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Stuart Baskerville Department of Science and Sport, University of Glamorgan, Pontypridd, Mid
Glam., UK, CF37 1DL. sbaskerv@glam.ac.uk
Wynne Evans Department of Science and Sport, University of Glamorgan, Pontypridd, Mid
Glam., UK, CF37 1DL ewevans@glam.ac.uk
Flame tests nitric acid. These "stock solutions" of the cations should
be retained for further tests.
A nichrome wire should be cleansed by heating in the
hottest spot of a Bunsen burner flame (the tip of the blue Reaction with NaOH (aq)
cone) until no color is observed in the flame. The wire is
then moistened with concentrated HCl and dipped into A solution of NaOH should be added drop-wise to a
the powdered mineral, so that a small amount adheres to sample of the stock solution and the presence/absence,
the wire. This end of the wire is then heated and the and color, of any metal hydroxide precipitate noted. If
presence of some substances will color the outer part of the stock solution has been prepared by dissolution in
the flame. Note that the wire must be thoroughly cleaned acid, it will be necessary to ensure that the solution has a
before further use. Because the K+ color is often masked pH>7 before precipitation can occur. As addition of
by Na+, the use of a blue glass filter to view the flame is NaOH(aq) proceeds, the students can monitor the rise in
recommended. Colors that may be observed are shown pH by using a glass rod to put a drop of the solution on to
in figure 1. Faint colors may be observed from other universal indicator paper. The white precipitates
metals such as Pb2+ (pale blue); however these can be produced as Pb(OH)2, Al(OH)3 and Zn(OH) 2 exhibit
misleading and the presence of the metal should be amphoteric behaviour and will dissolve in excess of
confirmed by other means. For this reason, both NaOH(aq) to produce the soluble Na+ salts: Na2Pb(OH)4,
possibilities (colored /not colored flame) are allowed for NaAl(OH)4, and Na2Zn(OH)4 respectively.
Pb2+ in figure 1. The flame test is extremely important for
the identification of Na + and K+ because their salts are Reaction with NH4OH(aq)
soluble; hence the cations cannot be identified by tests
that rely on the production of an insoluble product. This test can be used to differentiate Zn2+ from Pb2+ and
Al3+; the zinc cation will complex with excess NH3(aq) to
Solubility form a soluble compound. Drop-wise addition of
NH4OH(aq) to a stock solution containing Zn2+ ions will
Solubility in cold water can provide a valuable clue to the result in the formation of a white precipitate of Zn(OH) 2
identity of the mineral; students should be aware that all which dissolves in excess NH4OH(aq). The same
Na+, K+ and NO3- salts are soluble in water - however operation applied to solutions containing Al3+and Pb2+
solubility does not necessarily infer that the mineral will yield white precipitates of hydroxides that persist on
belongs to one of these three classes! Compounds that addition of excess solution. The reaction can also be used
prove to be insoluble in water should dissolve in dilute as a confirmatory test for Cu2+; addition of NH4OH(aq) to
a Cu2+ solution will result in the formation of a
green/blue precipitate of Cu(OH)2 that will dissolve in Add BaCl2(aq) to a solution of the suspect SO42- sample.
excess NH 4OH(aq) to form a solution of a distinctive A white precipitate (BaSO4) that persists in acid solution
deep blue copper complex ion. (not H2SO4!), confirms the presence of SO42-.
Test for Cl- Test for NO 3-
Add AgNO3(aq) to a solution of the suspect chloride. A To ca 2 ml of an aqueous solution of the mineral (note if it
white precipitate (AgCl), which persists on the addition doesn't dissolve in water it's not a nitrate!), in a boiling
of HNO3(aq), confirms the presence of Cl-. tube, add an equal volume of NaOH(aq), and a
spatulaful of Devarda's alloy. Warm carefully. Test for
Test for SO42- the evolution of NH3, by holding damp red litmus paper
at the mouth of the tube. A blue colour indicates the
presence of NH3; this is a product of the reduction of HARDNESS AND SPECIFIC GRAVITY
NO3- by the alloy.
When the students have correctly identified the ions in a
Test for CO32- sample, they are given values for the specific gravity and
hardness of that mineral (see Table 1). They should then
Carbonates "fizz" in acid solution and CO2 is evolved. consult an appropriate text (for example Dutrow, 2007)
The presence of the gas can be confirmed by shaking it available in the lab and definitively identify the mineral.
with limewater [Ca(OH)2(aq)] - the limewater goes At the end of the exercise, students should be made
"milky" due to precipitation of CaCO3. Since CO 2 is aware that, in analysis of minerals:
heavier than air, expensive delivery apparatus is not
required; the gas can be poured from the fizzing test tube There may be more than one metal cation present in a
into a test tube containing limewater - when the latter is mineral, for example minerals can be double salts such
shaken, the reaction occurs (Figure 3). as glauberite, Na2Ca(SO4)2.
Minerals will rarely be as pure as the powders they
Test for S2- have been given to analyse and may also contain trace
amounts of other metals over those given in the
If acid is added to a solution of the unknown mineral , the chemical formula - such small details may be of value
smell of H2S (rotten eggs) will be detected. Warming the in establishing the geological/geographical origin of
mixture will speed this process up. The H2S gas blackens the material.
damp Pb(CH3COO)2 (lead ethanoate) paper. Minerals may contain the same cation(s) and anion,
but have different crystalline structures or be in
Test for B4O72- hydrated or anhydrous forms - in these cases, they will
be different minerals with different properties. For
Dip a piece of turmeric paper into the suspect B4O72- example, calcite and aragonite are both forms of
solution, acidified with HCl(aq). Dry the paper at 100 C CaCO3 - but they have different crystalline structures;
- if the paper turns reddish brown, B4O72- has been and different values for hardness and specific gravity.
identified.
REFERENCES
Bajo, S., 1978, Volatilization of arsenic(III,V), antimony
(III, V) and selenium (IV, VI) from mixtures of
hydrogen fluoride and perchloric acid solution:
application to silicate analysis, Analytical
Chemistry, v. 50, p. 649 - 651.
Figure 3. Testing for CO2. Chao, T. T. and Sanzolone, R. F., 1992, Decomposition
techniques, Journal of Geochemical Exploration, v.
44, p. 65-106.
FURTHER WORK Dutrow, B. and Klein, C., 2007, Manual of mineral
science (manual of mineralogy 23rd edition), John
There are many more chemical "spot" tests than are listed Wiley and Sons, 656p.
in this exercise. For more experienced students, the work Knapp, E. P., Desjardins, S. G., and Pleva, M. A., 2003, An
can be extended to other minerals - but additional safety interdisciplinary approach to teaching introductory
measures may need to be employed. Examples would chemistry to geology students, Journal of Geoscience
include cassiterite, cerargyrite and aluminosilicates, Education, v. 651, p.481-483.
which are insoluble in most acids and do not lend Murray, R. and Tedrow, J, 1998, Forensic Geology,
themselves to analysis by the simple methods outlined Prentice Hall ECS Professional, 176p.
here. Instead, much more extreme conditions are Urben , P., 2006, Bretherick's Handbook of Reactive
required - dissolution in HF or fusion in alkalis as Chemical Hazards (7th edition), Academic Press
examples (Chao et al., 1992 and Bajo, 1978). Inc.,U.S, 2680p.
Svehla, G., 1996, Vogel's Qualitative Inorganic Analysis
CONCLUSIONS (7th edition), Longman, 310p.
The methods described in the lab exercise require only
basic "wet" laboratory facilities and, we feel, give
students good experience of the scientific method:
observation and inference gained from systematic and
methodical working. These are essential qualities for all
scientists, and not least for forensic practitioners. In
particular, geochemical analysis of the mineral content of
soils is an invaluable aid to tracing where the soil came
from and therefore to possibly identify the scene of a
crime - since soils from different locations can have
vastly different compositions (Murray, 1998). In the
exercise described, students also gain an appreciation of
the chemical and physical properties of the minerals in
question, which will aid them in their subsequent studies
of geoscience or chemically-related courses. The
investigation contributes towards 5% of the marks for the
module.
Other practical exercises, with their percentage
contribution to the final mark, include: microscopic
analysis of thin sections of different samples of sand and
rock, in an attempt to pinpoint their areas of origin (10%);
recognition of minerals using the petrological
microscope (5%) and forensic case studies where mineral
identification has contributed to the evidence (30%). In
addition to the coursework component described,
students are required to take a 2 h exam at the end of the
academic year (50%). The pass mark is 40% - depending
on the external examiner's approval. Pass results for this
module consistently compare favourably with other
modules the students study (for example, a 93% pass rate
at first attempt in 2007). Feedback is very positive; the
students seem to enjoy the investigative nature of the
practical exercises and appreciate their relevance to the