EXPLOsive
EXPLOsive
EXPLOsive
DDNP-Diazodinitrophenol
DNT-Dinitrotoluene
EGDN-Ethyleneglycoldinitrate
GC-Gas Chromatography
IR-Infrared spectroscopy
Lead Azide-Pb(N3 ) 2
NC- Nitrocellulose
NG-Nitroglycerine
RDX- Cyclotrimethelenetrinitramine
TATP- Triacetonetriperoxide
TNT-2,4,6-trinitro toluene
INTRODUCTION TO EXPLOSIVES
1.1 Title: Introduction to Explosive Materials
1.3 Purpose: To have a knowledge about the Nature, uses, characteristics, Classification
composition, chemical nature, Physical and chemical properties of explosive materials.
Generally, there are three categories of explosives i.e Chemical, Mechanical and Nuclear
explosives. (Ref.1 page 10).
Mechanical Explosives are those substances that tend to undergo physical change such
as overloading of container with compressed air stream.
Nuclear Explosives are the most powerful explosives. They areproducedby sustained
nuclear reactions while releasing a tremendous amount of heat and energy.
Explosives
Lead Azide
Lead
Boosters Main Charge
Styphnate
Mercury
ndustrial
Fulminate
PETN, Tetryl RDX,HMX,TNT
explosives
DDNP
Tetrazene ,DNT,ANFO,
HMTD Dynamite,
TATP Water gels
Emulsions
Slurry
explosives
9. Velocity of Detonation More than 1000 m s-1 Less than 1000 m s-1
(VOD)
High explosives are detonating explosives. Detonation is the explosion effect that is
caused by the transmission of high speed shock wave when the explosive compound or mixture
of compounds decomposes and liberates energy.The chemical reaction propagates with such
rapidity that the rate of reaction zone into the material exceeds velocity of sound and is greater
than 1000m/s. High explosives are further sub-divided in to two groups according to their
susceptibility to initiation i.e. Primary explosives and Secondary explosives. (Figure-1)
Primary explosives are among the most powerful and most sensitive of all chemical
explosives.These are the explosives which are used to start or initiate the explosion. These
compounds are easily detonated by mechanical shock, friction and heat and readily ignited by
direct contact with flame or electrical sparks. The main function of Primary explosives is to
initiate a secondary explosive by shock wave. Because of their sensitivity they are used in small
quantities. Initiators are mainly used in military detonators, industrial blasting caps and stab,
and shock primers. (ref 3, page15 ). Examples of primary explosives are Mercury Fulminate,
lead Azide, Lead Styphnate, Dizodinitrophenol (DDNP),Tetrazine etc.
Lead azide has a high temperature of ignition and less sensitive to shock and friction than
Mercury fulminate. It has good stability to heat and storage. Due to its high temperature of
ignition it is generally used in primary mixtures with Lead styphnate which is very easy to ignite.
Its contact with copper must be avoided because it leads to the formation of Copper azide.
Since it is a non-conductor it may be mixed with flaked graphite to form a conductive mixture
for use in low energy electrical detonator. (ref 3, page15).Some properties of compound is
given in Table-3
Lead styphnate is a toxic explosive which is thermally stable, non-corrosive and non-
hygroscopic. It is sensitive to flame and electrostatic discharge. It is therefore used to sensitize
lead azideand initiate burning in primer compositions. (ref 3, page 16 ). Chemical structure of
compound is given in figure-2 and some properties of compound is given in Table-4.
1.10.1.4Tetrazene:
DDNP is yellowish brown powder which is used for initiating high explosives in propellant
primary devices. The sensitivity of DDNP to friction is about the same as Lead azide but less
than Mercury fulminate.DDNP is used to form priming mixture where a high sensitivity to flame
or heat is desired. Some properties of compound is given in Table-6.
Secondary explosives are generally used as the main charge. These are relatively
insensitive to heat, flame and shock. They usually require a primary explosive to initiate
detonation. Secondary high explosives include boosters and main charge. The most
commonly used booster is PETN. TNT, RDX, HMX, Dynamites, Binary explosives, emulsions,
watergel etc. are used as main charge. The most important class of main charge is the
organic compounds which contain the nitro group.
It was used in large caliber shells in world war I. In world war II a mixture of ammonium
picrate and TNT was widely used in the press loading of armour piercing shells.(ref 2, pages
3-4).Chemical structure of compound is given in figure-4 and some properties of compound is given
in Table-7.
1.10.2.2 TNT(2,4,6-trinitrotoluene) :
TNT is one of the most commonly used High explosive in military weapons and in civilian
mining. It is frequently used as main charge in artillery projects, mortar rounds and aerial
bombsused military explosives. Its main features include low melting point, good chemical
and thermal stability, low sensitivity to impact, friction and high temperature and its
compatibility with other explosives. Chemical structure of compound is given in figure-5 and
some properties of compound is given in Table-8
1.10.2.3 Tetryl(2,4,6-trinitrophenylmethylnitramine ):
It is used in military boosters. (ref 2, page 4).Chemical structure of compound is given in figure-6
and some properties of compound is given in Table-9.
1.10.2.4 PETN(Pentaerythritoltetranitrate):
PETN is one of the strongest known High explosive. It is used as a base charge in blasting
caps and detonators, as the core explosives in detonating cord, in booster charges, in plastic
explosives, and as an ingredient in other explosives. The chemical stability of PETN is very
high and is considered to be more stable than all other nitrate esters. (ref 3, pages 9-10).
Chemical structure of compound is given in figure-7 and some properties of compound is given in
Table-10.
It is also known as cyclonite and hexogen. It is one of the most important military explosives
used today. It has high chemical stability and an explosive power.RDX is considerably more
susceptible to shock than TNT fordetonation. RDX is used as a component in mixtures with
other explosives such as TNT and as a plastic explosive also. A well-known plastic explosive,
Semtex is based on RDX and PETN. Mixtures of RDX and wax are used for booster charges in
many military ammunitions especially in artillery shells. (ref 3, pages 5-6). Chemical structure
of compound is given in figure-8 and some properties of compound is given in Table-11.
1.10.2.6 HMX(Cyclotetramethylenetetranitramine):
1.10.2.8 Dynamite:
Over the years, formulas for dynamite have been developed to hit every type of
rock blasting. Varieties have been developed for severe water conditions utilizing nitro
cotton to gel the NG (the gelatins are one branch of the dynamite family) for
cohesiveness to enable loading into up holes in mines, for safe usage in under- ground
coal mines (the permissible having salts of various types to cool the explosive reaction
as part of formula) and for economics by making formulas with very high ammonium
nitrate percentages (and thus no cohesiveness or water resistance) where severe field
conditions do not exists. Literally thousands of different formulas might be found, but
for years all had the commonality of having nitroglycerine as a component. Some
typical formulations have been shown in Table below (ref 2, pages 6-7).
Material Type*
1 2 3 4 5
Balsa 2.0 -- -- -- --
Microballoons -- -- -- 0.3 --
Typical slurry explosives contain ammonium nitrate (30 – 70% 0, Sodium nitrate ( 10-
15%), calcium nitrate(15-20%), aliphatic amine nitrate upto 40%, Al ( 10-1L%), TNT
or other explosives sensitizers (5-15%), gellants (1-2%), stabilizers (0.1- 2%), ethylene
glycol (3-15%) and water (10-20%). (ref 2, page 9 & ref 3, page 21).
1.10.2.13 Mixture
A vast number of explosives consisting of mixtures of various explosives compounds
were developed by combatants in world war II. Many of these combinations may
include materials such as HMX, RDX, TNT, Al powder, wax, and plasticizers with or
without other ingredients for special properties. A few worth mentioning are
C3 - RDX+TNT+DNT+MNT + Tetryl+NC
Low explosives are compounds or mixtures that deflagrate. These explosives have
propagation speed less than 1000m/s. Low explosives are mechanical mixtures of individual
ingredients. They are used mainly used as propellants because they tend to exert a rapid
pushing effect. Propellants are mixtures of one or more energetic materials, plasticizers,
stabilizer and inorganic additives (ref 3, page 17).The main applications of propellants are
in launching projectiles from guns, rockets and missile systems. Black powder (gun powder)
and smokeless powder are the most commonly used low explosives.
References:
1. Narayanan T.V (1996). Modern techniques of Bomb Detection and Disposal.
R.A.Security system, Delhi.
2. Alexander Beveridge. (1998).Forensic Investigation of explosions, Taylor and Francis Ltd,
Bristol.
3. Yinon.J. and Zitrin. S. (1993). Modern Methods and application of analysis of
Explosives, John Wiley and Sons, New York.
4. Yinon.J. and Zitrin.S. (1981).The analysis of explosives . Pergamon press,
New York
5. Ghosh.K.M. (1988). The Principles of fireworks, Economic enterprise, Ahmedabad.
6. Chladek J. The identification of organic peroxides. Advances in analysis an detection of
explosives. Proceedings of the 4th International symposium on Analysis and
detection of Explosives September 7-10: 1992; J Yinon edition. Kluwer academic
publishers, 1993;73-76
Improvised Explosive Devices are thosewhich are not manufactured by any fixed standards.
The materials of construction, composition of ingredients, Initiation method depends upon the
availability of resources, knowledge and skill of user. These devices are mainly used by anti-
social elements for insurgent activities.
1) Potassium chlorate + Arsenic sulphide + projectiles (iron nails, glass pieces , stone chips
etc.,) - Throw down device.
2) Potassium chlorate + sugar initiated by conc., Sulphuric acid - Acid bomb
(ref1).
3) Crude RDX or TNT as main charge.
Tiffin carrier, transistor, cement pipe, iron pipe, telephone, Television, toys, cell-phone,
computer, scooter, cycle, the articles which are easily available to the anti-social
elements. ( ref1 ,2&3)
3.2 Scope: Pre blast (Unexploded) and post blast (exploded) low and high explosives
3.4 Introduction:-
The systematic procedure for both pre blast and post blast explosive evidence is divided in to
Four major steps
1. Preliminary examination
2. Extraction of Explosive material
3. Detection of Inorganic explosives including pyrotechnic composition
4. Detection of organic explosives
2. Sample is examined for odour , colour, consistency and any visually observables
ingredients. Ingredients with characteristic odour such as mononitrotoulene may often be
detected at this stage. The colour and consistency may guide to find the general type of
particular explosive . Some ingredients such as fragments / components of the device
(pipe/container/wires/wrappers/fuses/ parts of timing devices/batteries etc)can be readily
identified by their characteristic appearance. Visible contaminants can also be observed at
this stage
The solvent extraction of the Post blast debris is a typical for extraction of explosive residues for further
testing. Pre blast explosives are directly dissolved in to the solvent on the basis of solubility. Four
extracts are required for identification of unknown explosive material/residues.
Acetone is universally accepted broad-spectrum solvent for majority of organic explosives such as RDX,
HMX, TNT, PETN etc. Other organic solvents like ether, benzene and chloroform are also used, which are
suitable for certain groups of organic explosives (nitro aromatic and some nitrate ester like EGDN or
NG). In some instances, methanol or other solvents or their mixtures may be used instead of
acetone.The extracts are concentrated and subjected to various analytical tests for detection and
identification of organic explosives (ref 2, page 221-222).
The residue left after acetone extract is treated with hot water and filtered. The inorganic residue
dissolves readily in hot water. The water extract is concentrated to a small volume. Chemical and other
analytical tests are performed for the detection of water soluble ingredients ( anions and cations ) in
explosives compositions such as low explosives, inorganic explosives and pyrotechnic compositions (ref
2, pages 222-223)
The residues left after water extraction often include metals, sulphides of arsenic and antimony, sulphur
carbon etc. A small portion of the dried material is extracted with 2N NaOH and filtered. The filtrate is
preserved for the detection of sulphide, arsenic, antimony, aluminum etc.(ref 5,page 309,229,231,252)
The following analytical scheme in the flow diagram may be applied in general. The scheme is intended
to serve as a general outline of the sequence of the examination.The scheme is intended to serve as a
general outline of the sequence of the examination. Not all of the tests listed in the scheme will be
required for every examination and other unlisted tests may be applicable as required by the
circumstances of individual cases (ref 1, page122)
Examination of vapors
Visual Examination
Microscopic Examination
CE – Capillary Electrophoresis, EDX – Energy Dispersive X-ray, GC–Gas Chromatography, HPLC – High Performance Liquid
Chromatography, IC – Ion Chromatography, IR – Infra-red Spectroscopy, GC MS – Gas Chromatography Mass Spectrometry,
SEM – Scanning Electro Microscopy, TLC – Thin Layer Chromatography, XRF – X-ray Fluorescence, XRD – X-ray Diffraction, ICP
– Inductively coupled plasma spectrometry, GC-IMS – Gas Chromatography – Ion Mobility spectrometry, AAS – Atomic
absorption spectrometry, UV-VIS – Ultra Violet –visible spectro photometry, LC-MS-MS-Liquid Chromatography tandem mass
spectrometry (ref 1, page 123)
4.3 Purpose: Detection and identification of anions and cationsin pre blast and post blast
inorganic explosives/ pyrotechnic compositions.
Requirements:
i) 2M Nitric acid
ii) Silver nitrate
iii) Lead acetate.
Preparation of reagents:
Reagent A: - Nitric acid (2M). Pour 128 ml conc.nitric acid into 500ml water, dilute to 1lit.
Reagent B: - Silver nitrate (0.1M). Dissolve 16.99 g of AgNO3 in water and dilute to 1lit.
Reagent C: - Lead acetate solution (0.25M).Dissolve 95 g lead acetate trihydrate in a mixture of
500 ml water and 10ml glacial acetic acid and dilute the solution with water to 1lit.
Procedure:
I. Take 1ml of water extract in a clean test tube. Add 2-3 drops of reagent A to it. Then add
2-3 drops of reagent B. White precipitate indicate the presence of chloride ion, which is
soluble in NH4 OH and insoluble in HNO3.
II. Take 1ml of extract in a clean test tube. Add 2-3 drops of reagent C to it. White
precipitate indicates the presence of Cl-
III. The about tests must be carried out along with the reference standard as well as blank.
(ref 1, pages 325-326).
Requirements:
i) Potassium dichromate
ii) Conc. H2SO4
iii) Diphenylcarbazide
Preparation of reagents:
Preparation of reagents:
Procedure :-
I. Take 1ml of extract in a clean test tube. Add 2-3 drops of reagent A to it and then the test
tube is kept in a water bath at 1000C for 5 minutes, then add 2-3 drops of reagent B to it. A
white crystalline precipitate indicates the presence of SO4.2-
II.Place 1 drop of reagent B upon filter paper, followed by a drop of freshly prepared solution of
reagent C. Treat the reddish-brown spot with a drop of acidified extract. The coloured spot
disappears.
III. The above test must be carried out along with the reference standard as well as blank. (ref 1,
pages 347-348 ).
Requirements:
i) Barium chloride
ii) Potassium permanganate
iii)Hydrogen peroxide
Preparation of reagents:
ReagentA;0.25M Barium chloride (Dissolve 61.1 g barium chloride dihydrate in water and
dilute to 1 lit.)
Procedure
Take 3 drops of extract in a semi-micro test tube . Add 2 drops of reagent B and 1 drop
of reagent A. a pink ppt appears. Add a few drops of reagent c and shake well. The colouredppt
becomes clearly visible. (Ref1 page 348).
i) Sulphanilic acid
ii) -Naphthylamine
iii) Acetic Acid
iv) Indole
v) Ethanol
vi) Sulphuric acid
Preparation of reagents:
Reagent A:- 1% sulphanilic acid in 30% acetic acid. It is prepared by dissolving 1 g of sulphanilic
acid in 100ml of warm 30% acetic acid.
Procedure:-
I. Place1 drop of neutral or acid extract on a clean spot plate. Add 1 drop of Reagent A and
then 1 drop of reagent B to it. Pink to red colour indicates the presence of NO -. (Griess test).
2
II.Place 1 drops of the extract in a semi micro test tube. Add 10 drops of the reagent C and 2
drops of the reagent D to it. A purplish-red colour indicators the presence of NO -. 2
III.The above tests must be carried out along with the reference standards as well as blank. (ref
1, pages 312-313 ).
Preparation of Reagents:
Reagent A: 1% sulphanilic acid in 30% acetic acid. Dissolve 1 g of sulphanilic acid in 100ml of
warm 30% acetic acid.
Reagent B: – naphthylamine Boil 0.3 g of -naphthylamine with 70ml of distilled water, filter
or decant and mix with 30ml of glacial acetic acid.
Procedure:-
1. Place 1drop of neutral or acidic extract in a clean spot plate. Add 1 drop of the reagent A
and then 1 drop of reagent B. Then add a pinch of zinc dust. Pink to red colour indicates
the presence of Nitrate. (Griess test).
2. Place a crystal of ferrous sulphate on a spot plate. Add a drop of extract and allow a drop of
conc. sulphuric acid to run at the side of the drop. A brown ring forms round the crystal of
ferrous sulphate indicating presence of nitrate.
N.B: If nitrite is present in the extract, then at first it is removed from the solution by
sulphamic acid or by sodium azide and then test for nitrate is performed.
The above tests must be carried out along with the reference standards as well as blank. (ref 1,
pages 334-337 )
Place a few drops of aqueous solution on a clean spot plate. Add one drop of conc. sulphuric
acid and small crystal of Brucine and stir the mixture with a glass rod . A blood red colour is
produced.
Note-Chlorate and Nitrites will interfere hence these ions to be eliminated before testing for
nitrates if they are suspected in exhibit as per 4.4.12.1 and 4.4.12.2
Requirements:
i) Cobalt nitrate ii) Acetone v) Chloroform
iii) Cupric sulphate iv) Pyridine
Preparation of Reagents
Reagent A: 0.5M Co (NO3)2. (Dissolve 146 g of cobalt nitrate in water and dilute to 1lit.)
Reagent B: 0.25 M CuSO4. (Dissolve 62.42 g of CuSO4.5 H2O in water and dilute to 1lit.)
Procedure:
I Mix one drop of the test solution in a micro-crucible with a very small drop of a reagent
A and evaporate to dryness. The residue whether thiocyanate is present or not is coloured
violet and the colour slowly fades. Add a few drops of acetone, A blue green or green
colouration is obtained.
II Add a few drops of pyridine to 3-4 drops of reagent B. Then introduce about 2ml of
chloroform, followed by 5-6 drops of the extract. Shake the mixture vigorously. The chloroform
layer will acquire a green colour (ref 1, pages 318-319)
III The above tests must be carried out along with the reference standards as well as blank.
Additional test :
Preparation of reagents:
Procedure:
I 1ml of extract is dried in a spot plate. After cooling add 2-3 drops of conc. Sulphuric acid.
Then add 2-3 drops of reagent A. Blue colour indicates the presence of chlorate ions.
II Place a drop of the extract in a micro crucible and add 1drop of the reagent B. Warm
rapidly over a micro burner and allow to cool. A violet coloration appears. Very pale coloration
may be intensified by adding a drop of reagent C. When a deep violet colour, due to an
oxidation product of the diphenylcarbazide is obtained.
Additional test:
Requirement:
i) Indigo
ii) conc. Sulphuric acid
iii)sodium sulphite or sulphurous acid
Preparation of reagent :
Reagent A : 1% Indigo in concsulphuric acid
Reagent B: 10% sodium sulphite solution in water
Preparation of Reagents:
Procedure:
I. Take 1 drop of the water extract in a clean test tube. Add 2 drops of reagent A and mix
it. To it add little KCl. The change of blue litmus paper to red indicates the presence of
thiosulphate. (ref 2, pages 319-320 )
II. Take 1ml of the neutral or slightly alkaline water extract in a clean test tube. Then add
2-3 drops of the reagent B to it. A crystalline violet ppt indicates the presence of thiosulphate.
(ref 1, pages 305-307 ).
III. The above tests must be carried out along with reference standard as well as blank.
Requirements :
Preparation of Reagents:
Procedure:
I. Apply a drop of water extract on a piece of filter paper impregnated with Reagent A -
Reagent B and spray the paper with Reagent C. Violet spot indicates the presence of
perchlorate.
NB:- Persulphates gives an analogous reaction. When they are present the test is carried
out on a TLC plate which is then heated for over 1 hour at 110 C to decompose the
persulphates. Violet spots obtained, following such treatment indicates the presence of
perchlorates. (ref 3, page 102-103 )
II. The above tests must be carried out along with reference standard as well as blank.
Requirements:
i) ZnSO4
ii) Potassium Ferrocyanide
iii) Sodium Nitroprusside
Preparation of Reagents:
Procedure:
Place a drop of reagent A on a spot plate. Add one drop of neutral test solution. The reagent is
decolourised. (Ref 1 page 304)
4.4.10 Test for Phosphate (PO 43-)
Requirements:
i) Ammonium molybdate
ii) Benzidine
iii) Conc. Nitric acid
iv) Glacial Acetic acid
v) Saturated solution of Sodium acetate
vi) Conc. Hydrochloric acid.
vii) Sodium hydroxide
Preparation of Reagents:
Reagent A: Dissolve 0.5g of Ammonium molybdate in 10ml of water. Add 3ml conc. HNO 3.
Reagent B: Dissolve 6.5g Benzidine in 10ml glacial acetic acid and dilute to 35ml with water.
Reagent C: Dissolve 16 g sodium hydroxide in 100 ml water.
Procedure:
Test for Phosphate:
I. Place one drop of water extract in a spot plate. Add one drop of reagent A, wait for 30
seconds. Add one drop of reagent B, wait for 30 sec. Again add 3 drops of saturated
solution of sodium acetate. Blue gray colour indicates the presence of phosphate.
II. The above tests must be carried out along with reference standard as well as blank.
i) Ammonium molybdate
ii) Benzidine
Preparation of Reagents:
Reagent A: Dissolve 0.5g of Ammonium molybdate in 10ml of water. Add 3ml conc. HNO 3.
Reagent B: Dissolve 6.5g Benzidine in 10ml glacial acetic acid and dilute to 35ml with water.
Reagent C: Dissolve 16 g sodium hydroxide in 100 ml water.
phosphorus is oxidized to phosphate by adding few drops of HNO 3–HCl (mixture 1:1),
boil for 5 minutes, cool and wait for 5 minutes. Place one drop of acidic sample solution on spot
plate and one drop of reagent C and one drop of reagent A and one drop of reagent B. wait for
30 sec. And then add 5 drops of saturated solution of sodium acetate. A blue or blue gray
colour indicates presence of phosphorus. (ref 3, pages 104-105 )
The chlorate obscure the test for nitrate. The nitrate is reduced to ammonia by boiling
the sample solution with zinc test and sodium hydroxide. The chlorate is also reduced to
chloride which is tested by silver nitrate solution .
Residue Filtrate
CdS and excess of CdCO3. Wash and Reject the Add strontium nitrate solution in slight excess.
washings. Digest the residue With dilute acetic Allow to stand overnight and filter.
acid to remove Excess carbonate. Yellow residue Residue Filtrate
Indicates sulphide. Confirm by warming With treat with dil. HCl and Acidify with dil. HCl
dilute HCl and test the evolved H2S with lead filter. Test the residue and boil SO2 is evolved
acetate paper (Sulphide for sulphate (sodium and sulphur is slowly
nitropruside test) and precipitated
filtrate for
Thiosulphate and
sulphite
I. Place a drop of neutral water extract on a black porcelain plate and add 8 drops of
reagent A. Stir with a glass rod when a yellow turbidity or pptappears. In case of smaller
amounts of sodium, place the porcelain plate under UV light. A bright fluorescenceindicate the
presence of sodium.
Requirements:
Reagent B: 0.167 M sodium cobaltinitrite solution (Dissolve 6.73g sodium cobaltinitrite in 100
ml water.)
Procedure:
I Place a drop of the water extract upon reagent A paper and add 2 drops of 0.1N HNO 3. A
red stain at the site of the spot appears while all other parts of the reagent paper turn bright
yellow.
NB: First test the suspected material for the presence of ammonium ion. If the extract contain
ammonium, evaporate it to dryness in a micro crucible. After cooling the residue moisten the
residue with water and carry out the test as above. Ammonium ion may be eliminated by boiling
the solution with dilute NaOH solution. (ref 3, pages 105-106 )
II. Take 5 drops of water extract in watch glass, evaporate to about 2 drops and cool, then
add 4 drops of reagent B and warm if necessary. Yellow precipitate insoluble in dilute
acetic acid, .indicates K+ (ref 1, page 289).
a) Test for Potassium ion in presence of ammonium ion, add water extract to a few drops
of perchloric acid white ppt. appears (Ref 1)
b) Add water extract to 1 ml of 10% (W/V) Sodiium hydroxide solution and boil. The
evolution of pungent smelling gas occurs, which produces deme white fume on contact with
Requirements:
i) Sodium Rhodizonate
ii) 0.5 N Sodium Hydroxide.
Preparation of reagents:
Reagent A: 0.2% aqueous solution of Sodium rhodizonate. Dissolve 0.2 g of Sodium
rhodizonate in 100ml of distilled water.
Requirements:
i) Potassium chromate
ii) Strontium rhodizonate
Preparation of reagents:
Reagent A: 0.2% aqueous solution of sodium rhodizonate.
Dissolve 0.2 g of sodium rhodizonate in 100ml of distilled water.
Reagent B: Saturated solution of potassium chromate.
Procedure:
I. Place a drop of neutral extract of sample on a filter paper or in a spot plate. Add a drop
of reagent A. A brownish red coloration or precipitate is produced.
If barium is also present proceed as follow. Impregnate the filter paper with reagent B
and dry it. Place a drop of extract on this paper and after a minute place a drop of
reagent A on the moistened spot. Brownish red spot or ring is formed. (ref 1, pages
281-282 )
II. The above test must be carried out along with the reference standard as well as blank.
4.5.6 Flame test for Sodium, Potassium, Barium, Calcium & Strontium.
Take small part of the water extract in a beaker, evaporate it to dryness and cool. Take
conc. HCl in a watch glass. Perform flame test by platinum wire in the non-luminous
flame of the burner. (ref 1, page 466 )
Ca2+ Brick-red
Ba2+ Yellowish-green
Sr2+ Crimson
I. Place a drop of neutral or weakly acidic water extract in a spot plate and add a drop of
reagent. An Orange brown precipitate indicates the presence of ammonium ion.
Procedure:
Post explosion Test Procedure:
I. Place a drop of water extract in the spot plate and add 2 drops of reagent A. (In an acidic
medium solution is orange colour). Add 2N NaOH until colour changes to violet.
Appearance of blue precipitate or tint that intensifies on standing indicates the presence
of Magnesium. (ref 3, pages 97-98 )
II. Place a drop water extract on a spot plate and add 1-2 drops of reagent B. Add one drop
of 2M NaOH. Blue precipitate is formed indicating the presence of magnesium. (ref 1,
page 288 )
III. The above tests must be carried out along with the reference standard as well as blank.
Preparation of Reagents:
Reagent A: Prepare saturated solution of Morrin reagent in 5ml of methyl alcohol in a small
bottle.
Reagent B: Aluminon reagent.(Dissolve 0.25 g of aluminon in 250ml of water.)
II. Take 1ml of the acidified water extract, add 1 ml 10M ammonium acetate solution and
2 ml 0.1% aqueous solution of reagent B. Shake, allow to stand for 5 minutes and add
excess of ammoniacal ammonium carbonate solution to decolourise excess dyestuff and
lakes due to traces of chromium hydroxide and silica. A bright red precipitate or
colouration persisting in alkaline solution indicates the presence of aluminium.
(ref 1, page 252 )
III. Place a drop of water extract on a reagent paper (reagent C). Hold it for a short time over
a bottle containing conc. ammonia solution and then over glacial aceticacid until the blue
colour just disappears and the unmoistened paper regains the brown colour of free
quanalizarin. A red-violet or red spot is formed. Blank test should also be performed.(ref
1, page 254 )
IV. The above tests must be carried out along with the reference standard as well as blank.
I. Dissolve the unknown metallic powder in 2 N NaOH and carry out the above tests.(ref 3,
page 90)
I. Place 2 drops of the test solution on a spot plate add 1 drop of reagent A and 2 drops of
conc. sulphuric acid. A blue or purple blue colour indicates the presence of sugar.
(ref 3, page 106)
II. A drop of the test solution is mixed with reagent B and 1 drop of reagent C in a test
tube. The mixture is boiled for 1-2 min. A red colour or precipitate indicates reducing
sugars. (ref 6, page 338).The above tests must be carried out along with the reference
standard as well as blank.
I. The procedure is same as above ( I) but a purple colour formation indicates a position
result.
Procedure:
I Gutzeit Method:-
Mix a drop of alkali extract with a few grains of zn and few drops of dilute sulphuric acid
in the micro test tube with a flat rim and place a small piece of filter paper moistened
with 20% silver nitrate solution on the flat surface. Gray stain will be obtained. (ref 1,
page 231)
If a bright copper foil is boiled with extract, acidified with at least one tenth of its bulk of
conc. HCl, the arsenic is deposited upon the copper as a gray film of copper arsenide.
Antimony, Mercury, Silver and other metals are also precipitated under similar
condition. It is therefore necessary to test for arsenic in the deposit in the dry way as
follow. Wash the copper strip having deposits with distilled water, dry between filter
paper and then heat gently in a test tube. A white sublimate of arsenic oxide appears
which is identified by examining under microscope when the sublimate appears as
octahedral and tetrahedral crystals (ref 1, Page 231).
Preparation of Reagents:
Reagent A: Add 0.01g Rhodamine-B in 100ml of distilled water.
Procedure:
Post explosion Test Procedure:
I. Take a small portion of NaOH extract in a spot plate. To it add 1-2 drops of conc. HCl and
a few mg sodium nitrite. Add 10 drops of reagent A and mix it. A change of colour from
bright red to violet indicates the presence of Antimony. (ref 3, page 92)
II. The test must be carried out along with reference standards as well as blank.
i) p-Amino dimethylaniline
ii) Ferric chloride
ii) Hydrogen sulphide
iv) Sodium nitroprusside
Procedure:
I. Place a drop of alkali extract on a spot plate, add a drop of conc. HCl, mix. Add 2-3
drops of reagent A to it. Add a drop of reagent C. A clear blue coloration appears
after a short time (2-3 minutes). (ref 1, page 310)
II. Mix on a spot plate a drop of the alkaline extract with a drop of reagent B. A violet
colour indicates the presence of sulphide. (Ref 1, page 309)
Alternatively filter paper impregnated with 2M ammoniacal solution of sodium
nitroprusside may be employed.
The tests must be carried out along with reference standards as well as blank.
Requirements:
i) 2M Sodium hydroxide
Procedure:
I. Take a small portion of pyridine extract in a small test tube and boil it for one minute.
Add a drop of 2M sodium hydroxide (add in a hot condition). A blue to green colour for
low and red to brown for high concentrations of sulphur is observed. (ref 3, page 107)
II. The above tests must be carried out along with the reference standard as well as blank.
The instrument Ion Chromatograph is calibrated and kept ready for analysis as per the
instrument manual.
Analysis of Anions
Column : Polystyrene/divinylbenzene copolymer, 250mm length, 4.6mm ID
Suppressor : Metrohm Suppressor Module (MSM, 20m mol/L H2SO4)
Analysis of Cations
Column : Spherical Silica gel with polybutadiene maleic acid groups, 125mm length, 4mm ID
Eluent : 4 Mmol/L Tartaric acid/0.75 Mmol/L Dipicolinic acid : 3 Mmol/L Tartaric
acid/0.5Mmol/L Oxalic acid for basic cations and nickel, zinc, cobalt : 8 Mmol/L Tartaric
acid/10% acetone for basic cations.
Flow rate : 1ml/min
Sample volume: 10 μL
pH range :2-7
The instrument is calibrated and kept ready for analysis as per the instrument manual.
Conditions:
Column : Fused silica capillary with 75m I D (Prepared for use by flushing for 2 minutes
with 100 mMNaOH.)
Detector: Scanning UV detector, dual wavelength mode at 280 nm and 205 nm.
Operating Voltage: 20 KV
Buffer: Add 0.53 g of potassium dichromate, 0.76 g of sodium tetraborate, and 2.47 g of
boric acid to 1 liter of de-ionised water, adjust to 7.65 with diethylenetriamine
(DETA) and filter through 0.45 m nylon filter. The resultant buffer solution is
2mM in borate , 40 mM in boric acid and 1.8 mM in dichromate.
Injection: Hydro dynamic injection
Injection time: 5 sec
Ions identified: Cl-, NO2-, ClO3-, NO3-, SO4-, SCN-, ClO4-, HCO3-
(ref 4, page 135 )
XRF Technique based on the emission of characteristic X-ray radiation when a sample is
exposed to exciting radiation from more energetic X-ray. The spectra are displayed as
intensity verses energy or wavelength.
- The sample is irradiated with a beam of primary X-ray knocks out an electron from the K
shell. An electron in the L shell drops into the K shell with concurrent emission of
radiation of characteristic wavelength, the secondary or florescent radiation. An
electron in the M shell drops into the vacancy in the L shell with the emission of
radiation. The process is repeated as an electron in the N shell drops into the newly
created vacancy in the M shell. Hence obtain spectrum consist of well defined peaks
due to these transitions, which are called K, K , K, L, and L for the transition L,
MK, NK, ML and NL. These peaks may have shoulders, because the electron in
the L or M shell can have one of three or five energies depending whether it is in a, s, p
or d sub shell but quantum mechanical selection rule allows two K and two K
transitions.
- The energy differences within a shell are very small compared with the differences
between various shells and these transitions show up. If at all, as extra peaks on the
main peaks, they are labeled K1, K2 and K 1 etc. The X-ray spectrum is thus highly
characteristic of an element.
- According to Moseley for a series of the same type the observed wave length is related
to the atomic number of the element. This leads to two conclusion of analytical
importance: (1) A spectrum of unknown sample will have a series of peaks whose
maximum wavelength is directly related to atomic number of the element in the
sample, i.e. quantitative analysis is simple. (2) The peaks are so characteristic of an
element that quantitative analyses can be carried out without prior separation, i.e.
method is specific.
- Furthermore, because the transitions are between inner shells, the valence state of the
element is of little consequence so that the total amount of an element can be readily
determined regardless of its chemical form.
ELEMENT K KB1 Kab L1 LB1 LB2 L1 Llab Lllab Llllb M1
C 0.277 0.284
Na 1.041 1.067 1.072
Mg 1.254 1.296 1.303
Al 1.487 1.553 1.56
S 2.308 2.464 2.471
Cl 2.622 2.816 2.82
k 3.313 3.59 3.608
Ca 3.691 4.013 4.038 0.341 0.345
Fe 6.4 7.058 7.111 0.705 0.718
As 10.532 11.727 11.865 1.282 1.317
Sr 14.142 15.837 16.108 1.807 1.872
Sb 26.279 29.725 30.486 3.605 3.844 4.101 4.348 4.699 4.382 4.132
Ba 32.071 36.381 37.458 4.466 4.828 5.157 5.531 5.996 5.623 5.247
Hg 70.167 80.249 83.1 9.989 11.823 11.924 13.83 14.843 14.251 12.287 2.195
Pb 74.243 84.921 87.995 10.552 12.614 12.623 12.623 15.855 15.205 13.041 2.346
5.2 Scope: Chemical tests and chromatographic methods for identification of Primary High
Explosives (Initiatory Composition)
5.3 Purpose: Detection and identification of Primary High Explosives (Initiatory Composition)
in pre blast and post blast residues.
Add an equal amount of Vanadium pentoxide to the sample on a spot plate and allow
one drop of concentrated hydrochloric acid to run into the mixture. Mercury fulminate
produces a violet coloration.
Add one drop of freshly prepared ferric chloride solution to the sample dissolved in
saturated ammonium acetate solution. A blood red colouration indicates Azide or Thiocyanate.
In case of azide the colour is discharged by hydrochloric acid but retained in case of
thiocyanate.
The presence of Lead styphnate is indicated by its characteristic yellow green colour.
Eluents:
1 2 3 1 2 3
MercuryII - - 0.14 Orange - Grey
Brown
Lead II 0.37 0.36 0.00 Yellow - Brown
Grey
Styphnate 0.73 0.71 0.89 Yellow without visualization
References :-
1.Yallop.H.J. Explosion Investigation 1980. Foren. Sci. Soc. Academic Press, U.K.
Requirements:
i) Diphenylamine ii) Sulphanilic acid
iii) Acetic acid iv) -Naphthlyamine
v) BrucineSulphate vi) Ethanol
vii) Thymol crystals viii) Nitrogen free conc.H2SO4
ix) Potassium hydroxide x) Tetramethylammonium hydroxide
xi) J-acid. xii) conc. Sulphuric acid
Preparation of Reagents:
IV Add 1 ml of extract to 2-3 drops of Reagent E in a clean test tube (ref 5, page 108).
TNT -- purple red Tetryl -- red violet
NB: Add one drop of a 1;1 acetone -alcohol mixture and one drop of 25% aqueous
tetramethylammonium hydroxide to 5-10 mg of test material. In the presence of 2,4-dinitrotoluene a
blue colour appears, and in the presence of TNT, a dark red colour. Since the colour will change with
time, the first observation is the decisive one.
V Take 200 mg crystals of thymol in a test tube and add 0.3 ml of conc. sulphuric acid
(nitrogen free) and 1ml of the sample extract, mix well, warm the tube for 5 minutes at
100 C and add 5-10 ml of ethanol.(ref 5, pages 95-96). Observe the colour for
conclusion.
NB: If the same test is repeated at 150 C RDX will produce blue colour whereas HMX
results in olive colour. Thus RDX can be distinguished from HMX.
VI Place a drop of reagent F on a glass filter paper followed by a drop of the test
solution in Acetone (ref 5, page 94) and observe the colour for conclusion.
Requirements:
TLC plates (20x20cm or 10x10cm) of Silica gel G layer thickness 250 m.
Developing solvents:
i) Chloroform
ii) Acetone
iii) Toluene
iv) Cyclohexane
v) Ethylacetate
vi) Trichloroethylene
Procedure:
1. Activate the pre-coated TLC plates by keeping it in air oven at a temperature of 110 0C
for 30 minutes.
3. Take 100ml of eluent in a developing chamber (for 20x20 cm TLC plate), cover with a lid
and allow it for saturation for at least 30 minutes.
4. The concentrated acetone extract of sample is spotted on the pre coated TLC plate
along with reference standard of high explosives, by leaving 2 cm from one edge of the
TLC plate and maintaining minimum distance of 1.5cm between two spots of
applications.
5. The TLC plate is placed in the developing chamber vertically and allowed to develop up
to 10cm from the spots by ascending method.
6. Then the plate is removed and kept aside for the eluent to evaporate at room
temperature.
A. Spray the TLC plate with 5% Diphenylamine (DPA) in 95% ethanol and note the
colour developed, (II) Then keep the TLC plate under UV light for some time note the
colour, (III) The plate is again sprayed with conc. sulphuric acid and the colour
developed is noted.
B. Spray the TLC plate with 1N NaOH in ethanol and keep at 100 0C for 10 minutes in an
air oven. Cool and spray with Griess reagent (0.25% sulphanilic acid and 0.1%. -
Naphthylamine in 1:1 aqueous acetic acid and observe the colour developed as
given in table-1.
C. KOH and Griess as spray reagent. Brown red for TNT, orange brown for tetryl
Eluents:
1. Benzene
Elution distance: 16 cm
Eluents:
Visualising reagent:
1% resorcinol in concentrated sulphuric acid. After elution, the plate is air-dried and sprayed.
After heating at 140-1500C for 15-20 minutes a yellow-green colour is produced.
1. The instrument HPLC is calibrated and kept ready for analysis as per the operating
instructions described in instrument manual.
Method 1: For TNT, RDX, HMX, PETN, NG, EGDN, Tetryl (ref 9)
Detection : UV at 214 nm
Detection : UV at 200 nm
The instrument GC-MS is calibrated and kept ready for analysis as per the operating
instructions given in instrument manual.
Column : fused silica capillary, 15m x 0.25 mm ID with 0.25 mm coating of DB-5.
Electron energy: 70 eV in electron impact (EI) and chemical ionization (CI) modes
General – Absorbing bands in IR range 4000-1300 cm-1 for specific functional groups. Below
1300 cm -1 fingerprint region
NO2 – Symmetric and asymmetric stretching vibrations of group give rise to two distinct
absorption bands – a highly diagnostic value.
Nitrate esters – NO2 stretching vibrations 1285 – 1270 cm-1 and 1660 – 1640 cm-1
Two stretching vibrations in Nitra amines i.e., 1310 – 1270 cm-1 and 1590 – 1530 cm-1( Ref 15)
1. The instrument HPLC MSMS is calibrated and kept ready for analysis as per the
operating instructions described in instrument manual.
2. A solution of standard of High Explosives Acetate adducts are prepared for RDX, HMX,
Tetryl, TNT, PETN in Acetonitrile of concentration of about 0.1ug/ml each and filtered.
5. The Samples were analyzed by Multiple Reaction Monitoring and Product Ion Scan
modes.
LC conditions MS conditions
References:
1. Yinon.J. and Zitrin .S. (1981).The Analysis of explosives, Pergamon press, New York.
3. Yinon.J. and Zitrin .S. (1993).Modern Methods and Application in Analysis of Explosives, John
Wiley and Sons, New York
4. Parker.R.G. Stephenson .M.O., McOwen. J.M. and Cherolis J.A. (1975). " Analysis of Explosives
and Explosive Residues Part-1. Chemical tests, Jr. Foren. Sci., 20, 3, 133.
8 Parker .R.G.(1975). " Analysis of Explosives and Explosive residues Part-3. Mono Methyl Aamine
Nitrate, Jr. Foren Sci. 20, 2, 257-260.
9. Lyter.A.H. III.(1983). A high performance liquid chromatographic (HPLC) Study of Seven Common
Explosive Materials, J.Foren.Sci. 28, 2,
446.
10. Tamiri.T. and Zitrin.S. (1986). Capillary column Gas chromatography/ Mass spectrometry of
Explosives. J. Energetic materials, l4, 215.
11. Yallop.H.J. Explosion Investigation 1980. Foren. Sci. Soc. Academic Press, U.K.
12. J.S.Gharia, R.K.Sinha, U.R.Nair, S.R.Nair *& R.M. Roy (2000) “ Tagging of Explosives for
Detection”, Defence Science Journal, 50, 1, 45.(PP 45-49)
13. Yehuda, Yinon, Forensic and Environmental Detection of Explosives, (1999) J Wiley & sons, N.
York.
14. Krishnamurthy R ; Malve M K., Shinde B M , Analytical Report on Bombay Blast cases . March
1993. Journal of Indian Academy of Forensic science 1996 (35) page 54-55.
15. Krishnamurthy .R, Bakre SM , Shinde BM , Simultaneous detection of High Explosives in Post
explosion debris by HPTLC with two successive mobile phases . Journal of Planar
Chromatography Vol 12 Sept –Oct 1999 Page 394-396.
16. Atul Bajaj, Cijo John, Meenu Singh, Explosive post blast analysis: A case study, European Journal
of Forensic Sciences, Issue 2, Vol 3, 2016, 1-5.
7.3 Purpose: To have a uniform guide lines for interpretation of results in Test Reports and
while presenting the evidence and the limitations involved.
7.4General
The explosive experts are required to provide in Test Reports thedetails of explosivesor
otherwise based on the analysis result. For bulk materials which are suspected to be explosives
the analysis and interpretationsare easy. However, for post explosion cases the prediction of
original explosive substance (s) based on trace analysis pose challenges due to various factors
namely, protection of explosion scene, use of large quantity of water during firefighting in case
of fire associated with explosion,sample collection, handling, packing, labelling, preserving,
transportation, avoidance of cross contamination and maintenance of chain ofcustody from the
scene of explosion to the laboratory. In the laboratory, also proper care has to be taken to
ensure for proper chain of custody, storage of exhibits, cases are to be opened under
supervision and exhibits are to be handled with utmost care to ensure the sample integrity,
avoidance of cross contamination, proper cleaning of surfaces of case opening area and
working space, un ambiguous labelling of exhibits as well as reagents and good laboratory
practices. The expert has to deal with very small amount of post explosion residues which many
a time deny the possibility of repetition. Also, re- examination of post explosion debris by same
laboratory or another laboratory with same exhibits often leads to inconclusive and misleading
results as most of the available material might have been utilized by the original laboratory by
using repeated solvent extraction process to extract the maximum available residues. Care has
to be taken while prioritization and sequence of examination, handling of items, selection of
test procedures etc. (ref 1)
7.5Interpretation of Results
7.5.1In case of organic explosives normally residues of original explosives substances are
detected in trace level. The selection of test methods are decided by the experts based on the
back ground data provided by the forwarding authority, availability of samples, target analytes,
matrix effects, control samples and availability of resources both internal and external. Hence,
the methods selected to be validated and ensured that it is capable of detecting the
7.5.2 In case of low explosive mixtures and pyrotechnic compositions, for pre blast samples the
ingredients can be detected by the methods mentioned in Chapter 4 of this manual. The
ingredients are identified in ionic forms and elemental form. It is well known that the low
explosives contain mixture of oxidizer and fuel along with flame modifiers, binders, stabilizers
etc. (ref 2,3).The post explosion residues of low explosives may contain ions of original
ingredients or reaction products depending up on nature of explosion and stoichiometric
proportion of oxidizer and fuel.
Table 24. Some Common Inorganic Improvised Explosive Devices and the Target Analytes in
post blast residues (ref 3 & 4)
#Sodium nitrate or Sodium Chlorate is also used in Homemade IEDs and cation may change
accordingly
Some inferences can also be drawn in respect of composition of inorganic anions and cations in
mixtures.
1. The presence of ammonium and phosphate can normally be due to ammonium phosphate
since this is the only phosphate likely to be present in an industrial blasting explosive.
2. The presence of ammonium and nitrate can normally be due to ammonium nitrate since
this is a very common constituent of industrial blasting explosives.
3. The presence of sodium and chloride can normally be due to sodium chloride since this is a
common major ingredient of coal mining explosives.
4. If ammonium, nitrate, sodium and chloride are all present this may mean ammonium
nitrate and sodium chloride or, alternatively, the reversed ion mixture i.e. ammonium chloride
and sodium nitrate. The former is far more likely since reversed ion mixture is very uncommon.
The point may be resolved, however, by extracting a portion of explosive with ether and
acetone and examining the residue microscopically for the characteristic cubic crystals of
sodium chloride(ref 5).
5. The presence of barium normally denotes barytes since this is the only barium salt normally
used as a constituent of industrial blasting explosives. By close observation and keen attention
in details, experienced operators can make other deductions with varying degrees of certainty.
After taking into account any known or suspected contaminants, the observations are then
compared with the specified compositions of explosives by manufacturers whose products are
normally used in the country in which the investigation is taking place in some other country, if
this appears relevant. This may be quickly and conveniently done if the components of the
various explosives are recorded on punched cards. It will often be found that only one explosive
has the particular combination of ingredients. When there are two or more observations of
colour, consistency will often resolve the question. But, if this is not so; then a quantitative
determination must be made. It is often not necessary, however, to determine all the
ingredients since normally there will be one ingredient that is present in markedly different
proportions in the possible explosives of a particular class.
1. Best Practice Manual for the Forensic Recovery, Identification and Analysis of
Explosive Traces (ENFSI-BPM-EXP-01) Version 01 November 2015 by the
European Network of Forensic Science Institutes (ENFSI)
5. E. Suresh Babu and Sukhminder Kaur A DSC Analysis of Inverse Salt-pair explosive
Composition Journal of Proppellants,Explosives,Pyrotechnichs 29 (2004) No.1 p 50-
55
8.2 Scope: -To identify explosives which are not commonly encountered
8.3 Purpose: To have a procedure to identify explosives which are not commonly used and
to keep the manual open document so as include procedures for new explosive materials.
Some of the miscellaneous explosive materials and their test procedures are mentioned below
8.3.1.1TATP-Triacetonetriperoxide (TATP)
Triacetonetriperoxide (TATP) is a white crystalline solid material .It is one of the most sensitive
explosive known. Being extremely sensitive to impact, temperature change and friction, It is
very easy to detonate. It is an organic peroxide containing neither metallic elements nor nitro
group. Therefore the presence of peroxide group cannot be detected by standard security
procedure like transmission and vapor detector.(ref 1&3).
The dark blue color of molybdenum hydrogen bronze suspension is changed to yellow upon
oxidation with TATP. The same reagent can also be used for quick neutralization of the sensitive
explosive: a lasting final blue color indicates complete neutralization. The reaction with TATP is
depicted in following equation (ref 4 P51)
6 Mo2O5 OH + Me2COO 3 12 MoO3 + 3 H2O + 3 Me2CO
TATP
HMTD
Urea Nitrate
Conditions
Column: Fused silica capillary Column 30mX 0.25 mm (id) coated with HP-5 MS (0.25m film)
Injector Temperature: 1800C
Column Temperature: programmed from 500C to 1800C at a rate of 150C/min,10 min at 1800C,
180-3000C at a rate of 250C/min and 5 min at 3000C.
Transfer Line was held at 2300C.
Ion Source Temperature: 1800C
Quadrupole Temperature: 1200C
Scan range: 29-350 Da
Scan Rate : 2.29 scans/s
Electron energy :70eV
Carrier gas: Helium
Injection: Split less mode
Preparation of xanthydrolalkylcarbamates (xantylurethanes)
Sample and xanthydrol are reacted according to the method described by Mc Cord and de
Perre (ref C.de Perre, B McCord, Trace analysis of urea nitrate by Liquid chromatography-
UV/fluorescence, Forensic Sci. Int.211(2011) 76-82) using three alcohols as solvents; methanol,
ethanol and 1-propanol.The products have been characterized in the reaction mixtures by GC-
MS.
8.3.3 Quantitative Estimation of Ammonium Nitrate
Vide Notification No. G.S.R. S.O. 1678(E) dated 21/07/2011, Ammonium Nitrate having the chemical
formula NH4NO3 or any combination containing more than 45 percent of ammonium nitrate by weight
including emulsions, suspensions, melts or gels (with or without inorganic nitrates) shall be deemed to
be an explosive under the meaning of the Explosives Act 1884. Provided that such ammonium nitrate or
any combination thereof shall not include those fertilizers from which ammonium nitrate cannot be
extracted by any physical or chemical means.(ref.12). Hence, it is important that the purity of
ammonium nitrate needs to be estimated to include it under the purview of the act or otherwise.
Outline of the Method- Ammonia from ammonium nitrate reacts quantitatively with excess of
formaldehyde to produce nitric acid
8.3.3. 1.Reagents
8.3.3.2 Procedure- Weigh exactly 0.4 g of sample into a 250 ml conical flask and dissolve in 20
ml of water. Add 50 ml of formaldehyde 1:1 reagent and warm the flask. Cool to room
temperature and titrate against standard alkali till permanent light pink colour appears. Drain
another 2 ml of alkali and note down the volume (V1). Keep it for 10 minutes and titrate against
standard hydrochloric acid using a calibrated micro burette till the solution becomes colourless
and note down the volume (V2). Repeat the same experiment till concordant values are
obtained
8.3.3.3 Calculations
N1
(100-moisture percent)
Where
Uncertainty of measurement for the quantitative estimation may be calculated as per ref. 13 by
considering all the contributory factors.
References
(Page 01 of 08)
Form No.
2. Date(s) of examination:
I Examination of High Explosives
Sample Alcoholic KOH Test DPA Test Thymol+ Ethylene diamine Test
Ex-No.
Ex No
Ex No.
Ex No
Solvent System A:
Solvent System B:
Solvent System C:
Spray Reagent:
HR f / λ max values
Results
Mobile Phase:
Column:
Flow Rate:
(b)Results
Column : fused silica capillary, 15m x 0.25 mm ID with 0.25 mm coating of DB-5.
Electron energy: 70 eV in electron impact (EI) and chemical ionisation (CI) modes
(b) Results
(b)Results
Extraction:
Name of the Name of the Test conducted Observation With Exhibit No.
Anions control
Na OH
extract
Mobile Phase A:
Mobile Phase B:
Mobile Phase C:
Column :
Flow Rate:
(b)Results-
(a)Experimental Condition
(b)Results-
Extraction:
Antimony
+3
(Sb )
Rhodamine-B Test
(a)Experimental Condition
Mobile Phase A:
Mobile Phase B
Mobile Phase C
Column :
Flow Rate:
(b) Result
(Page 07 of 08)
(b) Result
Note: Tests were carried out as per Working Procedure Manual Document No
Inference: