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LABORATORY EXPERIMENTS
IN MEDICAL CHEMISTRY
Edited by
GYRGY OSZBACH
PCS, 1995
CONTENTS
1. INTRODUCTION
Laboratory safety..................................................................................................... 3
Accident protection, fire protection, first aid .......................................................... 5
2. LABORATORY UTENSILS AND METHODS
Utensils.................................................................................................................... 9
Simple laboratory methods...................................................................................... 9
Laboratory measurements .................................................................................. 9
Heating ............................................................................................................... 9
Forming precipitates ........................................................................................ 12
Preparation of gases......................................................................................... 12
3. SIMPLE LABORATORY SEPARATION METHODS
14
Decantation............................................................................................................ 14
Filtration ................................................................................................................ 14
Drying.................................................................................................................... 15
4. CHEMICAL ANALYSIS
17
44
4.1.63
Reaction of sulphate ion.............................................................................53
4.1.64-66 Reactions of phosphate ion ........................................................................53
4.1.67
PREFACE
ince the English Program started at the University Medical School of Pcs in
1984, remarkable changes have been made in chemical education. Today,
there are appropriate textbooks available to support the lectures and seminars
in the fields of General, Organic and Bioinorganic Chemistry. In 1994, the
Department issued a handout on Inorganic Chemistry, but there was a lack of an
updated laboratory manual. (The former one was written in 1984 and the last reprint
was edited in 1991.) This edition is a translation of the Hungarian version ("Orvosi
kmiai gyakorlatok") issued this year.
The manual contains experiments much more than can be completed within
the limited time of the main course. Among them, there are practices to be replaced in
the future by another ones that cannot be performed for the time being. Some of the
experiments, mainly the instrumental ones, appear as demonstrations, which are
planned to be carried out by the students themselves.
When writing the lab manual, our main object was to enable students to work
independently in the laboratory, observe relevant phenomena, draw conclusions and
make notes, by which anyone can reproduce the experiment.
It is strongly recommended, that students carefully study Chapter 1,
"Laboratory Safety", before starting work in the laboratory to avoid accidents.
Chapter 2 ("Laboratory Utensils and Methods") and 3 ("Simple Laboratory
Separation Methods") comprise general laboratory methodology, which are to be
mastered so that it can provide a firm knowledge throughout the course. The
following "Chemical Analysis" section includes qualitative, quantitative, organic and
bio-organic analytical practices. In Chapter 5 ("Reaction Kinetics") and Chapter 6
("Chemical Equilibria") simple test-tube reactions help students comprehend the basic
concepts of the processes also important in life sciences. A separate chapter, number
7, is devoted to the most powerful separation method, chromatography, widely used in
biomedical practice and research. Chapter 8, "Instrumental Analysis", offers an insight
into the high-performance methods employed in modern diagnostic laboratories.
In Chapter 9 (Appendix) one can find an overview of Inorganic Chemistry,
particularly recommended in the first half of the course. Calculation Exercises are
attached to promote student's own preparation for the exams on General Chemistry.
Concentrations of reagent solutions used regularly in the practices, which are
prepared by technicians in the stock laboratory, are not indicated in the text. For a
better reproducibility, they are also available in the Appendix.
1. INTRODUCTION
LABORATORY SAFETY
Preparation in advance
a) Read through the descriptions of the experiments carefully. If necessary, do
study the theoretical background of the experiments from your chemistry book(s).
After understanding, write down the outline of the experiments to be performed in
your laboratory notebook. If any items you don't understand remain, do ask your
instructor before starting work.
b) Prepare your notebook before the laboratory practice. Besides description of
the outline of the experiments, preliminary preparation should also include a list of the
chemicals and procedures which need special care and attention to avoid laboratory
accidents during your work.
Laboratory rules
a) The laboratory instructor is the first to enter and the last to leave the
laboratory. Before the instructor's arrival students must not enter the laboratory.
b) Always wear laboratory coat and shoes in the laboratory. Sandals and opentoed shoes offer inadequate protection against spilled chemicals or broken glass.
c) Always maintain a disciplined attitude in the laboratory. Careless acts are
strictly prohibited. Most of the serious accidents are due to carelessness and
negligence.
d) Never undertake any unauthorized experiment or variations of those
described in the laboratory manual.
e) Maintain an orderly, clean laboratory desk and cabinet. Immediately clean
up all chemical spills from the bench and wipe them off the outer wall of the reagent
bottles with a dry cloth.
f) Smoking, drinking, or eating is not permitted during the laboratory practice.
Do not bring other belongings than your notebook, stationery, and laboratory manual
into the laboratory. Other properties should be placed into the locker at the corridor.
g) Be aware of your neighbour's activities. If necessary, warn them of improper
techniques or unsafe practices.
h) At the end of the lab, completely clean all glassware used in the
experiments, clear the laboratory bench of reagent bottles, glassware and equipment,
and clean it with a dry cloth. After putting back all your personal labware into your
cabinet, lock it carefully.
i) Always wash your hands with soap before leaving the laboratory.
point it at anyone. If you want to check the odour of a substance formed in a test tube
reaction, waft the vapours from the mouth of the test tube toward you with your hand.
c) Before heating glassware make sure that its outer wall is dry. Wet glassware
can easily break on heating. When heating liquids in a test tube, hold it with a piece of
tightly folded paper or a test-tube holder.
d) When heating liquids in an Erlenmeyer flask or in a beaker, support the
glassware on a wire gauze placed on an iron tripod, and put a piece of boiling stone
into the liquid to prevent bumping. Start heating with a law flame and intensify it
gradually.
e) When lighting the Bunsen burner, close the air-intake holes at the base of
the burner, open the gas cock of the outlet, and bring a lighted match to the mouth of
the burner tube until the escaping gas at the top ignites. (It is advantageous to strike
the mach first and then open the gas cock.) After it ignites, adjust the air control until
the flame is pale blue and the burner produces a slight buzzing sound.
f) If the Bunsen burner "burns in", which can be noticed from its green flame
and whistling (whizzing) sound, the gas valve of the outlet should be turned off
immediately. Allow the burner to cool, and light it again as described above.
g) When using an electric heater or other electric device, do not touch them
with wet hands and prevent liquids from spilling over them. If it accidentally happens
(e.g. a flask cracks on heating), unplug the device immediately and wipe off the liquid
with a dry cloth.
h) As a general rule, a flame should be used to heat only aqueous solutions.
Most organic solvents boil below the boiling point of water. A hot water bath can be
effectively used to heat these solvents.
i) When working with flammable organic solvents (e.g. hexane, diethyl ether,
petroleum ether, benzene) use of any open flame in the laboratory is prohibited. The
vapours of the flammable substances may waft for some distance down their source;
thus presenting fire danger practically in the whole laboratory.
j) In case of a smaller fire (e.g. a few millilitres of organic solvent burning in a
beaker or an Erlenmeyer flask), it can be extinguished by placing a watch glass over
the mouth of the flask. In case of a bigger fire and more serious danger, use the fire
extinguisher fixed on the wall of the laboratory. At the same time alarm the University
Fire Fighter Office by calling the N 1333 from the corridor or from the stock lab.
k) Never blow the fire. This way you might turn the fire up and the flame can
shoot into your face. Do not use water to smother fires caused by water-immiscible
chemicals (e.g. benzene) and alkali metals. Pouring water on a plugged electric device
is also prohibited.
l) If your clothing catches fire, you can smother the flames by wrapping
yourself in a wet towel or a laboratory coat.
m) In case of fire in the laboratory the main gas valve and the electric switch
of the laboratory should be turned off immediately. (They are located in the corridor
on the outer wall of the laboratory.) Besides fighting the fire, start giving the injured
first aid immediately.
First aid
a) In case of an accident or injury, even if it is minor, notify your laboratory
instructor at once. The urgent first aid is an absolute requirement for the prevention of
more serious adverse health effects.
b) Minor burns caused by flames or contact with hot objects should be cooled
immediately by flooding the burned area with cold water, then treating it with an
ointment. Severe burns must be examined by a physician.
c) In case of a cut, remove the contamination and the glass splinters from the
wound. Disinfect its boundary with alcoholic iodine solution and bind it up with
sterile gauze. In case of severe cases the wound should be examined and treated by a
physician.
d) Whenever your skin gets into contact with chemicals, wash it quickly and
thoroughly with water. In case of chemical burns, the chemical should be neutralized.
For acid burns, the application of a dilute sodium hydrogen carbonate, for burns by
alkali, the application of a dilute solution of boric acid is used. After neutralization,
wash the affected area with water for 5-10 minutes and apply an oily ointment if
necessary.
e) Concentrated sulphuric acid dripped onto your skin must be wiped away
with a dry cloth. Then the affected area should be treated as described for acid burns
above.
f) Acids splashed onto your clothes could be neutralized with diluted solution
of ammonia or sodium hydrogen carbonate.
g) If any chemical gets into your mouth, spit it out immediately, and wash your
mouth well with water. In case of acidic or basic chemicals rinse your mouth first with
a diluted solution of sodium hydrogen carbonate or that of boric acid, respectively, to
neutralize the acid or the base.
7
h) If any chemical enters your eyes, immediately irrigate the eyes with large
quantities of water. In case of any kind of eye damage consult a physician
immediately.
i) In case of inhalation of toxic chemicals the injured should be taken out to
fresh air as soon as possible.
j) In case of an electric shock, the immediate cutoff of the electric current
supply of the laboratory (main switch) is the most important step to avoid irreversible
health damage. The injured should get medical attention as soon as possible. If
necessary, artificial respiration should be given until the physician arrives.
UTENSILS
Laboratory Measurements
Heating
In the laboratories, both direct and indirect methods of heating are used. For
direct heating a free gas flame or an electric hotplate or an electric heating mantle, for
indirect heating mostly liquid baths (water, mineral oil, silicone oil, glycerol) are used.
One of the most common sources of heat is the gas Bunsen burner (Fig.2.1b).
Solid materials can be heated (or ignited) on a direct flame in porcelain or
metal crucibles placed onto an iron tripod by means of a clay triangle. Heating is
started with a small flame and intensified gradually. Ignitions under precisely
controlled conditions can also be performed in an electric furnace.
Smaller amounts of aqueous solutions may be heated and boiled on direct
flame keeping a test tube with not more than 3-4 cm3 of the solution into the mantle
of the flame by means of a strip of a triple-folded paper sheet or a test-tube holder.
First the upper part of the solution is heated and then the rest. Caution: Never turn the
opening of a heated test tube toward your face or toward other people working
nearby.
Larger amounts of nonflammable, not too volatile liquids can be heated and
boiled in an Erlenmeyer flask or a beaker placed onto an iron tripod by means of an
asbestos wire gauze. In case of boiling, a piece of pumice (boiling stone) is placed into
the solution to avoid bumping.
1. Test tube
3. Beaker
4. Wash bottle
5. Measuring cylinder
6. Glass funnel
7. Watchglass
8. Porcelain crucible
9. Petri dish
11.Narrow-mouthed reagent bottle
11
Forming Precipitates
Precipitates are produced mostly for analytical purposes. Then the visual observation
is very important. Therefore, the reagent is added gradually with shaking while the
changes are monitored. For a complete precipitation, the reagent should be added in
excess. Note that in case of amphotery or complex formation the excess of the reagent
can dissolve the previously formed precipitate.
Preparation of Gases
Laboratory gases (O2, N2, Cl2, H2, CO2, N2O, HCl, noble gases) on large scale are
put on the market in high-pressure cylinders. Smaller amounts of them can also be
prepared in the laboratory. The most widely used gas generator is the so-called Kipp's
apparatus which is suitable for producing gases from a solid, water-insoluble and a
liquid reactant (Fig. 2.2). It consists of two bulbs separated by a diaphragm and of a
long-stem funnel introducing the solution into the lower bulb. The apparatus functions
semi-automatically as follows:
12
The solid reactant is placed into the middle bulb and, from the upper funnel,
the liquid reactant is introduced into the lowest bulb. The lowest bulb can not be filled
because of the resistance of the compressed air in the two lower bulbs. Turning the
gas-outlet stopcock on, the hydrostatic pressure pushes the liquid reactant through the
diaphragm into the middle part and the reaction starts. If the gas cock is turned off, the
increasing pressure of the evolving gas presses the liquid back into the lowest part and
the reaction is stopped. However, the apparatus is then ready to function again if the
cock is turned on. Usually a wash bottle is attached to the gas outlet for washing out
the drops of the reagents and for flow control. A rate of not more than 2 to 3 bubbles
per second gas flow is advised.
Gases frequently prepared in Kipp's apparatus:
Hydrogen from granulated zinc and hydrochloric acid according to the equation:
Zn + 2 H+ = H2 + Zn2+
Hydrogen sulphide from iron(II) sulphide and hydrochloric acid:
FeS + 2 H+ = H2S + Fe2+
Carbon dioxide from cracked marble and hydrochloric acid:
CaCO3 + 2 H+ = Ca2+ + H2O + CO2
13
Decantation
The simplest way of the separation of a liquid from a solid phase is called decantation.
In this operation a suspension is allowed to stand until the precipitate settles down and
then the supernatant liquid is cautiously poured off. Then, the rest is suspended in
distilled water and the procedure is usually repeated twice to remove the dissolved and
adsorbed impurities. For the sedimentation of very fine suspensions, especially for
that of colloidal ones, centrifugation is used.
Filtration
Filtration means the separation of two phases with the aid of a filtering layer which
allows only one of the phases to pass through. Usually the solid phase is separated
from the liquid and rarely from the gaseous phase. In case of simple filtration,
hydrostatic pressure is enough to have the liquid pass through. To enhance the rate of
filtration, reduced pressure can be applied for vacuum filtration in the laboratory.
Rarely, filtration under pressure is also applied.
If simple filtration is performed at atmospheric pressure, smooth, conical and
short-stem funnels are used (Fig. 3.1).
14
Drying
Drying means the removal of an unnecessary liquid or its vapour from a solid, liquid
or gaseous material. In most cases, water is to be removed. The performance of drying
depends on the state of matter and the thermal stability of the substance to be dried.
Thus, gases and liquids are usually kept in direct contact with the drying agent. Solid
samples are usually placed into a closed space (desiccator) and the drying agent acts
through the common airspace (Fig. 3.6). A wide variety of hygroscopic materials are
used as dehydrating agents. Of hydrate-forming substances, anhydrous CaCl2,
Mg(ClO4)2, Na2SO4, K2CO3 cc. H2SO4, NaOH and KOH are widely used. Some
metals and a few oxides bind water by a chemical reaction, e.g. Na, K, CaO, P2O5.
Silica gel, which is coloured by a blue cobalt salt when prepared for drying, binds
water by adsorption. If silica is saturated with water, the blue colour of the cobalt salt
turns pink, indicating that silica should be reactivated by warming.
Gases can be dried by passing them through an adsorption tube with a solid
packing, e.g. P2O5 or silica or through a washing bottle filled with a liquid drying
agent, e.g. cc. sulphuric acid.
Liquids are usually dried by adding an insoluble solid dehydrating agent and
are allowed to stand for a longer period of time. The drying agent can be removed by
filtration or decantation. For the dehydration of certain organic solvents, azeotropic
distillation (see later, at "Distillation") is useful.
Demonstration: Desiccator, infrared lamp.
16
4. CHEMICAL ANALYSIS
The aim of chemical analysis is the qualitative recognition and the determination of
the quantity of the constituents (e.g. atoms, ions, groups) of substances or mixtures.
Accordingly, analytical chemistry can be classified into two main parts: qualitative
and quantitative analysis. However, in the modern natural science and industry it is
also requested to answer questions about the form, distribution and interactions of the
constituents. Therefore, the task of analysis is to answer all the questions about the
chemical composition, structures, etc. being important in the characterization or
usage.
Chemical analysis may be classified according to the nature of the substances
investigated. Thus, inorganic and organic analysis are different but not strictly
independent fields of analysis. Inorganic analysis may be subdivided into metal,
silicate, etc. analysis; organic analysis comprises hydrocarbon, protein, food,
pharmaceutical, etc. analysis.
Another way of classification is based on the applied methods. The two main
branches of quantitative analysis are gravimetry and titrimetry. Gravimetry is based on
the measurement of the mass of the samples, while the volumetric methods are based
on the measurement of volumes proportional with the amount of a gas or a dissolved
reactant. Many of the physical or physicochemical properties are known to give
measurable values proportional with the mass or the concentration of different
samples. These instrumental analysis methods allow to perform the gravimetric or
volumetric determinations more precisely and sometimes can be automated. On the
other hand, instrumental methods themselves are useful to determine concentration or
composition occasionally together with structure. Separation methods represent
another enormously developing field of analysis.
It should be noted that the modern, fast and high performance methods unify
the separation, detection and quantitative determination techniques as well. The
principles are the following:
a) During separation the components are identified and usually quantitatively
measured. (E.g. immunoelectrophoresis, affinity chromatography or the combined gas
chromatography-mass spectrometry in which the chromatographically separated and
quantitatively measured
spectrometer.)
17
b) Without separation, selective analysis methods are used for one or more
components of a mixture not being sensitive to other components present (e.g.
enzymatic determination of blood glucose).
18
19
DETECTION OF CATIONS
During the systematic qualitative analysis the test for cations always precedes
that of anions since the previous knowledge of the present cations simplifies the
analysis of anions.
The most common cations are classified into five analytical groups taking
advantage of the different solubility of their derivatives formed with the reagents
added subsequently in the order: hydrochloric acid, hydrogen sulphide, ammonium
sulphide and ammonium carbonate. The formulas of physiologically important
(essential or poisonous) ions are underlined. They will be studied in the laboratory
course.
20
GROUP 1a
Cl
NH2
+ Hg + Cl- + 2 H2O
Experiment 4.1.8
Adding NaOH solution, black mercury(I) oxide precipitates.
Hg22+ + 2 OH- = Hg2O + H2O
Experiment 4.1.9
Adding NH4OH solution, metallic mercury and basic mercury(II) amido
nitrate form as a black precipitate (disproportionation).
21
NH2
NO 3
+ 2 Hg + 3 H2O
GROUP 1b
Experiment 4.1.11
NaOH solution precipitates yellow mercury(II) oxide. Difference from
mercury(I) ion which turns black with NaOH.
Hg2+ + 2 OH- = HgO + H2O
Experiment 4.1.12
NH4OH solution precipitates white mercury(II) amido chloride.
Hg2+ + Cl- + NH4+ + 2 OH- = Hg
NH2
Cl
+ 2 H2 O
Experiment 4.1.13
Potassium iodide (KI) solution gives a red precipitate of mercury(II) iodide.
The precipitate dissolves in excess reagent to form colourless, water-soluble
tetraiodomercurate(II) ion.
Hg2+ + 2 I- = HgI2
22
HgI2 + 2 I- = [HgI4]2The alkaline solution of the complex salt is the so-called Nessler's reagent, which is
used for testing NH4+.
GROUP 2.
For testing the reactions of arsenic(III) ion, arsenic trioxide [As2O3] stock solution is
used.
Experiment 4.1.20
Bettendorf's test:
Bettendorf's reagent, tin(II) chloride (SnCl2) in cc. HCl solution (caution, very
caustic!), reduces arsenic compounds to elementary arsenic as a black precipitate or a
mirror on the wall of the test tube.
2 As3+ + 3 Sn2+ = 2 As + 3 Sn4+
Procedure:
Excess volume of Bettendorf's reagent is added to the test solution and is
allowed to stand for a few minutes.
23
Experiment 4.1.21
Gutzeit's test:
Elementary zinc (in hydrochloric acid medium) reduces the soluble arsenic
compounds to arsine gas (AsH3). Allowing the gas to come into contact with a filter
paper wetted with a drop of concentrated silver nitrate solution, a yellow spot appears
which turns black when applying a drop of water onto it.
AsO33- + 9 H+ + 3 Zn = AsH3 + 3 Zn2+ 3 H2O
AsH3 + 6 AgNO3 = Ag3As . 3 AgNO3 + 3 HNO3
Ag3As . 3 AgNO3 + 3 H2O = 6 Ag + H3AsO3 + 3 HNO3
Procedure:
To 1 cm3 As-containing solution a few cm3s of HCl, a few drops of CuSO4
and a piece of zinc metal are added. A wad of cotton wool is applied into the mouth of
the test tube as a filter and the tube is covered with a piece of filter paper wetted with
a drop of 50 % silver nitrate. A yellow spot develops within a few minutes which
turns black when a drop of water is added.
24
GROUP 3
For testing the reactions of iron(II) ion, iron(II) sulphate [FeSO4] stock
solution is used.
Experiment 4.1.35
NaOH solution precipitates greenish-white iron(II) hydroxide, which, allowed
to stand on air, is oxidized to brown iron(III) hydroxide.
Fe2+ + 2 OH- = Fe(OH)2
4 Fe(OH)2 + 2 H2O + O2 = 4 Fe(OH)3
Experiment 4.1.36
K3[Fe(CN)6], potassium-hexacyanoferrate(III) solution precipitates dark blue
iron(II) hexacyanoferrate(III).
3 Fe2+ + 2 [Fe(CN)6]3- = Fe3[Fe(CN)6]2
25
For testing the reactions of iron(III) ion, iron(III) chloride [FeCl3] stock
solution is used.
Experiment 4.1.38
NaOH solution deposits reddish-brown, gelatinous iron(III) hydroxide.
Fe3+ + 3 OH- = Fe(OH)3
Experiment 4.1.39
K4[Fe(CN)6], potassium hexacyanoferrate(II) solution precipitates iron(III)
hexacyanoferrate(II) (Prussian blue). The reaction is specific for Fe3+ ion.
4 Fe3+ + 3 [Fe(CN)6]4- = Fe4[Fe(CN)6]3
Experiment 4.1.40
NH4SCN, ammonium thiocyanate (ammonium rodanide) solution in slightly
acidic medium produces blood-red coloration. Iron(III) thiocyanate formed may be
extracted (transferred into another phase) by shaking with diethyl ether.
Fe3+ + 3 SCN- = Fe(SCN)3
26
GROUP 4
For testing the reactions of calcium ion, calcium chloride [CaCl2] stock
solution is used.
Experiment 4.1.42
(NH4)2(COO)2, ammonium oxalate solution in slightly basic, neutral or acetic
acid medium precipitates white Ca oxalate. This reaction is characteristic and very
sensitive to Ca2+ ion.
Ca2+ + (COO)22- = Ca(COO)2
Experiment 4.1.43
27
Flame test. The volatile Ca compounds colour the gas flame brick-red.
General procedure:
Into a porcelain crucible, 1 cm3 of the sample solution (or 0.1-0.5 g of a solid
sample) and a granule of elementary zinc are placed and the crucible is almost totally
filled with 20 % hydrochloric acid solution. The non-luminous flame of the Bunsen
burner held horizontally above the intensively bubbling solution changes its colour
(Fig. 4.1.1).
GROUP 5
Experiment 4.1.44
NaOH solution precipitates white, gelatinous magnesium hydroxide.
Mg2+ + 2 OH- = Mg(OH)2
In the presence of ammonium salts, due to the decrease of OH- concentration, the
precipitate does not form (see mass-action law; solubility product and Exps. 4.1.65
and 6.10).
Experiment 4.1.45
In the absence of other ammonium salts, (NH4)2CO3 or Na2CO3 solution
precipitates white crystals of basic magnesium carbonate.
4 Mg2+ + 4 CO32- + 4 H2O = Mg(OH)2.3 MgCO3.3 H2O + CO2
28
Experiment 4.1.46
Magnesia mixture (see Exp. 4.1.65 and Exp. 6.10) forms a white precipitate
with sodium hydrogen phosphate (a characteristic reaction of both magnesium and
phosphate ions).
Mg2+ + NH4+ + PO43- = MgNH4PO4
Reactions of sodium ion (Na+)
For testing the reactions of sodium ion, sodium chloride [NaCl] stock solution
is used.
Experiment 4.1.47
Flame test: (For the performance see Exp. 4.1.43.) Sodium chloride vapour
colours the flame intense yellow (very sensitive for sodium).
Experiment 4.1.48
In a neutral or slightly alkaline medium potassium hexahydroxoantimonate(V)
solution precipitates white sodium hexahydroxoantimonate(V).
Na+ + [Sb(OH)6]- = Na[Sb(OH)6]
Reactions of potassium ion (K+)
For testing the reactions of potassium ion, potassium chloride [KCl] stock
solution is used.
Experiment 4.1.49
In a not too dilute solution sodium hydrogen tartrate precipitates potassium
hydrogen tartrate as white crystals.
29
COO K+ +
COOK
CH OH
CH OH
COOH
CH OH
CH OH
COOH
Experiment 4.1.50
Na3[Co(NO2)6], sodium hexanitritocobaltate(III) solution precipitates yellow
potassium hexanitritocobaltate(III). Note: The reagent solution is dark.
3 K+ + [Co(NO2)6]3- = K3[Co(NO2)6]
Experiment 4.1.51
Flame test: (For the performance see Exp. 4.1.43.) Potassium chloride vapour
colours the flame pale violet. Traces of sodium may obscure the colour, but viewed
through a cobalt glass the yellow colour of sodium can be filtered.
Experiment 4.1.52
On addition of a strong base, e.g. NaOH, ammonia gas evolves. Stick a piece
of wet red litmus paper into the middle of the convex side of a watch glass. In another
watch glass mix 2-2 drops of ammonium chloride and sodium hydroxide solutions
and cover the watch glass with the first one. The blue colour of the litmus paper
indicates the evolution of ammonia gas. (Difference from potassium ion.)
NH4+ + OH- = NH3 + H2O
30
Experiment. 4.1.53
Na3[Co(NO2)6] solution, precipitates yellow ammonium
cobaltate(III).
3 NH4+ + [Co(NO2)6]3- = (NH4)3[Co(NO2)6]
hexanitrito-
Experiment 4.1.54
The most sensitive reaction of ammonium ion is the Nessler reaction. In
strongly basic medium potassium tetraiodomercurate(II), [HgI4]2- produces brown
precipitate or brownish-yellow coloration depending on the concentration of the test
solution. Basic mercury(II) amido iodide forms.
NH4+ + 2 [HgI4]2- + 4 OH- = HgO Hg
31
NH2
I
+ 7 I- + 3 H2O
DETECTION OF ANIONS
32
GROUP 1
For testing the reactions of carbonate ion, sodium carbonate [Na2CO3] stock
solution is used.
Experiment 4.1.58
Barium-nitrate solution precipitates white barium carbonate. The precipitate
dissolves in dilute acids with the evolution of carbon dioxide gas. (Difference from
SO42- and PO43- ions.)
Ba2+ + CO32- = BaCO3
BaCO3 + 2 H+ = Ba2+ + CO2 + H2O
Experiment 4.1.59
The water-soluble carbonates hydrolyze making the solution considerably
basic. The solution dropped with phenolphthalein turns intense pink (difference from
soluble hydrogen carbonates).
CO32- + 2 H2O
2 OH- + H2CO3
33
Experiment 4.1.61
Hydrogen carbonate ion is less basic than carbonate ion. Phenolphthalein
shows pale pink colour only.
HCO3- + H2O
OH- + H2CO3
34
GROUP 2
Experiment 4.1.65
Magnesia mixture in alkaline medium precipitates magnesium ammonium
phosphate as white crystals. The precipitate dissolves in acids (see also Exps. 4.1.46
and 6.10).
35
Experiment 4.1.66
In a solution acidified with HNO3, large excess of ammonium molybdate
precipitates yellow ammonium phosphomolybdate, (NH4)3[P(Mo3O10)4]. To 1-2
drops(!) of phosphate solution, 1 cm3 nitric acid is added, followed by a gradual
addition of ammonium molybdate until a yellow colour develops. In a few minutes,
yellow crystals separate.
4 H2[Mo3O10] + PO43- + 3NH4+
(NH4)3[P(Mo3O10)4] + 4 H2O
GROUP 3
36
The precipitate is divided into four test tubes and the following tests are performed:
a) When adding nitric acid, the precipitate does not dissolve,
b) adding ammonia, the precipitate dissolves partly forming diamminesilver complex
ion,
c) adding sodium thiosulphate solution, the precipitate dissolves easily in the form of
complex dithiosulphatoargentate ions,
d) allowed to stand, the yellow precipitate turns gradually grey due to the
photosensitivity of silver salts:
AgI + 2 NH3 = [Ag(NH3)2]+ + IAgI + 2 S2O32- = [Ag(S2O3)2]3- + I2 AgI + h = 2 Ag + I2
Experiment 4.1.69
Chlorine water sets free elementary iodine from iodides.
2 I- + Cl2 = 2 Cl- + I2
The brown solution is divided into two test tubes and
a) starch solution is added to form a blue inclusion complex. The reaction is extremely
sensitive to iodine.
b) carbon tetrachloride is added and the mixture is shaken. In the water-insoluble,
oxygen-free organic solvent iodine shows violet colour.
37
Experiment 4.1.70
Bromine water acts similarly to chlorine.
2 I- + Br2 = 2 Br- + I2
GROUP 4
For the tests of nitrite ion, sodium nitrite [NaNO2] stock solution is used.
Experiment 4.1.71
A little NaNO2 solution is acidified with acetic acid, and FeSO4 solution is
added. The solution turns brown due to the formation of (unstable) nitroso iron
sulphate, [Fe(NO)SO4]. (Nitrate reacts similarly but only in presence of cc. H2SO4.)
Experiment 4.1.72
To 1-2 cm3 distilled water 1-2 drops of NaNO2 solution are added. Then,
1-1 cm3 of Griess-Ilosvay 1 and 2 reagent solutions in this order. In dilute nitrite
solution intense red colour develops. (At higher concentrations nitrite ion oxidizes the
red dye and the solution turns pale yellow.)
In acidic medium aromatic amines like sulphanilic acid (reagent 1) are
diazotized by nitrous acid and the diazonium salt formed reacts with other aromatics
like -naphthylamine (reagent 2) in an azo-coupling reaction resulting a deeply
coloured dye.
HOS O2
+
NH2 + HNO 2 + H
N N
HOS O2
+
HOSO 2
N N
HOSO 2
NH2
38
N N
+
+ 2 H2O
NH2 + H +
For the tests of nitrate ion, sodium nitrate [NaNO3] stock solution is used.
Experiment 4.1.73
To a little NaNO3 solution cc. H2SO4 is added carefully, the solution is
cooled under the tap and iron(II) sulphate solution is carefully layered on. A brown
ring forms known from the reactions of nitrite ion (see Exp. 4.1.71).
Experiment 4.1.74
On addition of Zn + HCl, nitrate ion can be reduced to nitrite and gives
positive Griess-Ilosvay reaction (see Exp. 4.1.72).
Procedure:
Repeat Exp. 4.1.72 with sodium nitrate solution, adding zinc powder to the
reaction mixture.
NO3- + Zn +H+ = NO2- + Zn2+ +H2O
39
Experiment 4.1.76
Simple analysis of cations and anions
The simple analysis of cations and anions of medical importance in cases
when only one cation and one anion are present is performed as shown in Tables 1
and 2.
Procedure:
Prior to the systematic analysis it is strongly recommended that preliminary
tests be carried out with a small portion of the sample (colour, odour, crystal form,
etc.). Then, 0.5-1 g of the sample is dissolved in 30-40 cm3 water. One-third of this
stock solution is used to test for cations, another third for anion analysis, the rest is put
aside. It is advisable to check the pH of the stock solution before systematic analysis.
First the cations are identified, since their knowledge limits the number of the
possible counterions. E.g., if the sample is water-soluble and Hg22+ cation has been
found, the presence of Cl- and I- ions should be excluded.
After the identification of the ion according to Tables 1 and 2, all the
characteristic reactions of the suspected ion should be positive to accept the analysis
correct. The analysis process should be described in details in the notebook, including
visual observations and chemical equations.
40
II
Reagent
Observation
Ion?
white precipitate
Pb2+ or Hg22+
X + NaOH:
white precipitate
black precipitate
Pb2+
Hg22+
solution I + H2S:
yellow precipitate *
As3+
X + NH4OH:
III
X + (NH4)2S:
black precipitate
Hg2+ or Cu2+
white precipitate
Hg2+
blue precipitate
Cu2+
white precipitate
Zn2+
Cr3+
black precipitate
greenish precipitate
Fe2+
brown precipitate
Fe3+
blue precipitate
Co2+
X + Na2CO3:
white precipitate
Ca2+ or Mg2+
X: flame test:
brick-red
Ca2+
negative
Mg2+
yellow
Na+
pale violet
K+
X + NaOH:
IV
X + Nessler's reagent:
brown precipitate
X + acid-base indicator:
acidic
NH4+
H+
* In presence of oxidative ions (Fe3+or NO2-), milky colloidal solution of sulphur may form.
41
Reagent
+ HCl
Observation
Ion?
CO32-, HCO3-
gas evolution
or ClO-
the gas
CO2:
CO32- or HCO3ClO-
+ Ba(NO3)2
white precipitate:
(CO32-) *,
SO 2- or PO 34
a) prec. + HNO3
+ HNO3 + AgNO3
dissolves:
(CO32-) *
PO 3-
insoluble:
SO42-
precipitate:
Cl- or I-
a) prec. + NH4OH
b) prec.+Na2S2O3
soluble in b) only:
+ Griess-Ilosvay reagent
ClI-
red colour:
NO2-
red colour:
NO3-
42
SELF-TEST QUESTIONS
1.
Why can the sulphides of the cations of the first two analytical groups be
precipitated with H2S in acidic medium?
2.
3.
4.
5.
6.
7.
Write equations for the reactions of potassium iodide with Hg2+, Pb2+ and
Cu2+ ions.
8.
10.
How can Hg22+, Hg2+, Pb2+, Cu2+, Fe2+, Fe3+, Mg2+ and NH4+ ions be
distinguished using a single reagent?
11.
12.
How could you prepare Nessler's reagent and which ion is detected with it?
13.
14.
Write down the reactions suitable to distinguish Fe2+ and Fe3+ ions.
15.
During storage, iron(II) ions are easily oxidized to iron(III) ions by the
atmospheric oxygen. Propose a reaction to check the purity of an iron sulphate
sample.
16.
17.
18.
19.
20.
21.
43
22.
What are the common reagents for the Group 1, 2 and 3 anions?
23.
How can you detect and explain the basicity of CO32- and HCO3- solutions?
24.
25.
How could you detect and distinguish SO42- and PO43- ions?
26.
27.
44
45
9. APPENDIX
46
CLASSIFICATION OF THE INORGANIC COMPOUNDS
The scientific classification of the inorganic compounds is based on their bonding systems
and crystal types: Ionic compounds usually form ionic crystals; covalent compounds are of
network or molecular crystals; the so-called intermetallic compounds exist in the form of a
metallic crystal lattice. This grouping allows a rather easy understanding of structure-property
relationships but exceeds our requirements. Considering that most of the inorganic compounds
are either hydrogen and/or oxygen compounds or salts, the following classification may be
useful:
Hydrogen compounds
Hydrogen forms so-called binary hydrides with almost all elements.
Ionic hydrides are formed with the elements of the lowest electronegativity values (sblock elements) in which hydride anion (H-) exists (NaH, CaH2). These salt-like hydrides are
strong bases (proton acceptors, electron pair donors) and strong reducing agents (electron
donors).
The hydrides of the non-metallic elements (p-block elements) are covalent compounds
(volatile, of molecular crystal lattice). Their properties depend strongly on the partner atoms.
Thus, the hydrogen halides are polar, soluble in water, their solutions are acidic and their acid
strength increases with the atomic number of the halogen. Hydrides of the oxygen group elements
are slightly acidic (H2S), H2O is amphoteric. The elements of the nitrogen group form basic
hydrides (NH3, PH3), the carbon group hydrides are neutral. The hydrides of silicon, aluminium
and boron represent a transition between the covalent and salt-like ones.
Hydrides of the d-block elements (transition metals) are of metallic type in which
hydrogen atoms(!) occupy the space between the metal ions in the crystal lattice.
Oxygen compounds
The oxygen compounds are classified as oxides, hydroxides and oxoacids. Salts of
oxoacids will be discussed separately.
Oxides
a./ Basic oxides are the oxides of the elements of lowest electronegativity, reacting with
water to form the corresponding hydroxide bases, i.e. they are base anhydrides. Examples: The
47
oxides of the s-block elements (Na2O, K2O, CaO, BaO), a few of the p-block elements (Bi2O3)
and of the transition metals of lower oxidation state (FeO, MnO, CoO).
b./ Acidic oxides: To this group belong the oxides of the highly electronegative nonmetals and metalloids (SO2, SO3, P2O3, P2O5, As2O3, As2O5, CO2, SiO2, NO2, N2O3, N2O5,
etc.) and a few of the transition metals at higher oxidation state (CrO3, Mn2O7, V2O5, OsO4).
These oxides are acid anhydrides; They hydrolyze with water to form acids.
c./ Neutral oxides: This group comprises first of all H2O (amphoteric), NO, CO, N2O
(not being anhydrides) and the water-insoluble oxides ( Al2O3, Fe2O3).
Hydroxides and oxoacids
The basic oxides react with water to form bases, the acidic oxides to form oxoacids. In
aqueous solution, bases dissociate into hydroxide ion and a metal ion, the acids into hydrogen
(oxonium) ion and an oxo-anion. Acids and bases react to form water and a salt. The basic
strength of hydroxides increases with the atomic radius of the metal atom, the acid strength
increases with the oxidation number of the central atom. There is an intermediate group of
hydroxides (amphoteric hydroxides) exhibiting both weakly acidic and basic reactions depending
on the medium.
Acid-base character of X(OH)n compounds
Oxidation
number of X
General
formula
Basic
Amphoteric
Acidic
+1
XOH
Li, Na, K,
Cl
+2
X(OH)2
+3
X(OH)3
Fe, Bi
B, P
+4
X(OH)4
Pb, Sn
C, Si, S, Se
As
P, N, Cl, Br, I
H2XO3
+5
H3XO4
HXO3
48
+6
H2XO4
+7
HXO4
Mn, Cl, I
A few examples:
Hydrolysis of a basic oxide:
CaO + H2O
= Ca(OH)2
Ca(OH)2
Ca2+
CO2
H2O
2 OH=
H2CO3
Certain acidic oxides, depending on the stoichiometric ratio of added water, form different acids:
Adding maximum amount of water orthoacids, with less amounts pyro- and metaacids are
produced respectively, e.g.:
P2O5
3 H2O
2 H3PO4
orthophosphoric acid
P2O5
2 H2O
H4P2O7
pyrophosphoric acid
P2O5
H2O
metaphosphoric acid
2 HPO3
There are acid anhydrides which disproportionate during hydrolysis. These are regarded as the
common anhydrides of two different acids, e.g.:
2 NO2
H2O
HNO3
Dissociation of an acid:
H2CO3
Ca(OH)2
+
=
HNO2
2 H+
CO32-
Basic oxides react with acids, acidic oxides with bases and basic oxides with acidic oxides,
respectively, also to form salts.:
Basic oxide with an acid:
CaO + H2CO3
CO2
= CaCO3
Ca(OH)2
CaO + CO2
+ H2O
= CaCO3
=
CaCO3
+ H2O
49
Salts
Salts are regarded as products of the acid-base (neutralization) reactions (i.e. they are not
oxygen containing compounds by all means. See, e.g. NH3 + HCl = NH4Cl). Salts can be
classified as follows:
a./ Normal salts: Salts resulted in a stoichiometric neutralization reaction:
2 NaOH
H2SO4
Na2SO4
2 H2O
3 KOH
H3PO4
K3PO4
3 H2O
b./ Acid salts: Salts formed by an incomplete neutralization of a polybasic acid. The
name: acid salt refers to the composition, not to their hydrolysis! (Their reactions in aqueous
solution are not acidic by all means!):
KOH
H3PO4
KH2PO4
H2O
2 KOH
H3PO4
K2HPO4
2 H2O
NaOH
H2CO3
NaHCO3
H2O
KOH
H2SO3
KHSO3
H2O
c./ Base salts are products of a partial neutralization of a polyvalent (polyacidic) base.
The name: base salt refers to the composition, not to their hydrolysis! (Their aqueous solutions
are not basic by all means!):
Bi(OH)3
HNO3
Bi(OH)2NO3
Sb(OH)3
HCl
SbOCl
H2O
+ 2 H2O
d./ Mixed salts: Salts formed in a reaction of one base with two acids:
Ca(OH)2
Cl2
CaClOCl
H2O
50
e./ Double salts: Occasionally, from a solution of two different salts, uniform crystals are
obtained. The composition of these crystals is stoichiometric, according to the sum of the two
formulas and, when dissolved, dissociate into all ionic components:
K2SO4
Al2(SO4)3
2 KAl(SO4)2
(alum)
or, e.g .
KAl(SO4)2
(NH4)2SO4
+FeSO4
K+
Al3+
2 SO42-
2 NH4+
Fe2+
+ 2 SO42-
[Ag(NH3)2]Cl
When dissolved:
[Ag(NH3)2]Cl = [Ag(NH3)2]+ + Cl-
(diamminesilver(I) chloride
= 3 Na+
[Ag(S2O3)2]3-
Thio compounds
In both inorganic and organic chemistry, compounds having divalent sulphur atom(s)
instead of oxygen atom(s) of a structurally analogous, known compound, are called thio
compounds. Thus, the thio analogue of water is hydrogen sulphide (H2S), those of oxides are the
sulphides (CO2 / CS2, CaO / CaS etc.), that of sulphuric acid is thiosulphuric acid (H2SO4 /
51
H2S2O3), that of arsenous acid is thioarsenous acid (H3AsO3 / H3AsS3), that of cyanic acid is
thiocyanic acid (rodanic acid) (HOCN / HSCN), etc..
Acyl groups
Acyl groups, as imaginary derivatives of oxoacids, can be obtained by the removal of the
hydroxyl groups (not hydroxide ions!) from the acid molecules. Thus, acyl groups have free
valence (-ies) useful to construct formulas of acid derivatives, e.g. acyl halides:
A few examples:
Oxoacid
Acyl group
Acyl chlorlide
nitrosyl chloride
ClNO
nitric acid:
NO2
nitryl chloride
ClNO2
=SO
sulphinyl chloride
Cl2SO
or thionyl group
or thionyl chloride
sulphonyl chloride
carbonyl chloride
Cl2SO2
or sulphuryl chloride
=CO
COCl2
or phosgene
phosphoric a.: H3PO4
phosphoryl g.
PO
phosphoryl chloride
or phosphorus oxychloride
POCl3
52
53
Table 1. Examples of naming inorganic compounds
F
Cl
Br
Formula
Name
Latin name
Anions
( trivial name )
...........................ide
.....................atum
fluoride
chloride
bromide
fluoratum
chloratum
bromatum
iodide
iodatum
CN
OH
cyanide
hydroxide
cyanatum
hydroxydatum
O 2
S 2
oxide
sulphide
oxydatum
sulfuratum
hydride
hypo...........ite
hypochlorite
...................ite
hypo..................osum
hypochlorosum
....................osum
ClO2
NO2
chlorite
nitrite
chlorosum
nitrosum
SO32
sulphite
sulfurosum
arsenite
.......................ate
arsenicosum
............................icum
ClO3
BrO3
chlorate
bromate
chloricum
bromicum
IO3
NO3
iodate
nitrate
iodicum
nitricum
CO32
SO42
carbonate
sulphate
carbonicum
sulfuricum
S2O32
thiosulphate
thiosulfuricum
PO4
AsO43
phosphate
arsenate
phosphoricum
arsenicum
MnO42
OCN
SCN
manganate
cyanate
thiocyanate (rodanide)
manganicum
cyanicum
thiocyanicum
OCl
AsO3
per...............ate
MnO4
ClO4
permanganate
perchlorate
hyper................icum
hypermanganicum
hyperchloricum
54
Acids
HCl
Name
hydrogen chloride
Latin name
acidum chloratum
HI
HCN
hydrogen iodide
hydrogen cyanide
H 2S
HOCl
HClO2
hydrogen sulphide
hypochlorous acid
chlorous acid
ac. hypochlorosum
ac. chlorosum
HClO3
chloric acid
ac. chloricum
HClO4
HNO2
perchloric acid
nitrous acid
ac. hyperchloricum
ac. nitrosum
HNO3
H2SO3
nitric acid
sulphurous acid
ac. nitricum
ac. sulfurosum
H2SO4
sulphuric acid
ac. sulfuricum
H3PO3
H3PO4
H2CO3
orthophosphorous acid
orthophosphoric acid
carbonic acid
ac. phosphorosum
ac. phosphoricum
ac. carbonicum
H2SiO3
silicic acid
ac. silicicum
KOH
potassium hydroxyde
kalium hydroxydatum
Ca(OH)2
Fe(OH)2
calcium hydroxyde
iron(II) hydroxyde
calcium hydroxydatum
Fe(OH)3
iron(III) hydroxyde
Bases
Salts
NaCl
salt)
NaClO3
As2S3
sodium chlorate
arsenic(III) sulphide
As2S5
arsenic(V) sulphide
CaSO4
calcium sulphate
calcium sulfuricum
(gypsum)
MgSO4
Na2SO4
magnesium sulphate
(bitter salt)
sodium sulphate
magnesium sulfuricum
natrium sulfuricum
(Glauber's salt)
CuSO4
FeSO4
copper(II) sulphate
iron(II) sulphate
cuprum sulfuricum
ferrosum sulfuricum
55
Fe2(SO4)3
Hg2Cl2
HgCl2
iron(III) sulphate
mercury(I)chloride
hydrargyrum chloratum
(calomel)
mite
mercury(II)chloride
(sublimate)
Formula
NaH2PO4
Name
sodium dihydrogen
Latin name
phosphate
Na2HPO4
disodium hydrogen
phosphate
Na3PO4
Bi(OH)2NO3
trisodium phosphate
bismuth dihydroxide
bismuthum subnitricum
nitrate
(basic bismuth nitrate)
Complexes
[Fe(CO)5]
pentacarbonyliron(0)
[Ag(NH3)2]Cl
diamminesilver(I)
chloride
Na3[Ag(S2O3)2]
sodium
dithiosulphatoargentate(I)
K4[Fe(CN)6]
potassium
hexacyanoferrate(II)
K3[Fe(CN)6]
potassium
hexacyanoferrate(III)
K2[HgI4]
potassium
tetraiodomercurate(II)
Fe3[Fe(CN)6]2
iron(II)
hexacyanoferrate(III)
Fe4[Fe(CN)6]3
iron(III)
hexacyanoferrate(II)
For the practice, one of the most important properties of compounds is their solubility.
The water-solubility of the most common inorganic salts is tabulated below.
56
Anion
Solubility
Soluble in water
NO3
Cl
Br
most of bromides are soluble except: AgBr, Hg2Br2, HgBr2 and PbBr2
most of iodides are soluble except: AgI, Hg2I2, HgI2 and PbI2
I
SO42-
ClO3
C2H3O2
S2
most of sulphides are insoluble except alkali-, alkali earth metal and ammoniumsulphides
OH
most of hydroxides are insoluble except: alkali hydroxides and Ba(OH)2, Sr(OH)2,
Ca(OH)2
CO3
SO3
PO43
most of carbonates are insoluble except: alkali metal and ammonium carbonates
most of sulphites are insoluble except: alkali metal and ammonium sulphites
most of phosphates are insoluble except alkali metal and ammonium phosphates.
57
Concentrations of reagent solutions made by the technicians in the stock laboratory and not
indicated in the text can be seen below.
Acetic acid
Alcoholic -naphthol
Alum
Ammonia
Ammonia-ammonium-chloride
buffer
Ammonium acetate
Ammonium carbonate
Ammonium chloride
Ammonium iron(III) sulphate
Ammonium molybdate
Ammonium oxalate
Ammonium sulphide
Ammonium thiocyanate
Arsenic trioxide
Barium chloride
Barium nitrate
Benzoic acid
Bettendorf's reagent
Bismuth chloride
Bromine in carbon tetrachloride
Bromine-water
Calcium chloride
Calcium hydroxide
Chlorine-water
Chromium(III) sulphate
Cobalt(II) nitrate
Copper(II) sulphate
Dimethyl glyoxime
2,4-Dinitrophenyl hydrazine HCl
3,5-Dinitrobenzoic acid
Disodium hydrogen phosphate
Eriochrome black T
Ethanolic silver nitrate
12 %
5%
5%
5%
0,8 % ammonium-chloride + 0,33 % ammonia
8%
10 %
10 %
5%
5 %, in 4 % ammonia solution
3%
5 % ammonia solution saturated with H2S gas
0,90 %
0.5 % (dissolves in hot water!)
5%
9%
0,12 %
10 % tin(II) chlorde in cc. HCl
4 % + cc. HCl until dissolves
5%
1%
11 %
5%
distilled water saturated with chlorine gas
6%
10 %
4%
1 % in ethanol
2 %, in 40 % ethanol
0,21 %
7%
1 %, in 70 % isopropanol
2%
58
Fehling I
Fehling II
Formaldehyde
Fructose
Glucose
Glycine
Glycogen
Griess-Ilosvay I
Griess-Ilosvay II
Hydrochloric acid
Hydroquinone
Iodine
Iron(II) sulphate
Iron(III) chloride
Lactose
Lead(II) acetate
Lead(II) nitrate
Lecithin
Magnesia mixture
Magnesium chloride
Magnesium sulphate
Mercury(I) nitrate
Mercury(II) chloride
Methanolic -naphthol
Methyl orange
Methyl red
Methylamine HCl
-Naphthol
Nessler-reagent
Nickel sulphate
Ninhydrin
Nitric acid
ortho-Toluidine
Phenol
Phenolphtalein
Phenylhydrazine HCl
Picric acid
Potassium chloride
Potassium chromate
Potassium chromate (acidic)
4 % copper(II) sulphate
20 % K-Na-tartarate in 15 % NaOH solution
38 %
5%
10 %
1%
1%
1 % sulphanilic acid in 40 % acetic acid
3 % -naphthylamine in 30 % acetic acid
5%
5%
1 % +2 % KI
10 %
8%
5%
10 %
8%
0,2 %
10 %; see also Exp. 6.10!
10 %
5%
3 %, + nitric acid until dissolves
1,5 %
1%
0,10 %
0,2 %, in 60 % ethanol
40 %, acidified with a little HCl
5%
6 % Hg(II) chloride + 7,5 % KI in 20 % NaOH
5%
0,2 % in ethanol
20 %
6 % + 0,15 % thiocarbamide in cc. acetic acid
5%
1 % in 70 % ethanol
10 %
5%
8%
3%
3 %, in 20 % sulphuric acid
59
Potassium chromium(III) sulphate
Potassium hexacyanoferrate(II)
Potassium hexacyanoferrate(III)
Potassium
hexahydroxoantimonate(V)
Potassium iodide
Potassium permanganate
Protein
Rubeanic acid
Saccharose
Salicylic acid
Silver nitrate
Sodium acetate
Sodium acetate, concentrated
Sodium carbonate
Sodium chloride
Sodium dihydrogen phosphate
Sodium hexanitritocobaltate(III)
Sodium hydrogen carbonate
Sodium hydrogen tartarate
Sodium hydroxide
Sodium hypochlorite
Sodium nitrate
Sodium nitrite
Sodium nitroprusside
Sodium thiosulphate
Starch
Sulphosalicylic acid
Sulphuric acid
Thymol blue
Thymolphthalein
Trichloroacetic acid
Trisodium phosphate
Tryptophane
Zinc sulphate
5%
2%
2%
2%
2%
0,3 % in 5 % sulphuric acid
4-5 egg-whites in 1 dm3 water
0,1 %, in 65 % ethanol
20 %
1%
0.8 %
11 %
32 %
5%
8%
5%
40 %, in 3 % acetic acid
9%
8%
5%
2%
5%
5%
1 %; unstable!
10 %
1 %-os, + 0,1 % salicylic acid
20 %
10 %
0,5 % in ethanol
0,1 %, in 50 % ethanol
0,16 %
5%
0,5 %
4%