Katanax X-FLUXER User manual

Automatic fluxer

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Thank you for having chosen the X-300 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 84 for contact
details).
© September 2020, Katanax inc. All rights reserved.

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Index
Index ...............................................................................................2
Installation......................................................................................5
Box contents............................................................................................ 5
Location................................................................................................... 5
Leveling ................................................................................................... 7
Connection............................................................................................... 7
Mold size.................................................................................................. 7
Crucible holder setup................................................................................ 7
Questions ?.............................................................................................. 7
Introduction....................................................................................8
Fusion basics............................................................................................ 8
Automatic fluxers ..................................................................................... 8
The X-300 fluxer ...................................................................................... 8
Main features of the Katanax X-300 ........................................................ 11
Precautions ...................................................................................13
How the unit works ......................................................................14
Heating.................................................................................................. 14
Multiple configurations............................................................................ 14
Access to the furnace ............................................................................. 14
Agitation and pouring of the melt ............................................................ 15
Cooling .................................................................................................. 15
Solution agitation ................................................................................... 15
Using the X-300 (basic) ...............................................................16
Operation of the safety shield.................................................................. 16
The main running screen ........................................................................ 17
Loading a program ................................................................................. 20
During a fusion....................................................................................... 21
The right ingredients .............................................................................. 22
Care of the platinumware ....................................................................... 25
Crucible installation ................................................................................ 26
Mold installation ..................................................................................... 27
A general fusion ..................................................................................... 28
Making solutions..................................................................................... 29
Description of the fusion steps ................................................................ 30
Programming the X-300 (advanced)...........................................32
Viewing the fusion parameters ................................................................ 32
Unlocking the advanced mode ................................................................ 36
Managing fusion methods ....................................................................... 37
Preparing a fusion program..................................................................... 38
Heating steps ......................................................................................... 38
Pouring step........................................................................................... 39
Cooling steps ......................................................................................... 40

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On-the-fly editing ................................................................................... 41
Global parameters ........................................................................43
Language............................................................................................... 43
Holding temperature offset ..................................................................... 43
Startup tolerance.................................................................................... 44
End beep ............................................................................................... 44
Automatic shut-off delay......................................................................... 44
Safety shield protection .......................................................................... 45
Fusion counter ....................................................................................... 45
Special parameters.......................................................................46
Accessing the Special parameters ........................................................... 46
Offsets................................................................................................... 46
Loop operation ....................................................................................... 47
Movement testing................................................................................... 47
Fusion troubleshooting.................................................................48
Disk cracks............................................................................................. 48
Disk crystallizes...................................................................................... 48
Incomplete disk...................................................................................... 48
Non-homogenous disk............................................................................ 49
Bubbles in disk ....................................................................................... 49
Periodic inspection .......................................................................50
Warning................................................................................................. 50
Inspection schedule table........................................................................ 50
Flux spillage on holders........................................................................... 50
Holders alignment and functionality......................................................... 51
Air filter for the molds cooling ................................................................. 52
Furnace chimney cleaning....................................................................... 52
Element terminal connections ................................................................. 53
Furnace cleanliness ................................................................................ 53
Thermocouple junction ........................................................................... 54
Swing motion system ............................................................................ 54
Service operations ........................................................................56
Warning................................................................................................. 56
Crucible holder removal .......................................................................... 56
Crucible holder installation ...................................................................... 57
Mold holder removal............................................................................... 57
Mold holder configuration, assembly and alignment ................................. 58
Heating element replacement ................................................................. 60
Top/back panel removal ......................................................................... 62
Side panel removal................................................................................. 63
Bottom panels removal........................................................................... 64
Appendix A –Technical specifications.........................................66
Electrical ................................................................................................ 66
Physical ................................................................................................. 66
Appendix B –Warranty ................................................................67
Appendix C –Firmware and program transfers..........................68
Preset programs..................................................................................... 68

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Backup or restore by USB ....................................................................... 69
Appendix D –CPLive : Data logging ............................................71
Introduction to data logging.................................................................... 71
Installing EasyConverter ......................................................................... 71
Enable data logging ................................................................................ 72
Sample tracking ..................................................................................... 73
Copying logs to a USB drive................................................................... 74
Accessing logs through FTP..................................................................... 75
Structure of the data log files .................................................................. 76
Error / warning codes listing ................................................................... 77
Appendix E –CPLive : Networking...............................................78
Connecting the fluxer to your LAN........................................................... 78
Appendix F –CPLive : Remote access .........................................80
Controlling the fluxer from a remote device ............................................. 80
Allowing Katanax support to access your fluxer........................................ 82
Contacting Katanax ......................................................................84

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Installation
Congratulations on your acquisition of the X-300 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 several 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 X-300
1 instruction manual (this booklet)
USB memory stick and hex key set
Additionally, if you have ordered a X-300 with solution-making capability, you will
find:
3 unbreakable PTFE beakers, #KP0010A
magnetic stirring bars (one is included with each beaker)
the rest of the solution-making assembly is pre-installed into the instrument,
and is 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 from combustible materials
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.

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The lowest part of the funnel shall sit 45 to 60 cm above the instrument (96 to
111 cm above the tabletop).
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.
Table
The counter on which the instrument is to be used must be able to safely
withstand a weight of 54 kg (120 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 several persons carry the instrument to avoid back injuries.
IMPORTANT: The instrument can be carried by its bottom plate, or by the two
large handles on each end of the unit top. The safety shield handle shall NOT be
used to carry the instrument.
96-111 cm
(38-44 in.)
30 cm
(12 in.)

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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.
Your local fire code may require different clearance distances; please check with
your local regulations.
Leveling
In order to obtain glass beads with a uniform thickness, it is important that the
molds be reasonably horizontal upon pouring. If in doubt, place a bubble spirit
level on top of the fluxer and adjust the instrument’s feet to compensate for
possible slant. (Also see page 27 for mold installation details. If mold is correctly
leveled but beads are still incomplete, please refer to Fusion troubleshooting, at
page 48.)
Connection
The X-300 works on 195-250 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.
Mold size
On the X-300, the user can easily re-configure the mold holder to accept any mold
nominal size from 30 to 40 mm. Please refer to page 58, Mold holder
configuration, assembly and alignment for details.
Crucible
holder setup
Once the mold holders are configured and installed, you may proceed to page 57,
Crucible holder for details on how to properly assemble the parts that make up
the crucible holder, and install the latter in the instrument.
Questions ?
Should you have any question regarding the proper installation and start-up of
your instrument, please contact Katanax directly (see information on page 84) 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 X-300.
Fusion basics
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
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, or cause damage to the furnace insulation.
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.
The X-300
fluxer
General view
Enter the X-300, the fusion machine that combines the safety and accuracy of
electrical heating with unprecedented flexibility and simplicity. It is also a very
sturdy unit, as it shares many of its industrial-grade components with its larger
brother, the six-position X-600.

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Three variants of X-300 fluxers are available, depending on the number of
samples that can be processed in a single cycle:
X-300M –“Mono”, is a single station fluxer (one sample)
X-300D –“Duo”, is a double station fluxer (two sample)
X-300T –“Trio”, is a triple station fluxer (three samples)
and it is possible to upgrade from one version to the next by adding one or two
expansion kits (p/n KP8000A), available from Katanax.
The X-300 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 43.)
Safety shield
Crucible
LCD
interface
Mold

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Crucible holder
Unlike some other units, this fluxer involves no moving part to insert and lock the
crucible in place. 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 then
inserted into the crucible holder.
Mold holder
Platinum molds are installed under each crucible, in a separate holder device.
Unlike most other mold holders on the market, this design allows the user to re-
configure each position to independently accept 30, 32, 35 or 40-mm molds
without the need to purchase additional parts.
Crucible
“Fork”
“Hoop”
Mold

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Please refer to page 58, Mold holder configuration, assembly and alignment for
details, to learn how to change mold size.
The crucible holder and the mold holder are referred to collectively as the
platinumware holders.
Fusion sequence
When the user instructs the X-300 to launch the actual fusion, the instrument first
checks that the initial temperature is reached (see page 43, 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
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 left-to-right 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 further, to empty their contents into the molds.
A set of three blowers located underneath cool 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. KP8001A).
Some fusion types, such as peroxide and pyrosulfate, do not even require
pouring. The X-300 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
X-300
Accuracy
Entirely automated
Fully reproducible fusion methods
Outstanding temperature uniformity, thanks to a position-corrected heating
profile
Drift-free durable platinum-rhodium thermocouple
Perfect reproducibility using a closed electric furnace: all crucibles and molds
are exactly at the same temperature
Non-contaminating ceramic holders for crucibles and molds
Automatic compensation against power outlet voltage variations
Real-time temperature display
Safety
Integrated locking safety shield with glass viewport

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No gases used, so no post-combustion products released
Minimal heat dissipation; no need for a powerful vent hood
No hazardous voltage on the sealed heating elements
Versatility
Expandable from 1, 2 to 3 positions
Makes glass disks for XRF and can also readily do peroxide or pyrosulfate
fusions
Stores up to 32 different fusion programs
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
Accept mold sizes from 30 to 40-mm nominal diameters
Productivity
Simultaneous processing of up to three (3) samples for XRF or ICP/AA
Throughput of up to 15 samples/hour (when preparing acid solutions)
Fast initial heat-up time of about 15 minutes
Productivity is enhanced by a user-adjustable holding temperature.
Therefore, the temperature between fusions can be maintained to minimize
initial ramping time
Individual mold blowers for fast cooling after the fusion
Automatic detection of failed heating elements
Heating elements can be replaced without cooling the furnace down
Durability
Sealed, non-brittle heating elements are impervious to flux
All-ceramic platinumware holders without moving parts
Ability to continue working even with a failed element
Chimneys vent out corrosive halogen gases
Sturdy industrial-grade modular electronics
Robust IP65 rated industrial interface
Dedicated PLC-based programming (not Windows®dependent)
Low-maintenance
Simplicity
Easy installation, easy use
Single-phase power, no separate power supply
Intuitive touch-screen color LCD graphics interface
Easy icon navigation
Multilingual interface
A simple, intelligent, high-performance furnace
Easy component access
USB-upgradeable firmware
CPLive™ remote 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 inside the furnace. 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 nominally powered by 220 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 26, 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 set of
state-of-the art heating elements, whose resistive wire is sealed within a ceramic
sheath. Hence, the element filament is protected from chemical vapors,
projections and spills at all times.
During heating, temperature is controlled by means of a highly durable platinum
thermocouple. This same thermocouple also allows the furnace to be kept at a
preset, constant temperature to quicken initial ramping before a fusion.
Multiple
configurations
Since the X-300 fluxer is available in various configurations (for 1, 2 or 3 samples
per fusion cycle), the size of the heating cavity, the number of heating elements
and the position of the platinumware holders will change.
Number of
positions
Model
number
Furnace cavity and
holders location
Number of
heating elements
1
X-300M
Center
(33% of full cavity is used)
3
2
X-300D
Left + center
(66% of full cavity is used)
2 + 3 = 5
3
X-300T
Left + center + right
(100% of full cavity is used)
2 + 3 + 2 = 7
It is possible to upgrade from one version to the next by adding one or two
expansion kits (p/n KP8000A), available from Katanax.
Access to the
furnace
At the beginning of a fusion cycle, 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.

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Agitation and
pouring of the
melt
A mixing motion of the sample and flux is produced by the alternate rotation of a
stepper motors located behind the crucible holders. This motor drives push-bars,
which in turn drives the crucible holders with a left-to-right motion to agitate the
melt.
At the moment of pouring, the rocking motor rotates the crucible holder 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 immediate transfer of the hot
melt into another container.
Cooling
When the pendulum motion system moves the platinumware holders out of the
furnace, the molds are stopped just above cutouts. At a programmed moment,
blowers located underneath those cutouts push 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 KP8001A.
IMPORTANT: Before attempting to make solutions, it is necessary to remove
the mold holders, 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 agitation wells before 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 solution will agitation will be automatically started at the
appropriate moment..

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Using the X-300 (basic)
Operation of
the safety
shield
The safety shield is the partition that stands between the furnace and the user
during a fusion, to protect against accidental burns when the red-hot
platinumware holders swing forward at the end of the cycle.
The shield must be manually pulled up to access the platinumware holders. Once
ready to start another fusion, the shield must be manually pulled down, until it
rests in lower and locked position.
Automatic lock operation
When the unit is first powered on, the safety shield automatically unlocks; it will
automatically lock when the shield is manually opened and eventually re-closed
before starting a fusion. The shield will unlock by itself again at the very end of the
fusion cycle, when the cooling fans stop.
A detector ensures that the shield is properly closed 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 necessary. Refer to
Safety shield protection on page 45 for details.
Electronic unlocking
When the user opens the shield and re-closes it, the fusion instrument assumes
that it is ready to start a fusion, and so the shield locks. In case the user wants to
re-open the shield before the fusion is started, simply press on the “Shield unlock”
button:
The instrument will then indicate that the shield is unlocked and ready to be
opened by showing the icon with a green halo:
When the above icon is shown (with the green halo), you may push then pull the
shield open. It will re-lock when closed again.

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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 picked through an oblong opening on the front of the
unit, at the left of the shield. Use a thin tool (like the 2.5-mm hex key provided in
the tool kit) and reach for the cylindrical part in the top section of the oblong hole.
Gently push this cylindrical part upwards, to unlatch the shield, and then pull the
safety shield open.
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 access
Thin tool

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Here is a short explanation of the various zones and buttons:
The graph zone shows the outline of
the crucible temperature as a function
of time.
The “Start” button, quite obviously, is
used to launch the currently selected
fusion program.
This button is used to unlock the
safety shield (see Operation of the
safety shield, page 16).
This “sleep” button allows the user to
put the fluxer in smooth shutdown
mode. Pressing it will turn the heating
power off but keep the furnace door
closed, so that the furnace cools very
slowly. This can help extend the life of
the insulation.