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Quick Assays in Mineral Identification

Quick Assays in Mineral Identification

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04/18/2013

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The good news first: for the most important tests you need only a few chemicals and
normally only a very small amount of each. Generally minute amounts, a pinch or a knife–
pointful, are used for a test. Thus a sufficient supply may be stored in approx. 5 ml volume
plastic tubes with a tight-fitting hinged lid. All chemicals should be carefully labelled!

The bad news:
- If you want to do all possible spot tests, you have to keep more than 50 different
chemicals in store.
- Although you will use very small amounts of any chemical, suppliers sell only large
packages, much bigger than you need!

The simplest way to overcome these difficulties is to have a friend who works at a chemical
laboratory, preferably at an university laboratory. Some of the chemicals are sold in small
quantities by pharmacies. Another way is to place a joint order together with other interested
collectors. Some hints about suppliers are given in part II.

Solid reagents.

Sodium carbonate, Na2CO3 (soda); Na2CO3 10H2O (natron) is also available.-
Dry sodium carbonate should be preferred. It melts at 854° C. The melt decomposes most
chemical compounds, thus producing the sodium salts of the anions, the cations are
transferred to carbonates, oxides or other compounds. NaHCO3, which is sold as baking soda
at pharmacies, may be used as well.

Sodium tetraborate, Na2B4O7 ; Na2B4O7 10 H2O (borax) is also available.-
The dry reagent melts at 742° C. The melt cools to a clear glass. Sodium tetraborate melt
dissolves various substances, especially metal oxides, in many cases yielding characteristic
colours.

Ammonium sodium hydrogen phosphate, NH4NaHPO4 4H2O, is sometimes called
phosphorous salt or microcosmic salt.-
On heating, this salt changes to sodium metaphosphate NaPO3 by losing water and NH3.
If available NaPO3 should be preferred. The melting point is 628° C, again a clear glass is
obtained. Many oxides give a distinct colour to the glass.

13

The origin of the name microcosmic salt.

Beads of sodium metaphosphate saturated with some oxides cool to a clear glass. Small crystals grow
in the glass on repeated heating and cooling. A microscope with a 80 to 100 x magnification is needed
to inspect these crystals with various morphologies. Such beads resemble a microcosmos. Some
authors tried to use the effect for analytical purposes in the 19th

century, but these efforts failed. Borax

beads sometimes show the same effect.

Potassium hydrogen sulphate KHSO4 –
This compound melts at 210° C, it decomposes according to:
2 KHSO4 ⇒ K2S2O7 + H2O and K2S2O7 ⇒ K2SO4 + SO3 .
A variety of minerals are decomposed by fusion with the reagent. Such fusions may be made
either in a platinum wire loop, on a magnesia rod, in porcelain, on glazed clay dishes, or in a
test tube.

Ammonium hydrogen sulphate, NH4HSO4 –
Melting point 147° C. This compound or its concentrated solution can be used instead of
concentrated sulphuric acid in some cases.

Potassium nitrate, KNO3 (nitre) –
It is used only in a mixture with three parts of sodium carbonate in sensitive reactions for
chromium and manganese.

Tin(II) chloride, SnCl2 2H2O –
It is used in reductions.

Potassium oxalate, K2(COO)2 –
Is used for reducing melts, mostly together with sodium carbonate.

Tin, Sn / zinc, Zn –
These metals are used for reductions. The granulated metals are preferred, thin foil is useful,
too. Don't use soldering tin, since this is an alloy!

Magnesium, Mg –
Magnesium ribbon is useful for detecting phosphoric acid in minerals.

A mixture of one part ammonium chloride NH4Cl and two and a half parts of ammonium
nitrate NH4NO3 has a melting point of approx. 140° C. It may be used like aqua regia, which
is a mixture of concentrated nitric and hydrochloric acid. The solid mixture should be kept
dry, any contact to metals or reducing chemicals should be avoided! Melting should be done
in porcelain or glass vessels or on a magnesia furrow.

Cobalt nitrate, Co(NO3)2 –
Just before use, the required amount of this salt is dissolved in 10 parts of water. The solution
is used to identify some oxides.

Ammonium heptamolybdate, (NH4)6Mo7O24 4H2O –
It is used for the detection of phosphates, arsenates, and silicates.

14

Liquid reagents

You will need distilled water, which is sold at pharmacies or filling stations. It is convenient
to keep a supply of distilled water in a washbottle of the type used in chemical labs.

Hydrochloric acid, HCl –
Concentrated HCl is sold with either 32 or 36 weight%. A 1:1 dilution is generally used.

Nitric acid, HNO3 –
Concentrated nitric acid has 65 weight%. It is extremely corrosive, keep it away from skin,
fabric, metal and paper. Generally a dilution of 1 volume conc. HNO3 with 2 volumes of
water is sufficient.

Sulphuric acid, H2SO4 –
A diluted sulphuric acid 30 weight% is sold for lead batteries at filling stations in nearly all
countries. This acid is sufficient for nearly all tests. – Some drops of the concentrated acid
may be prepared by heating no more than 1 ml of the 30% acid in a test tube, shaking
vigorously till white fumes are produced. Use and handle the remaining liquid only after
cooling! - In most cases it is possible to use ammonium hydrogen sulphate instead of
concentrated sulphuric acid.

The concentrated acids described above should be stored in small glass bottles with ground-
glass-stoppers. The diluted acids can be stored in polyethylene bottles with screw tops. Before
filling please leak-proof the bottle and the screw; fill with water, screw shut, and squeeze the
bottle gently holding the neck of the bottle downward.

Ammonium hydroxide, NH4OH –
The concentrated solution has 34 weight%, a 1:1 dilution is sufficient.

Methanol, CH3OH –
It is used for a special boron test, or as a solvent for organic compounds, it is poisonous when
swallowed! Denatured ethanol may be used instead.

Hydrogen peroxide, H2O2 –
A diluted solution is used in some tests for Ti, Cr, V, or Mn. – You may use a freshly
prepared solution of sodium perborate instead. This is a constituent of tablets sold for cleaning
dentures. Look for the name sodium perborate on the label showing the ingredients. A
common brand is Kukident. A tiny part of a tablet dissolved in 1 – 2 ml water is sufficient for
each test.

It is advisable to store only a very small amount of all wet chemicals, bottles holding 30 or
50 ml are sufficient! If you need only a few drops, use a dropper to take the amount from the
bottle. - A glass tube with a narrow inner diameter (3, 4, or 5 mm) is heated in the middle over
a flame, turning it slowly so that the glass will be uniformly heated. When the glass becomes
quite soft, the tube is removed from the flame and quickly pulled in two parts. Break off the
thus formed capillary in order to get a narrow opening. Soak the liquid by means of a rubber
bulb, it is a good auxiliary construction to fix a plastic tubing to the end of the glass dropper
and close the end of the plastic tubing by a glass rod (figure 6).

15

For transport of any kind the leakproof plastic bottles should each be wrapped in a plastic
bag secured by sellotape. Put this in a tin with a tight lid and fill the free volume at least partly
by an absorbent material like silica gel. You can also use the super-absorbent material from a
modern diaper like the brand pampers. Again the lid of the tin should be fastened with
adhesive tape.

The transport of any corrosive liquids, acids and strong alkaline solutions on an aircraft is
strictly prohibited by international air traffic regulations. You may overcome this difficulty by
using 30% sulphuric acid for lead batteries which is available worldwide and can be bought at
your destination.

- On dissolving 4.3g of NaCl in 10 ml of such acid and adding 10 ml of water you get a

15% HCl.

- A solution of 6.1g of ammonium nitrate in 10 ml of sulphuric acid 30% can be used
instead of nitric acid.

- If you dissolve 2 g of NH4Cl and 1.4g of NaOH in 10 ml of distilled water, you may use
this solution like ammonium hydroxide.

Weigh these chemicals at home and seal or weld them separately in plastic for transport. Do
not forget to label them correctly. Mark a volume of 10 ml by a waterproof pen on a test tube.
The additional ions in these solutions must be considered only in the case of a few wet tests.
If you only need an acid to detect calcium carbonate, you may use vinegar, or, better a 10%
solution of citric acid in water.

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