Analytical cosmetics:BIS specification and analytical methods for shampoo, skin-cream and toothpaste, Indian standards, Schedule S and Schedule Q, Drugs and cosmetic act, standards for heavy metals in cosmetics, standards for coloring agents in cosmetics, annexures, list of approved colours and dyes as per schedule Q Part 1, list of colours permitted to be used in soaps, types of toothpaste, general requirements for ECO mark and BIS mark, BIS certification marking
2. BIS-stands for Bureau of Indian Standards
The quality and safety by Central Drugs Standard
Control Organization (CDSCO) (Regulatory control
over the quality of drugs, cosmetics and medical
devices)
As per Drug and Cosmetics Act 1940 and rules
1945, cosmetic means ‘Any article intended to be
rubbed, poured, sprinkled or sprayed on, or
introduced into, or otherwise applied to the human
body or any part thereof for cleansing, beautifying,
promoting attractiveness or altering the
appearance, and includes any article intended for
use as a component of cosmetic’.
3. Cosmetic products in India are regulated under
the D & C act 1940 and rules 1945 and labelling
declaration by BIS.
BIS sets standards for cosmetics for the products
which are under Schedule S of Drugs and
Cosmetics rules 1945.
BIS is the national standards body of India
working under the aegis of Ministry of Consumer
Affairs, Food and Public Distribution, Government
of India.
4. According to IS 6608:200, if all the raw materials
requiring a test for heavy metals have been so tested
and comply with the requirements, then the
manufacturer may not test the finished cosmetic for
heavy metals and arsenic.
There should be a declaration for heavy metals and
hexachlorophene (anti-bacterial) content for
registration of cosmetic products.
The test report should include result of lead, arsenic,
mercury, other heavy metals and if any microbiological
test.
Undertaking from the manufacturer stating compliance
of all the materials/pigments used, heavy metals (with
the specified limits) and Hexachlorophene content in
products with BIS and D & C rules 1945.
5. While manufacturing skin creams and lipstick
if dyes colour (pigments like lakes) are used
then they shall comply with IS 4707 (Part I)
It should be according to Schedule Q (which
describes the list of dyes, colours and
pigments permitted to be used in cosmetics
and soaps) and CDSCO.
6. Schedule Q is divided into 2 parts:-
1. PART I:-It consists of the list of dyes,
colours and pigments permitted to be used
in cosmetics and soap as per amended by
the BIS from time to time.
2. PART II:-It consists of list of raw materials
not permitted and not safe to be used in
cosmetics
7. As per Schedule Q synthetic organic colours
and natural organic colours used in cosmetics
that are permitted for use shall not contain
more than-
-2 ppm of Arsenic (calculated as Arsenic
Trioxide)
-20 ppm of Lead (calculated as Lead)
-100 ppm of heavy metals other than Lead
8. Guinea green B
Tartrazine
Flaming red
Amaranth
Orange G
Deep red (Maroon)
Indigo
Eosin TS
Deep maroon (Fanchon Maroon)
Food yellow 18
Natural orange
Lake red D
Acid fast green
9. Phthalocyanine blue
Citrus red No. 2
Pigment yellow 3
Oil red no. 1/Solvent red 24/Oil red 3R
Aqueous green paste
Pigment orange 5
10. Other ingredients must comply with the provisions
of IS 4707 (Part II)
Rule 134 of D & C rules prohibited on the use of
cosmetics containing dyes, colours and pigments
other than those specified by the BIS (IS 4707 Part I
as amended) and Schedule Q
According to Rule 145 of D & C Rules, the use of
lead and arsenic compounds in cosmetics for the
purpose of colouring is prohibited.
The import of cosmetics in which a lead or arsenic
compound has been used for the colouring
purpose is not allowed under Rule 135.
Cosmetics containing mercury compounds are not
manufactured and imported under Rule 145 D and
135 D
11. IS 6356:2001. This standard prescribes the requirement and
the methods of sampling and test for toothpaste.
DENTIFRICE- It is any substance or combination of
substances specially prepared for the public for cleaning the
accessible surfaces of teeth.
TOOTHPASTE- It is defined as a dentifrice in the form of a
smooth, semi-solid, homogeneous mass containing
acceptable ingredients such as abrasives/polishing agents,
surfactants, humectants, binding agent and other
appropriate substances for oral health maintenance. The
product can be opaque, transparent or combination thereof,
colored or white, packed in a suitable container from which
it can be extruded in the form of a continuous mass.
12. TYPES:-Type 1-Non-fluoridated
Type 2-Fluoridated
SPECIFICATIONS
1.Composition:-The toothpaste shall not contain
mono or disaccharides, e.g. sucrose or other
readily fermentable carbohydrates. All the raw
materials used shall conform to respective IS
wherever they exist.
2.Dispensing:-The paste shall extrude from the
collapsible tube or any other suitable container in
which it is packed, at 27±2ºC in the form of
continuous mass with the application of normal
force, without the application of excessive force
which would cause injury to the tube or
container. It shall be possible to extrude the bulk
of contents from the tube or container from the
crimped end of the tube by rolling the tube
gradually.
13. 3.Stability:-The toothpaste shall not show any
physical sign of deterioration during normal
conditions of storage and use. When
subjected to a temperature of 45±2ºC for a
period of 28 days the toothpaste should meet
the requirements of the standard.
4.Packaging Material Inertness:-The collapsible
tube or any other suitable container used for
packaging should not corrode, deteriorate or
cause contamination of the toothpaste during
normal condition of storage and use. There
should be no sign of corrosion, chemical
attack or other damage.
14. 5.Acceptance test:-Toothpaste should comply
with the requirements given in Table 1, when
tested according to the methods given in
Annexure B to Annexure G.
6.Shelf Life:-It should be declared by he
manufacturer for all types of toothpaste.
Manufacturing date (month and year) should
be mentioned on tube and carton. The expiry
date or “Best before use” shall be mentioned
on the tube and carton. During the shelf life
the product will meet the requirement of the
standard.
15. 7.Additional requirements for the ECO-mark
(Optional)
(a)GENERAL REQUIREMENTS
The product shall conform to the
requirements for quality, safety and
performance prescribed under the general
requirements
All the ingredients that go into the
formulation of cosmetics shall comply with
the provisions of IS 4707 (Part 1 and 2). The
product shall meet other specific
requirements as given in the standard.
The product package shall display a list of
key ingredients in descending order of
quantity present.
16. The product should not be manufactured
from any carcinogenic ingredients.
The manufacturer should produce to BIS
environmental clearance from the concerned
state pollution control board as per the
provisions of the Water (Prevention and
Control of Pollution) Cess Act, 1977 and the
Air (Prevention and Control of Pollution) Act,
1981 along with the authorization, if required
under the Environment (Protection) Act, 1986
and the Rules made there under, while
applying for ECO-mark. Additionally,
provisions of the D & C Act, 1940 and the
rules there under shall be complied with.
17. (b)SPECIFIC REQUIREMENTS
Heavy metals like Lead and Arsenic shall not
exceed 20 and 2 ppm respectively when tested
by the respective method prescribed in IS.
8.Abrasivity (Type test):-The toothpaste shall not
exceed the limits of dentin abrasivity that of 2.5
times when tested as per the procedure given in
Annex H.
It may be noted that type test is recommended to
be done on the formulation only once to pass the
above criterion. This test need not be done for
each and every batch. However, this test is a
must if the abrasive system is changed in the
formulation. It is not required for the new
formulation as long as abrasive components are
not changed.
18. 9.PACKING AND MARKING:-
Packing:-Toothpaste shall be packed in
collapsible tube or in any other suitable
containers like sachets, pumps or other
suitable dispensing systems. When packed in
containers, the containers shall be properly
sealed and have a leak-proof cap or closure.
The containers, if necessary, may further be
packed in cartons or any other suitable
packaging material.
The material for product packaging shall
meet the parameters evolved under the
scheme of labelling environment friendly
packaging/packaging materials.
19. Marking:-The tubes and the cartons should be
legibly marked with the following information:-
Name and type of toothpaste
Name and address of the manufacturer
Net mass or volume of the material in the tube
Batch number, in code or otherwise
Month and year of manufacture
Fluoride ion content in ppm for Type 2
toothpaste
Expiry date or “Best use before…..”
Foaming/Non-foaming
List of key ingredients
*Note:-this is exempted in case of pack sizes of
30g/60 ml or less
20. 10.BIS certification marking:-
(a)The use of the standard mark is governed by the
provisions of the Bureau of Indian Standards Act,
1986. and the Rules and regulations made
thereunder. The details of the condition under
which the license for the use of the standard
mark may be granted to manufacturers or
producers may be obtained from the Bureau of
Indian Standards.
(b)If the product is covered under ECO-Mark
(optional), it shall be suitably marked with ECO-
Mark logo besides Standard mark. The label may
clearly specify that ECO-Mark is applicable to the
contents or the package or both, as the case may
be.
21. 11.Sampling:-
Representative test samples of the material
shall be drawn as prescribed in IS 3958.
Number of tests and criteria for conformity-
the tests for abrasivity, stabililty and
container’s inertness shall be type tests and
shall be performed for product approval
whereas tests for dispensing, fineness, pH,
heavy metals, arsenic, foaming power,
fluoride content and microbial counts shall be
carried out on each batch for acceptance of
the product.
22. 12.Quality of Reagent:-unless specified
otherwise, pure chemicals and distilled water
(IS 1070) shall be employed in tests.
*Note- ‘Pure chemicals’ mean chemicals that
do not contain impurities., which affect the
result of analysis.
23. S.NO. CHARACTERISTIC REQUIREMENT
FOR NON-
FLUORIDATED
REQUIREMENT
FOR
FLUORIDATED
METHOD OF
TEST,
ANNEXURE
1. Fineness
(a)Particles
retained on 150μ IS
sieve, % by mass,
Max
(b) Particles
retained on 75μ IS
sieve, % by mass,
Max
10
2.5
1
2.5
B
-
2. pH of aqueous
suspension
5.5-10.5 5.5-10.5 C
24. S.NO. CHARACTERISTIC REQUIREMENT
FOR NON-
FLUORIDATED
REQUIREMENT
FOR
FLUORIDATED
METHOD OF
TEST,
ANNEXURE
3. Heavy metals (Lead),
ppm, Max
20 20 D
4. Arsenic, ppm, Max 2 2 E
5. Foaming power, ml,
Min
50 50 F
6. Available fluoride ion,
ppm, Max
50 1000 G
7. Microbial counts
(a)Total viable counts
per gram, Max
(b)Gram negative
pathogens per gram,
Max
1000
Absent
1000
Absent
IS 14648
IS 14648
25. Raw materials used in the toothpaste
formulation fall into the following categories
1. Polishing agents
2. Surfactants
3. Humectant
4. Binding agent
5. Others as per IS 4707 (Part 1 and Part 2)
26. Squeeze the toothpaste and feel the presence
of the particles/agglomerates/granules.
Subject the toothpaste suspension to an
ultrasonic treatment and pass through
fineness test.
Ultrasonification loosens out the
agglomerates/granules into the constituent
materials.
28. The colour produced with thioacetamide
reagent in test solution is matched against
the obtained with standard Lead solution
ANNEXURE E (DETERMINATION OF ARSENIC)
29. Strict attention should be paid to all the
details of the procedure in order to ensure
concordant results
A suspension of the material in water is taken
in a graduated cylinder and it is shaked 12
times under prescribed conditions
The volume of the foam formed is observed
after keeping the cylinder for 5 minutes.
30. Water soluble species are converted to
fluoride ion by acid hydrolysis.
The fluoride ion activity is then determined
potentiometrically with the help of fluoride
ion sensitive electrode.
31. This annexure identifies the procedure for
determination of dentifrice abrasivity using the
RDA laboratory method.
RDA-Relative Dentin Abrasivity (it is a scale that
assigns the dentifrice a abrasivity value relative to
standard reference abrasive)
Abrasives include fluorides such as Sodium
Fluoride, Stannous Fluoride or carbonates such as
Calcium carbonate, Magnesium carbonate or
oxides such as Aluminium oxide
ANNEXURE J (LIST OF ADJUNCT INDIAN STANDARDS)
32. IS 7884:2004 (specification for surfactant based
shampoo)
S.NO. REQUIREMENTS DETAILS
1 Description Shampoo shall be in liquid, emulsion or a paste
form. It may be coloured and perfumed
2 Physical
characteristics
When visually examined it should be free from
any sediments. If it is in the form of any
emulsion, it should be stable. When it is in the
form of a paste, it should be free from
agglomerated particles
3 Ingredients Raw materials should conform to the
requirements prescribed in IS
33. S.NO. REQUIREMENTS DETAILS
3.1 Dyes It should comply with the provisions of IS
4707 (Part I), subject to the provision of
Schedule Q of the Drugs and Cosmetics act,
issued by Government of India
3.2 Other ingredients Shall comply with the provisions of IS 4707
(Part 2)
3.3 List of ingredients
used
conventionally in
formulation of
shampoo
Annexure A
3.4 Compliance with
Table 1 when
tested in
accordance with
the method
prescribed
34. 3.5. Additional requirements for ECO mark:-
3.5.1.The product shall conform to the requirements for
quality, safety and performance
3.5.2.All the ingredients that goes into the formulation of
cosmetics shall comply with the provisions of IS 4707 (Part I
and Part II)
3.5.3.The product package shall display a list of key
ingredients in descending order of the quantity present.
3.5.4.The product shall not be manufactured from any
carcinogenic ingredients
3.5.5.The manufacturer shall produce to BIS environmental
consent clearance from the concerned State Pollution
Control Board as per the provisions of the Water (Prevention
and Control of Pollution) Cess Act, 1977 and the Air
(Prevention and Control of Pollution) act, 1981 along with
authorization, if required under the Environment
(Protection) act, 1986 and the rules made there under shall
also comply with.
35. 3.6.Specific Requirements:-
3.6.1.Product shall be dermatologically safe when
tested as per IS 4011
3.6.2.Biodegradable agents wherever used in
cosmetic formulations shall be as per their limit
finalized for synthetic detergents for ECO mark by
the technical committee
3.6.3.Heavy metals calculated as Lead and Arsenic
shall not exceed 20 and 2 ppm respectively when
tested by the respective method prescribed in
relevant Indian standards.
3.6.4.The material for product packaging shall
meet the parameters evolved under the scheme of
labelling environment friendly
packaging/packaging materials.
36. 4.Packing and Marking:-
4.1.Shampoo shall be packed in glass or plastic
containers or any other suitable containers
4.2.The container shall be legibly marked with the
following information:
1. Name of the material
2. Manufacturer’s name and/or his recognized
trademark, if any;
3. Net content in volume for liquids and emulsions
and in mass for pastes
4. Month and year of manufacturing/packing
5. Batch or lot number in code or otherwise
6. ‘Best before use…’ (month and year to be
declared by the manufacturer)
37. 4.3.BIS Certification marking- the container may also be
marked with the standard mark.
4.3.1.The use of the standard mark is governed by the
provisions of BIS act, 1986 and the rules and
regulations made there under. The details of conditions
under which the license for the use of Standard mark
may be granted to manufacturers or producers may be
obtained from the BIS
4.3.2.If the product is covered under ECO mark
(optional), it shall be suitably marked with the ECO
mark logo besides the standard mark. The label may
clearly specify that ECO mark is applicable to the
contents or the package or both, as case may be. If the
product package or both, as case may be. If the
product package is not separately covered under ECO
mark scheme, it shall be clearly mentioned on the
product that ECO mark label is applicable to contents
only.
38. 5.SAMPLING
5.1.Representative samples of the material
shall be drawn as prescribed in IS 3958
5.2.Tests for all the requirements shall be
carried out on a composite sample
5.3.The shampoo shall be taken t have
conformed to this standard if the composite
sample passes all the tests.
39. 6.Quality of reagents
Unless specified otherwise, pure chemicals and
distilled water (see IS 1070) shall be employed
in tests.
‘Pure chemicals’ shall mean chemicals that
don’t contain impurities which affect the
results of analysis.
40. ANNEXURE A (List of raw materials used in the
formulation of surfactant based shampoo)
A.1.DETERGENTS
1. Sodium or potassium or ethanolamine salts of
lauryl sulphonic acid
2. Lauryl ether sulphates
3. Sulphated monoglycerides
4. Sodium alkyl sulpho-acetate
5. Alkyl benzene polyoxyethyl sulphonates
6. Sodium n-lauryl sarcosinate
7. Sodium alpha olefin sulphonates
8. Other synthetic detergents
41. A.2.FOAM STABILIZERS
1. Ethanolamides or isopropanolamides of
fatty acids
2. Amine oxides
3. Cocobetaines
4. Cocoamidopropyl betaines
A.3.CHELATING AGENTS
1. Sodium polyphosphates
2. Sodium salt of Ethylenediamine tetra acetic
acid (EDTA)
45. ANNEXURE B- (Determination of non-volatile alcohol
soluble matter)
B-1 GENERAL
This method determines the amount of non-volatile
alcohol matter in surfactant based shampoos.
B-2 REAGENTS
B-2.1 Ethyl alcohol-Neutral, conforming to IS 321
B-2.2 Methyl red indicator solution-Dissolve 0.1 g of
methyl red in 300 ml of ethyl alcohol and 200 ml
of water
B-2.3 Potassium chromate solution-10% solution
B-2.4 Nitric acid dilute-1:4 (w/v)
B-2.5 Silver nitrate solution-0.1 M
46. B-3 PROCEDURE
B-3.1
Weigh accurately about 10 g of the sample into a
150 ml beaker.
Evaporate on a steam-bath to almost complete
dryness. Digest with 50 ml of 96% ethanol by
heating on a steam bath for 2 min.
Filter the hot alcoholic solution through a sintered
glass filter funnel fitted to a Buchner flask to
which suction is applied.
Wash the beaker and the residue in the sintered
glass funnel 5 times with 30 ml portions of hot
ethanol.
47. B-3.2
Transfer the filtrate in the buchner flask to a
weighed wide mouthed flat-bottomed flask.
Evaporate nearly to dryness on a water bath and
drive off the remaining alcohol by directing a
gentle steam of dry air into the flask whilst
continuously rotating the latter in the water bath.
Heat the flask in an air over at a temperature of
105ºC until constant mass.
Calculate mass percent of residue obtained
Mass (% residue γ)=Mass of residue obtained ×100
Mass(g) of the material taken for test
48. B-3.3
Dissolve the residue in 50 ml of distilled water and
add to it 2 drops of methyl red indicator solution.
If the solution is yellow in colour, neutralize it by
adding dilute nitric acid drop by drop to get pink
colour.
Titrate the solution with AgNO3 solution using 2.5
ml of Potassium chromate solution as indicator, till
a brown colour is obtained.
Carry out a blank determination using the same
quantity of all reagents except the sample.
49. B-3.4 Calculate the chloride content in
shampoo in terms of molecular mass of NaCl
in % by formula:-
NaCl (in % X)= V×0.584
M
Where, V=Volume (in ml) of standard AgNO3
solution required for the material minus
volume (in ml), of standard AgNO3 solution
required for the blank.
M= Mass (in g) of the material taken for
test.
50. B-3.5 Calculation
To calculate % non-volatile alcohol soluble
matter, subtract the mass percent of NaCl as
determined in B-3.4 (X) from the mass
percent of the residue (Y) obtained in B-3.2.
% Non-volatile alcohol soluble matter=Y-X
51. ANNEXURE C (Determination of pH)
pH meter equipped with glass rod. Determination
of pH to be done at 27ºC
52. ANNEXURE D (Determination of foam height)
Requirement for shampoo that is surfactant
based:-
S.NO CHARACTERISTICS REQUIREMENT METHOD OF
TEST (REFER TO
ANNEXURE)
1. Non-volatile alcohol
soluble matter (% by mass)
10 B
2. pH 4-9 C
3. Foam height for 2 %
solution, Min
150 mm D
53. ANNEXURE E (Ideal properties of shampoo)
Ease of application
Rinsing
Easy wet combing
Manageability
Lustre
Fragrance
Low level of irritation
Well preserved
Good stability
Economical
54. IS 6608:2004 (Indian standards skin-cream
specification)
IS 4707 (Part 1 and Part 2)
REQUIREMENTS
(1)Description:-Skin cream shall be in the form of a
thick emulsion or unctuous mass (having
greasy/oily/soapy feel) with a pleasant odour. It
shall be white or pigmented or of uniform colour.
55. (2)Ingredients:-Unless specified otherwise, all the
raw materials used in the manufacture of skin
creams shall conform to the requirements
prescribed in the relevant Indian Standards where
such standards exist.
a) The dyes, colours (pigments, lakes etc.) if used in
the manufacture of skin creams shall comply with
IS 4707 (Part 1) subject to the provision of
Schedule Q of Drugs and Cosmetics Act, issued
by Government of India.
b) Other ingredients shall comply with the
provisions of IS 4707 (Part 2)
56. (3)The material shall also comply with the requirements
given in Table 1 when tested as prescribed in Table 1
Table 1:Requirements for skin-cream
S.NO. CHARACTERISTICS REQUIREMENT METHOD OF TEST
(REFER TO ANNEXURE)
1. Thermal stability To pass the test A
2. pH* 4-9 B
3. Total fatty substance
content (% by mass),
Min.
5 C
4. Total residue (% by
mass), Min.
10 D
5. Heavy metals** (as Pb),
ppm, Max.
20 E
6. Arsenic**,ppm, Max. 2 F
7. Microbial content/limit
(a)Total viable count
(b)Gram –ve pathogen
NMT 1000
Less than 10
IS 14648
IS 14648
57. *for creams based on beeswax and borax, pH shall
be between 5-10
**if all the raw materials requiring test for heavy
metals and arsenic have been so tested and comply
with the requirements, then the manufacture may
not test the finished cosmetic for heavy metals and
arsenic.
58. Requirements for quality, safety and performance prescribed
under this section
1. All the ingredients that go into formulation of cosmetics shall
comply with the provisions of IS 4707 (Part 1 and Part 2). The
product shall also meet specific requirements as given in the
standard
2. The product package shall display a list of key ingredients in
descending order of quantity present.
3. The product shall not be manufactured from any carcinogenic
ingredients.
4. The manufacturer shall produce to BIS environmental consent
clearance from the concerned State Pollution Control Board as
per the provisions of the Water (Prevention and Control of
Pollution) Cess Act, 1977 and the Air (Prevention and Control of
Pollution) act, 1981 along with authorization, if required under
the Environment (Protection) act, 1986 and the rules made
there under shall also comply with.
59. SPECIFIC REQUIREMENTS
1. Product shall be dermatologically safe when
tested as per IS 4011
2. Heavy metals calculated as Lead (Pb)-NMT 20
ppm and Arsenic 2 ppm, when tested by the
respective method prescribed in Indian
Standards.
60. PACKING AND MARKING
1. Packing:-Material should be packed in suitable well-
closed containers
2. Marking:- The container shall be legibly marked with
the following information:-
(a) Name of the material
(b)Manufacturer’s name and/or his recognized
trademark, if any;
(c)Net content
(d)Month and year of manufacturing/packing
(e)Batch or lot number in code or otherwise
(f)‘Best before use…’ (month and year to be declared by
the manufacturer)
(g)List of key ingredients and NOTE-This is exempted in
case of pack sizes of 30 g/60 ml or less
(h)Any other information required by statutory
authorities.
61. SAMPLING
1. Representative samples of the material shall be
drawn as prescribed in IS 3958
2. Tests for all the characteristic shall be carried out
on the composite samples as per methods
referred in table 1
3. The material shall be taken to have conformed to
the standard if the composite sample passes all
the tests.
62. QUALITY OF REAGENTS
1. Unless specified otherwise, pure chemicals
and distilled water (see IS 1070) shall be
employed in tests.
2. ‘Pure chemicals’ shall mean chemicals that
don’t contain impurities which affect the
results of analysis.
63. ANNEXURE A (Test for thermal stability)
A humidity chamber/incubator controlled at 60-
70% relative humidity and 45±1ºC.
The sample shall be taken to have passed the test,
if on removal from the incubator shows no oil
separation or any other phase separation
64. ANNEXURE B (Determination of pH)
A digital pH meter equipped with a glass
electrode can be used.
65. ANNEXURE C (Determination of total fatty
substance content)
The emulsion is broken with dilute mineral
acid and the fatty matter is extracted with
petroleum ether. It is weighed after removal
of the solvent.
66. ANNEXURE D (Determination of residue)
Weigh accurately about 5g of the material in a
weighed, clean and dry squat form weighing
bottle and dry to constant mass at 105±1ºC.
Cool in a desiccator and weigh.
67. ANNEXURE E (Test for heavy metals)
The colour produced with hydrogen sulphide
solution is matched against that obtained
with standard lead solution.
68. ANNEXURE F (Determination of Arsenic)
Arsenic present in a solution of the material is
reduced to arsine, which is made to react with
mercuric bromide paper. The stain produced
is compared with the standard stain.