Staining of thin-sections for feldspars: Workflow
Getting started
---prepare uncovered thin sections leaving it a bit thicker (yellow quartz)
---polish with 600-grit SiC (may use finer powders, the finer the better)
---clean with dilute ethanol (to remove SiC rests, fat, dust etc.)
---read and sign security warning about HF usage (ask István for such)
---set up your staining facility near a sink; the beakers should have the appropriate size and shape to serve as chemical baths into which your thin sections will be dipped. Now prepare all the reagents except HF:
In a 100 ml beaker, solve 0.02 g K-rhodizonate in 60 ml distilled water.
In a 100 ml beaker, solve 4.4 g BaCl2 in 80 ml distilled water.
In a 100 ml beaker, solve 36 g Na-cobaltinitrite in 60 ml distilled water.
---Fill a large (e.g. 500 or 1000 ml) beaker with distilled water and put it in the sink. (Water is used for rinsing the thin sections between the individual staining steps.) Allow a gentle stream of water to flow out of the tap which gradually replaces the water in the beaker. If possible, use distilled water.
---Set up lab wipes or paper towels with something to rest the sections against so that they dry on their edges rather than on flat sides.
---Finally, in the fume hood, prepare a bottle of HF (48 to 50%). Whenever working with HF, be very careful, calm and patient as it is extremely aggressive and toxic. Work only in the hood and keep all the security regulations.
Etching
---pour 48% HF into the etching vessel, with about 1 cm liquid height.
---close the vessel and place your section onto the aperture which has the appropriate size for your sections; take care that it fits precisely into the frame, leaving no leakage gap. (Fig. 1)
---never touch the section by hands; use a flat tweezers
---cover the dish with an upside-down plastic bowl to keep off air currents.
---etch for 45 sec; increase time if HF appears to attenuate (it remains strong for min. ~30 min.). The sections should never touch the HF liquid itself, only the vapor.
Staining
---complete etching of all sections, and keep them in the fume before proceeding to stain. The etched surfaces should not get in contact with any object.
---drop a section into Na-cobaltinitrite solution; remove after 45 sec
---rinse thoroughly in distilled water
---shake off excess water and blot section edge with many-times folded lab wipes or paper towels
---dip the section into BaCl2 solution, agitate shortly, remove after 2 sec
---rinse in distilled water, for 10 sec
---check whether there is a fine, thin, even water film covering the whole surface of the section
---place several drops of K-rhodizonate on the slide, in a very rapid succession. Help the solution distributing on the surface by agitating or tilting it gently
---after 3 sec (may vary upon plag composition), rinse in distilled water
---shake off excess water and blot section edge and dry gently with compressed air
---examine the plags with a microscope to determine whether they are sufficiently stained. If they are light grey/very light pink then cover briefly again with K-rhodizonate and rinse again. Always work with wetted surface and use short contact times (1-3 sec)
Covering
---cover just as the ordinary slides. Be careful; the stained surface is very fragile and fingers, and even water, could rub off the stain.
Some remarks
The role of reagents:
---Quartz remains unstained.
---Plagioclase will be stained by K-rhodizonate, turning them into pink.
---K-feldspar will be stained by Na-cobaltinitrite, turning them into yellow.
---BaCl2 is needed between these two staining steps, for fixing.
Stability of reagents:
---K-rhodizonate: 1-2 hours max. Always prepare it freshly (pure crystalline material is hygroscopic, thus clumps tend to form. You may have to filter the solution first).
---Na-cobaltinitrite: about 6 months (after use, filter and keep in a brown bottle)
---BaCl2: stable, but BaCO3 may form and precipitate due to contact with CO2.
Intensity of staining:
---The K-rhodizonate stain may be too pale. If so, repeat staining as many times as desirable.
---If you have a fine-grained sample, (very fine sand, silt) the plagioclase stain tends to pervade the thin section and thus obscure some quartz grains.
---Staining intensity is proportional to An%; the more calcic the plag, the more stain it takes up. Pure Ab is not expected to take up the K-rhodizonate stain.
Tamás Mikes
This compilation is largely based on:
Houghton, H. F. 1980. Refined techniques for staining plagioclase and alkali feldspars in thin section. Journal of Sedimentary Petrology 50, 629-631.
http://www.union.edu/PUBLIC/GEODEPT/COURSES/petrology/staining_feldspars.htm
Fig. 1