Maintenance and care of platinum-ware

This document is prepared for one of the most prevalent type of platinum-ware used for
borate fusion technique. The information found in this document is to be use with 95%
platinum and 5% gold alloy. The platinum-wares used in labs are considered as consumables
in fusion. The best way to preserve them is to make a regular maintenance of your
platinum-ware and to have good knowledge of the fusion to run your samples. The only way
to keep them as new is to avoid fusion cycles!!

Normal use and maintenance:

Molds
When preparing beads, the most important thing is to take care of the mold.
Damaged surface of mold (scratches, little dots) can directly affect the XRF results by
decreasing the intensity of certain elements up to 0,2%. A polishing schedule should be
adopted when the production of beads is regular (ex. every week, every 50 fusions, etc).
Stress produced by temperature cycling can slowly induce deformation of the mold. The
mold surface can become convex with time. Here again, the analyzed surface of the bead
will be modified and will have a direct incidence on the XRF results (decreasing the
intensity). To resolve this problem, you can use reinforced mold (thicker mold) and/or
straighten your mold with special press equipment.

Crucible
The crucible's scratches and little dots are less important in the analytical point of
view. They will not have a direct impact on the results if we compare them with the molds.
However, old and used crucibles can trap sample and lose their non sticking behavior. The
incidence on analytical results can then be related to carry over. Normally, the crucible is
thinner than the mold so you must be careful when polishing. At least, the polish treatment
should be less regular than the molds. If you use ‘‘mouldibles’’ crucibles, you can treat them
as molds for the polish treatment (reinforced bottom). However,, the behavior of sample
during fusion will be very important to know because if you induce irreversible damages to
your mouldible crucibles, you will lose your crucible and your mold at the same time!
Acid cleaning:

Cleaning your platinum-ware with acid can help to dissolve residues like flux and
surface sticking/inclusions of certain elements. Here are some suggestions of acid treatment
you can use to clean your platinum:

Soft cleaning:
- HCl 20% or more, hot solution with stirring for about 30min-1hour
- H2SO4 20% or more, hot solution with stirring for about 30min-1hour
- NH4NO3 saturated solution, hot solution with stirring
- Citric acid, hot solution in sonic bath
- Blank fusion (flux and NWA only)

Heavy cleaning:
- HNO3 conc. (hot and stirring), rinse  HCl Conc. (hot and stirring)
(Never use HNO3 and HCl together, it can dissolve platinum!! (Aqua regia))
- Fusion with K2S2O7 (between 5 and 10g) at 550˚C. Rinse with hot water after the
fusion

In all cases, it’s very important to rinse well your platinum-ware after cleaning them to
eliminate any residual traces of acid. At high temperature, the acid vapors can damage your
platinum. It can also damage parts of your fusion instrument.

Polishing:

Polishing treatments are used to restore the surface of the platinum. You cannot
remove deep scratches or little dots. You will be able to remove light scratches, surface
oxidation of platinum (whitish film) and shallow dots. Severe damages to platinum-ware will
require refurbishing and/or replacement. The good news is that platinum is still worth money
even if you cannot use it anymore for fusion (big hole in the bottom of your crucible for
example). You will not have to pay the entire price to replace it if you send back your ‘‘old’’
platinum in exchange.
You will find on the market many suppliers offering polisher. A lot of other fusion labs
have developed their own polish station. Many prefer to use a rotating tool (DREMEL) with
special brush tips and diamond paste. This way, we can make a general polishing or
concentrate our work on specific zones when it is needed.
Here is the method we suggest to polish platinum-ware:

1. Start with a coarse brush tip of 320 Mesh for rotating tool. Other coarser brush
types exist (180-220 Mesh) but the quantity of platinum removed will be higher.
The starting size of the Mesh always depends of the platinum deterioration.

2. Change your DREMEL tip for a foam pad. You can start to use diamond paste with
mineral oil or water (depending if your diamond paste is oil soluble or water
soluble). Add a bit of diamond paste 575 Mesh in your platinum and add few
drops of oil or water. Use your DREMEL foam pad tip and brush your platinum
with the mix.

3. Rinse well your platinum between each diamond paste operation. We strongly
recommend not to use the same foam pad for different diamond paste Mesh size.
Change your foam pad and use a diamond paste of 1000-1200 Mesh and redo a
pass of brushing.

4. After 1000-1200 mesh, you better use a softer rub tools like a tissue paper
‘‘Kleenex’’ or cotton wool because the DREMEL coarse foam pad risk to create
scratches at this point. You can now use 8000 Mesh diamond paste and rub
manually for few minutes.

5. Increase again the Mesh size to 60 000 – 100 000 to have a very nice mirror
finish. Your platinum surface will look like new.

Polishing is always a question of rubbing with a slow rise of Mesh size. You cannot start from
545 Mesh and jump right away to 60 000 because it will leave scratches. Depending of the
platinum surface ‘‘damage’’ or scratching, you can start with higher mesh size and slowly
increase. Lower mesh size (<320 Mesh) will remove deeper scratches and deep dots, but
will remove also more platinum.
 Platinum surface oxidized Platinum after polishing

The best precaution is to know what you fuse!

The majority of accidents and severe damages that happen to platinum are caused
by the sample itself. Platinum is a noble metal and he is recognized to have a low reactivity
with the majority of products (acids, oxides, etc). Unfortunately, this is not the case for all
kind of materials. You should always be cautious when you work with new samples
containing bright metallic particles (reduced metals).

The most important reactivity aspect to know with platinum is the possibility to
create low melting point alloys with other type of metal. Sometime these alloys can melt at
temperature as low as 600˚C! (ex. Pt-As 597˚C, Pt-Si 986˚C, Pt-P 588˚C).

Here is a list of reduced elements that you should fear if your sample contains at
least one of them:

- Ag - Pb - Sb
- Ni - Zn - Ferroalloys (FeSi, FeTi, FeCr, etc)
- Cu - Sn - Carbide (SiC)
- Al - Cr - Carbon (high temperature)
- Ti - As
- Si - P
 Of course, it’s not because your sample contains those kinds of elements that you
cannot use the fusion technique to prepare your sample. You just need to oxidize your
sample before or during the fusion. Here are the most common techniques to oxidize
samples containing poisonous elements for platinum:

- Pre-heating: This consists to oxidize the sample by heating in a furnace at high

temperature for a certain period of time
- Acid pre-oxidation: This consists to oxidize the sample using an acid (HCl, HNO3,
H2SO4, etc) before the fusion cycle.
- Solid oxidizer: This consists to oxidize the sample during the fusion cycle using a
solid oxidizer (LiNO3, Li2CO3, NaCO3, Sr(NO3)2, LiOH, combination of solid
oxidizers, etc)

Warning!!!

Some solid oxidizers can partially oxidize the platinum (LiOH, NaOH, sulphides). You must
take caution to protect your platinum surface from the oxidation reaction when you use a
solid oxidizer during the fusion. Here are two suggestions to dispose the products to protect
your platinum crucible during the oxidation:

‘‘On Top’’ ‘‘Sandwich Style’’

Crucible Crucible

Sample-oxidizer mix Sample-oxidizer mix

Flux Flux
Sample-oxidizer mix Sample-oxidizer mix
Flux Flux
Conclusion

We hope this document will help you to have a better understanding of the precious
tools you work with. If platinum-ware is well treated, it can stay in good shape for
thousands and thousands of fusion cycles. With a good knowledge of fusion chemistry, you
should be able to avoid bad experiences like ruined your brand new platinum crucible in a
single fusion (real story!).

Don’t hesitate to communicate with us if you need specific information about the
present document. It will be a pleasure to help you take caution of your platinum (and
instrument) by sharing our experience and knowledge.

Benoit Bouchard, Chemist

Application specialist

Katanax inc.
100-2022 Lavoisier
Quebec QC
Canada G1N 4L5

Tel: +1-418-657-6201
Fax: +1-418-657-6203

www.katanax.com