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Mineral Identification by Chemical Testing

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

ABSTRACT DESCRIPTION OF THE EXERCISE


We present the details of a qualitative chemistry exercise In this exercise, each student is given two different,
that can be used for mineral identification and requires unknown samples (labelled by letters and/or numbers)
relatively simplistic laboratory facilities. The exercise is to identify in a two-hour laboratory session. About sixty
used as part of a forensic earth science module for second students take the course each year, but lab classes contain
year BSc Forensic Science students who previously have no more than twenty students at a time supervised,
had a basic chemical education but little experience of typically, by two members of academic staff and a
classical inorganic analysis. We suggest that it could be laboratory technician.
adapted for use with students studying beginning Initially, pure chemicals are given to the student; this
geoscience courses who could usefully increase their avoids the expense, and time-consuming powdering, of
knowledge of chemistry. Flow charts that guide the genuine mineral samples and gets the students familiar
students through the investigation are provided. For with the observations involved. In addition, for
more experienced students, references are provided that simplicity, the students are required to identify one
illustrate more advanced "wet" analytical techniques. metal cation and one anion in each sample. A periodic
table is a useful aid to demonstrate color/solubility
trends in various groups and blocks of metals. The
INTRODUCTION students are given flow diagrams to guide them through
the tests (figures 1 and 2); for further information, the
Sophisticated instrumental techniques such as X-ray tests are described in more detail in a standard inorganic
diffraction, electron microscopy, ICP-MS analysis and analysis text (Svehla, 1996). Students are made aware
X-ray fluorescence are commonly used to identify that they should record the results of all tests and that
mineral samples. However simple chemical testing, in negative results, as well as positive ones, can give
conjunction with determination of hardness and specific valuable clues to the identity of an unknown species. The
gravity, can give valuable information about the nature students are given a standard report sheet to fill in on
of a mineral. It has also been widely recognised (Knapp which they record the code identity of the sample and
et al., 2003 and references therein) that basic chemistry their name and/or enrolment number (the university
courses are desirable components of earth science gives them an opportunity to have their work
programmes. Here we describe a mineral identification anonymously marked). They then complete a table in
laboratory exercise that is presented to second year BSc which they record their tests, observations and
Forensic Science students as part of a forensic earth inferences for each sample. On completion of this part of
science module, but could be equally successfully the exercise the students are expected to use hardness
incorporated into beginning geoscience courses. The and specific gravity data to identify the mineral, as
half module "Forensic Earth Science" was created in subsequently described.
order for the students to appreciate the role of earth
science data in the forensic examination of crime scenes. SAFETY
It contains the identification of rocks and minerals by the
use of the petrological microscope and chemical analysis Students should wear appropriate dress: laboratory
as well as a background to stratigraphic (including soil) coats or overalls, safety glasses and safety gloves.
analysis and the role of clast, crystal and particle analysis Instructors should complete appropriate risk
in informing forensic investigation. The module assessments before the commencement of the exercise
comprises thirty-six hours of class contact time and is (see, for example, Bretherick's Handbook of Reactive
delivered via formal lectures, tutorials and practical Chemical Hazards, 2006). All chemicals should be
exercises and assessed through examination and regarded as potentially harmful by inhalation or
practical coursework. This account describes one such ingestion. Any tests that involve sulfides should be
practical assignment. The students have already had carried out in a fume hood in case of deliberate or
basic experience with theoretical and practical chemistry accidental generation of toxic H2S. Concentrations of
in year one; they will have knowledge of formulae, solutions used are typically 1 mol L-1, except: AgNO3 ( 0.1
equations, stoichiometry, bonding theory and crystal mol L-1) and BaCl2 (0.5 mol L-1).
structures as relevant examples. The aim of this module
is to demonstrate how relevant these chemical concepts ADDITIONAL NOTES ON TESTS
are to both their understanding of fundamental
geological processes (such as the importance of Color of solid or solutions
dissolution and precipitation in both the creation and
destruction of limestones) and the rigors of forensic Colors frequently indicate the presence of a transition
investigation. metal ion such as Cu 2+, Fe2+ or Ni2+.

302 Journal of Geoscience Education, v. 56, n. 4, September, 2008, p. 302-306


Mineral Chemical Name Ions Present Hardness Specific Gravity
Saltpeter/niter Potassium nitrate K+ NO3 - 2.0 2.1
Mirabilite/Glauber salt Sodium sulfate Na+ SO4 2- 1.5 - 2.0 1.5
Rock salt/halite Sodium chloride Na+ Cl- 2.0 - 2.5 2.2
Chile saltpeter Sodium nitrate Na+ NO3- 1.5 - 2.0 2.3
Borax Sodium tetraborate Na+ B4 O72- 2.0 -2.5 1.7
Witherite Barium carbonate Ba2+ CO32- 3.5 4.3
Calcite Ca2+ CO32- 3.0 2.7
Aragonite Calcium carbonate 3.5 - 4.0 2.9
Gypsum Ca2+ SO42- 1.5- 2.0 2.3
Anhydrite Calcium sulfate 3.0 - 3.5 2.9
Morenosite Nickel sulfate Ni2+ SO42- 2.0 - 2.5 2.0
Malachite Copper(II) carbonate Cu2+ CO32- 3.5 - 4.0 3.9 - 4.0
Chalcanthite Copper(II) sulfate Cu2+ SO42- 2.5 2.1 - 2.3
Atacamite/remolinate Copper(II) chloride Cu2+ Cl- 3.0 - 3.5 3.7 - 3.8
Epsom salts/epsomite Magnesium sulfate Mg2+ SO42- 2.0 - 2.5 1.7
Websterite/aluminite Aluminium sulfate Al3+ SO42- 1.0 - 2.0 1.7
Melanterite Iron(II) sulfate Fe2+ SO4 2- 2.0 1.9
Pyrite Iron(II) disulfide Fe2+ S22- 6.0 - 6.5 4.8 - 5.1
Pyrrhotite Iron(II) sulfide Fe2+ S22- 3.5 - 4.5 4.4 -4.7
Strontanite Strontium carbonate Sr2+ CO32- 3.5 - 4.0 3.6 - 3.7
Galena Lead(II) sulfide Pb2+ S2- 2.5 7.4 - 7.6
Cerussite Lead carbonate Pb2+ CO32- 3.0 - 3.5 6.6
Smithsonite Zinc carbonate Zn2+ CO3-2 4.0 - 4.5 4.3 - 4.5
Spahlerite Zinc sulfide Zn2+ S2- 3.5 - 4.0 3.9 - 4.2

Table 1. Minerals suitable for identification in the chemical tests described.

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

Baskerville and Evans - Mineral Identification by Chemical Testing 303


Figure 1. Identification of cations.

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

304 Journal of Geoscience Education, v. 56, n. 4, September, 2008, p. 302-306


Figure 2. Identification of anions.

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.

Baskerville and Evans - Mineral Identification by Chemical Testing 305


field of forensic science. Comments received on
end-of-module evaluation forms have included:
"I found the coursework challenging, [it] kept me
thinking which I enjoy"
"The exercises are good. Overall I found the chemistry
interesting"
"I didn't realise that soils and sands could be so different"

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

306 Journal of Geoscience Education, v. 56, n. 4, September, 2008, p. 302-306