ICS 71.100.40  
Y 43  
                                                         GB 
National Standard of the People’s Republic of China   
    GB8372 – 200x  
Replacing GB8372 -2001  
_______________________________________________________________  
 
 
Toothpaste  
 
(Draft  for Approval)  
 
 
 
 
 
 
 
 
 
 
 
 
 
Issue date: 200×-××-××                     Implementation date: 200 ×-××-×× 
____________________________________________________________________  
 
Issued  
by General Administration of Quality Supervision,  Inspection 
and Quarantine of The People’s Republic of China  
 Forward  
 
     The indicators of odour, paste squeeze pressure and foam volume set out in 
Table 4.2, packaging in Subsection 7.2, and transportation in Subsection 7.3 are 
recommendatory clauses. All other clauses are mand atory.  
     This Standard refers to the international Standard ISO11609: Dentistry –– 
Toothpastes –– Requirements, test methods and marking 1995 (E).  
     This Standard replaces GB8372 -2001, “Toothpaste”.  
Compared with GB 8372 -2001, the main changes to this  Standard are as 
follows:  
–– the scope of application of the Standard has been verified;  
     –– the terms and definitions have been increased;  
     –– it is specified that the raw materials used in the manufacture of toothpaste 
should meet “Requirements f or toothpaste - use raw materials”;  
     ––the requirements of the total number indices of mould and yeast have been 
increased;  
     –– it is specified that the micro -organism  index test should conform to the 
requirements of “ Hygienic Standard for Cosmetics ”; 
     –– requirements regarding foam volume index of children’s toothpaste have 
increased;  
     –– the pH index has been revised;  
     –– requirements regarding total fluorine volume index have been revised;  
–– requirements regarding soluble fluorine or free fluorine volume index have 
been revised;  
     –– requirements regarding the total fluorine volume index of children’s fluoride 
toothpaste have been revised;  
     –– requirements regarding soluble fluorine or free fluorine volume index of 
children’s fl uoride toothpaste have been revised;  
     –– it is specified that net contents should be finished according to the Order No 
75 [2005] of the General Administration of Quality Supervision,  Inspection and 
Quarantine, the People’s Republic of China , “Measurem ent, supervision and 
management methods of quantitative packed products”;  
     –– part of the marking, packaging and storage requirements has been revised.  
 
     Appendix A to this Standard is a standardised appendix.  
     This Standard was proposed by the  General Administration of Quality 
Supervision,  Inspection and Quarantine of the People’s Republic of China .      The organisation in charge of this Standard is the  National Toothpaste and Wax 
Products Standardisation Centre.  
     The main drafting unit fo r this Standard is the General Administration of 
Quality Supervision,  Inspection and  Testing of Toothpaste and Wax Product  Light 
Industry.  
     The main drafters of this Standard are: Sun Dongfang, Ma Xuan, Li Xianbo, 
Shen Erui, and Meng Yu.  
     Previous versions of this Standard to be replaced by this Standard are:  
     –– QB592 -81, GB8372 -87, GB8372 -1995, and GB8372 -2001.  
     As from the date of implementation, this Standard replaces the original national 
Standard GB8372 -2001 “Toothpaste”, implemented b y the  General Administration of 
Quality Supervision,  Inspection and Quarantine of the People’s Republic of China . Toothpaste  
 
1   Scope  
 
     This Standard sets the terms and definition, requirements, test methods, 
inspection rules, marking, packaging, tr ansportation and storage of toothpaste.  
     This Standard applies to different kinds of toothpaste for cleaning and caring 
for the mouth.  
 
2   Normative references  
 
     The provisions of the following documents become provisions of this Standard 
after be ing referenced. For dated reference documents, all later amendments 
(excluding corrigenda) and versions do not apply to this Standard; however, the 
parties to the agreement are encouraged to study whether the latest versions of these 
documents are applicab le. For undated reference documents, the latest version apply 
to this Standard.  
GB 7917.2  Standard methods of hygienic test for cosmetics Arsenic . 
GB 191  Packaging  –– Pictorial marking for handling of goods  (EQV ISO 780: 
1997).  
GB/T 601   Chemical reagent  –– Preparati ons of standard volumetric solutions . 
GB/T 602   Chemical reagent  –– Preparations of stock standard solutions  (NEQ ISO  
6353 -1: 1982).  
GB/T 603   Chemical reagent  –– Preparations of reagent solutions for use in test 
methods (NEQ ISO 6353 -1: 198 2). 
GB/T 6682  Water for analytical laboratory use  –– specification and test methods  
(NEQ ISO 3696: 1987).  
     GB/Z ×××× -200×  Requirements for toothpaste -use raw materials.  
     No 172 [1997] issued by the National  Quality and Technical Supervision  
Bureau,  “Provisions on indicating product identification .” 
     Order No 75 [2005] of the General Administration of Quality Supervision,  
Inspection and Quarantine, the People’s Republic of China , “Measurement, 
supervision and management methods of quantitative pa cked products.”  
     JJF1070 -2005   Measurement and inspection rules for net contents of 
quantitative packaged products.  
     “ Hygienic standard for cosmetics ,” 2007 Version issued by the Ministry of 
Health of t he People’s Republic of China .  
3   Terms and  definitions  
     This Standard adopts the following terms and definitions.  
3.1 
     Toothpaste  
     A substance in paste form mixed with and composed of friction agent, 
moisturiser, thickening agent, foaming agent, aromatics, water and other additives 
(including ingredients for improving the health conditions of the mouth).  
 
4   Requirements  
     The raw materials used for producing toothpaste should meet the 
“Requirements of toothpaste -use raw materials.”  
4.1   Hygiene indices  
     Hygiene indices should meet the requirements set out in Table 1.  
4.2  Sensory, physical and chemical indices  
     Sensory, physical and chemical indices should meet the requirements set out in 
Table 2.  
4.3   Net contents  
     The net contents of toothpaste should conform to Orde r No 75 [2005] of the 
General Administration of Quality Supervision,  Inspection and Quarantine of the 
People’s Republic of China , “Measurement, supervision and management methods for 
quantitative packaged products.”  
 
Table 1  
Item Requirement  
Total number of bacterial colony  (CFU/g)          500 
Total number of  mould and yeast (CFU/g)          100 
Faecal  coliform group / g  Nil 
Pseudomonas aeruginosa  / g Nil Micro -organis m 
Index  
Staphylococcus aureus  / g Nil 
Heavy metal (in Pb) content / (mg/kg)             15 Toxic substance 
limit  Arsenic (As) conte nt / (mg/kg)                   5 
Remarks:  The words set in bold characters are mandatory indices.  
 
Table 2  
Item Requirement  
Paste  Clean, even, tight, normal colour  Sensory 
Index  Odour  Meet the specified odour type  Thic kness / mm  9 ~ 33  
Paste squeeze pressure / kPa     40 
Foam volume / mm            
 60 
120 (applicable to children’s toothpaste)  
pH value  5.5 ~ 10.0  
Stability  The paste does not leak out of the tube,  
no liquid is separated from the paste,  
odour  and colour are normal.  
Excessively hard grain  No scratches are found on the glass.  
Total fluorine vol./%  0.05~0.15 (applicable to fluoride toothpaste)  
0.05~0.11 (applicable to children’s fluoride 
toothpaste)  Physical 
and 
Chemical 
Indices  
Soluble fluorine or free fluorine 
vol./%  0.05~0.15 (applicable to fluoride toothpaste)  
0.05~0.11 (applicable to children’s fluoride 
toothpaste)  
Remarks:  The words set in bold characters are mandatory indices.  
 
4.4   Requirements of packaging appearance  
4.4.1 Pliable tube or other packaging  
4.4.1.1 The tube body is clean -cut, neat, firmly welded, and undamaged. Images and 
words are printed clearly and completely. The colour process is accurate, without any 
obvious printing defects or ink loss;  
4.4.1.2 The cap is clean, neat, with even colour, a nd without fading. The cap and the 
thread at the tube mouth are tightly matched, but not loosened or stripped. The part of 
the easy -to-open cap that is lifted is firmly connected to the body of the cap, and 
tightly sealed up, without any disclosure of the paste;  
4.4.1.3 The tube end is firmly sealed without leakage;  
4.4.1.4 If there is a sealing film at the mouth, it is clean, complete, and can be torn off 
easily.  
4.4.2  Box (applicable to toothpaste packaged in small boxes)  
4.4.2.1 The surface of the box i s clean -cut, neat, with patterns printed clearly and with 
accurate colour process.  
4.4.2.2 The body of the box should be flat, has no cracks and no delaminating.  
 
5   Test methods  
     Unless otherwise specified, both the reagents and water used in this St andard 
are analytical reagents and water which meet the requirements set out in GB/T6682.  
     Unless otherwise specified, the standard solution for use in the analysis, the solution for impurity determination, the making agent and products for test method s 
should be prepared according to the requirements set out in GB/T601, GB/T602 and 
GB/T603.  
     Regarding the calculation of the index of the final test result according to the 
method of weighing, 20 mm of the paste should be firstly squeezed out and disc arded.  
After that, squeeze out the weighted volume as the sample.  
5.1  Micro -organism  index  
     Inspection should be carried out according to the methods set out in “ Hygienic 
Standard for Cosmetics .” 
5.2  Heavy metal (counted in Pb) content  
     This met hod belongs to arbitration inspection method.  The non -arbitration 
inspection can be based on the method specified in the normative Annex A.  
5.2.1  Toothpaste containing calcium carbonate and calcium phosphate as basic 
substances  
5.2.1.1 Reagents  
     a) N itric acid;  
     b) Nitric acid solution: 5 mol / L;  
     c) Nitric acid solution: 0.2 mol / L;  
     d) Nitric acid solution: 0.01 mol / L;  
     e) Hydrogen peroxide solution content: 30%;  
     f) Ammonia water: ammonia content 25%~28%;  
     g) 1% ammonium  hydroxide solution: add water to 4ml of ammonia water to a 
dilution of 100 ml;  
     h) 10% ammonium sulphamate solution: weigh and take 10 g of ammonium 
sulphamate. Add water to dilution to 100 ml;  
     i) 2% APDC solution: APDC (ammonium pgrroline dithio carbamate) is the 
atomic absorption analytical reagent. Weigh and take 500 mg of APDC. Add 25 ml of 
water and dissolve. The solution must be poured into a brown bottle, which is then 
stored in the refrigerator. One week later, a re -blend shall be made;  
     j) Standard lead reserve liquid: contain 1 mg/ml of lead;  
     k) Standard lead solution: absorb 10.0 ml of lead reserve liquid into a 100 ml 
volumetric flask. Dilute it by 0.01 mol/l of nitric acid solution until reaching the 
graduation (contain 100 g/ml of lead). Separate the dilution using 0.01 mol/l of nitric 
acid solution, making lead become the standard solutions at 1g/ml, 3g/ml and 
5g/mL;  
     l) Chloroform;  
m) Hg2+ solution: weigh and place 0.537g of mercuric oxide into a small beaker, 
and then add 1ml of nitric acid to dissolve it. Add around 50ml of water, and filter it.  Use some water to clean the beaker and funnel. Add around 480ml of water. Use 
5mol/l and 0.2mol/l of nitric acid solution to adjust the pH to 1.6. Add water to 500ml.  
The solution contains 1,000 g/ml of Hg2+. 
5.2.1.2 Instruments  
     a) pH meter: accuracy at 0.02pH. Use buffer solution pH=4.00 for calibration;  
     b) Atomic absorption spectrophotometer: at a wavelength of 283.3nm.  
5.2.1.3 Preparation and determination of sample  
     Take a tube of toothpaste at random to use as the sample. Weigh 2g of 
toothpaste, and accurately place 0.01g into a 150ml Erlenmeyer flask . Add 5ml of 
water and 5ml of nitric acid. Heat the flask under a low flame and shake until the 
paste inside is dissolved. After i t is gradually cooled down, add in 1.5ml of 30% 
hydrogen peroxide solution, and shake the flask. Heat under a low flame until the 
hydrogen peroxide is completely broken down. If any nitrogen dioxide smoke appears 
in a brick red colour, immediately add 2ml of 10% ammonium sulphamate solution 
and heat until the solution is slightly boiling. Rapidly add water to make up to 50ml 
so that it cools down quickly. Add 3ml of ammonium water. After this has cooled 
down to room temperature, pour the solution into a 100 ml beaker. Use 10ml of water 
to clean the  Erlenmeyer flask  twice. Use ammonium water and 1% ammonium 
hydroxide solution to adjust the pH to 1.1 ~ 1.2. During this time, the solution will 
appear to be slightly turbid. Filter this though a 125ml separator fu nnel. Use 5ml of 
water to clean the beaker and funnel. 1ml of 2% APDC solution is added to the 
solution. Shake the flask evenly. Allow it to stay in quiescence for 3 minutes. Add 
10ml of chloroform, and shake the flask for 2 minutes. After layering, the ch loroform 
is transferred to another separator funnel. Again, use 10ml of chloroform to repeat the 
extraction. Combine the extracted solutions. Add 10.0ml of Hg2+ solution, and shake 
the flask for 2 minutes. After layering, the upper -layer water phase is sup plied to 
conduct the determination of flame atomic absorption. Meanwhile, take 0.01 mol/l of 
nitric acid as being blank. Determine the absorption of the standard lead series: 
1g/ml, 3g/ml and 5g/ml. Using lead concentration as the horizontal coordinate and 
lead absorption as the vertical coordinate, draw a standard curve.  
5.2.2 Toothpaste with aluminium hydroxide and silica as the basic substances  
5.2.2.1 Reagents  
     Sulphuric acid.  
     Other reagents are the same as Subsection 5.2.1.1.  
5.2.2.2 Instru ments  
     The same as Subsection 5.2.1.2.  
5.2.2.3 Preparation and determination of samples  
     a) Aluminum hydroxide toothpaste: take a tube of toothpaste at random as the sample. Weigh 2g of toothpaste, and accurately place 0.01g into a 250ml Erlenmeyer  
flask . Add 15ml of nitric acid and 1ml of sulphuric acid and heat until nitrogen 
dioxide gas is produced in a brick red colour. Take down the flask and allow it to cool 
down for a while. Add 2ml of hydrogen peroxide solution, shake the flask and allow it 
to cool down to room temperature. Add 10~15ml of water and 1ml of hydrogen 
peroxide solution and boil for 5~6 min. While boiling, the flask should be shaken 
continuously to remove the hydrogen peroxide. Add in 2ml of 10% ammonium 
sulphamate solution. After  it cools down slightly, take it down. Rapidly add water to 
60ml, and allow it to cool down to room temperature. After the pH value of the 
solution is adjusted to 1.0, move it to a 125ml separator funnel.  Add in 1mL of 2% 
APDC solution and 10ml of chlorof orm, and shake the flask for 2 min. After layering, 
chloroform is transferred to another separator funnel. Again, use 10ml of chloroform 
to repeat the extraction. Combine the extracted solutions. Add 10.0ml of Hg2+ solution, 
and shake the flask for 2 min. After layering, the upper -layer water phase is supplied 
to conduct the determination of flame atomic absorption. Meanwhile, take 0.01 mol/l 
of nitric acid as being blank. Determine the absorption of the standard lead series: 
1g/ml, 3g/ml and 5g/ml. Use lead concentration as the horizontal coordinate and 
lead absorption as the vertical coordinate to draw a standard curve.  
     b) Silica toothpaste: take a tube of toothpaste at random as the sample. Weigh 
2g of toothpaste, and accurately place 0.01g into a  250mL Erlenmeyer flask . Add 5ml 
of water and 5ml of nitric acid and heat under a low flame until the paste is dissolved.  
After it has gradually cooled down, add 1.5ml of hydrogen peroxide solution, and 
shake the flask. Heat under a low flame until hydrog en peroxide gas in a red brick 
colour is created. Add 2ml of 10% hydrogen peroxide solution. After it has been 
slightly heated, take it down. Add 20ml water to cool it down to room temperature.  
Use two layers of filter paper to conduct filtering. Use 15ml  of water and clean the 
Erlenmeyer flask several times , the inner wall of the Buchner funnel, and clear the 
sediments. The filtered solution is poured into the 100ml beaker. Use 10ml of water to 
clean the filtering flask twice. Adjust the pH value to 1.2. Regarding the following 
operation, with the exception of the addition of 5.0ml of Hg2+ solution for back 
extraction, the rest of the complexing, extraction and determination are carried out by 
aluminium hydroxide toothpaste.  
5.2.3 Admissible error  
     The  admissible error between the results acquired from two times of parallel 
determination is ± 5%.  
5.3 Silicon content  
     According to the silicon speck inspection method of GB7919.2.  
5.4 Paste       Take two tubes of toothpaste at random as the samples. Di ssect the tube, and 
carry out a visual test according to the index requirements.  
5.5 Odour  
     Identify the odour by smelling.  Identify the flavour by using tongue -tasting 
method.  
5.6 Thickness  
5.6.1 Instruments  
5.6.1.1 Thermostat:  Accuracy at ± 2oC; 
5.6.1.2 Stop watch;  
5.6.1.3 Standard cap: there is a small hole at a diameter of 3mm at the centre. The 
inner diameter and thread of cap should be consistent with the corresponding tube 
type of toothpaste;  
5.6.1.4 Thickness measurement shelf: the rectangular  metal shelf is installed with 13 
stainless steel wires at a diameter of 1.5mm. The first steel wire is installed at the end 
of the metal shelf. The central distance between the second and first wires is 3mm, 
and the distance between the third and second w ires is 6mm. After that, for each 
increase of a stainless steel wire, the distance is increased by 3mm, until the total 
length of 36mm. The distance figure of each stainless steel wire is just the reading of 
the thickness. The first wire is 0, the second w ire is 3, the third wire is 6, the fourth 
wire is 9, and so on and so forth.  
5.6.2 Determination procedures  
5.6.2.1 Place 3 samples of toothpaste tubes in a thermostat at 45oC ± 2oC.  Then, 
place another 3 samples of toothpaste tubes at room temperature. A fter 24 hours, these 
tubes of toothpaste are to be determined.  
5.6.2.2 The samples to be determined are sealed by standard caps. Discard the first 
20mm of toothpaste squeezed out. Allow the paste to cross over the steel wires in fine 
threads on the thickn ess shelf from the first one to the rest of them. When the paste is 
squeezed out, the paste in fine threads should hang vertically on the steel wires, and 
the squeezing speed should be even and consistent. From each tube of toothpaste, 
three threads of pas te are squeezed out continuously. After squeezing, allow the paste 
to remain hanging for 1 min., and observe the falling situation of the paste.  
5.6.2.3 Indication of results  
     a) Among the three paste dangles, the greatest distance in mm between 2 
unbroken paste dangles both horizontally crossing over the steel wires is considered 
the determination result of a single tube of toothpaste. If the thickness of the three 
hanging paste threads is different, the middle value is taken as the determination resul t 
of the single tube of toothpaste.  
b) After three tubes of toothpaste have been determined, two of them having the same thickness are taken as the final results.  If the determination results of three 
tubes of toothpaste are different, the middle value is  taken as the final result.  If the 
determination result is smaller than 9mm or greater than 33mm, the toothpaste is 
judged as failed; and if it is at the range of 9~33mm, the toothpaste is judged as 
passed.  
5.7 Paste squeeze pressure  
5.7.1 Instruments  
5.7.1.1 Refrigerator: accuracy at ± 1oC; 
5.7.1.2 Determined paste squeeze pressure;  
5.7.1.3 Condensation pump;  
5.7.1.4 Pressure gauge: accuracy at 1 Pa, measurement range at 0~40kPa;  
5.7.1.5 Standard cap: the same as Subsection 5.6.1.3.  
5.7.2 Determination p rocedures  
     Take two tubes of toothpaste at random as the samples. Place them in a 
refrigerator at -8oC ± 1oC for 8 hours, and then remove them. Use hand to squeeze out 
around 20mm of toothpaste and discard it. The mouth of the toothpaste tube is 
screwe d into the standard cap of the paste squeeze pressure determiner. Then, tightly 
screw the standard cap together with the toothpaste into the air cylinder of the paste 
squeeze pressure determiner, and no air should leak out. Slowly press air into the air 
cylinder through the condensation pump. When 1mm~2mm of the paste is squeezed 
out, stop the air supply. Open the exhaust piston of the air cylinder, and let the 
pressure gauge resume to zero. Use a small knife to scrape the mouth of the pliable 
tube to strik e off the paste squeezed out, and close the exhaust piston.  Press in air 
again. When 1mm~2mm of paste is squeezed out, record the pressure reading on the 
pressure gauge immediately. The absolute difference of the parallel determination 
values should not b e greater than one. Take the greatest determination value as the 
determination result.  
5.8 Foam volume  
5.8.1 Instruments  
5.8.1.1 Super thermostatic water bath:  Accuracy at ± 1oC; 
5.8.1.2 Ross -Miles foam determiner.  
5.8.2 Preparation of test fluid  
Take a t ube of toothpaste at random as the sample. Weigh and take 10g of 
toothpaste from it, and accurately place 0.01g into a 100ml beaker. Meanwhile, add 
100ml of distilled water for heating to 40oC ± 1oC.  First of all, use a small amount 
of distilled water to blend the sample to be in thick liquid state. Pour the sample in 
thick liquid state into a 1,000ml porcelain cup, and clean the beaker several times.  
Finally, pour the remaining distilled water into the 1,000ml porcelain cup, and stir it slightly and even ly. Pour into a 40oC ± 1oC thermostatic water bath to keep it warm, 
and then wait for the results.  
5.8.3 Determination procedures  
5.8.3.1 Preparation work  
     Turn on the super thermostatic water bath circulation device that connects with 
the graduated tu be jacket of Ross -Miles foam determiner, and keep the foam 
determiner at 40oC ± 1oC. First of all, use a clean and well -prepared drip tube to hold 
200ml of distilled water at 40oC ± 1oC to clean the inner wall of the graduated tube.  
Then, use the test sol ution to wash along the wall. The washing should be complete.  
Pour the test solution being preheated to 40oC ± 1oC to the lower end of the graduated 
tube, and adjust the surface of test solution to the graduation of 50ml.  
5.8.3.2 First test  
     Use the d rip tube to absorb accurately 200ml of test solution. Next, place it on 
the graduated tube carrier and allow it to be vertical to the cross -section of the 
graduated tube, making the test solution reach the central position of solution surface 
inside the gr aduated tube when being poured into the tube. Open the piston of the drip 
tube, and let the test solution drip down once. Upon the dripping of the test solution, 
immediately record the high and low peak values of foam. Calculate the average 
mathematical va lue of two peak values, and take it as the test result of this time.  
5.8.3.3 Second test  
     Repeat the procedures of Subsections 5.8.3.1 and 5.8.3.2, and carry out the 
second test.  
5.8.3.4 Calculation results  
     The absolute difference between the test  results of the first and second tests 
should be smaller than 5mm. Take the average mathematical value of the two test 
results as the determination result.  
5.9 pH value  
5.9.1 Instruments  
5.9.1.1 pH meter:  Accuracy at 0.02pH unit;  
5.9.1.2 Thermometer:  Acc uracy at 0.2oC; 
5.9.1.3 Balance:  Accuracy at 0.01g.  
5.9.2 Determination procedures  
    Take a tube of toothpaste at random as the sample. Weigh and take 5g of 
toothpaste from the tube, and accurately place 0.01g into a 50ml beaker. Add 20ml of 
the pre -boiled and cooled distilled water for stirring thoroughly and evenly, and 
determine it by the pH meter under 20oC. 
5.9.3 Indication of results  
     The absolute difference between the parallel determination values should not be greater than 0.2pH unit. Take t he average mathematical value as the determination 
result.  
5.10 Stability  
5.10.1 Instruments  
5.10.1.1 Refrigerator: accuracy at ± 1oC; 
5.10.1.2 E lectro -heating standing -temperature cultivator : accuracy at ± 1oC. 
5.10.2 Reagent  
     Filter paper: 102 at med ium speed.  
5.10.3 Determination procedures  
     Place a toothpaste sample in a refrigerator at -8oC ± 1oC for 8 hours. Then, 
remove it and place it in a standing -temperature cultivator  at 45oC ± 1oC. After 8 
hours, remove it and allow it to reach room temp erature again. Open the cap, and the 
paste should not leak out of the tube mouth. Squeeze out all the paste on a white filter 
paper. No liquid should be separated from the paste, and the odour and colour should 
be normal.  
5.11 Excessively hard grain  
5.11.1  Instruments  
5.11.1.1 A determiner of excessively hard grain;  
5.11.1.2 Microslide: 75mm× 25mm.  
5.11.2 Determination procedures  
     Take a tube of toothpaste at random as the sample. Weigh and take 5g of 
toothpaste on a microslide without any scratch mark.   Place the microslide into the 
fixed tank of the determiner.  Press on the friction copper billet, and turn on the 
switch. After the copper billet has undergone forward and backward motion friction 
100 times, remove the friction and take out the microslid e. Use water or 1+1 hot nitric 
acid to clean the microslide, and then observe whether any scratches appear on it.  
5.12 Instruments  
5.12.1.1 Ion meter:  Attached with fluoride  ion-selective electrode  and reference 
electrode. The division value of potential measurement should not be greater than 
0.2mV;  
5.12.1.2 pH meter:  Accuracy at 0.02 pH;  
5.12.1.3 Ion precipitator;  
5.12.1.4 Diffusion chamber (see Figure 1).  
5.12.2 Reagents  
5.12.2.1 Hydrochloric acid solution: 4 mol/l;  
5.12.2.2 Sodium hydroxide solution: 4  mol/l;  
5.12.2.3 Potassium hydroxide solution: 2 mol/l;  
5.12.2.4 Perchloric acid solution: 0.4 mol/l;  5.12.2.5 H examethyl disiloxane  saturated p erchloric acid solution:  Pour 58% 
perchloric acid solution into a separator funnel, and add in h examethyl disil oxane  
(HMDS).  After drastic shaking of the funnel, let it stay in quiescence for layering.  
The lower layer is just the  hexamethyl disiloxane  saturated p erchloric acid solution;  
5.12.2.6 Citrate buffer solution: 100g of trisodium citrate, 60mL of glacial acetic acid, 
60g of sodium chloride, and 30g of sodium hydroxide are dissolved by water.  
Adjust the pH value to be 5.0~5.5, and use water to dilute it to be 100mL;  
5.12.2.7 Fluoride  ion standard solution: Accurately weigh and take 0.1105g of 
standard sodi um fluoride (drying at 105oC ± 2oC for 2 hours). Use deionised water to 
dissolve it, and obtain a predetermined volume to 500ml. Shake it and store in a 
polyethylene plastic flask for later use The concentration of the solution is 100mg/kg.  
5.12.3 Preparat ion of sample  
     Take a tube of toothpaste at random as the sample. Weigh and take 20g of 
toothpaste, and accurately place 0.01g into a 50ml plastic beaker. Gradually add in 
deionised water to stir it until it is dissolved. Transfer it to a 100ml plastic  volumetric 
flask. Dilute it until reaching the graduation, and shake it. Pour it into two separate 
graduated 10ml centrifuge tubes, at equal weight. After being centrifuged in the 
centrifuge machine (2000r/min.) for 30 min., it is cooled down to room temp erature.  
Its supernatant liquid is used for the analysis of free fluorine and the concentration of 
soluble fluorine, whereas its suspension is for the analysis of the concentration of total 
fluorine.  
5.12.4 Drawing of standard curve  
     Accurately absorb  0.5, 1.0, 1.5, 2.0 and 2.5mL of fluoride ion standard solution, 
and move them into five 50ml plastic volumetric flasks. 5ml of citric buffer solution 
is added to each of them. Use deionised water to dilute it until reaching the graduation. 
After this, eac h solution is poured in a 50ml plastic beaker. When the solutions are 
being stirred by magnetic force, measure the potential values E, record them, and 
draw an E -logC (C is the concentration) standard curve.  
 
 
 
 
 
 
 
 
 
  
 
 
1 – diffusion chamber cover    2 – diffusion chamber    3 – absorption pool  
Diffusion chamber cover:  110mm × 20mm  
Diffusion chamber:  d110 mm × 60mm  
Absorption pool:  L × S × H = 75mm × 50mm × 35mm  
Figure 1   Diffusion chamber  
5.12.5 Determination of free fluorine  
     Absorb 10ml of su pernatant liquid, and place it in a 50ml plastic volumetric 
flask.  Add in 5ml of citric buffer solution. Use deionised water to dilute it until 
reaching the graduation. Transfer it to a 50ml plastic beaker. When it is being stirred 
by a magnetic force, me asure its potential value. On the standard curve, check its 
corresponding fluorine content, and then calculate the concentration of free fluorine.  
5.12.6 Determination of soluble fluorine  
     Absorb 0.5ml of supernatant liquid, and transfer it into a 2mL of micro 
centrifuge tube. Add 0.7ml of 4 mol/l hydrochloric acid. Cover the centrifuge tube.  
Put it in water bath at 50oC for 10 min. Transfer it to a 50ml volumetric flask. Add 
0.7ml of 4mol/l sodium hydroxide for neutralising.  Then, add in 5ml of citra te 
buffer solution. Use deionised water to dilute it until reaching the graduation.  
Transfer it to a 50ml plastic beaker. When it is being stirred by magnetic force, 
measure its potential value. On the standard curve, check its corresponding fluorine 
content, and then calculate the concentration of soluble fluorine.  
5.12.7 Determination of total fluorine content  
5.12.7.1 The connecting place between the diffusion chamber and the chamber cover 
is applied with Vaseline. The chamber is placed at an inclined p osition (see Figure 2), 
forming three small chambers separating from each other, as shown in Figure 2.  
Absorb 0.5ml of suspension and transfer it to the left chamber of the diffusion 
chamber.  Add in 5ml of 0.4 mol/l of perchloric acid solution, and stir it for a while.  
Add 0.5ml of 2mol/l potassium hydroxide.  Transfer 5ml of  hexamethyl disiloxane  
saturated p erchloric acid solution to the right chamber.  Seal the diffusion chamber 
tightly by the cover.  Thoroughly blend the solutions of the left and righ t chambers, 
and let it stay in quiescence for above 7 hours.  
5.12.7.2 Open the diffusion chamber. Remove the solution of the central chamber.  
Transfer the solution to a 50ml volumetric flask. Add 0.25ml of 4 mol/l hydrochloric 
acid for neutralizing. Add i n 5ml of citrate buffer solution. Use deionised water to 
dilute it until reaching the graduation. Transfer it to a 50ml plastic beaker. When it is 
being stirred by magnetic force, measure its potential value. On the standard curve, check its corresponding fluorine content, and then calculate the concentration of total 
fluorine.  
5.12.8 Calculation formulas  
     Free fluorine = antilog c × (50 / 10) × (100 / m) …………………. (1)  
     Soluble fluorine = antilog c × (50 / 0.5) × (100 / m) ………..……. (2)  
     Total flu orine = antilog c × (50 / 0.5) × (100 / m) …………..……. (3)  
 
 
 
 
 
 
 
Figure 2   Placement of diffusion chamber  
Remarks:  Material of diffusion chamber:  polystyrene  
In the formulas:  antilog c –– anti -logarithm value, which is acquired from the 
logarithm value of fluorine content found on the 
standard curve  
               m –– mass of sample, in grams.  
     Finally, the above calculation results in mg/kg are converted to percentage 
concentration.  
5.12.9 For the statement, “Absorb 0.5ml of suspension” in Su bsection 5.12.7.1, the 
suspension can also be replaced by 0.2g~0.3g of paste being added with small volume 
of deionised water. Its calculation equation is:  
     Total fluorine = antilog c × (50 / m) …………..…………………….. (4)  
5.12.10 Admissible error  
     The ad missible error between the parallel determination results of the two is ± 
5%.  Their average arithmetic value is taken as the determination result.  
5.13 Determination of net contents  
     Carry out the inspection according to methods set out in JJF1070.  
 
6 Inspection rules  
6.1 Inspection categorisation  
6.1.1 Type inspection  
     The inspection of toothpaste type includes all the items of this Standard. Type 
inspection should be carried out at least once every season of normal production.  
Under one of the f ollowing circumstances, type inspection should also be carried out:  
6.1.1.1 When the technical conditions or prescription of raw material has any tremendous change that may affect the performance of product;  
6.1.1.2 When a product resumes its production af ter suspended production for a long 
time;  
6.1.1.3 When there is a greater difference between the ex -factory inspection result and 
the type inspection of the last time;  
6.1.1.4 When the national quality supervision institution has the request of type 
inspec tion. 
6.1.2 Ex-factory inspection  
     Before a product is delivered from the factory, it must pass the inspection by the 
production factory. Ex -factory inspection items are physical and chemical indices, 
sensory index, as well as the requirements of net c ontents and package appearance 
specified in Section 4.  
6.2 Batch and sampling, judgment rules  
6.2.1 Toothpaste should be delivered batch by batch. Products of the same technical 
conditions, variety, specifications and production date are considered to be a  batch.  
The consignee can also take the delivered products for once as a batch.  
6.2.2 Sampling  
     Take carton as the unit. Confirm the samples according to the size of batch and 
based on Table 3.  
Table 3  
Batch (No. of Cartons)  Sampling (No. of Cartons)  
 500  5 
501 ~ 1,000  8 
> 1,000  13 
     Randomly take cartons of samples at the delivery place or the warehouse of the 
finished products of toothpaste. When inspecting the packaging quality, inspect all the 
small packages inside the carton, and carry out the inspection according to Subsection 
4.4.2. The total judgment rate of the passed products is 10%. After this, take 2~4 
medium boxes at random from each carton, and then take the same number of tubes 
from each medium box, making the total number of sampl es to be no less than 40 
tubes.  
6.2.1.1 If the inspection is not passed, samples can be taken out from 2 times of the 
carton samples to carry out re -inspection of the failed items.  If the re -inspection 
results are still failed, this batch of products is r egarded as being failed.  
6.2.1.2 When the consignor and consignee have argument over the inspection result, 
arbitration inspection can be carried out, and the arbitration result is the final 
reference.  
7   Marking, packaging, transportation, storage  7.1 M arking  
7.1.1 The package for sale should contain the following marking:  
7.1.1.1 Name and brand of product;  
7.1.1.2 Net contents;  
7.1.1.3 Name and address of production factory;  
7.1.1.4 Execution standard number;  
7.1.1.5 Guarantee period and production date  or expiry date and production batch 
number;  
7.1.1.6 Odour type;  
7.1.1.7 The ingredients of the toothpaste should be indicated with the standard names 
of the raw materials. Fluoride toothpaste should be indicated with the amount of 
added fluorine. Children ’s fluoride toothpaste should be indicated with warning 
words.  
7.1.1.8 The marking of travellers’ toothpaste should be according to No. 172 [1997] 
issued by National  Quality and Technical Supervision  Bureau, “ Provisions on 
indicating product identification .” Regarding the travellers’ toothpaste with a 
marketed package at a net weight of less than or equal to 10g, the package can be 
indicated with only the name, brand, net contents, name of production factory, 
guarantee period and production date or expiry d ate and production batch number, 
with no need to indicate the odour type, adopted standard number, and so on.  
7.1.2 Large package should include the following marking:  
7.1.2.1 Name of product;  
7.1.2.2 Name and address of production factory;  
7.1.2.3 Number of cartons, gross weight;  
7.1.2.4 Production date or expiry date and production batch number;  
7.1.2.5 The specifications of packaging carton should meet the requirements of 
GB/T191;  
7.1.2.6 Identifications such as “Upward,” “no rainfall,” “no sunshine,” an d so on 
should meet the requirements of GB/T191.  
7.2 Packaging  
     The enterprise may decide whether toothpaste in pliable tubes shall be packed 
in little boxes or not, and whether the medium -sized packaging box is made out of 
contracted packaging or pape r box. For large packaging cartons, it should adopt the 
material that will not damage the materials of the products inside the carton.  
7.3 Transportation  
    Loading and unloading should be carried out lightly. Cartons should be piled up 
according to the a rrowheads. Avoid intense vibration, bumping, sunshine, rainfall and 
damage caused by pressurising.  7.4 Storage  
7.4.1 Store the products in the ventilated and dry warehouse. Do not place the product 
close to sources of water or heating systems. Products sho uld be stacked no less than 
8cm above the ground or 50cm from the wall. In the middle of warehouse, there 
should be an aisle. Cartons should be stacked according to the arrowheads, and should 
not be placed upside down.  
7.4.2 Guarantee period  
7.4.2.1 The gu arantee period should be indicated along with the production date 
shown according to the order of year, month and date, and no reversal of the order is 
permitted. Years should be indicated by 4 -digit figures, e.g. 2000;  
7.4.2.2 Limited period of use and pr oduction batch;  
     The guarantee period is fixed by the enterprises, but should not exceed 5 years.  Appendix A  
(Standardised Appendix)  
Lead content determination of samples directly injected from 
graphite oven  
 
A1 Instruments and reagents  
A1.1  An atomi c absorption spectrometer (attached with graphite oven).  
     Conditions of the machine:  
     Wavelength: 283.3nm, lamp current 3.5mA, and slit 1.0. Use deuterium light to 
deduct the background.   
     The determination conditions of graphite oven are show n in Table A1.  
A1 
Item Temperature, oC Retention time, s  Temperature rise speed, oC/s 
Dry 
Cineration  
Atomisation  90~120  
700 
1,750  80 
50 
2.0 - 
- 
400 
A1.2  A 10ml microsyringe.  
A1.3  A magnetic force stirrer.  
A1.4  Balance:  Accuracy at 0.001g.  
A1.5  A 50 ml straw.  
A1.6  Several 100ml beakers.  
A1.7  (1+1) nitric acid (of excellent grade and pure).  
A1.8  Prepared standard lead solution: weigh 0.1598g of lead nitrate. Use 
appropriate amount of (1+1) nitric acid solution for dissolving it. Use distilled water 
to dissolve it, and obtain a predetermined volume to 1,000ml. The concentration of 
the solution is 100g/ml.  
A1.9 Diluter: take appropriate volume of agar, ammonium dihydrogen phosphate , and 
dispenser, which are dissolved by distilled water to  obtain a cer tain predetermined 
volume.   
A2 Handling of sample  
     Take a tube of toothpaste at random as the sample. Weigh 2.00g of toothpaste, 
and place it in a 100ml beaker. Add 50ml of diluter and 1.0ml (1+1) nitric acid. Stir 
well on the magnetic force stirrer un til an even solution is formed (taking around 20 
min.).  
A3 Determination of sample  
     Under the condition that the sample is being stirred on the magnetic force stirrer, 
use the microsyringe to absorb 10ml (do not absorb the bubble), and fill it into the  
graphite tube. Turn on the switch of the graphite oven, and carry out determination of the sample. Record the absorption value, and carry out blank test.  
A4 Drawing of standard curve  
     According to the absorption value of sample, prepare 3~5 standard l ead 
solutions with the corresponding concentration.  Determine the absorption value, 
deduct the blank absorption value, and draw the curves of concentration and 
absorption value.  
A5 Calculation  
     The sample absorption value is deducted by the blank abso rption value.  From 
the standard curve, check the corresponding concentration, which is multiplied by the 
multiple, resulting in the lead content in the sample toothpaste (mg/kg).  
Calculation equation:  
                            X = K • c  ………………………………  ( A1) 
where, X –– lead content in toothpaste, mg/kg;  
      K –– diluted multiple of sample;  
      c –– corresponding concentration checked from the standard curve, mg/kg.  
A6 Admissible error  
     The admissible error between the results acquired from both pa rallel 
determinations is ± 5%.  
 
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