Katanax K2 Prime User manual

®
Automatic fluxer
2

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Thank you for having chosen the K2 Prime fusion machine from Katanax. To enjoy
years of reliable, efficient and safe use of this time-saving instrument, please read
this manual thoroughly and keep it in a safe and handy place for future reference.
Should you have any question regarding the use, maintenance or repair of your
instrument, kindly contact Katanax directly for assistance (see page 91 for contact
details).
© February 2015, Katanax inc. All rights reserved.

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Index
Index ...............................................................................................2
Installation......................................................................................5
Box contents............................................................................................ 5
Location ................................................................................................... 5
Leveling ................................................................................................... 7
Heating element protection....................................................................... 7
Hi-throughput “HX” version....................................................................... 8
Connection............................................................................................... 8
Questions ?.............................................................................................. 8
Introduction....................................................................................9
The fusion theory ..................................................................................... 9
Automatic fluxers ..................................................................................... 9
The K2 Prime fluxer................................................................................ 10
Main features of the Katanax K2 Prime.................................................... 12
Precautions ...................................................................................14
How the unit works ......................................................................15
Heating.................................................................................................. 15
Access to the furnace ............................................................................. 15
Agitation and pouring of the melt ............................................................ 15
Cooling .................................................................................................. 16
Solution agitation ................................................................................... 16
Using the K2 Prime (basic) ..........................................................17
Operation of the safety shield.................................................................. 17
The main running screen ........................................................................ 18
Electro-mechanical pushbuttons.............................................................. 20
Loading a program ................................................................................. 21
During a fusion....................................................................................... 22
The right ingredients .............................................................................. 23
Care of the elements .............................................................................. 26
Care of the platinumware ....................................................................... 27
Crucible installation ................................................................................ 27
Mold installation ..................................................................................... 29
A general fusion ..................................................................................... 29
Making solutions..................................................................................... 30
Description of the fusion steps ................................................................ 31
Programming the K2 Prime (advanced)......................................33
Viewing the fusion parameters ................................................................ 33
Unlocking the advanced mode ................................................................ 37
Managing fusion methods ....................................................................... 38
Preparing a fusion program..................................................................... 39
Heating steps......................................................................................... 39
Pouring step........................................................................................... 41

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Cooling steps ......................................................................................... 42
On-the-fly editing ................................................................................... 43
Global parameters ........................................................................44
Language............................................................................................... 44
Holding temperature offset ..................................................................... 44
Startup tolerance.................................................................................... 45
End beep ............................................................................................... 45
Automatic shut-off delay......................................................................... 45
Safety shield protection .......................................................................... 46
Fusion counter ....................................................................................... 46
Special parameters.......................................................................47
Accessing the Special parameters ........................................................... 47
Twisting correction ................................................................................. 47
Offsets................................................................................................... 48
Cam assisted.......................................................................................... 49
Movement testing................................................................................... 49
Fusion troubleshooting.................................................................51
Disk cracks............................................................................................. 51
Disk crystallizes...................................................................................... 51
Incomplete disk...................................................................................... 52
Non-homogenous disk............................................................................ 52
Bubbles in disk ....................................................................................... 52
Periodic inspection .......................................................................53
Warning................................................................................................. 53
Inspection schedule table........................................................................ 53
Flux spillage on holders........................................................................... 54
Holders alignment and functionality......................................................... 55
Visual integrity of heating elements......................................................... 56
Element terminal connections ................................................................. 56
Door springs tension check ..................................................................... 57
Furnace cleanliness ................................................................................ 57
Thermocouple junction ........................................................................... 58
Door Safety switch ................................................................................. 58
Linear motion system ............................................................................. 59
Service operations........................................................................60
Warning................................................................................................. 60
Platinumware holders service.................................................................. 60
Crucible holder removal .......................................................................... 60
Crucible holder assembly ........................................................................ 62
Crucible holder Installation...................................................................... 63
Mold holder removal............................................................................... 64
Mold holder assembly ............................................................................. 67
Mold holder installation ........................................................................... 68
Adjustment of holders ............................................................................ 68
Heating element replacement ................................................................. 77
Element tube replacement...................................................................... 79
Furnace top/back removal ...................................................................... 80
Spring position adjustment ..................................................................... 81
Furnace door removal............................................................................. 81

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Furnace backwards flipping..................................................................... 82
Blower box removal................................................................................ 83
Base compartment access ...................................................................... 84
Linear carriage lubrication....................................................................... 85
Firmware and program transfers.................................................86
Preset programs..................................................................................... 86
Backup or restore by USB....................................................................... 87
Technical specifications................................................................89
Electrical ................................................................................................ 89
Physical ................................................................................................. 89
Warranty .......................................................................................90
Contacting Katanax ......................................................................91

5
Installation
Congratulations on your acquisition of the K2 Prime fluxer, from Katanax. Please
read the following section for proper commissioning of your instrument. Do not
hesitate to contact Katanax with any question you might have with this crucial
step.
IMPORTANT: It is advisable that at least two persons carry this instrument to
avoid injuries. Do not drop instrument.
Box contents
The instrument comes with its essential accessories. In addition to optional items
you might have ordered, the box should contain:
1 fluxer (K2 Prime main unit),#K2Pn-dd [n=5 or 6 positions, dd=mold diam.]
1 accessories box containing the parts to assemble the platinumware holders
1 instruction manual (this booklet) and other instructions
Additionally, if you have ordered a K2 Prime with solution-making capability, you
will find:
5 unbreakable PTFE beakers, 5x#KP0010A
5 magnetic stirring bars (included with KP0010A)
1 crucible holder middle section (to hold 5 crucibles)
Note that the rest of the solution-making devices are permanently installed into
the instrument, and are not packaged separately.
Location
Vent hood
Molten flux, additives and some samples may produce vapors and gases that
need to be extracted. In particular, the use of excessive amounts of halogen-
based non-wetting agent will potentially cause the deterioration of the fluxer if the
corrosive fumes are not properly vented out.
In order to minimize airflow around the unit, the hood shall ideally be of the
canopy type, i.e. with sides and front open. If the sides are closed or otherwise
occupied by other instruments, a clearance of 30 cm shall be maintained on either
sides and to the back of the instrument.
Sash-type hoods should preferably not be used; or if unavoidable, the sash shall
be kept open, so as not to create front-to-back air movements.
The funnel (intake section) of the hood shall be approximately equal (or slightly
larger than) the size of the instrument's footprint, and centered above it to avoid
sideways airflow around the fluxer.
The lowest part of the funnel shall sit 45 to 60 cm above the instrument (93 to
108 cm above the tabletop).

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Fume hood air speed, measured at the base of the intake funnel, shall be around
0.5 m/s.
Given the nature of the exhausted gases (halogen compounds), Katanax
recommends that the piping be internally coated with a corrosion-resistant finish,
PTFE-coated piping being the optimal. (Other corrosive-resistant coatings may be
allowed by your local fire codes.) The same applies to the fan / impeller and any
other part in contact with the gas flow.
Motor and fan / impeller sizing information can unfortunately not be provided by
Katanax, as those strongly depend on factors linked to each individual installation
(pipe diameter, pipe distance to the outside, exhaust baffle type, etc...). Those will
need to be calculated locally for each installation by HVAC engineers.
In all cases, the vent hood must be centered above the fluxer. Failure to comply
with this requirement could create temperature uniformity issues and/or
premature degradation of the platinumware holders.
Table
The counter on which the instrument is to be used must be able to withstand a
weight of 68 kg (150 lbs). It is recommended to use the instrument from a
standing position, and adjust table height accordingly.
The tabletop shall be made of a non-combustible material, horizontally flat, rigid,
and stable.
It is advisable that at least two persons carry the instrument to avoid back
injuries.
Safety clearance
Because your new fluxer will produce heat, a minimal safety clearance must be
provided to prevent surrounding material from heating and potentially catching
fire. All around the instrument, a minimum distance of 30 cm (12’’) must be free
from combustible materials. Similarly, a clearance of at least 45 cm (18’’) must be
provided above the top of the instrument.
93-108 cm
(37-43 in)
30 cm
(12 in)
30 cm
(12 in)
30 cm
(12 in)

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Leveling
In order to obtain glass beads with a regular thickness, it is important that the
molds be reasonably horizontal upon pouring. If in doubt, place a lightweight
bubble spirit level on the molds and adjust instrument’s feet to compensate for
possible slant. (See page 29 for mold installation details.)
Heating
element
protection
To protect the heating elements, especially during the initial fusion method
development phase, different protection devices are available. They represent a
simple way of shielding the elements from the sputtering that may occur during a
fusion that is not optimally set yet.
Katanax offers a protective plate, made of a dark-colored ceramic, and clear
tubes. The plate covers all bottom elements simultaneously, while tubes can be
installed over top elements and/or bottom elements (when no plate is installed).
The dark ceramic plates is very resistant to flux and chemicals, and can be used in
all types of sample preparation. This is the protection method that Katanax
recommends.
Alternatively, two clear tube material choices are available: Quartz and Sapphire.
The Quartz tubes (part number KP5010E, sold as a pack of 8) are inexpensive,
but while these tubes will normally last very long, they are not the best choice if
you plan on using Iodine-based releasing/non-wetting agent in your fusion
recipes. Indeed, those compounds (LiI, KI, NH4I…) will evaporate almost entirely
their iodine, which readily attacks quartz (SiO2).
Hence, if you are using (or plan on using) an Iodine-based releasing agent, we do
not recommend to install quartz tubes; rather, if you want a protection on the
elements, use Sapphire tubes or a protective plate.
In short:
1. If you do not use iodine-based non-wetting agent:
a. You can install optional Quartz tubes (p/n KP5010E) or Sapphire
tubes (p/n KP5011E) –or
b. You can install an optional protective plate (p/n KP1200A), with or
without tubes protecting the top elements –or
c. You can use the instrument without any optional protection
2. If you want to use iodine-based non-wetting agents:
a. You cannot use Quartz tubes.
b. You can order/install optional Sapphire tubes (p/n KP5011E) –or
c. You can install an optional protective plate (p/n KP1200A), with or
without Sapphire tubes protecting the top elements –or
d. You can use the instrument without this optional protection

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Please refer to page 79, Element tube replacement for additional instructions on
tube installation and replacement.
Hi-throughput
“HX” version
The K2 Prime is available at:
the original 15A, 3000W rating, or
at a boosted 20A, 4000W rating (with the addition of factory-installed
KP5201A or field-installed KP5200A).
We call this higher-power unit the “HX version”. This HX version allows not only a
faster heat-up rate, but also boasts a second mold cooling blower. The combined
effect of those two features can save up to 20% fusion cycle time.
Additionally, the HX version includes the protective plate for bottom elements.
However, the electrical current drawn by the HX version is higher than the regular
version, and so the power line, outlet and breaker must be chosen accordingly.
Connection
The K2 Prime works on 220-240 VAC, 50/60 Hz. Note that the in-wall power line
and corresponding wall breakers or fuses must be designed to carry at least 15 A
for the regular version(20 A for the HX version), with GFCI protection.
While it is technically workable to use the instrument at 208 VAC (standard in
some areas), heat-up times will be longer than in the recommended voltage
range. Katanax offers step-up transformers that can overcome such local
limitations.
IMPORTANT: This instrument is to be connected to a GFCI (Ground Fault
Circuit Interrupt) breaker, which provides necessary protection to the fluxer
installation.
Questions ?
Should you have any question regarding the proper installation and start-up of
your instrument, please contact Katanax directly (see information on page 91) for
assistance.

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Introduction
This section intends to introduce the reader to the fusion technique and to
familiarize him or her to the K2 Prime.
The fusion
theory
Fusion is a technique used to prepare inorganic samples, with a view to analyze
them by x-ray fluorescence (XRF), inductively coupled plasma (ICP) atomic
absorption (AA) or any traditional wet chemistry method. Typical samples include:
cements, ores, slag, sediments, soils, rocks, ceramics, pigments, glasses and
even metals.
A fusion can produce either a small, homogenous solid glass disk (or “bead”) for
XRF, or an acid solution for other analytical methods.
The process of fusion as a sample preparation method exhibits many advantages
over other methods, as it does not produce mineralogy, grain size or orientation
effects and the result is perfectly homogenous.
In sample preparation by fusion, the sample never actually melts. It is merely
dissolved into a solvent. This solvent, generally a lithium borate flux, is solid at
room temperature and must be molten to dissolve anything. This is the only
reason the process requires heat.
Therefore, the peak temperature of a sample preparation by fusion is
determined only by the type of flux, not the type of sample.
Katanax does not recommend exceeding 1050°C when using lithium borates.
Katanax does not recommend exceeding 1000°C when using sodium borates.
Heating above those temperatures could cause flux evaporation that could bias
the subsequent analysis.
Automatic
fluxers
Because of the potential risk of manipulating red-hot samples and to increase
repeatability of temperature, mixing and duration, the industry has now adopted
the automated fusion machine as the standard equipment to prepare samples by
fusion.

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The K2 Prime
fluxer
General view
Enter the K2 Prime, the fusion machine that is the evolution of the original K2,
which was the first and only fully automated electric fluxer. Based on this success,
Katanax has updated the concept, making it sturdier and easier-to-use than ever.
The K2 Prime comes pre-loaded with various fusion methods that can be used as
is, or can be customized. All fusion methods can be saved, renamed, deleted or
copied, just like computer files. Only the preset methods are protected to avoid
accidental overwriting.
Upon turning the instrument on, the furnace will start heating up to prepare for
the first fusion cycle. If left idle for an extended period of time, the furnace will
automatically turn off. (Holding temperature and automatic shutoff features are
further discussed in the Global parameters section, at page 44.)
Crucible
Mold
LCD
interface
Furnace
Furnace
door
Safety shield

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Crucible holder
Unlike the first K2 Prime units, this newer version has a fixed locking bar on top of
the crucibles. Locking is achieved automatically due to the dynamic geometry
during pouring.
The straight-walled platinum crucibles are loaded with a few grams of powdered
sample, an appropriate flux and often other agents. The crucibles are inserted into
the crucible holder, and held in place by a locking bar.
Mold holder
Platinum molds are installed under each crucible in a separate holder. This holder
can only accommodate one size of molds at a time.
The crucible holder and the mold holder are referred to collectively as the
platinumware holders.
Fusion sequence
When the user instructs the K2 Prime to launch the actual fusion, the instrument
first checks that the initial temperature is reached (see page 44, Holding temp for
more details on this setting). If not, the processor waits until the furnace is ready.
Then, the furnace door automatically opens, the platinumware holders enter the
Crucible
Locking bar
“BlackDisk”
End-plate
Mold

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furnace, the door closes and all heating steps are automatically started in
sequence. Temperature is constantly monitored and displayed.
Once the flux is molten (after a programmable time), a back-and-forth rocking of
the crucible holder continuously mixes the flux with the sample.
The liquid flux starts dissolving the sample. When all sample is dissolved (after the
programmed time), the furnace door opens, the platinumware holders move
forward and, during the time the door closes, the crucibles are tilted forward to
empty their contents into the molds.
If set so in the fusion program, it is possible for the now-full molds to be re-heated
in the furnace, before they are pulled out again. (This operation is called annealing
and is needed in very special cases only.)
A blower located underneath cools the molds, while the furnace remains powered,
readying for the next cycle. When the molds are completely cooled, the user picks
up perfectly homogenous glass beads, ready for analysis by XRF.
For solution preparation, the hot melt is poured into unbreakable beakers (instead
of molds), which contain a dilute acid that is automatically stirred by a magnetic
system (optional, item no. KP5001A).
Some fusion types, such as peroxide and pyrosulfate, do not even require
pouring. The K2 Prime is also designed for such fusions, where the whole crucible
is dipped into an acid, after the fusion, to prepare a solution by leaching.
Main features
of the Katanax
K2 Prime
Accuracy
Entirely automated
Fully reproducible fusion methods
Perfect reproducibility using a closed electric furnace: all crucibles and molds
are exactly at the same temperature
Real-time temperature display
Safety
Integrated locking safety shield
No gases used, so no post-combustion toxic products released
Minimal heat dissipation; no need for a powerful vent hood
Versatility
Makes glass disks for XRF and can also readily do peroxide or pyrosulfate
fusions
With optional solution agitation module, can also prepare solutions
Ready to fuse with built-in methods for oxides, minerals, metals, alloys,
sulfides, fluorides and more
Can perform solid oxidations
Fully customizable fusion methods
USB connectivity

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Productivity
Simultaneous processing of up to six (6) samples (depending on options)
Throughput of 20 to 25 samples/hour
Productivity is improved by a user-adjustable holding temperature. Therefore,
the temperature between fusions can be maintained to minimize initial
ramping time
Simplicity
A simple, intelligent, high-performance furnace
Easy installation
Intuitive touch-screen color LCD graphics interface
Easy icon and menu navigation
Low maintenance; easy component access
1-year limited warranty

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Precautions
High temperature
Although this instrument has been built to be very safe, it is still capable of
reaching temperatures up to 1200ºC. Care must be taken in order to avoid
touching hot surfaces.
Even though crucibles and molds are supposed to be cool at the end of a fusion
cycle, in order to avoid risks of burns, use appropriate gloves, laboratory tongs or
some other adapted tool to manipulate the crucible, mold and glass disk.
User is advised that this instrument remains very hot for a long time, even after
turning it off.
High voltage
This instrument is powered by 240 Volts AC. Although the elements are
interlocked with a safety device that removes power when opening the furnace
door, reasonable precautions must be taken.
Disconnect power cord before attempting any cleaning, maintenance or repair
operation.
Be careful that no liquid infiltrate into the unit’s casing.
Acid spills
When making solutions, user is strongly discouraged to use glass beakers, as acid
spills in instruments are dangerous and not covered by warranty. Use only
unbreakable PTFE beakers; otherwise, there is a risk of user injury, due to flying
glass shards or acid splatter.
Heavy instrument
It is advisable that at least two persons carry this instrument to avoid injuries. Do
not drop instrument.
Crucible installation
To ensure safe operation, proper installation of the crucibles needs to be checked
by the user before each fusion. See page 27, Crucible installation, for detailed
instructions.
Damaged / dirty holders or platinumware
Never run a fusion if platinumware or their holders are damaged or soiled.
Replace damaged items or clean dirty parts immediately.

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How the unit works
Heating
Heating of both the mold and the crucible supports is achieved using a state-of-
the art heating element alloy coiled around rigid ceramic rods. These rods run
along a semi-soft, highly insulating material. These parts are then assembled into
an aluminum shell.
During heating, temperature is controlled by means of a platinum thermocouple.
This same thermocouple also allows the furnace to be kept at a preset, constant
temperature to quicken initial ramping before a fusion.
Access to the
furnace
Stepper motors automatically open the door, move the platinumware holders into
the furnace, and finally re-close the door. Upon pouring, the same sequence is
repeated in reverse order.
During a fusion, the safety shield remains locked, to prevent accidental burns
when the platinumware holders move in and out of the furnace.
Agitation and
pouring of the
melt
Homogenization of the sample into the flux is produced by the rotation of two
synchronous stepper motors located at the far right and left of the instrument.
These motors directly drive the crucible holder with a back-and-forth motion to
agitate the melt.
Just before the final pouring motion, both motors drive the crucible holders as if to
“pour backwards”, but the motion is stopped by a mechanical bumper. This
ensures perfect alignment of both ends of the crucible holder. (This is called
twisting correction.)
At the moment of pouring, the motors rotate the crucible holder forward to an
adjustable pouring angle, at an adjustable speed. The melt pours naturally into
the molds, and this can be helped with an optional shaking of the crucible in
pouring position.
The crucible holder is then automatically brought back to the vertical, ready for
another fusion.
The pouring step can also be completely disabled, for procedures such as
pyrosulfate or peroxide fusions, which do not need transferring the melt into
another container.

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Cooling
When the linear motion system moves the platinumware holder out of the
furnace, the molds are stopped just above a cutout designed to receive the
beakers.
At a programmed moment, a blower located on the back side of those wells
pushes fresh air upwards and under the molds, to cool them.
Solution
agitation
Making solutions requires that the instrument be fitted with the optional solution
agitation module, item number KP5001A.
IMPORTANT: Before attempting to make solutions, it is necessary to remove
the middle section of the mold holder, which can otherwise interfere with the top
of the beakers.
When making solutions, the hot melt is poured directly into beakers containing an
acid. Those beakers are to be placed into the cooling wells at the beginning of the
fusion. This acid solution must be agitated to improve the dissolution speed of the
crystallized flux and sample.
To do so, alternatively powered magnetic coils produce a rotating magnetic field
under the beakers. By placing a laboratory-type magnetic stirring bar in the acid
before fusion, the agitation will be automatically started at the appropriate
moment.

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Using the K2 Prime
(basic)
Operation of
the safety
shield
The safety shield is the large curved part that stands between the furnace and the
user during a fusion, to protect against accidental burns when the red-hot
platinumware holders slide out at the end of the cycle.
The shield must be manually pulled up to access the platinumware holders. In the
fully open position, the shield will rest against a stopper, in the near-vertical
position.
Once ready to start another fusion, the shield must be manually pulled down until
it rests in lower position.
Automatic lock operation
In normal use when the unit is powered, the safety shield is unlocked when no
fusion is ongoing, and will automatically lock when a fusion is started. The shield
will unlock by itself at the very end of the fusion cycle, when the cooling fans stop.
A detector ensures that the shield is in place before allowing the fusion to start.
Katanax recommends working in that default configuration, but it is also possible
(at the user’s risk) to entirely disable the locking mechanism if preferred. Refer to
Safety shield protection on page 46 for details.
Manual override
When there is no power (e.g. when cleaning or packing the unit), it is possible to
override the locking mechanism to manually open the safety shield.
The locking latch bolt can be reached behind the shield, on the left-hand side near
its bottom. Use the eraser end of a pencil (or the non-writing end of a pen) to
push the latch bolt inwards to the right, and then gently open the safety shield.
You can also use your hand to push the latch bolt if you have long slender fingers,
but be careful not to pinch the tip of your finger while opening the shield.

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The main
running screen
After the booting screen, you will obtain a display similar to the following (not all
buttons/icons will appear, depending on the instruments’ settings):
Safety shield
Latch bolt