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Katanax K1 PRIME Manual

Automatic fluxer
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Summary of Contents for Katanax K1 PRIME

  • Page 1 ® Automatic fluxer...
  • Page 3 Thank you for having chosen the K1 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.

  • Page 4: Table Of Contents

    Introduction ..................6 The fusion theory ..................6 Automatic fluxers ..................6 The K1 Prime fluxer .................. 7 Main features of the Katanax K1 Prime ............ 10 Precautions ................... 12 High temperature ................... 12 High voltage ................... 12 Acid spills ....................12 Heavy instrument ...................
  • Page 5 Crucible heating element replacement ............. 43 Mold heating element replacement ............47 Firmware and program transfers..........50 Preset programs ..................50 Backup or restore by USB ............... 51 Technical specifications ..............53 Electrical ....................53 Physical ....................53 Warranty ..................54 Contacting Katanax ..............55...

  • Page 6: Installation

    Installation Congratulations on your acquisition of the K1 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.

  • Page 7: Leveling

    (See page 22 for mold installation details.) Connection The K1 Prime works on 117-127 or 220-240 VAC, 50/60 Hz.  When used at 117-127 VAC, the power line must be able to provide 12 A.

  • Page 8: Introduction

    Introduction This section intends to introduce the reader to the fusion technique and to familiarize him or her to the K1 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.

  • Page 9: The K1 Prime Fluxer

    Mold heater interface Enter the K1 Prime, the fusion machine that is the evolution of the original K1, which was the first and only fully automated electric resistance fluxer. Based on this success, Katanax has updated the concept, making it sturdier and easier-to- use than ever.
  • Page 10 Crucible heater Crucible lid Locking bar Crucible Spill protector Crucible heater A straight-walled platinum crucible is loaded with a few grams of powdered sample, an appropriate flux and often other agents. The crucible is inserted into the crucible heater, and locked by the locking bar’s crucible lid. A removable spill protector is provided, so that any pouring residue can easily be cleaned.
  • Page 11 Mold heating/cooling unit Mold Mold holder Element Mold heater Blower Banana plug A platinum mold in a special holder is then installed in the removable mold heater. The mold is actually placed in a metal holder, which is available in various sizes to accommodate all typical mold diameters.

  • Page 12: Main Features Of The Katanax K1 Prime

    Fusion sequence When the user instructs the K1 Prime to launch the actual fusion, 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 heater continuously mixes the flux with the sample.
  • Page 13 Productivity  Throughput of 5 to 7 samples/hour Simplicity  Simple, intelligent, high-performance heaters  Easy installation  Intuitive touch-screen color LCD graphics interface  Easy icon and menu navigation  Low maintenance; easy component access  1-year limited warranty...

  • Page 14: Precautions

    Precautions High temperature Although this instrument has been built to be very safe, it is still capable of reaching temperatures up to 1150ºC. Care must be taken in order to avoid touching hot surfaces. Even though the mold is 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 mold and glass disk.

  • Page 15: How The Unit Works

    How the unit works Heating Heating of both the mold and the crucible is achieved in separate heaters, using a state-of-the art alloy heating elements coiled around rigid ceramic rods. These rods run along a semi-soft, highly insulating material. These parts are then assembled into an aluminum container.
  • Page 16 To do so, alternatively powered magnetic coils produce a rotating magnetic field under the beaker. By placing a laboratory-type magnetic stirring bar in the acid before fusion, the agitation will be automatically started and stopped.

  • Page 17: Using The K1 Prime (Basic)

    Using the K1 Prime (basic) 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): Here is a short explanation of the various zones and buttons:...
  • Page 18 crucible temperature icon depicted with  the actual measured temperature (in orange), and  the target temperature, which the crucible heater is in the process of reaching (in gray) Similarly, the mold temperature icon is shown with corresponding actual (orange) target (gray) temperatures.

  • Page 19: During A Fusion

    The padlock icon/button shows the state fusion program parameters. A closed padlock means that the parameters locked, password required unlock parameter access. Conversely, open padlock means that parameters freely changed. More details are given at page 27, Programming Prime (advanced). Entering the password is also required access Global...

  • Page 20: The Right Ingredients

    The Pause button is used to temporarily “freeze” the ongoing fusion. In pause mode, timers are suspended, and the current furnace temperature is maintained. Any ongoing motor motion will be continued or completed. This can be useful when some extra time is required to complete an oxidation or dissolution reaction, for example.
  • Page 21 Sample preparation Besides the traditional specifications of a sample to be representative, uncontaminated and dry, Katanax recommends that the sample be ground to <100µm. This is to ensure that the fusion be completed within a reasonable time. Additionally, the sample must be fully oxidized before heating the crucible containing the sample.
  • Page 22 After the choice of the right flux, the flux-to-sample ratio is probably the second hardest question to answer. This section intends only to explain general concepts. For more specific information, the customer is invited to contact Katanax directly. To obtain the best readability possible on the analytical instrument, one wishes to put as much sample as possible in the preparation.

  • Page 23: Care Of The Elements

    (see page 27, Programming the K1 Prime (advanced) for details on ramping). The amount of selected reagent will depend on the sample contents and can be estimated stoichiometrically.

  • Page 24: Crucible Installation

    A general fusion Here are the steps required to perform a fusion on the K1 Prime fluxer. 1. Turn the instrument on by flipping the rocker switch at the back of the instrument. The main screen appears when booting is complete.

  • Page 25: Making Solutions

    7. Add the non-wetting agent if it is not already integrated within the flux. 8. Place crucible in its heater. Important: make sure that it is properly locked in place. See page 22, Crucible installation, for details. 9. Place mold on its holder, using appropriate mold holder ring. Important: do not forget to install the mold! See page 22, Mold installation, for details.

  • Page 26: Description Of The Fusion Steps

    Description of the fusion steps All fusion programs in the K1 Prime are built the same way, and have nine (9) steps. Here is the list of those steps, along with the corresponding icon:...
  • Page 27 Heating 1 Typically used to pre-heat the sample, with little or no agitation. Heating 2 Typically used to oxidize the sample at low temperature (e.g. using nitrates), with little or no agitation. Heating 3 Typically used oxidize sample higher temperature (e.g. using carbonates), again with little or no agitation.
  • Page 28 Cooling 2 Used for blower-cooling of the mold Each step is launched when the preceding one is completed. It is also possible for a step to have a null duration (i.e. zero seconds), useful when one wants to increase crucible temperature with no rocking (the rocking parameter must be set to 0).

  • Page 29: Programming The K1 Prime (Advanced)

    Programming the K1 Prime (advanced) When specific sample types do not seem to be easily processed by a preset fusion method, it is necessary to manually modify the parameters of critical fusion steps. Viewing the fusion parameters Without risking to change a parameter, any user can check the current values and settings of the current program, step-by-step.
  • Page 30 Let us now understand the meaning of each symbol. We are now familiar with the graph zone, which shows the outline of the crucible temperature as a function of time. fusion step being edited represented as the portion of curve between the two vertical red lines.
  • Page 31 The crucible with angle symbol is used to refer to two rocking parameters. The top one is the amplitude of the rocking. The bottom one is the rocking speed. The icon in the lower left corner has now switched to a graph icon. Pressing this button will bring you back to the main running screen.
  • Page 32 This block of icons shows that the pouring is On (thus the “green light”). The parameters to the right show the crucible angle degrees) upon pouring, the pouring motion speed (in percent) well mold temperature. This section indicates the number of “knocks”...

  • Page 33: Unlocking The Advanced Mode

    Unlocking the advanced mode Before being allowed to manage fusion program and edit parameters, one must enter the correct password. To do so, click on the padlock icon/button. After touching the padlock button, a numeric keypad will pop up, ready for password entry. Type the password, which is 2014.

  • Page 34: Preparing A Fusion Program

    Heating 1 and Heating 2, or Heating 1 and Heating 3, and so on, without affecting anything. For standardization purposes, Katanax tends to use the last heating steps, and leave the first ones empty when not needed.

  • Page 35: Pouring Step

    IMPORTANT: No fusion should require temperatures in excess of 1100°C. Please contact Katanax if you feel your sample type needs higher temperatures. Duration Step duration (mm : ss) is also adjusted by pressing on the plus and minus buttons.

  • Page 36: Cooling Steps

    Pouring can be completely turned off and on by pressing the red and green vertical switch. The mold temperature can also be adjusted here. Note that entering a mold temperature of 20°C switches to “solution” mode. If pouring is on, the crucible tilting angle and speed can be controlled with the plus and minus buttons.

  • Page 37: Solution Programs

    As explained earlier, in a cooling step, the two crucible-related parameters are not used to control the crucible rocking motion, but rather to control the straightening up of the crucible heater, after the pouring. Typically, the tilting angle of “Cooling 1” will be the same as the pouring (typically 120°), and the tilting angle of “Cooling 2”...

  • Page 38: Global Parameters

    Global parameters In addition to program-specific parameters, your fluxer provides extra versatility through flexible parameters that will apply to all fusion programs. To access the global parameters screen, first unlock the advanced mode (see page 31, Unlocking the advanced mode), then touch the Global Parameters icon that is now available on the main display screen.

  • Page 39: Fusion Troubleshooting

    Glass disk sticks to the mold If disk top surface is concave (disk adheres to the mold walls), add non-wetting agent at the beginning or during the fusion. Katanax recommends lithium bromide. Glass disk contains undissolved particles Some sample may not be completely dissolved.

  • Page 40: Incomplete Disk

    this single point on the surface and radiate outwards. Cleaning the instrument’s base and surroundings will correct the problem. Incomplete disk This symptom causes disks that have the shape of a moon crescent, i.e. a circle with a missing section. It is caused by the mold not containing enough flux, or by the mold not being leveled.

  • Page 41: Periodic Inspection

    If unsure, do not hesitate to get in touch with a Katanax technician (see page 55, Contacting Katanax). Note that no modifications of the instrument, except those explicitly described and permitted in this manual, are allowed.

  • Page 42: Visual Integrity Of Heating Elements

    IMPORTANT: Always disconnect the instrument from the power outlet when working with panels removed. Risk of electrocution! In the K1 Prime, heating elements build a surface oxide layer over the metallic coil, which protects it from degradation and lengthens its lifespan. However, this oxide is extremely sensitive to molten flux.

  • Page 43: Element Terminal Connections

    Element terminal connections IMPORTANT: Always disconnect the instrument from the power outlet when working with panels removed. Risk of electrocution! 1. To check the integrity of the element ceramic connectors and terminals, do the following: Unplug instrument (Caution – risk of death by electrocution) and let the heaters cool down completely.
  • Page 44 1. This inspection consists in verifying the junction of thermocouple for visible damage. Unplug K1 (Caution – risk of death by electrocution). Look inside the crucible heater, where the crucible would normally sit. The thermocouple is the cylindrical prong, with a tiny metallic wire running through its top end.

  • Page 45: Service Operations

    Should you have any question, or need further assistance, please do not hesitate to contact us (see page 55, Contacting Katanax). Warning IMPORTANT: Some of the procedures described in the following pages imply a risk of death by electrocution;...
  • Page 46 Remove the terminal screws (circled below), their lock washer and their contact brackets. You should have in your hand two screws, two washers and two small contact brackets. Terminal screws Manually tilt the crucible heater back to the upright position. 5.
  • Page 47 6. Now remove the top ring, and the five ceramic top plates (see picture below). Ceramic plates Black ceramic cylinder Heating element 7. Remove the inner “Black Ceramic” cylinder that protects the element. 8. Gently pull the element upwards. Heating element installation From the instructions above, the crucible heater is in a partially disassembled state.
  • Page 48 3. Inspect the heater cavity, and look for molten flux spills. If molten flux is found, scrape the insulation clean, or replace the soft insulation completely. IMPORTANT: Remember that molten flux on the soft insulation could transfer onto the new element and ruin it rapidly. Ensure that the heater’s cavity is completely clean before installing a new element.

  • Page 49: Mold Heating Element Replacement

    Mold heating element replacement IMPORTANT: Always disconnect the instrument from the power outlet when working with panels removed. Risk of electrocution! The mold heating element comprises a single wire, wound in a spiral around two ceramic screws. The resulting assembly is inserted into a soft thermal insulation shell.
  • Page 50 Top ring Ceramic plates Heating element Thermocouple Ceramic connector Thermocouple cover Banana connectors 10. To remove the clear tubes from the heating element (if they are clean and you intend on re-using them), you will need to remove the screw at the ends of the heating element.
  • Page 51 3. Inspect the heater cavity, and look for molten flux spills. If molten flux is found, scrape the insulation clean, or replace the soft insulation completely. IMPORTANT: Remember that molten flux on the soft insulation could transfer onto the new element and ruin it rapidly. Ensure that the heater’s cavity is completely clean before installing a new element.

  • Page 52: Firmware And Program Transfers

    Preset programs This section lists the methods that are factory programmed into the K1 Prime. It is not possible for the user to alter or delete them. Note that Katanax cannot be held responsible for any damage to platinumware or fluxer incurred by the use of those methods.

  • Page 53: Backup Or Restore By Usb

    This can also be useful to transfer fusion programs among several fusion instruments. Alternately, you might have received from Katanax a firmware upgrade that you want to install on your instrument. You can also contact Katanax to obtain instructions on how to download firmware updates. Backup fluxer to USB drive 1.
  • Page 54 “USBDISK”, then click on its sub-directory, named “disk_a_1”. If the data was created in another (sub-)directory, you will need to browse to reach it. In particular, firmwares obtained from Katanax (via Web or email) are located in a sub-directory named “Firmware K1P…” ; you must select (highlight) this folder at this step.

  • Page 55: Technical Specifications

    Technical specifications Electrical Voltage ......117-127 VAC or 220-240 VAC Frequency ...... 50-60 Hz Electric power ....1300 W (max consumption) Main fuse......@ 115 VAC : 12 A ........@ 230 VAC : 10 A Physical Weight ......30 kg (66 lbs) Height ......

  • Page 56: Warranty

    Katanax reserves the right to make changes in the design or to make additions or improvements with respect to its product without incurring any obligation to...

  • Page 57: Contacting Katanax

    Contacting Katanax Katanax sales and technical staff can be reached at the following address: Katanax inc. 2500 Jean-Perrin, suite 100 Quebec City, QC Canada G2C 1X1 Tel.: (+1) 418-915-4848 E-mail: info@katanax.com Web: www.katanax.com When contacting us, kindly have the serial number of the instrument at hand.

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