CHAPTER 6 – CHEMICAL

ASPECT OF QUESTIONED
DOCUMENTS
At first impression, it seemed that the
examination of questioned documents is
hardly within the scope of a forensic
chemist, but if we consider the fact that
the essential materials in a document
examination of any kind are the PAPER
and INK or PENCIL, and the chemical
examination of inks, erasures, alterations
and sequence of writing are all associated
with such examination. It will be evident
that there is a large amount of purely
chemical work in the field of document
examination.
DOCUMENT =

Is an original, official ,written or printed

paper furnishing information that is used
as a proof of something else.
WHAT IS A QUESTIONED DOCUMENT?
It is any object that contains handwritten
or typewritten markings whose source or
authenticity is in doubt.
PACKING, PRESERVATION and
TRANSPORTATION of DOCUMENTS
Documents are precious things and
therefore should be treated accordingly:
1. Documents should be handled, folded
and marked as little as possible.
2. If folding is necessary to send to the
laboratory, the fold should be made
along old lines. Place it in manila paper
envelope or brown envelope or in a
transparent plastic envelope.
3. As a receipt, the document should be
placed between 2 sheets of plain white paper
and place it in the folder.
4. Documents should not be touched with
pencil, pen or anything that could be possibly
mark them.
THE EXAMINATION OF QUESTIONED
DOCUMENTS
Examination and Comparison of Paper
The essential materials in a document
examination of any kind are the paper and ink
or pencil or writings. The examination of paper
ma be necessary if we want to know the age
of the document, the presence of alterations,
erasures and other forms of forgery.
 PROBLEMS ENCOUNTERED IN THE
ANALYSIS OF PAPER
1. Determination of whether two pieces of
paper originated from the same source.
2. Determination of the probable age of the
paper.
3. Determination of the composition of the
paper.
1. Fiber Composition - practically all the papers
may be classified from the standpoint of their
basic fiber composition into sets of fiber mixtures
namely:
a. Mechanical pulp = ground wood- sulfite
mixture, this is pulp from coniferous and
dicotyledonous wood in combination with sulfite
chemical pulp from conifers.
b. Soda-Sulfite Mixture =chemical pulp from
dicotyledonous woods.
c. Rag Sulfite =cotton rag or linen rag.
2. Sizing Material = added to paper to improve its
texture. Examples of sizing materials are rosin
casein gelatin and starch. It serves as binder.
3. Loading materials= added to paper to give
weight. It partially fills the pores between the fibers
of the paper. example's of this are calcium sulfate
and barium sulfate.
 Substances Used for Writing:
Egyptian Papyrus – one of the earliest
substance used for writing. It is from the name
papyrus that the word paper was derived. After
papyrus came parchment and velum then
linen rag followed by mixture of linen and
cotton or cotton only. Paper made from a
variety of fibrous materials started about the
middle of the 19th century.
a. 1800 – straw was first used.
b. Between 1845 and 1880 – from soda pulp
c. 1869- from mechanical wood pulp
d. Between 1880 and 1890 from sulfite wood
pulp
At present, a thin sheet of matted or felted
vegetable fiber ( usually wood pulp ) with filler
as clay and sizing material as rosin or starch.
 THE EXAMINATION OF PAPER
FROM the examination and comparison of paper
may determination the following:
1. The age of paper as compared with the age of
known document
2. Whether a paper is identical with or different from
another paper whose history is known.
3. Whether two sheets of paper of the sane
manufacturer were made at the same time. In this
case we have to know when the form was printed or
when the paper was first made that bears a particular
mark.
 THE FOUR TESTS FOR PAPER
1. Preliminary Examination
2. Physical test causing no perceptible change
3. Physical test causing a perceptible change
4. Chemical test
1. Preliminary Examination – deals with the
appearance of the document and the following are
observed:
a. Folds and creases
b. Odor
c. Impression caused by transmitted light – gives
indication of the color, translucency where
tampering is made, change in tint which indicates
substitution of sheets of paper, watermarks and wire
marks.
d. Presence of discoloration in daylight and under
the ultraviolet light.
Watermark – if present, is one of the most important
features in the comparison of paper. It is distinctive
mark or design placed in the paper at the time of its
manufacture, by a roll usually covered by wire cloth
known as dandy roll which serves as a means
whereby the paper can be identified as a product
of a particular manufacturer.
Wiremark – Marks produced on a paper by the
flexible wire soldered to the surface of the dandy roll
that carries the watermarks.
2. Physical Test Causing No Perceptible Change –
a test applied on paper without perceptible
changing or altering the original appearance of
the document.
a. Measurement of length and width – to
indicate that they originated from the same
manufacturer if two pieces are found to be
exactly the same.
b. Measurement of thickness
 c. Measurement of weight/unit area or the
(grammage) or gsm or g/m²
d. Color of the paper – It is closely related to its
brightness. A side by side comparison maybe
made in well diffused light. Observation of color is
influenced by the texture, gloss, finish, type of
illumination and the element of human error.
e. Texture
f. Gloss – gloss and texture may be determined
by visual observation in good daylight or under
different kinds of illumination.
 g. Opacity – the quality of the paper that does
not allow light to pass through or which prevents
dark objects from being seen through the paper.
h. Microscopic examination/inspection – for
possible presence of dirt, foreign particles,
imperfections, wiremarks or certain unusual fibers.
These maybe a deciding factors in determining
whether or not the same manufacturer made two
pieces of paper.
3. Physical Examination Causing a Perceptible
Change – this is done only if sufficient samples are
available and if prior authorization from the court is
required this can be done.
a. Bursting strength or Pop test – the apparent
pressure necessary to burst a hole in a sheet when
properly inserted in a suitable instrument.
b. Folding endurance test – it is obtained on
an instrument that registers the number of
alternate folds the paper will stand before
breaking.
 c. Accelerated aging test – there are some
methods of aging a document artificially namely:
1. soaking in coffee solution
2. soaking in tea solution
3. exposure to charcoal
4. ironing
5. heating in an oven
6. exposure to ultraviolet light
 d. Absorption test – maybe made to determine
either the rate of absorption or the total absorption
of paper. A strip of paper is suspended in water or
ink or other liquid.
4. Chemical test – this test determines the fiber
composition, the loading material and sizing
material used in the paper.
A. Fiber composition – the examination is purely
microscopic and it determines the material used
and nature of processing. This maybe determined
by boiling a small piece of the document in 5%
sodium hydroxide.
The liquid poured off and the fragment of paper
washed and teased out on the glass slide and
stained with the following and the color observed
under the microscope.
Reagents:
a. 2 grams potassium iodide, 1.5 grams iodine,
2ml glycerine and 20 ml water
b. 1) 20 grams zinc chloride and 10 ml water
2) 2 grams potassium iodide, 1 gram iodine
and 5 ml water
 Mix 1 and 2 allow the mixture to stand and
decant clear supernatant liquid for use. (the solution
is zinc chloriodine)
c. 1 gram phloruglucine, 25 ml water and 5 ml
conc HCl
d. 10% solution of aniline sulfate

B. Sizing material – the sizing material maybe tested

by:
Procedure and Results:
1. Gelatine is extracted by boiling the paper in
water. The solution is tested with dilute tannic acid
solution. Positive result is yellow precipitates.
2. Rosin – this is extracted by heating the paper
on a water bath with 95% alcohol. The solution
obtained is evaporated to dryness and the residue
dissolved in acetic anhydride, cooled, transferred
to a porcelain dish and strong sulfuric acid is
added.
POSITIVE RESULT: reddish violet color that
quickly change to red brown.

SIMPLE test for ROSIN: Place a few drops of

ether on the paper and if ROSIN is
present, a brown ring will be formed
when ether evaporates.
 3. Starch – add a dilute iodine solution on the
paper. Blue color is produced if starch is present.
4. Casein – it can be detected by addition of
Millon’s reagent on the paper. Pink color appears if
casein is present.
 THE ANALYSIS OF INK

Some of the most important questions that arise in

the analysis of ink are:
1. Whether the ink is the same or like or different in
kind from ink on other parts of the same
documents or on the other documents.
2. Whether two writings made with the same kind
of ink were made with identical ink, or inks of
different qualities or in different conditions.
3. Whether an ink is as old as it purports to be.
4. Whether documents of different dates or a
succession of differently dated book entries show
natural variations in ink writing or whether the
conditions point to one continues writing at one
time under the same condition.
 TYPES OF INK
1.Gallotannic ink or iron-nutgall ink (blue) – today
the most frequently used ink for making entries in
record books and for business purposes.
Gallotonic ink is made of a solution of iron salt
(ferrous sulfate) and nutgall (iron gallotannate).
This ink can penetrate into the interstices of the
fiber and not merely on the surface thus making
its removal more difficult to accomplish. The color
changes undergone by this ink in the process of
oxidation provides a valuable means of estimating
the approximate age of writing.
Blue – with the naked eye; very recent
Violet – less recent
Black – still less recent
2. LOGWOOD INK-(black) the color is
dependent on the inorganic salt added,
but on drying and standing they turn black.
It is made of saturated solution of logwood
to which very small amount of Potassium
Dichromate is added. HCl is also added to
prevent formation of precipitate. Phenol is
added as preservative. This ink is
inexpensive, does not corrode steel, will not
wash off even fresh, flows freely.
3. NIGROSINE INK OR ANILINE INK (blue
black or purple black)- made of coal tar
product called nigrosine dissolved in water.
It easily smudge, affected by moisture,
maybe washed off from paper with little
difficulty.
(hindi magandang ink,kapag binura
kumakalat ang dumi)
4.CARBON INK/CHINESE INK/ INDIAN INK (black)=
the oldest known ink material. Uses finely divided
carbon in colloidal suspension used to produce
deep black drawing and writing ink. Made of
carbon in the form of lampblack.
 Does not penetrate deeply into the fibers
of the paper so that it may easily washed
off. Not affected by the usual ink testing
reagents.

Used in diplomas.
5. COLORED WRITING INK – today almost
all colored inks are composed of synthetic
aniline dyestuffs dissolved in water. In
certain colored inks ammonium vanadate
is added to render the writing more
permanent.

6. BALLPOINT PEN – made of light fast dyes

soluble in glycol type solvents like
carbitol, glycol or oleic acid.
 TEST FOR INK
1.Physical method/Test – applied to
determine the color and presence of
alterations, erasures, destruction of sizes of
the use of stereoscope, handlens,
microscope.
2.Chemical Test or Spot Test – a simple test
wherein different chemicals or reagents
are applied on the ink strokes and the
chemical reactions or characteristic color
reactions or the other changes in the ink
are observed.
REAGENTS USED: 5% hydrochloric acid,
10% oxalic acid, tartaric acid, 2% sodium
hydroxide,10% sodium hypochlorite,
chlorine water, water, etc.
3. PAPER CHROMATOGRAPHY TEST – a
reliable procedure which can be adopted
to identify and compare ballpoint pen ink.
DETERMINATION OF APPROXIMATE AGE
of DOCUMENT
1. AGE of INK- no definite procedure which
can be given for this determination except
when the color is black, because on the
observation that within a few hours, the
color of ink writings become darker and the
dye contained therein is influenced by the
light or the room, oxygen of the air, acidity
or alkalinity of the paper.
THERE ARE SEVERAL METHODS OF
DETERMINING THE DEGREE OF OXIDATION OF
THE INK WRITING.THESE ARE:
A. PHYSICAL test (PHENOMENA) such as
matching the color of the ink writing with
standard colors or with itself over a period
of time.
 B. CHEMICAL RXN that may reveal some
information concerning the length of time
the ink has been on the paper.
2. AGE of PAPER
a. through watermarks
b. in some cases, based from the
composition of the paper
The detection and deciphering of illegible
writing is one of the major problems in
document examination
ILLIGIBLE WRITING- is an unnecessary
writing which is not capable of being read
usually found on checks, birth certificates,
passport, transcript of records,etc.
EXAMPLE OF ILLIGIBLE WRITINGS:

1. ERASURE- the removal of writing. It can be

done mechanically or chemically.
2. OBLITERATION- the obscuring of writing by
superimposing ink, pencil or other
marking materials
3. SYMPATHETIC INK- substance used for
invisible writing
4. INDENTED WRITING- term applied to the
partially visible depression appearing on a
sheet of paper underneath the one in
which the visible writing appears.
5. WRITINGS ON CARBON PAPER-writings
produced even by used carbon paper
6. CONTACT WRITING- blank paper may
contain traces of ink because of
previous contact with some writings.