IS 3584:2007

Indian Standard
CAMPHOR — SPECIFICATION
( Second Revision)

ICS 71.100.60

@ BIS 2007

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SI-iAH ZAFAR MARG
NEW DELHI 110002

June 2007 Price Group 2

Natural and Synthetic Fragrance Materials Sectional Committee, PCD 18

FOREWORD
This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards, after the drafl finalized
by the Natural and Synthetic Fragrance Materials Sectional Committee had been approved by the Petroleum,
Coal and Related Products Division Council.
This standard was first issued in 1966 and subsequently revised in1984. In the first revision the wet method for
determination of total ketones using 2, 4-dinitrophenyl hydrazine was replaced by gas chromatog~aphic method.
The two grades were redesignated as pure and technical.
In this revision, modified GC method has been incorporated. A test has also been included to check adulteration
of camphor with hexamine.
Camphor (C ,OHIGO),is a naturally occurring bicyclic ketone, which is principally present in the volatile oils of
camphor ex Cinnamomum camphora (Linn.) Nees at Ebermaier, fare. Lauraceae and of ocimum from Ocimum
kilimand.wharicwn Guerke, fare. Labiatae. It is also obtained synthetically. It is represented by the following
structural formula:

&
o

Camphor (Molecular Mass 152.23)

Natural camphor is usually obtained from the oil of camphor or the oil of ocimum by first congealing and filtering
it before fractional distillation, and for final purification, pressing and sublimation are restored to. This material
is used in the manufacture of cellulose, films and in pharmaceutical preparations. It is also used as incense in
religious ceremonies and for other domestic purposes.
Synthetic camphor is usually obtained from alpha-pinene. Beta-pinene can also be used for this purpose, though
this is not the normal practice. Synthetic camphor is generally marketed as powder, tablets or THAL. THALS
consist of circular discs of the material about 250 mm in diameter and 60 to 100 mm thick. They are prepared
through a process of sublimation and cooling of the material to desired shape.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final value
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
IS 2:1960 ‘Rules for rounding off numerical values (revise@’. The number of significant places retained in the
rounded off value should be the same as that of the specified value in this standard.
 IS 3584:2007

Indian Standard
CAMPHOR — SPECIFICATION
( Second Revision)

1 SCOPE 3 TERMINOLOGY

This standard prescribes the requirements and the For the purpose of this standard, the definitions given
methods of sampling and test for camphor largely used in IS 6597 shall apply.
in trade and industry.
4 GRADES
2 REFERENCES
4.1 This standard covers two grades of camphor,
The following standards contain provisions which, namely, pure and technical.
through reference in this text, constitute provisions of
4.1.1 Technical material shall be only the synthetic
this standard. At the time of publication, the editions
product.
indicated were valid. All standards are subject to
revision and parties to agreements based on this 5 REQUIREMENTS
standard are encouraged to investigate the possibility
of applying the most recent editions of the standards 5.1 Description
indicated below. 5.1.1 The material shall be either natural or synthetic,
[S No. 7Ule translucent or opaque and shall consist of crystals,
granules or crystalline mass of tough consistency and
265:1993 Hydrochloric acid ~ourth revision)
pulverulent character, known as ‘flowers of camphor’,
326 Methods of sampling and test for having pungent, aromatic taste followed by a sensation
natural and synthetic perfumery of cold, and a characteristic penetrating odour.
materials:
(Part 1): 1984 Sampling (second revision) 5.1.2 Technical material may also be in the form of”
powder, tablets or any other form.
(Part 2): 1980 Preliminary examination of
perfumery materials and samples 5.1.3 The material shall also be tested olfactorily and
(second revision) especially for bynotes as prescribed under 4 and 5 of
(Part 4): 2005/ Determination of optical rotation IS 2284.
1S0 592:1998 (third revision)
5.2 Identification
(Part 6): 2005/ Determination of volubility in
ISO 875:1999 ethanol (third revision) The material shall bum readily with a bright smoky
(Part 10) : 2005/ Determination of residue on flame and volatilize slowly at room temperature.
1S04715 :1978 evaporation (third revision)
5.3 Volubility
(Part 16) :1989 Determination of melting point and
melting range (second revision) 5.3.1 One gram of the material shall dissolve in 800 ml
(Part 19) :1998 Gas chromatographic analysis of of water on being stirred mechanically at room
perfumery materials temperature for 3 h. The solution thus obtained shall
be clear. The same amount shall also dissolve separately
1070:1992 Reagent grade water (third revision)
in 1 ml of ethyl alcohol (95 percent by volume), 0.5 ml
1745:1978 Specification for petroleum of chloroform and in 1 ml of ether at 27 + 2°C. It shall
hydrocarbon solvent (second also be freely soluble in carbon disulphide and in fixed
revision) ancJvolatile oils [see IS 326 (Part 6)].
2284:1988 Method for olfactory assessment of
natural and synthetic perfumery 5.3.2 Volubility in Petroleum Hydrocarbon Solvent
materials (first revision) (60/80)

6597:2001 Glossary of terms relating to One gram of the material shall give a clear solution in
fragrance and flavour industry 10 ml of petroleum hydrocarbon solvent (60/80) (see
(second revision) IS 1745).

1—111 Bls/ND/07
IS 3584:2007

5.3.3 Detection of Adulterant (Hexamine) 6.1.1 Technical material may also be supplied in the
form of powder, tablets or any other form.
5.3.3.1 Principle
6.2 The particular source, natural or synthetic, from
Hexamine is insoluble in acetone.
which the material has been obtained and the grade,
5.3.3.2 procedure shall be marked on each container.
Take 1g sample of camphor in a test tube and add 5 ml 6.3 The material shall be protected from light and
of acetone. Shake the mixture well for 3 to 5 min at room stored in a cool and dry place.
temperature and allow the tube to stand for 30 min.
6.3.1 BIS Certzjication A4arking
5.3.3.3 Result
The containers may also be marked with the Standard
A clear solution with completely dissolved crystals Mark.
indicates absence of aduherant, hexamine. This volubility
6.3.1.1 The use of the Standard Mark is governed by
Imethoddetects hexamine in camphor as low as 1percent. the provisions of the Bureau of Indian Standards Act,
5.4 The material shall also comply with the requirements 1986 and the Rules and Regulations made thereunder.
given in Table 1. The details of conditions under which a licence for
the use of the Standard Mark may be granted to
5.5 Additional Requirements for Pure Grade manufacturers or producers, maybe obtained from the
Camphor Bureau of Indian Standards.
5.5.1 Acidity 7 SAMPLING
The material shall be tested for mineral acidity as 7.1 Representative samples of the material, each
described in 5.5.1.1. If the testis negative, it shall also containing not less than 200 g, shall be drawn as
be tested for organic acidity as described in 5.5.1.2. prescribed in IS 326 (Part 1).
5.5.1.1 Mineral acidity 7.2 Number of Tests
Weigh 20 g of the material and dissolve the same in 7.2.1 Tests for determination of melting range and
100 ml of ethyl ether. Transfer the solution to a camphor content shall be conducted on each of
separating funnel and wash with two 50 ml portions of individual samples.
distilled water. Combine the aqueous extracts and add 7.2.2 Tests for the determination of all other
a drop of methyl orange. The colour of the extract shall characteristics shall be conducted on the composite
not show acid reaction. samples.
5.5.1.2 Organic acidity 7.3 Criteria for Conformity
Weigh 20 g of the material and dissolve in 50 ml of 7.3.1 For Individual Samples
ethanol. Titrate the solution with N/10 barium
hydroxide solution with phenolphtha]ein as indicator. A lot shall be declared as conforming to the
requirements of melting range and camphor content, if
Carry out a blank and apply necessary correction. The
acidity calculated as sulphuric acid (HZSOJ shall not each of the individual test results satisfies the relevant
requirement given in Table 1.
exceed 0.005 percent.
7.3.2 For Composite Samples
5.5.2 Chlorides
For declaring conformity of a lot to the requirements of
Dissolve of camphor in 2 ml of 50 percent aqueous
1g
other characteristics tested on the composite sample, the
ethanol. Add two drops of 10 percent silver nitrate test results on each of the characteristics shall satisfy the
solution. The opalescence, if any, shall not be greater relevant requirements given in 5.1,5 .2,5.3 and Table 1.
than that in a blank similarly prepared.
8 TEST METHODS
5.5.3 Salphates
8.1 Tests shall be conducted as prescribed under 5.1
Dissolve 1 g of camphor in 2 ml of 50 percent aqueous to 5.5 and appropriate references specified in COI5 and
ethanol. Add two drops of 10 percent barium chloride CO16 of Table 1.
solution. The turbidity, if any, shall not be greater than
that in a blank similarly prepared. 8.2 Quality of Reagents
Unless specified otherwise, pure chemicals and distilled
6 PACKING AND MARKING water (see IS 1070) shall be employed in tests.
6.1 The material shall be packed in air-tight containers NOTE — ‘Pure chemicals’ shall mean chemicals that do not
as agreed to between the purchaser and the supplier. contain impurities which affect the results of analysis.

2
 IS 3584:2007

Table 1 Requirements for Camphor

(Clauses 5.4,7 .3.1,7.3.2 and 8.1)

SI Characteristic Requirement for Method of Test, Ref to

No. ~~
Pure Technical IS No. Annex
(1) (2) (3) (4) (5) (6)

i) Colour Colorless or white, Colorless or white, 326 (Part

2) —
crystalline material crystalline material
ii) Melting range, “C 174to 179 165 to 179 326 (Part 16) —
iii) Optical rotation [10 percent (rr/v)] a) Natural +410 to +43° –1.5” to +1.5” 326 (Part 4) .
solution in 95 percent alcohol b) Synthetic –1 .5° to +1.5°
iv) Non-volatile matter, percent by 0.05 0.1 326 (Part 10) —
mass, Max
v) Camphor, percent by mass, A, Min 96 90 — A
vi) Freedom from halogens To pass test To pass test — B

NOTE — Flash point of camphor is 64°C.

ANNEX A
[Table 1, S1No. (v)]
GAS CHROMATOGRAPHIC ANALYSIS FOR CAMPHOR

A-1 GENERAL
.
A-IS The chromatographic conditions given here are
for guidance only.

A-1.2 Outline of the Method

A sample of the material is dissolved in a suitable
solvent (for example, cyclohexane and acetone) and is
injected into the gas chromatographywhere it is carried
by the carrier gas from one end of the column to the
other. During its movement the constituents of the
Key
sample undergo distribution at different rates and
1 – Solvent
ultimately get separated from one another. The
2- Isofenchone
separated constituents emerge from the end of the 3 – Camphor
column one atlter another and are detected by suitable 4- Isoborneol
means whose response is related to the amount of a 5- Borneol
specific component leaving the column [see IS 326
(Part 19)].
A-2 APPARATUS
Any gas chromatography capable of being operated
under conditions suitable for resolving the individual
2 45
constituents into distinct peaks may be used. The typical
chromatogram for camphor using a chromatography
with the following chromatographic conditions is FIG. 1 Tvncw CRROMATOGRAM OF CAMPHOR —
shown in Fig. 1. TECHNICAL

3
IS 3584:2007

Sample Camphor (dissolved in the suitable solvent) at injection port

Column where it is vaporized and well mixed with the carrier
Material Stainless steel gas. This is led into the chromatographic column
Length 3m wherein vaporized constituents of the sample are
Orifice 0.32 mm separated out by virtue of their differing interaction
Stationary phase FFAPIJ, 10 percent with the stationary phase, As the different constituents
by mass pass through the detector, they give signals
Solid support Chromosorb WHP corresponding to the amount of particular constituents
100-120 mesh having the column. The detection signals on
Carrier Gas Nitrogen transmission to the recorder, plots the chart. From the
Flow rate 30 ml/min specific area under various peaks corresponding to
Conditions specific constituents the quantities of different
Column temperature isothermal 150”C constituents are determined.
Injection port temperature 230”C
A-4 CALCULATION
Detector
Type FID Peak areas are calculated either by the most commonly
Temperature 250°C used triangular method or automated integration. When
an electronic integrator is used, concentrations of the
A-3 PROCEDURE constituents on the basis of the peak areas on
Conduct the flow of the carrier gas and inject the sample chromatogram are automatically calculated and
presented as a print out. For specific constituents,
!)F~~efatty acid pllw,e (FFAP)is carbowax 20 M treated with internal standard method is employed for higher
nitrophthal ic acid. accuracy.

ANNEX B
[Table 1, S1No. (vi)]
TEST FOR FREEDOM FROM HALOGENS

B-1 GENERAL B-4 PROCEDURE

B-1.l Outline of the Method B-4.1 Mix 100 mg of the material accurately weighed
with 200 mg of sodium peroxide in a clean, dry, hard
The material is fused with sodium peroxide. The residue
glass test-tube. Suspend the tube at an angle of about
is dissolved in nitric acid and treated with standard
45” by means of a chimp placed at the upper end and
silver nitrate solution. The turbidity produced is
gently heat the tube, starting at the upper end gradually
compared with a standard blank in which definite
quantity of hydrochloric acid is precipated with silver bringing the best towards the lower part of the tube
nitrate solution. until fusion is complete. Dissolve the residue in 25 ml
of warm water, acidify with dilute nitric acid and filter
B-2 APPARATUS the solution into a Nessler tube. Wash the test tube and
B-2.1 Test ‘hbe, of hard glass and of about 25 mm filter using two portions of 10 ml each of hot water,
internal diameter and 20 cm in length. adding the washing to the filtered solution. To the
filtrate add 0.5 ml of silver nitrate solution, dilute with
B-2.2 Nessler Cylinders, two, 50 ml capacity, water to 50 ml, mix thoroughly and compare the
B-3 REAGENTS turbidity with control tube.

B-3.1 Sodium Peroxide B-4.1.1 The material shall be deemed to have passed
the test if the turbidity produced in the testis not greater
B-3.2 Silver Nitrate Solution — 0.1 N. than that produced in a control test with the same
B-3.3 Standard Hydrochloric Acid — 0.2 N (see quantities of the reagents and 0.05 ml of 0.02 N
IS 265). hydrochloric acid.

GMGIPN—111 BIS/ND/07—300
Bureau of Indian Standards

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harmonious development of the activities of standardization, marking and quality certification of goods
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Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed
periodically; a standard along with amendments is reaffkmed when such review indicates that no changes are
needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards
should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of
‘BIS Catalogue’ and ‘Standards : Monthly Additions’.

This Indian Standard has been developed from Doc : No. PCD 18 (2322).

Amendments Issued Since Publication

Amend No, Date of Issue Text Affected

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