DEAS 187: 2017  
ICS 71.100.70  
 
© EAC 2017                                                                                                                              2ndEdition  2017   
 DRAFT EAST AFRICAN STANDARD  
Toothpaste  — Specification  
EAST AFRICAN COMMUNITY  DEAS 187: 2017  
ii © EAC  2017  – All right s reserved  
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Violators may be prosecuted . DEAS 187: 2017  
© EAC 2017  – All rights reserved  iii 
 Contents  Page 
Foreword  ................................ ................................ ................................ ................................ .............................  v 
1 Scope  ................................ ................................ ................................ ................................ ......................  1 
2 Normative references  ................................ ................................ ................................ ............................  1 
3 Terms and definitions  ................................ ................................ ................................ ...........................  1 
4 Requirements for toothpaste  ................................ ................................ ................................ ...............  2 
4.1 Composition  ................................ ................................ ................................ ................................ ...........  2 
4.2 Consistency  ................................ ................................ ................................ ................................ ...........  2 
4.3 Homogeneity  ................................ ................................ ................................ ................................ ..........  2 
4.4 Toxicity  ................................ ................................ ................................ ................................ ...................  2 
4.5 Stability  ................................ ................................ ................................ ................................ ...................  2 
4.6 Effect of container  ................................ ................................ ................................ ................................ . 3 
4.7 Fluorine derivatives  ................................ ................................ ................................ ...............................  3 
4.8 Other requirements  ................................ ................................ ................................ ...............................  4 
4.9 Microbiological requirements  ................................ ................................ ................................ ..............  4 
5 Prohibition or restrictions on clinical claims  ................................ ................................ .....................  4 
6 Sampling, testing and compliance with the standard.  ................................ ................................ ...... 4 
6.1 Sampling  ................................ ................................ ................................ ................................ .......................  4 
6.2 Testing  ................................ ................................ ................................ ................................ ....................  5 
7 Packing and labelling requirements  ................................ ................................ ................................ .... 5 
7.1 Packing  ................................ ................................ ................................ ................................ ...................  5 
7.2 Labelling  ................................ ................................ ................................ ................................ .................  5 
Annex  A (normative)  Determination of lead content  ................................ ................................ .....................  6 
A.1 Principle  ................................ ................................ ................................ ................................ .................  6 
A.2 Apparatus  ................................ ................................ ................................ ................................ ...............  6 
A.3 Reagents  ................................ ................................ ................................ ................................ ................  6 
A.3.1  Concentrated nitric acid  ................................ ................................ ................................ .......................  6 
A.3.2  Hydrofluoric acid - 40% (m/m)  ................................ ................................ ................................ ..............  6 
A.3.3  Citric acid  ................................ ................................ ................................ ................................ ...............  6 
A.3.4  Bromophenol blue indicator  ................................ ................................ ................................ ................  6 
A.3.5  Coppersulphate  ................................ ................................ ................................ ................................ ..... 6 
A.3.6  Hydrogen sulphide gas from Kipp's apparatus  ................................ ................................ .................  6 
A.3.7  Dilute nitric acid - approximately one per cent  ................................ ................................ ..................  6 
A.3.8  Ammonium hydroxide ................................ ................................ ................................ ...........................  6 
A.3.9  Thymol blue  indicator  ................................ ................................ ................................ ...........................  6 
A.3.10  Potassium cyanide solution -10% (m / v).  ................................ ................................ ............................  6 
A.3.11  Hydrogen sulphide solution.  ................................ ................................ ................................ ................  6 
A.3.12  Standard lead solution  ................................ ................................ ................................ ..........................  6 
A.4 Procedure  ................................ ................................ ................................ ................................ ...............  7 
A.4.1  preparation of sample  ................................ ................................ ................................ ...........................  7 
A.4.2  Method I  ................................ ................................ ................................ ................................ ..................  7 
A.4.3  Alternative method of test for lead contents  ................................ ................................ ......................  7 
Annex B  (normative )  Determination of pH  ................................ ................................ ................................ .. 10 
B.1 Apparatus  ................................ ................................ ................................ ................................ .............  10 
B.1.1  Analytical balance  ................................ ................................ ................................ ...............................  10 
B.1.2  pH meter with appropriate glass/calomel electrode assembly  ................................ ......................  10 
B.1.3  Stirrer  ................................ ................................ ................................ ................................ ....................  10 
B.2 Procedure  ................................ ................................ ................................ ................................ .............  10 
B.3 Expression of results  ................................ ................................ ................................ ................................  10 DEAS 187: 2017  
iv © EAC  2017  – All right s reserved  
 Annex C  (normative)  Test for stability  ................................ ................................ ................................ .........  11 
C.1 Apparatus  ................................ ................................ ................................ ................................ ............  11 
C.2 Procedure  ................................ ................................ ................................ ................................ ............  11 
C.3 Expression of results  ................................ ................................ ................................ .........................  11 
Annex D  (normative)  Determination of corrosion of the container  ................................ ..........................  12 
D.1 Procedure  ................................ ................................ ................................ ................................ ............  12 
D.2 Expression of result  ................................ ................................ ................................ ...........................  12 
Annex E (normative)  Determination of extrusion  ................................ ................................ ........................  13 
E.1 Procedure  ................................ ................................ ................................ ................................ ............  13 
E.2 Calcul ation and expression of results  ................................ ................................ ..............................  13 
Annex F (normative)  Determination of fluoride content  ................................ ................................ .............  14 
F.1 Principle  ................................ ................................ ................................ ................................ ...............  14 
F.2 Reagents  ................................ ................................ ................................ ................................ ..............  14 
F.2.1  Hydrochloric acid, concentrated.  ................................ ................................ ................................ ...... 14 
F.2.2  n-Pentane solution  in toluene (soln A).  ................................ ................................ ............................  14 
F.2.3  Standard fluoride solution (soln B).  ................................ ................................ ................................ .. 14 
F.2.4  Trimethylchlorosilane.  ................................ ................................ ................................ .......................  14 
F.3 Apparatus  ................................ ................................ ................................ ................................ ............  14 
F.3.1  Gas chromatograph  ................................ ................................ ................................ ............................  14 
F.3.2  Centrifuge  ................................ ................................ ................................ ................................ ............  15 
F.3.3  Microsyringe , 1μl ................................ ................................ ................................ ................................  15 
F.4 Determination of response factor of the apparatus  ................................ ................................ ........  15 
F.5 Procedure  ................................ ................................ ................................ ................................ ............  15 
F.5.1  For soluble fluoride  ................................ ................................ ................................ ............................  15 
F.5.2  For total fluoride  ................................ ................................ ................................ ................................ . 15 
F.5.2.3  Expression of result  ................................ ................................ ................................ ...........................  16 
Annex G (normative)  Determination of fineness  ................................ ................................ .........................  17 
G.1 Procedure  ................................ ................................ ................................ ................................ ............  17 
G.1.1  Equipment  ................................ ................................ ................................ ................................ ...........  17 
G.1.2  Determination  ................................ ................................ ................................ ................................ ...... 17 
G.1.3  Calculation  ................................ ................................ ................................ ................................ ...........  17 
G.2 Procedure II  ................................ ................................ ................................ ................................ .........  17 
G.2.1  Equipment  ................................ ................................ ................................ ................................ ...........  17 
G.2.2  Determination  ................................ ................................ ................................ ................................ ...... 17 
G.2.3  Calculation  ................................ ................................ ................................ ................................ ...........  17 
Annex  H (normative)  Determination of arsenic  ................................ ................................ ...........................  18 
H.1 modified Gutzeit method  ................................ ................................ ................................ ....................  18 
H.1.1  Outline of the method  ................................ ................................ ................................ .........................  18 
H.1.2  Reagents  ................................ ................................ ................................ ................................ ..............  18 
H.1.3  Procedure  ................................ ................................ ................................ ................................ ............  18 
Annex I (normative)  Sampling  ................................ ................................ ................................ .......................  19 
I.1 General requirements of sampling  ................................ ................................ ................................ ... 19 
I.2 Sampling of packages  ................................ ................................ ................................ ........................  19 
Bibliography  ................................ ................................ ................................ ................................ .....................  21 
 DEAS 187: 2017  
© EAC 2017  – All rights reserved  v 
 Foreword  
Development of the East African Standards has been necessitated by the need for harmonizing requirements 
governing quality of products and ser vices in the East African Community. It is envisaged that through 
harmonized standardization, trade barriers that are encountered when goods and services are exchanged 
within the Community will be removed.  
The Community has established an East African Sta ndards Committee (EASC) mandated to develop and 
issue East African Standards (EAS). The Committee is composed of representatives of the National 
Standards Bodies in Partner States, together with the representatives from the public and private sector 
organi zations in the community.  
East African Standards are developed through Technical Committees that are representative of key 
stakeholders including government, academia, consumer groups, private sector and other interested parties. 
Draft East African Standa rds are circulated to stakeholders through the National Standards Bodies in the 
Partner States. The comments received are discussed and incorporated before finalization of standards, in 
accordance with the Principles and procedures for development of East African Standards. XXXXXX.  
East African Standards are subject to review, to keep pace with technological advances. Users of the East 
African Standards are therefore expected to ensure that they always have the latest versions of the standards 
they are impl ementing.  
The committee responsible for this document is Technical Committee EASC/TC 078, Healthcare and medical 
devices.  
Attention is drawn to the possibility that some of the elements of this document may be subject of patent 
rights. EAC shall not be he ld responsible for identifying any or all such patent rights.  
This second edition cancels and replaces the first edition (EAS 187:2000), which has been technically revised.  DEAS 187: 2017  
vi © EAC  2017  – All right s reserved  
 Introduction  
The need for the development of an East African Standard on toothpast e has arisen from the fast expanding 
toothpaste industry within the region. Toothpaste assists in the removal of daily accumulation of debris and 
deposits from the exposed surface of the teeth without causing injury to the teeth and mucous membrane of 
the mouth. In addition it may remove stain and odour but it shall not remove enamel of the teeth.  
 EAST AFRICAN STANDARD  DEAS 187: 2017  
 
© EAC 2017  – All rights reserved  1 
 Toothpaste — Specification  
1 Scope  
This Draft East African Standard specifies the requirements , sampling and test methods  for toothpaste 
(fluoridated and non -fluoridated) for use with a tooth brush in the cleaning of natural teeth . 
2 Normative references  
The following documents are referred to in the text in such a way that some or all of their content constitutes 
requirements of this document.  For dated referen ces, only the edition cited applies. For undated references, 
the latest edition of the referenced document (including any amendments) applies.  
EAS 377, Cosmetics and cosmetic products  
ISO 4833, Microbiology of the food chain -- Horizontal method for the en umeration of microorganisms  
ISO 6634 , Fruits, vegetables and derived products -- Determination of arsenic content -- Silver 
diethyldithiocarbamate spectrophotometric method  
ISO 6579 -1, Microbiology of the food chain -- Horizontal method for the detection, enumeration and serotyping 
of Salmonella -- Part 1: Detection of Salmonella spp  
ISO 21150 , Cosmetics -- Microbiology -- Detection of Escherichia coli  
3 Terms and definitions  
For the purposes of this document, the following terms and definitions apply.  ISO and IEC maintain 
terminological databases for use in standardization at the following addresses:  — ISO Online browsing 
platform: available at http://www.iso.org/obp  
3.1  
bulk pack  
A pack containing two or more produc t units of the same nominal volume  
3.2  
defective  
A product unit that fails to meet one or more of the requirements as set out in 4 and 7 . 
3.3  
dentine  
The calcified tissue, tubular in structure that forms the bulk of a tooth . 
3.4 
dentifrice  
any substance or combination of substances specially prepared for the public for hygiene of the accessible  
surfaces of teeth and surrounding tissues  DEAS 187: 2017  
2 © EAC  2017  – All right s reserved  
 3.5  
enamel  
highly calcified tissue, prismatic in structure that covers the crown of a tooth . 
3.6  
lot 
Collection of prod uct units of the same size, type and style which have been manufactured under essentially 
the same conditions  
3.7  
product unit  
One unit of the final product consisting of the closed tube filled with toothpaste. The tube may be contained in 
a box (usually carton). . 
3.8  
toothpaste  
any semi -solid dentifrice preparation presented in the form of a paste, cream or gel  
3.9 
toothbrush  
device, with the working end of which carries filaments primarily for cleaning surfaces within the oral cavity  
4 Requirements for toothpaste  
4.1 Composition  
4.1.1  The toothpaste shall not contain sucrose or other readily fermentable carbohydrates. Artificial 
sweeteners, if used, shall comply with the specifications given by FOA/WHO Joint expert committee of food 
additives.  
4.1.2  Colouring matter, if used, shall comply with the requirements of EAS 377 -3: 
4.1.3  All ingredients shall be of acceptable quality and shall meet the requirements of the EAS 377.  
4.2 Consistency  
The toothpaste shall be smooth and free from lumps or particles, w hich are palpable in the mouth as separate 
or discrete particles.  
4.3 Homogeneity  
The paste shall extrude from the tube at 27°C ± 2 °C in the form of a homogeneous mass with the application 
of normal force starting from one end of the tube.  
4.4 Toxicity  
4.4.1 The toothpaste shall not contain ingredients in sufficient concentration to cause a toxic or irritant 
reaction when used in the oral cavity, nor shall it be otherwise harmful in normal use.  
4.5 Stability  
The toothpaste shall not ferment, segregate or o therwise deteriorate, during normal conditions of storage and 
use. When tested in accordance with annex C, the fore mentioned defects shall not occur.  DEAS 187: 2017  
© EAC 2017  – All rights reserved  3 
 4.6 Effect of container  
4.6.1 Tooth paste shall be packed in suitable tubes of material which shall not c orrode, deteriorate, or 
cause contamination of the tooth paste during normal conditions of storage and use. The paste shall be 
examined visually by extruding part of the contents. The internal surface of the tube when examined in 
accordance with Annex D sh all show no visible signs of corrosion or deterioration and the toothpaste shall 
show no sign of contamination.  
4.6.2 The lead content of the paints on the tube shall not exceed 250 mg/kg, when tested in accordance 
with Annex A.  
4.6.3 The toothpaste shall extrude to the extent of 94 % of the nominal volume, when tested in accordance 
with Annex E.  
4.7 Fluorine derivatives  
The total fluorine derivative and water -soluble fluorine derivative in fluoridated toothpaste (both determined as 
fluoride ion) shall comp ly with the requirements given in Table 1. The values given in the table are considered 
acceptable for toothpaste formulated to contain 1000 mg/kg expressed as fluoride ion. Fluoridated Toothpaste 
for children, shall be formulated to contain 500 mg/Kg of f luoride expressed as fluoride ion  
NOTE — The therapeutic effectiveness of a fluoride toothpaste may be influenced by the combination of fluorine 
containing  additive, abrasive agent and other constituents in toothpaste. Combinations additional to those in t he table are 
acceptable  provided that the product complies with all requirements of this standard with specific reference to clause 
4.Table 1 — Total and water soluble fluorine derivatives  
Predominant abrasive agent in toothpaste  Permitted range of total f luorine derivatives as fluoride 
ion, mg/kg  
Fluoride agent: Stannous fluoride  
Insoluble sodium metaphosphate  
Silica Calcium pyrophosphate   
Childrena: 600 to 800  
Adults: 900 to 1 500 
Fluoride agent: Sodium  
Monofluorophosphate  
Alumina  
Calcium carbonate  
Dical cium phosphate  
Insoluble sodium  
metaphosphate  
Silica   
) 
) Children: 600 to 800  
 
)Adults 90 0 to 1 500 
) 
) 
Fluoride agent: Sodium fluoride  
High betaphase calcium  
Pyrophosphate  
Polymethacrylate spheres   
) 
) Children: 600 to 800  
 
)Adults 90 0 to 1 500 
) 
) 
a Children shall imply ages 3 to 6 years  
 
For non -fluoridated toothpaste, Table 1 shall not apply.  DEAS 187: 2017  
4 © EAC  2017  – All right s reserved  
 Toothpaste with the fluoride level up to 50 mg/kg shall be regarded as non -fluoridated toothpaste.  
Test methods specified in Annex F are suitable for sodium mono fluorophosphate formulations. If formulations 
involving other fluoride agents are used, then the test methods have to be approved by the respective partner 
states National Standards Bodies.  
4.8 Other requirements  
The toothpaste shall also comply with requi rements given in Table 2.  
Table 2 — Requirements for tooth paste  
S/N  Characteristic  Requirements  Method of test  
1 Lead (Pb) mg/kg, max  0.5 Annex A  
2 pH 5.5 to 10.5  Annex B  
3 Fineness   
0.1  
Annex G  Particles retained on a 150 micron  
sieve, per cent b y mass, max  
Particles retained on a 75 micron  
sieve, per cent by mass, max  2.0 
 Arsenic (As2O3) mg/kg, max  2 Annex H  
4.9 Microbiological requirements  
The toothpaste shall also comply with requirements given in Table 3 
Table 3 — Microbiological requi rements for toothpaste  
Characteristic  Requirements  Method of test  
Total aerobic bacteria, per gram, max.  100 ISO 4833  
Salmonellae per 25 g  Absent  ISO 6579 -1 
Escherichia coli per 1g grams  Absent  ISO 21150  
5 Prohibition or restrictions on clinical claims  
The toothpaste shall not be claimed to control the amount of dental plaque, remove calculus, reduce dentine 
hypersensitivity, reduce the incidence of or treat caries or periodontal disease or any other oral diseases, 
unless such benefits have been clearly  demonstrated by clinical trials or other  scientific evidence that are 
acceptable to the respective partner states National Standards Bodies.  
6 Sampling, testing and compliance with the standard . 
6.1 Sampling  
Sampling shall be done in accordance with annex  I DEAS 187: 2017  
© EAC 2017  – All rights reserved  5 
 6.2 Testing  
6.2.1  The toothpaste recovered from the extrusion test shall be well -mixed into a composite sample that will 
be used for all relevant tests on toothpaste.  
6.2.2  A suitable number of empty tubes shall be taken from the sample to test for lead  in paint.  
7 Packing and labelling requirements  
7.1 Packing  
7.1.1  Toothpaste shall be packaged in containers that shall neither show defects nor contaminate the 
toothpaste during the normal shelf life of the product.  
7.1.2  The containers shall be further p acked in individual carton boxes or other protective materials.  
7.2 Labelling  
The immediate container (i.e. tube) and outer container shall  be legibly and indelibly marked with the following 
information:  
a) name of the toothpaste or registered trade mark;  
b) the name, in chemical nomenclature, of any ingredient for which special therapeutic properties are  
claimed, together with the concentration present in the toothpaste;  
c) nominal volume of contents or weight of contents;  
d) code number or batch number;  
e) name and addr ess of manufacturer;  
f) date of manufacturer;  
g) country of manufacture;  
h) in the case of fluoridated toothpaste, the words "FLUORIDE TOOTHPASTE" shall be given in ; 
i) expiry date ; and  
j) safety notice regarding the use by children below six years of age.  DEAS 187: 2017  
6 © EAC  2017  – All right s reserved  
 Annex  A 
(normative)  
 
Determination of lead content  
A.1 Principle  
The material is brought into solution. The brown colour produced with aqueous hydrogen sulphide solution i s 
matched with that produced with a standard lead solution.  
A.2 Apparatus  
Nessler tubes -100 ml capacity  
A.3 Reagents  
A.3.1  Concentrated nitric acid  
A.3.2  Hydrofluoric acid - 40% (m/m)  
A.3.3  Citric acid  
A.3.4  Bromophenol blue indicator  
Dissolve 0.1 g of br omophenol blue in 100 ml of rectified spirit . 
A.3.5  Coppersulphate  
A.3.6  Hydrogen sulphide gas from Kipp's apparatus  
A.3.7  Dilute nitric acid - approximately one per cent  
A.3.8  Ammonium hydroxide  
Dilute one volume of liquor ammonia (sp. gr. 0.92) with 10 v olumes of water . 
A.3.9  Thymol blue indicator  
Dissolve 0.1 g of thymol blue in 100 ml of rectified spirit.  
A.3.10  Potassium cyanide solution -10% (m / v).  
A.3.11  Hydrogen sulphide solution.  
Freshly prepared, saturated solution.  
A.3.12  Standard lead solution  
Dissolve 1.600 g of lead nitrate in water and make up the solution to exactly 1 000 ml. Transfer 10 ml of the 
solution by means of a pippete into a 1000 ml flask and dilute to the mark. One millitre of the final solution 
contains 0.01 mg of lead (Pb). The solution should be freshly prepared.  DEAS 187: 2017  
© EAC 2017  – All rights reserved  7 
 A.4 Procedure  
A.4.1  preparation of sample  
A.4.1.1  Accurately weigh 2.000 g of the toothpaste, in a platinum dish and incinerate for about 2 h at 525 
°C to 550 °C. Cool, then add 10 ml of concentrated nitric acid and hea t on a steam bath for 2 h.  
A.4.1.2  Evaporate off the nitric acid as far as possible, then add 5 ml of water and evaporate to dryness.  
A.4.1.3  Take the residue to fumes on a hot plate with three successive portions of hydrofluoric acid. Cool 
and dilute wit h water.  
A.4.1.4  Filter the solution, if necessary, with suction through a fine fritted glass filter and dilute the filtrate 
and washings to 200ml in a graduated flask. This solution shall be used in the test in A.4.2 and H.3.  
A.4.2  Method I  
A.4.2 .1 Take in a beaker 100 ml of the solution prepared in A.4.1. Add 10 g of citric acid and adjust  to pH 
3.0 to 3.4 by adding ammonium hydroxide (to give a yellow purple colour with bromophonol  blue indicator).  
A.4.2.2  Add about 10 mg of copper sulphate to act a co -precipitant. Precipitate sulphides by  passing 
hydrogen sulphide until solution is saturated.  
A.4.2.3  Dissolve the sulphides, without previous  washing, with 5 ml of hot dilute nitric acid, drawing 
solution through filter into the original flask; wash  with hot water and collect the washing along with the 
solution in nitric acid.  
A.4.2.4  Boil to remove sulphureted  hydrogen. Add 5 g of citric acid previously dissolved in water, make 
ammoniacal to pH between 8.5  and 10 (bluish) green to blue towards drop of t hymol blue indicator) and add 5 
ml of potassium  cyanide solution.  
A.4.2.5  Transfer to a Nessler tube, add 10 ml of hydrogen sulphide solution, dilute to the  mark and shake. 
Carry out a control test using 2 ml of standard lead solution and the same quantit ies of other reagents as used 
in test with the material.  
A.4.2.6  The toothpaste shall be taken as not having exceeded the limit  prescribed if the intensity of colour 
produced in the test with the material is not greater than that produced in the control te st. 
A.4.3  Alternative method of test for lead contents  
A.4.3.1  Principle  
Lead in toothpaste is extracted with acid after low temperature ashing. The ammonium pyrrolidine 
dithiocarbamete (APDC) complex is formed, extracted into 4 - methylpentan -2-one and th e lead is determined 
by atomic absorption spectroscopy.  
A.4.3.2  Precautions  
All apparatus and reagents shall be lead free. Avoid contamination, particularly from atmospheric dust. To avoid 
volatilization of lead it is essential that ashing be carried out a t a low temperature 450°C is recommended, 500 °C 
maximum.  
A.4.3.3  Apparatus  
The following apparatus is required:  
A.4.3.3.1  Beakers - 100 ml capacity, borosilicate glass or silica evaporating dishes.  DEAS 187: 2017  
8 © EAC  2017  – All right s reserved  
 A.4.3.3.2  Flasks - conical, I 00 ml capacity.  
A.4.3.3.3  Funnels - separating 100 ml capacity.  
A.4.3.3.4  Muffle furnace  
A.4.3.3.5  Atomic absorption spectrophotometer and lead hollow cathode lamp  
A.4.3.3.6  Pipette - Pasteur type  
A.4.3.3.7  Pipette 10 mI  
A.4.3.4  Reagents  
The following reagents shall be used and all shall be of recognized analytical reagent quality.  
A.4.3.4.1  Acetone  
A.4.3.4.2  Ethanol  
A.4.3.4.3  4-methylpentan -2-one (isobutyl methyl ketone)  
A.4.3.4.4  Nitric acid - concentrated  
A.4.3.4.5  Nitric acid - 5M 
A.4.3.4.6  Ammonia solution - 5M solution is recom mended but a more dilute solution may be used 
if preferred  
A.4.3.4.7  APDC one percent solution - Wash about 1. 5 g of ammonium pyrrolidine  
dithiocarbamate, (APDC) with 20 ml acetone in a P4 sintered glass crucible. Suck dry, weigh 1 g of the 
washed APDC an d dilute to 100 ml with water.  
A.4.3.4.8  Standard lead solution - (1 000 mg/kg lead)  
A.4.3.5  Procedure  
A.4.3.5.1  Destruction of organic matter  
A.4.3.5.1 .1 Accurately weigh about 2 g of the toothpaste into a 100ml beaker or a silica evaporating dish.  
A.4.3. 5.1.2  Slurry with 10 ml to 15 ml ethanol and evaporate to dryness on a water bath.  
A.4.3.5 .1.3 Place in muffle furnace at 100 °C. Slowly raise the temperature by 50 °C steps to 450 °C to 
avoid ignition. Complete ashing at 450 °C  
A.4.3.5.1.4  If the ash is d ark coloured, wet it with a few drops of concentrated nitric acid and reheat -in the 
furnace at, 450 °C for 30 s to 1h.  
A.4.3.5.2  Acid extraction of the ash  
A.4.3.5.2 .1 Add 5 ml water and 10 ml 5 M nitric acid to the cooled ash and boil gently for 5 min.  
A.4.3.5.2.2  Filter the solution into a 100ml conical flask rinsing with two 5 ml portions of water and 
retaining as much as possible of any insoluble matter in the beaker or dish.  DEAS 187: 2017  
© EAC 2017  – All rights reserved  9 
 A.4.3.5.2.3  Add 10 ml 5M nitric acid to the beaker or dish and boil gently for  5 min.  
A.4.3.5.2.4  Filter into the same conical flask rinsing with two 5 ml portions of water.  
A.4.3.5.3 Determination of lead  
A.4.3.5.3 .1 Adjust the pH value of the acid solution to 3 to 4 with the ammonia solution, transfer to a 
separating funnel and co ol to room temperature.  
NOTE  The effect of the pH value on extraction of lead is indicated in table A.1  
Table A.1 — The effect of the pH value on extraction of lead  
pH Peak height (mm)  
 
1 
2 
3 
4 
5 
6 
7 
8 0.5 g/ml 1.0g/ml 
55 
55 
72 
68 
66 
54 
44 
50 100 
122 
142 
136 
108 
115 
92 
90 
 
A.4.3.5.3 .2 Add 2 ml of APDC solution, mix and set aside for 5 min.  
A.4.3.5.3 .3 Add 10 ml of 4 methylpentan -2-one, measured accurately usin g pipette, and shake vigorously 
for 1 min.  
A.4.3.5.3 .4 Allow to separate, remove the clear or ganic layer with a Pasteur pipette.  
A.4.3.5.3 .5 Aspirate the organic layer into the atomic absorption spect rophotometer fitted with a lead 
hollow cathode lamp set at 283.3 N/m.  
A.4.3. 6 Calibration  
Submit aliquot portions of standard lead solution containin g, 0 to 20 μg Pb to the procedure in A.4.3.5.3 . 
Construct a new curve for each set of measurements.  
A.4.3.7 Calculation  
Relate the test result to the calibration curve and calculate, μg Pb/9 (mg/kg).  DEAS 187: 2017  
10 © EAC  2017  – All right s reserved  
 Annex B  
 
(normative )  
 
Determination of pH  
B.1 Apparatus  
B.1.1  Analytical balance  
B.1.2  pH meter with appropriate glass/calomel electrode assembly  
B.1.3  Stirrer  
B.2 Procedure  
B.2.1  Weigh 5.0 g ± 0.5 g of toothpaste into a 100 ml beaker. Slurry with 20 ml ± 0.1 ml of distilled water.  
B.2.2  Determine the pH valu e of the slurry at a temperature of 23 °C ± 2 °C using the glass/calomel 
electrode assembly, about 3 min after the commencement of slurrying.  
B.3 Expression of results  
Report the pH value of the toothpaste.  
 DEAS 187: 2017  
© EAC 2017  – All rights reserved  11 
 Annex C  
 
(normative)  
 
Test for stability  
C.1 Apparatus  
Oven  
C.2 Procedure  
C.2.1  Transfer a suitable quantity of the composite sample of the tooth paste into each of two glass test 
tubes and stopper them.  
C.2.2  Heat the two tubes for 72 hours in an oven maintained at 45 °C ± 1 °C. Allow to cool and exam ine 
the contents visually for homogeneity and for signs of fermentation or other deterioration or both.  
C.3 Expression of results  
Report the result as pass or fail  
 DEAS 187: 2017  
12 © EAC  2017  – All right s reserved  
 Annex D  
 
(normative)  
 
Determination of corrosion of the container  
D.1 Procedure  
D.1.1  Heat the tube of toothpaste at 45 °C ± 1 °C for ten days and then test as follows:  
D.1.2  Extrude a portion of the paste and examine it for visible contamination. Slit the tube, remove the paste 
and examine the surfaces of the tube for signs of corrosion, chemic al attack or other damage.  
D.1.3  Disregard surface staining by colouring agents in the toothpaste.  
D.2 Expression of result  
Report the result as pass or fail  
 DEAS 187: 2017  
© EAC 2017  – All rights reserved  13 
 Annex E  
(normative)  
 
Determination of extrusion  
E.1 Procedure  
E.1.1  Maintain the tube of toothpas te at 23 °C ± 2 °C for at least 2 hours and then test as follows: Remove 
the cap and invert the tube over a plastics beaker for which a tare has been recorded.  
E.1.2  Press -out the paste from the fold of the tube in the direction of the shoulder, holding th e tube between 
thumb and index finger of the left and right hand.  
E.1.3  When the tube is almost emptied, the mantle of the tube is to be pulled over an edge, removing the 
rest of the paste in the shoulder by nipping it off rectangular. The extrusion shall be carried out without the 
application of abnormal force.  
E.2 Calculation and expression of results  
E.2.1  Record the mass, m, of toothpaste extruded. Use a suitable method to determine the density of the 
toothpaste and hence calculate the volume of toothpa ste extruded.  
E.2.2  The extrusion, expressed as % (V/V) of the nominal volume, is given by the formula  
100 volumealminnom
 
Where  
m is the mass of toothpaste extruded;  
ρ is the density of the toothpaste  DEAS 187: 2017  
14 © EAC  2017  – All right s reserved  
 Annex F  
(normative)  
 
Determination of fluoride content  
F.1 Principle  
The fluorine derivative species in a sample of toothpaste (for total fluoride analysis) or in the aqueous extract of the 
toothpaste (for soluble fluorid e analysis) is allowed to react with trimethylchorosilane under acidic conditions to 
produce trimethylfluorosilane. This derivative is extracted into toluene containing n -pentane as internal standard.and 
the organic phase is analysed by gas chromatography.  
F.2 Reagents  
Use only analytical reagent grade and distilled or demineralized water.  
F.2.1  Hydrochloric acid, concentrated.  
F.2.2  n-Pentane solution in toluene (soln A).  
0.6 g of n -pentane made up to 1 litre with toluene.  
F.2.3  Standard fluoride solution (soln B).  
An aqueous solution of sodium fluoride containing 1.0 mg F/mL.  
F.2.4  Trimethylchlorosilane.  
F.3 Apparatus  
F.3.1  Gas chromatograph  
A suitable gas chromatograph equipped with a flame ionization detector, and having a column oflength about 
1.5 m and  nominal outside diameter 6 mm packed with 10%, methyl silicone (100%) on 80 -100 mesh flux 
calcined diatomite, acid washed.The recommended GC instrument conditions are as follows:  
Temperatures - Column 50 °C  
Injector 80 °C  
Detector 100 °C  
Carrier gas - Nitrogen, flow rate 20 ml/min  DEAS 187: 2017  
© EAC 2017  – All rights reserved  15 
 F.3.2  Centrifuge  
F.3.3  Microsyringe , 1μl 
F.4 Determination of response factor of the apparatus  
F.4.1  Pipette 1 ml of the fluoride solution into a 50 ml plastics flask. Using a measuring cylinder, add 8 ml of 
concentrated hydrochl oric acid, stopper the flask and mix the contents. Add from a burette 2.0 ml of the 
trimethylchlorosilane.  
F.4.2  Securely stopper the flask, mix well by shaking and allow to stand for 15 min to cool. Using a safety 
pipette, pipette 5 ml of the toluene solu tion of n -pentane into the flask and stopper. Mix thoroughly by shaking 
vigorously for 2 min.  
F.4.3  Transfer the contents of the flask to a centrifuge tube, stopper and centrifuge at 2500 r/min for 5 min. 
Inject 0.6 μl of the upper layer onto the column and allow the chromatogram to develop.  
F.4.4  Draw tangent base lines to the peaks of interest, and measure the heights of the trimethylfluorosilane 
and n -pentane peaks. ((Alternatively, determine the areas of the relev ant peaks).  
The response factor (k) is given by the formula  
B solutionofmlin fluorideof gramsA solutionofmlinetanPennof grams
etanPennof height Peaklorosaline trimethylfof height Peak
15 
 
F.5 Procedure  
F.5.1  For soluble fluoride  
F.5.1.1  Weigh accurately 5.0 ± 1.0 of toothpaste into a centrifuge tube. Add approximately 15 ml of water, 
slurry with a glass rod and centrifuge for 10 min. Decant the supernatant liquid into a 50 ml volumetric flask. 
Repeat this extraction process an additional two times and bring the volume of the supernatant liquid up to 50 
ml with water.  
F.5.1.2  Pipette 10 ml of the above solutio n into a plastics centrifuge tube. Add 8 ml of concentrated 
hydrochloric acid and immerse in a boiling water bath for I min and let stand for 10 min. Then coot under 
running water.  
F.5.1.3  Add 1 ml of trimethylehlorosilane, cap, mix and let stand for 15 m in. Pipette 5 ml of n -pentane 
solution into the tube, mix centrifuge and inject 0.6 μL of the upper layer.  
F.5.1.4  The mass of fluoride, in grams, is given by the formula  
kA solutionofmlinetanPennof grams
etanPennof height Peaklorosaline trimethylfof height Peak 5 
 
F.5.2  For total fluoride  
F.5.2.1  Weigh accurately 1.0 ± 0.1 g of toothpaste into a plastics  centrifuge tube. Add several glass 
beads and 8 ml of concentrated hydrochloric acid in parts. Cap and shake, pausing several times to release 
pressure.  
F.5.2.2  Add 8 ml of water, cap and mix. Immerse in a boiling water bath for 1 min. Mix and let stand f or 2 
min, then cool under running water.  DEAS 187: 2017  
16 © EAC  2017  – All right s reserved  
 F.5.2.3  Add I ml of trimethylchlorosilane, mix and let stand for 15 min. Pipette 5 ml of n -pentane solution 
into the tube, mix, centrifuge and inject 0. 5 µl of the upper layer.  
The mass of fluoride, in grams, is giv en by the formula  
B solutionofmlin fluorideof gramsA solutionofmlinetanPennof grams
etanPennof height Peaklorosaline trimethylfof height Peak
15 
 
F.5.2.3  Expression of result  
Report the results of total and soluble fluorine derivative of the sample tested as mg/kg of fluoride ion . DEAS 187: 2017  
© EAC 2017  – All rights reserved  17 
 Annex G  
(normative)  
 
Determination of fineness  
G.1 Procedure  
G.1.1  Equipment  
On 150 -micron sieve  
G.1.2  Determination  
D.1.2.1  Place about 10 g of the toothpaste, accurately weighed, in a 100 ml beaker. Add 50 ml of water 
and allow to stand for 30 min. with occasional stirring until the tooth -paste is completely dispersed.  
D1.2.3  Transfer to a 150 -micron sieve and wash by means of a slow stream of running tap water and 
finally with a fine stream from a wash bottle until all the matter that can pass through the sieve has passed.  
D.1.2.4  Let the water drain from the sieve and then dry t he sieve containing the residue in an oven. If 
there is any residue on the sieve, carefully transfer it to a tared watch glass and dry it to constant mass in an 
oven at 105 °C ± 2 °C.  
G.1.3  Calculation  
Material retained on 150 -micron  
% by mass = 
21100
MM  
Where  
M1 is the mass in g of residue retained on the sieve;  
M2 is the mass in g of the material taken for the test.  
G.2 Procedure II  
G.2.1  Equipment  
On 75 -micron sieve  
G.2.2  Determination  
Weigh accurately about 10 g of the toothpaste and pro ceed as in G.1.2, using a 75 -micron sieve. If there is any 
residue on the sieve carefully transfer it to a tared watch glass and dry it to constant mass in an oven at 105 °C ± 2 
°C. 
G.2.3  Calculation  
Calculate as in G.1.3 . 
 DEAS 187: 2017  
18 © EAC  2017  – All right s reserved  
 Annex  H 
(normative)  
 
Determination of arsenic  
H.1 modified Gutzeit method  
H.1.1  Outline of the method  
H.1.1 .1 The modified Gutzeit method of test of Arsenic shall be employed in cases where arsenic content is 
not needed and only a knowled ge of is desired. In cases where the actual arsenic content is to be determined, 
silver diethyldithiocarbamate method outlined in ISO  6634  shall be followed.  
H.1.1.2 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 a standard stain.  
H.1.2  Reagents  
H.1.2.1  Mixed acid  
Dilute one volume of concentrated sulphuric acid with four volumes of water, and add to this 10 g of sodium 
chloride for each 100 ml of the  solution.  
H.1.2.2 Ferric ammonium sulphate solution  
Dissolve 84 g of ferric ammonium sulphate in water containing 10 ml of mixed acid and make up to one litre.  
H.1.2.3  Concentrated hydrochloric acid  
H.1.2.4  Stannous chloride solution  
Dissolve 80 g of stan nous chloride (SnCl 2.2H 2O) in 100 ml of water containing 5 ml of concentrated 
hydrochloric acid.  
H.1.3  Procedure  
H.1.3.1  Place 2g of toothpaste sample accurately weighed in a platinum dish and incinerate for about  2 
hours at 525 °C to 550 °C. Cool and add 1 ml to 2 ml of  hydrochloric acid and 0.5 ml nitric acid and evaporate  to 
dryness on the steam bath.  
H.1.3.2  Dissolve the residue in  5 ml hot water, evaporate to dryness and treat it with  hydrofluoric acid. 
Evaporate again to dryness.  
H.1.3.3  Dilute  it with water (about 50 ml). Filter the solution, if  necessary, with suction through a fine 
fritted glass filter  and dilute the filtrate and washing to 100 ml in a  graduated flask.  
H.1.3.4 Carry out the test by adding into the Gutzeit bottle 2 ml of ferric ammoniu m sulphate solution, 0.5 ml 
of stannous chloride solution and 50 ml of the solution as prepared in A.4.1 . For comparison, prepare a stain 
using 0.001 mg of arsenic trioxide.  DEAS 187: 2017  
© EAC 2017  – All rights reserved  19 
 Annex I  
(normative)  
 
Sampling  
I.1 General requirements of sampling  
In drawing, pr eparing, storing and handling samples, the following precautions and directions shall be 
observed.  
I.1.1 Samples shall be taken in a protected place not exposed to damp air, dust or Soot.  
I.1 2 The sampling instrument shall be clean and dry.  
I.1.3 The s amples, the material being sampled, the sampling instrument and the containers for samples 
shall be protected from adventitious contamination.  
I.1.4 The samples shall be placed in clean and dry glass containers. The sample containers shall be of a 
size su ch that they are almost completely filled by the sample.  
I.1.5 Each container shall be sealed air -tight after filling and marked with full details of sampling, batch or 
code number, name of manufacturer, and other important particulars of the consignment.  
I.1.6 The samples shall be stored in such a. manner that the temperature of the material does not vary 
unduly from the normal temperature and they are protected from light.  
I.1.7 Sampling shall be done by a person agreed to between the purchaser and the supplier, and in the 
presence of the purchaser or his representative and the supplier or his representatives.  
I.2 Sampling of packages  
I.2.1 General - The sampling procedure for packages shall consist essentially in selecting and drawing, a 
sufficient num ber of unit packs.  
I.2.2 Lot - In a single consignment, all the packages containing toothpaste of the same type and form, 
representing the same batch of manufacture, shall constitute a lot. If the consignment consists of packages 
containing toothpaste of different types or forms or batches of manufacture, then the packages containing 
products of the same type, form and batch of manufacture shall be grouped together; each group shall 
constitute a separate lot.  
I.2.3  Scale of Sampling -For ascertaining the  conformity of a lot to the requirements prescribed in the 
specifications for individual toothpaste and toilet goods, tests shall be carried out on each lot separately. The 
number ( n ) of packages to be selected for drawing the samples shall depend on the  size ( N) of the lot in 
accordance with Table I.1. DEAS 187: 2017  
20 © EAC  2017  – All right s reserved  
 Table I.1 — Scale of sampling for packages  
No. of packages in the lot(N)  No. of packages to be selected,(n)  
Upto 3  Each container  
4 to 50  3 
51 to 150  4 
151 to 300  5 
301 to 500  6 
501 and above  7 
 
I.2.4 The packages shall be selected at random and to ensure randomness of selection, random number 
tables shall be used. In case such tables are not available, the following procedure may be adopted: ‘Starting 
from any package, count all the packages in on e order as 1,2,3 . . . . . . . . . up to r and so on, where r is the 
integral part of N/n.  Every rth package thus counted shall be withdrawn to give a sample for purposes of test ‘.  DEAS 187: 2017  
© EAC 2017  – All rights reserved  21 
 Bibliography  
[1] IS 6356:2001, Toothpaste — Specification (Third Revision)  
[2] ISO 11609:2017 , Dentistry -- Dentifrices -- Requirements, test methods and marking   
[3] PS: 1721, 2009, Specification for tooth paste (1st Revision)  
[4] SANS 1302:2008, Toothpaste  DEAS 187: 2017    
 
© EAC 2017  – All rights reserv ed