Before You Start:

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Instrument:

Instructions:

***These instructions are available as a pdf document [English]:* *click here***

***These instructions are available as a pdf document [German]:* *click here***

The machine: Claisse M4®

The M4 casts glass beads in standardized dimension (4 cm) in a single automated procedure. The casting powder (mixture of sample and flux) is rapidly heated with a Bunsen burner. Automated agitation homogenizes the material and removes gas bubbles from the melt. The actual casting is isothermal, casting dish and crucible are heated up to the same temperature. This prevents early crystallization of the sample. The vitreous solidification of the melt is done with cool air from ventilators underneath the casting dish.

The whole process needs between 10-15 minutes for 3 samples cast synchronically. In general the machine can be used again immediately after a run. The product can be analysed directly; no subsequent polishing is necessary.

For instructions on preparation of casting powders, go here.

Casting with Claisse M4®

Start-up and operation

Important:

- The machine must never be loaded with more than 11 g total mass (powder + flux). (Otherwise the melt will overflow upon casting and the Bunsen burners will be damaged.)
- Work with M4 only with safety goggles (the pill can burst at all the time)
- Crucible and casing dish should NEVER be touched on the inner side!!! (even small scratches are leading to contamination of the following samples)

The operation of the machine is done through a panel of the operation microprocessor.

a. open the gas valve (do not change anything on the in-between valve!!)

b. press the ‘on’ button

c. Make sure that the ultrasonic bath is filled with water (level up to 3 cm below rim, see mark) and plug it in.

d. Switch the used burners on.

e. Employ the casting dish

f. employ the crucible with the weighted powder

g. put down the pivot arm (position 20°above horizontal)

h. Choose the suitable program

P 8 for silica and alumina
P 3 for rocks
P 10 for solutions

i. close the security shutter

j. start the machine through pressing the ‘start’- button

k. after the program is finished, pick up the pill using the suction cup.

In emergency case: press the ‘STOP’-button (reset the machine by pressing the ‘reset’-button)

The M4 conducts a self-test of the electronics and the supply lines (gas) after the start-up. If the settings do not meet the requirements, the start of the machine will be interrupted automatically. The panel shows an error message (how to solve problems see below).

In such a case, please try first to fix it yourself with the helping manual further on. If it is an extraordinary fault, contact immediately the responsible lab assistant

The menu and available programs

After start-up, a total of 10 main menus can be used. The most frequently used are mentioned above. For choosing a program, press ‘P’-Button followed by the wanted number.

If you want to cast different rock compositions, you must seek advice with the lab assistant first. The following materials are not allowed for processing:

NO slags und cinders (e.g., flying ashes)
NO ores (especially sulphides)
NO sulphates
NO flint or chert

The use of these materials leads to partial destruction of the platinum dish and crucible. A separate preparation protocol for rocks with oxide ore content >3%vol (dilution with standardized quartz powder) exists and has to be individually assigned by the lab assistant. No guarantee can be given for its success.

Changes on the working programs are only done by the assistant, because they are code protected.

Activation of a casting program

Place the crucible containing the powder softly into its holder. Insert the crucible from the top. With one hand, open the holder und put the crucible softly in between the triangle carrier. Check that the crucible is sitting correctly, wrong placed crucible could be scratched or fall out while rotating. Be very careful during insertion!!! If you have cast pills before, take care when placing the crucible, because the holder is extremely hot. Always use the special crucible tongs but never let the tongs touch the inside or upper rim of the crucible! Only touch the outside. Melt drops will be almost impossible to remove from scratches and will contaminate further samples.

With the same tongs, touch only the casting dish on the rim, but never on the casting surface. Any scratches will be on the glass bead measurement surface, and will cause the incident X-Ray beam to be out of focus. Open the holder with one hand (can be hot) and place the dish from above softly into position. Make sure the holder encloses the dish safely and check the correct placement. Wrong placed casting dishes can be scratched or lost while rotating.

Topple over the pivot arm (position 20°above horizontal) into the right position. The machine will rotate the dish into casting position after start of a program. Choose the desired program (‘P+number’) and then press the green 'Start' Button on the panel. From here on, everything is automated.

During operation, the remaining time can be read from the display:

You can read the following details:

12.3.0 means the remaining time is 12min 30s.

F 4.32 means the used function remains for 4min 32s.

GO means the program has been started.

Sequence of events during casting

The currently available programs comprise the following steps:

First Fusion: Melting of the powder while turning slowly

Second Fusion: Homogenisation of the powder using higher axial triangle and higher velocity.

Slow down: The crucible dish is pivot into the flame and heated up. As soon as the crucible and the dish have the same temperature the rotating is stopped.

Casting: The casting dish is pivot down and the crucible is pivot the melt into the dish.

Cooling: Short time afterwards, the fans underneath start and the melt is cool down.

Handling after the program: As soon as the fans stopped, you can pick up the pills using the suction cup.

Note: Never touch the slightly convex side of the glass bead with your fingers. You will experience elevated sodium values in your analysis. If it occurs, gently wipe the surface with a soft Kimwipe dipped in alcohol.

Cleaning and proper treatment of platinum material

Cleaning

For use of the machine, 3 casting dishes and 3 crucibles are handed out to the user. During the in between program time, the last used crucible is placed in warm (not boiling, ca. 80°C) hydrochloric acid (HCl 5%). 5 minutes are enough to clean the crucible if the antecedent program has been finished properly (this means, that the crucible has been shocked) and shortly placed in the ultrasonic bath. A hot plate (max. set dial to 6), glass beaker and acid are in the lab.

Under normal conditions of use, the casting dish doesn’t have to be cleaned by this procedure. It is only placed into the acid after the last sample for a few minutes. This is mainly to keep the lower side of the dish clean and reflective.

Never place the dish into the acid bath together with the crucibles! Their rims would scratch the inner casting surface of the dish.

If the room is left for any short time, switch the hot plate off and leave the platinum in the acid bath. As well switch the main gas supply off if you leave the room (in door frame, red button = OFF and green = ON)

Waste acid has to be poured into the white 10 L waste acid container next to the sink. Place container into the sink, unscrew top, pour waste acid in (GLOVES, SAFETY GOGGLES, LAB COAT!!!). If the container filling reaches the marked top level (ca. 10 cm below top), inform lab assistant for proper disposal. Do not pour waste acid into the sink. NEVER pour water into the waste acid container, explosion hazard!

Proper Handling:

Under no circumstances are the inner parts of the crucible or the casting dish ever to be touched by the tongs!! Even slightest contacts scratch the platinum surface. On these scratches, small melt drops remain, leading to lesser quality melts and contaminated glass beads. The platinum crucibles and/or dish would have to be replaced which takes a long time (>1 month) and is extremely expensive (depending on platinum price ca. 5000, - CHF per item!). After extensive use, the casting dish will deform to leave a convex surface on the analytical side of the glass bead. Scratches and uneven surface can be flattened and polished by about 4 hours work. Uneven surface leads to a defocused incident beam during analysis.



WRONG !!		WRONG !!

RIGHT !!	RIGHT !!

Troubleshooting and Error messages

Casting problems

Because the M4 is new, we do not know all the established problems. Please tell us what kind of problems you had, so we can improve the programs or manuals.

a. The bead does not cover the entire floor of the casting dish:

The bead was caste a few degrees too cold. Check if the valve on the gas bottle is open, make new powder mixture and cast again.

The whole mass is too small (6g instead of 9g flux and sample). Cast the pill again with the exact amount of flux and sample (1.5g sample/7.5g flux)

The melt is too viscous. Add a few drops of a non-wetting agent to a new weighted solution and cast again. (Still in experimental mode)

b. Small melt remnants stay behind in the crucible:

The melt is too viscous. Add to the beginning powder a non-wetting agent (2 drops of LiBr) and cast the pill again. (Still in experimental mode)

c. The bead has a small gas bubble trapped in its rim:

The bubble won’t change the quality of the analysis, because the outer millimetres of the bead are not incorporated into the measurement grid. Treat the casting dish for 5-10 minutes in warm acid.

d. The pill splits

The casting dish is too cold. Open the gas valve until the maximum is reached (do not touch the in-between valve!!) and cast the pill again.
There are external particles in the casting dish or the melt. Clean the casting dish before the next cast by putting it for 5 min in the warm hydrochloric acid bath.
The measurement of the powder was too improper (not 1:5 rate sample-flux). Cast the pill again with exacter measurements.

Error Messages

The machine is given out 2 error messages (‘Fail’ or ‘Err?). If it displays these messages, all application stop immediately. After the error is eliminated, you can ‘reset’ the machine with pressing the ‘reset’-button and the machine is ready for the normal use.

Possible error messages and how to fix it:

ERR:

a. the pivot arm is left in the position high. Put down the pivot arm (position 20° above horizontal) into initial position.

b. Switch the machine off/on and if ’ERR’ still occur, ask your lab assistant.

FAIL:

is displayed on the panel, if one or all of the used Bunsen burners couldn’t ignite. Open the gas valve (do not change anything on the in-between valve!!), push the ‘reset’-button and start the casting run again.

ARM7:

The pivot arm is in position high. Put down the pivot arm (position 20° above horizontal) into initial position.

Instructions for Users:

Automated Glass Bead Casting[Old PerlX3 Manual still online!]