell.
from the fingers, hold the window with the fingers at the top and bottom and wipe
from side to side so that if any grease is picked up, it is not deposited on the surface.
Do not use rubber gloves to hold the window. Gloves invariably have oils and short
chain polymers in the surface; some of these oils, especially silicone components,
are more difficult to remove than finger smears. Never bring silicone products
into close contact with glass optical components. Clean hands are best.
Caution!
If any silicone oils are deposited on the glass surface they adhere so
strongly that it is impossible to clean them off, ruining the component.
Cleaning steps
Depending upon the quality and cleanliness of the windows, use the appropriate
cleaning technique as described. Read through the below steps to determine the
correct techniques required; these are described in order of severity and contami-
nation.
It is recommended to inspect the cell window in reflected light from a fluorescent
tube or other light source.
Gritty surface If the surface has fingerprints on it or has not been cleaned
particles / for a long time, assume there is grit present. First wash the
Smeared surface surface then wipe it as described; refer to the Washing cell
- with grit windows and Wiping cell windows sections.
Dusty surface If the surface is just dusty use a clean air aerosol duster or
soft brush; refer to the “Clean air” aerosol dusters and
Brushing optical surfaces sections below. If marks are pre-
sent afterwards wipe the surface as described in Wiping cell
windows.
Smeared surface If the surface is smeared and you are sure there is no grit on
- no grit it, wipe the surface as described below in Wiping cell win-
dows.
Caution!
The outer faces of the windows have an anti-reflective coating and are
more prone to scratching than the inner surfaces. Be careful not to touch
the faces of the windows or put them down on dirty surfaces.
Caution!
Never use acetone for cleaning optical components as the adhesives used
to bond them may leach out and be deposited across the component, ren-
dering it useless. Ethanol is much safer.
3. Use each tissue for one pass only. This is the only way to ensure a clean
undamaged surface. If a wipe has done its job it will be loaded with grease from
the surface. Wiping the surface again will just deposit the grease back on the
surface. Worse, if the wipe has lifted off some remaining grit this could scratch
the clean surface.
4. Marks from the o-rings usually form an oily line around the outer part of the
optical surface. With surfaces contaminated in this way, wiping from the centre
outwards prevents the oily mark from being spread from an unimportant area
across the window centre. If there are smears associated with starting the pass
in the centre of the surface, once the o-ring marks have been completely
removed give the surface a single wipe from side to side.
5. Re-inspect the window; if it’s still marked, repeat the procedure with a new
clean tissue.
Note
If marks remain, use a liquid cleaner such as Ethanol or Propan-2-ol. This
can be soaked on a cotton wool bud and wiped across the window gently.
After one pass over the window discard the bud to avoid scratching. Re-
inspect the window and repeat until clean.
Caution!
When changing the tubing do not allow any dispersant or sample to come
into contact with the system covers. Some samples can cause permanent
damage to the surfaces.
Warning!
Do not allow dispersant or sample to come into contact with the skin.
Some dispersants and samples may cause injury.
If organic solvents are regularly used as dispersants, the flexible tubing that con-
nects the dispersion unit to the wet cell may become hard and discoloured. When
tubing loses its elasticity, air will leak into the system at the connections to the sam-
ple unit and cell. The resulting bubbles in the system cause instability in the back-
grounds and sample measurements.
When tubing hardens, moving a dispersion unit relative to the optical unit may
cause the tubing to become detached.
To change the tubing, first ensure that the dispersion unit, wet cell and tubing are
fully drained; and then remove. Push the new tubing onto the pipe boss to a mini-
mum of 7mm. Then secure, where fitted, with the aluminium tubing connectors
The standard sample tubing used with the system will be a grade of Tygon tubing
(available from Cole-Parmer Instrument Company). Tygon is chemically compati-
ble with a wide range of materials and Malvern can supply various grades of Tygon
tubing depending upon the application or solvent being used. Contact the manu-
facturer for full information on compatibility.
To retain chemical compatibility, always replace tubing with tubing of the same or
better grade. Always check the compatibility of new tubing with the samples in
use before connecting and using the system. Refer to the Appendix chapter of this
manual for information on chemical compatibility.
The specification of the tubing supplied with the dispersion unit is:
Warning!
Never put fingers in the tank when the pump/stirrer shaft is rotating.
Usually the measurement’s cleaning routine is sufficient to keep the tank clean.
However, over time deposits may accumulate in the tank.
Inspect the tank once a week. If it requires cleaning, disconnect the dispersion unit
from the mains power and use a bottle brush to clean it. Use a detergent (e.g.
Decon 90) for cleaning if required.
Make several clean flushes to clear all traces of detergent and deposits in the tank.
Note
The cuvette must not be taken apart for cleaning. users should only follow
the maintenance procedures specified.
Note
The cuvette and stirrer bar should be cleaned thoroughly before first use
and before performing any subsequent measurements.
ill 8865
Place the cuvette upside down in the washstation. Ensure correct orientation
and the cuvette is firmly in place. The spout should face away from the waste
exit/dispersant input.
Caution!
Ensure the cuvette is fitted correctly before continuing and using
the syringe, otherwise you may be sprayed with dispersant or other
cleaning chemicals. It is advised that eye protection is used.
Using the washstation, clean the cuvette with IPA or Acetone depending
upon the dispersant used in the analysis. Note it may be required to use a
glass syringe.
Discard the IPA or Acetone from the cuvette.
Repeat 2 to 3 times as required.
With clean dispersant that is to be used in the analysis, fill the cuvette as
described in the filling the cuvette section.
Discard the dispersant from the cuvette.
Repeat 2 to 3 times as required.
Clean the stirrer bar first with IPA or acetone depending upon the disper-
sant used in the analysis, then clean again using the analysis dispersant.
The cuvette and stirrer bar can now be used for the next analysis.
Cleaning and storing after all analysis have been completed:
Discard the sample and dispersant from the cuvette.
Using the washstation, clean with IPA or Acetone depending upon the dis-
persant used in the analysis. Note it may be required to use a glass syringe.
Discard the IPA or Acetone from the cuvette.
Repeat 2 to 3 times as required.
Clean the stirrer bar with IPA or acetone depending upon the dispersant
used in the analysis.
Leave the stirrer bar, and the cuvette to dry upside down on a clean sheet of
lint free cloth.
Cuvette cleaning - Intensive internal window clean
For more intensive cleaning of the internal faces and edges of the cuvette, use
optics quality cleaning cloth and the cuvette cleaning spatula. These are
included in the consumable kit supplied with the SV
First clean the cuvette with the washstation as described above, to ensure any
grit, if present, is removed. Cleaning by first using the spatula may scratch the
windows if any grit, etc. is present.
Wrap a small sheet of “low shedding” optics quality cleaning cloth around the
spatula. wet with IPA or Acetone and push into the cuvette opening until it
meets the base
Slide the spatula along the cuvette left and right, ensuring the spatula reaches
along each side and the bottom of the cuvette. Do this 3 to 4 times as required
using a fresh sheet of optics cloth, and then remove spatula.
Finally, using IPA, use the washstation again to remove any loose and dis-
lodged contaminants.
Caution!
The outer faces of the cuvette windows are optically coated; treat them
with the same care as a camera lens.
Caution!
The outer faces of the windows have an anti-reflective coating and are
more prone to scratching than the inner surfaces. Be careful not to touch
the faces of the windows or put them down on dirty surfaces.
Note
The cuvette must not be taken apart for cleaning. users should only follow
the maintenance procedures specified.
demagnetize the stirrer bars coupling to the stirrer motor thus affecting its
rotation and dispersion performance.
Never run the stirrer motor if a dry cuvette is fitted with the stirrer bar
inserted. The stirrer bar will spin directly on the windows possibly scratching
the cuvette windows.
It is recommended to only run the Hydro SV only as long as the dispersion or
measurement is required.
Caution!
The surfaces of the system may be permanently damaged if samples or dis-
persants are spilt on them. If a spillage occurs, disconnect the system from
the power supply before carefully cleaning it up.
Consumable kits
Consumable kits and additional spares for maintaining the Hydro series wet sam-
pling dispersion units are available from your Malvern representative. Please con-
tact them for full details and requirements.
The consumable kits include the following components:
Hydro LV consumable kit
SV cell
10ml disposable syringe and needle
attachment
Stirrer bar
Lint free wipes
Pipette
Cuvette cleaning spatula and cloth
Washstation drain tube
Appendix
Specification
The following tables detail the specification of the Hydro series wet dispersion
units and Hydro series wet cell. Full specifications of the optical unit and the Mas-
tersizer as a complete system can be found in the Mastersizer User Manual and
Basic Guide.
All specifications correct at time of publication, but may be subject to alteration.
Hydro MV / Hydro LV
Dispersion type Wet
Capacity
-- Hydro MV 120ml
-- Hydro LV 600ml
Typical applications
-- Hydro MV Solvent-based suspensions, Pharmaceuticals.
-- Hydro LV Minerals, fillers, chemicals, foodstuffs, emulsions
Sonication power / fre- 40W max, 40kHz (nominal)*
quency * Dispersant dependent.
Hydro EV
Dispersion type Wet
Capacity 600ml / 1000ml (using a standard laboratory
beaker)
Sonication power / fre- 40W max, 40kHz (nominal)*
quency * Dispersant dependent.
Hydro SM
Dispersion type Wet
Capacity 120ml maximum
Typical applications Solvent-based suspensions, Pharmaceuticals.
Minerals, fillers, chemicals, foodstuffs, emulsions
Dispersion mechanisms Continuously variable pump / stirrer
Modes of operation Manual via controller unit
Weight 9.75kg
-- Controller unit 1kg
-- Dispersion unit 8.75kg
Dimensions
-- Controller unit Width: 70mm / Height: 225mm / Depth: 170mm
-- Dispersion unit Width: 390mm / Height: 140mm / Depth: 175mm
Power Supplied via CAN cable from the Optical unit
Power consumption 5W - Standby / 10W - Nominal*
96W - Maximum operating power**
* The power recorded on a typical unit using maximum pump
speed, with water as the dispersant.
** The maximum power available through the CAN ports.
Hydro SV
Dispersion type Wet
Capacity 7ml maximum
Typical applications Solvent-based suspensions, Pharmaceuticals.
Minerals, fillers, chemicals, foodstuffs, emulsions
Dispersion mechanisms Continuously variable stirrer
Modes of operation Automatic via SOPs.
Manual via Front panel control dial
Weight
-- SV cell and cuvette 3.05kg
-- Washstation 1.5kg
Dimensions Width: 110mm / Height: 280mm / Depth: 210mm
Power Supplied via CAN cable from the Optical unit
Power consumption 2W - Standby / 5W - Nominal*
* The power recorded on a typical unit using maximum pump
speed, with water as the dispersant.
Chemical compatibility
Components of the dispersion unit that may come into contact with the sample are
manufactured from materials that are considered to give the widest protection from
chemical attack. However, it is important to check that any sample, dispersant or
titrant used is chemically compatible with the materials mentioned. The tables
below indicate the components of the Hydro series of wet dispersion units that
may come into contact with either sample or dispersant.
Warning!
It is advisable that the chemical compatibility is checked against the materi-
als identified below before inserting a sample. It is also recommended that
a test is performed on the material with the sample before more permanent
usage is undertaken.
Any cleaning and maintenance procedures necessary are described in the Mainte-
nance chapter of this manual.
Hydro EV
Component Materials
Pump assembly Stainless steel 316
Stirrer PEEK (Glass fibre reinforced)
Impeller Stainless steel 316 / PEEK
Ultrasonic transducer Stainless steel 316 / Titanium nitride /
PTFE
Sample flow pipework (internal) Stainless steel 316 / PEEK (Natural) /
FFKM / PTFE/
Sample flow tubing (external to wet Tygon
cell)
Wet cell assembly Borosilicate Glass / Stainless steel 316
/ FKM / FFKM
Sample beaker Glass
Drip tray PEEK (Glass fibre reinforced)
Beaker holder Stainless steel 316
Wet cell assembly Borosilicate Glass / Stainless steel 316
/ FKM or FFKM
Hydro MV / Hydro LV
Component Materials
Splash guard Acrylic
Tank surround PEEK (Glass fibre reinforced)
Tank and pump chamber PEEK (Glass fibre reinforced)
Pump shaft Stainless steel 316
Stirrer PEEK (Glass fibre reinforced)
Impeller PEEK (Glass fibre reinforced)
Ultrasonic transducer Stainless steel 316 / Titanium nitride
Dispersant input tubing (External) PTFE / (TUB0007)
Dispersant input tubing, pipework and Stainless steel 316 / FEP/ PTFE/ Kalrez
fittings (Internal)
Dispersant input valve (regulator) Stainless steel 316 / PTFE
Solvent (non-aqueous) input pipework Stainless steel 316
(internal)
Drain Valve Stainless steel 316 / PTFE / FFKM
Drain tubing (internal) Stainless steel 316 / PTFE
Drain tubing (external) PTFE / Acetal
Sample flow tubing (internal) Stainless steel 316 / FEP/ PTFE/ FFKM
Sample flow tubing (external to wet Tygon
cell)
Tubing connectors Aluminium
Wet cell assembly Borosilicate Glass / Stainless steel 316
/ FKM or FFKM
i
Note
For the Hydro MV / LV Fluoroelastomer (FKM) seals in the wet cell can
be upgraded to Perfluoroelastomer FFKM to improve the chemical com-
patibility. Contact the Malvern representative for details.
Component Materials
Dispersant input tubing (External) Tygon (MH2075 / HC F-4040-A) - Sol-
vent compatible*
Hydro SM
Component Materials
Tank, pump chamber and body PEEK (Glass fibre reinforced)
Pump shaft Stainless steel 316
Stirrer PEEK (Glass fibre reinforced)
Impeller PEEK (Glass fibre reinforced)
Drain Valve assembly Stainless steel 316 / PTFE / FFKM
Sample flow tubing (external to wet Tygon (St R-3603) - standard*
cell) Tygon (MH2075 / HC F-4040-A) - Sol-
(*sample dependent) vent compatible*
Tubing connectors (at cell) Aluminium
Wet cell assembly Borosilicate Glass / Stainless steel 316
/ FKM or FFKM
Hydro SV
Components of the SV unit that may come into contact with the sample are manu-
factured from Perlast® perfluorolastomer solvent-resistant seals, glass, 316 stainless
steel, PTFE, chemically resistant epoxy resin. These include:
Component Materials
Cuvette Borosilicate Glass / Stainless steel 316
Stirrer bar PTFE
Washstation Stainless steel 316
Note
For chemical compatibility of the Mastersizer 3000 optical unit, refer to
the Mastersizer 3000 basic guide.
Regulatory Information
Regulatory information for all Mastersizer 3000 instruments and dispersion units,
can be found in the Mastersizer 3000 basic guide.
www.malvern.com
PARTICLE SIZE
MASTERSIZER 3000
HYDRO SERIES
WET DISPERSION UNITS
MAN0479
MRK1955-01