Some standard content:
GB8372--2001
The fragrance in table 4.1, paste extrusion pressure in 5.4, foam volume in 5.5 and packaging and packaging form in 7.2 of this standard are recommended, and the rest are mandatory.
This standard is the revised version of GB83721995 "Toothpaste". This standard has requirements for toothpaste quality tolerances, sampling methods for sample toothpaste, methods for expressing consistency results, methods for calculating the final result of consistency, methods for expressing fluoride content, heavy metal content indicators, stability, toothpaste packaging, and labeling of toothpaste packaging. Ten issues including shelf life and shelf life were revised and supplemented.
This standard will replace GB8372-1995 from the date of implementation. Appendix A of this standard is a reminder appendix.
This standard is proposed by the State Light Industry Bureau
This standard is under the jurisdiction of the National Toothpaste Wax Products Standardization Center. The drafting unit of this standard is: National Standardization Center for Toothpaste and Wax Products. The main drafters of this standard: Li Shun, Ma Xuan, Shen Erui, Luo Ximing. 293
1 Scope
National Standard of the People's Republic of China
Toothpaste
GB 8372—2001
replaces GB8372--1995
this standard It stipulates the technical requirements, test methods, inspection rules and marking, packaging, transportation, storage and other requirements for toothpaste. This standard applies to various toothpastes for intraoral application. 2 Referenced standards
The provisions contained in the following standards constitute provisions of this standard by being quoted in this standard. At the time of publication of this standard, the versions indicated were valid. All standards are subject to revision and parties using this standard should explore the possibility of using the latest version of the standard listed below. GB/T601-1988 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T603-1988 Preparation of preparations and products used in chemical reagent test methods GB/T7917.2--1987 Hygienic Chemistry Standard Test Method for Cosmetics Monument Cosmetics Standard test method for microorganisms Determination of total bacterial count GB/T 7918. 2-1987
GB/T 7918. 3-1987
Standard test method for microorganisms in cosmetics Fecal coliforms GB/T 7918. 4-1987
7 Standard Test Methods for Microorganisms in Cosmetics Pseudomonas aeruginosa GB/T 7918.5-—1987
Standard Test Methods for Microorganisms in Cosmetics Staphylococcus aureus State Bureau of Technical Supervision Order No. 43 "Regulations on Measurement Supervision of Quantitative Packaged Goods" 》1995) 3 Product Classification
According to usage performance, it is divided into ordinary toothpaste and fluoride toothpaste. 4 Technical requirements
4.1 Sensory indicators, physical and chemical indicators and hygienic indicators are shown in Table 1. 4.2 Net content
The net content of single quantitative packaging commodities should comply with the State Administration of Quality and Technical Supervision Order (95) No. 43 Table (1); the average deviation of bulk and quantitatively packaged goods is ≥0.
4.3 Packaging appearance requirements
4.3.1 Hose or other packaging
a) The tube body is smooth, clean, even in thickness, without obvious scratches, and the color is consistent with the standard sample. b) The seal must be firm and straight, without openings, wrinkles, etc. The end of the tube must be tightly sealed and without leakage. c) The cap should be straight and smooth, with no cracks, burrs or bursts, the color should be uniform and not fade, the threads and the hose should have a sound matching structure, and should not be skewed or slippery.
a) The box surface is smooth and straight, the pattern printing is clear, the color registration is accurate, there must be no obvious scratches or burrs on the bottom, and the color is uniform. Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on October 24, 2001 | Wrinkles, missing edges, missing corners, and cracks. Table 1
Sensory indicators
Physical and chemical indicators
Hygienic indicators
5 test methods
Consistency, mm
Paste extrusion pressure, kPa| |tt||Foam volume, mm
Stability
Excellent particles
Total fluorine content.%
Soluble fluorine or floating fluorine content, %||tt ||Total number of bacteria, individuals/8
Fecal coliforms, individuals/g
Pseudomonas aeruginosa, individuals/8
Staphylococcus aureus, individuals/g||tt| |Heavy metal content (Ph), mg/kg
Arsenic content (As), mg/kg
Clean, uniform, delicate, normal color
Conforms to specified fragrance||tt ||The paste does not overflow the nozzle, does not separate water, and has normal fragrance and color, and no scratches on the glass
(Applicable to fluoride toothpaste)
(Applicable to fluoride toothpaste)
No detection allowed
No detection
No detection
The following sampling method should be adopted for the indicators that calculate the final test results according to the weighing method. a) Single-phase tube toothpaste: First squeeze out 20mm of paste, discard it, and then squeeze out a sample to measure its quality. b) Multi-phase tube toothpaste: First squeeze out 20mm of paste, discard it, and then take out the separated parts from each phase according to the marked proportion. If there is no marked proportion, take an average sample from each phase, mix it and weigh it. 5.1 Set
Take any 2 tubes of sample toothpaste, squeeze them all into strips on white paper or white porcelain board, and inspect visually. 5.2 Aroma
Determine by tasting.
5.3 Consistency
5.3.1 Main instruments
a) Thermostat, 1 set;
b) Stopwatch, 1 set;
c) Standard 1 cap, with a small hole with a diameter of 3mm in the center. The inner diameter and thread of the cap should match the corresponding toothpaste tube type; d) 1 consistency measuring frame, with 13 diameter rods installed on the rectangular metal frame It is a 1.5mm stainless steel wire. The first steel wire is installed at the end of the metal frame. The center distance between the second wire and the first wire is 3mm, and the distance between the third wire and the second wire is 6mm. For each additional stainless steel wire in the future, the distance increases by 3mm until 36mm. The distance between each stainless steel wire is the thickness reading. The first wire is 0, the second wire is 3, the third wire is 6, the fourth wire is 9, and so on. 5.3.2 Measurement procedure
GB 8372--2001
5.3.2.1 Place 3 tubes of sample toothpaste into a 45°C thermostat, and take another 3 tubes of sample toothpaste and place them at room temperature. Place separately for 24 hours before testing.
5.3.2.2 Screw on the standard caps of the samples to be tested, first squeeze out 20mm of toothpaste and discard it, then squeeze out the toothpaste, and move the paste strips from the first steel wire on the consistency rack to the The remaining steel wires are crossed so that the paste strips are placed horizontally on the steel wires. Each toothpaste is squeezed out 3 strips continuously. After squeezing, wait for 1 minute to observe the paste breaking off.
5.3.2.3 Calculation of measurement results
5.3.2.3.1 The maximum distance (mm) between two of the three identical paste strips that are not broken across the steel wire is considered as a single Measurement results. 5.3.2.3.2 After all three toothpastes have been measured, take the two toothpastes with the same consistency as the final result. If it is less than 9mm or greater than 33mm, it will be judged as unqualified. If it is between 9mm and 33mm, it will be judged as qualified. 5.4 Paste squeezing pressure
5.4.1 Main instruments and equipment
a) Refrigerator, 1 set,
b) Paste squeezing pressure measuring instrument, 1 set;
c ) Compression pump, 1 set;
d) Pressure gauge, 0~40kPa, 1 piece, accuracy 1Pa; e) Standard cap, the same as 5.3.1c.
5.4.2 Measurement procedure
Take 2 tubes of sample toothpaste at will, put it in an 8℃ refrigerator for 8 hours, take it out, squeeze out about 20mm of the paste by hand and discard it, remove the mouth of the toothpaste tube Twist the standard cap of the squeezing pressure measuring instrument, and then screw the standard cap and toothpaste tightly into the air storage cylinder of the squeezing pressure measuring instrument to make it airtight, and slowly press air into the air storage cylinder through the compression pump. . When the strip is squeezed out by 1mm ~ ~ 2mm, stop the air intake, open the exhaust piston of the air reservoir, return the pressure gauge to zero, use a knife to scrape the extruded paste up to the mouth of the hose, and close the exhaust piston , press the air again, and when the body is squeezed out by 1 mm to 2 mm, immediately record the pressure number of the pressure gauge, and take the maximum measured value as the measurement result. 5.5 Foam volume
5.5.1 Main instruments
a) Super constant temperature water bath, 1 set;
b) Roche foam measuring instrument, 1 set.
5.5.2 Preparation of test solution
Take 1 tube of toothpaste from the sample and weigh 10g of toothpaste from it (accurate to 0.01g) in a 100mL beaker, and heat 1000mL distilled water to 40℃ at the same time. First, use a small amount of distilled water to make the sample into a slurry, pour the slurry sample into a 1000mL porcelain cup, and wash the beaker several times. Finally, pour the remaining distilled water into the 1000mL porcelain cup, gently stir evenly, and put it in a 40℃ constant temperature water bath to keep warm for testing.
5.5.3 Determination procedure
5.5.3.1 Preparation
Turn on the super constant temperature water bath circulation device connected to the graduated tube jacket of the Roche foam tester, keep the foam tester at 40℃, first rinse the inner wall of the graduated tube with 40C distilled water, and then rinse along the wall with the test solution. The rinse must be complete, and the test solution preheated to 40℃ is injected into the lower end of the graduated tube, and the test solution liquid level is adjusted to 50mL scale. 5.5.3.2 First test
Use a dropper to accurately draw 200mL of test solution, and then place it on the top of the graduated tube rack and perpendicular to the cross section of the graduated tube, so that the test solution can reach the center of the liquid surface in the graduated tube when it flows in, open the piston of the dropper, and let the test solution flow down at once. When the test solution flows out, immediately record the peak value and low peak value of the foam, and calculate the average value of the two peak values. 5.5.3.3 Second test
Use a dropper to accurately draw 200mL of test solution, and then place it on the top of the graduated tube rack and perpendicular to the cross section of the graduated tube, so that the test solution can reach the center of the liquid surface in the graduated tube when it flows in, open the piston of the dropper, and let the test solution flow down at once. When the test solution flows out, immediately record the peak value and low peak value of the foam, and calculate the average value of the two peak values. 5.5.3.4 Calculation results
The arithmetic mean of the two tests is the determination result. 5.6 pH
5.6.1 Main instruments
a) Acidity meter, 1 unit, accuracy ≥ 0.02; b) Thermometer, 1 unit, accuracy 0.2℃;
c) Pan balance, 1 unit, accuracy 0.01g. 5.6.2 Determination procedure
Take a sample toothpaste, weigh 5g of it and put it in a 50mL beaker, add 20mL of pre-boiled and cooled distilled water, stir well, and immediately measure it with an acidity meter at 20℃. 5.7 Stability
5.7.1 Main instruments
a) Refrigerator, 1 unit;
b) Electric constant temperature incubator, 20℃~60℃, 1 unit, accuracy 1℃. 5.7.2 Determination procedure
Put a tube of sample toothpaste in a refrigerator at -8℃, take it out after 8 hours, and then put it in a constant temperature incubator at 45℃, take it out after 8 hours, and return it to room temperature. Open the lid, the paste should not overflow from the tube; squeeze all the paste on white paper, and no water should be separated; the aroma and color are normal. 5.8 Hard particles
5.8.1 Main instruments
One hard particle tester.
5.8.2 Determination procedure
Take a tube of sample toothpaste at random, weigh 5g of toothpaste from it and put it on a scratch-free slide (255mm×75mm), put the slide into the fixed groove of the tester, press the friction copper block, start the switch, make the copper block rub back and forth 100 times, stop rubbing, take out the slide, wash the slide with water or hot nitric acid (1:1), and then observe whether the slide is scratched. 5.9 Free fluorine, soluble fluorine and total fluorine content 5.9.1 Main instruments and tools
a) Fluoride ion selective electrode, 1 piece;
b) Calomel reference electrode, 1 piece;
c) PHS-3C acidity meter, 1 piece, or 720AORION acidity meter, 1 piece;
d) BD-Z ion precipitator, 1 piece;
e) Diffusion box (see Figure 1), 1 set.
Diffusion box cover: 110mm×20mm
Diffusion box: d110mmX60mmz
GB8372—2001
1-Diffusion box cover, 2-Diffusion box; 3-Absorption cell; L×S×H=75mm×50mm×35mmFigure 1 Diffusion box
5.9.2 Reagents
a) Hydrochloric acid solution (cHcl=4 mol/L); b) sodium hydroxide solution (cNaOH=4mol/L); c) potassium hydroxide solution (ckOH=2mol/L); d) perchloric acid solution (cHcio,=0.4mol/L); e) saturated perchloric acid solution of hexamethyldisiloxane: pour 58% perchloric acid solution into a separatory funnel, add hexamethyldisiloxane (HMDS), shake vigorously, and let it stand to separate. The lower layer is the saturated perchloric acid solution of hexamethyldisiloxane; f) citrate buffer: 100g trisodium citrate, 60ml. glacial acetic acid, 60g sodium chloride, 30g sodium hydroxide, dissolve in water, adjust pH=5.0~5.5, and dilute with water to 1000mL; g) fluoride ion standard solution: accurately weigh 0.1105g standard sodium fluoride (dried at 105℃ for 2h), dissolve in deionized water and make up to 500ml, shake well, and store in a polyethylene plastic bottle for later use. The concentration of this solution is 100mg/kg. 5.9.3 Sample preparation
Take any one tube of toothpaste for sample, weigh 20 g (accurate to 0.001 g) from it and place it in a 50 mL plastic beaker. Gradually add deionized water and stir to dissolve. Transfer to a 100 mL volumetric flask, dilute to the scale, shake well, and pour into two 10 mL centrifuge tubes with scales respectively to make them equal in weight. Centrifuge in a centrifuge (2000 r/min) for 30 min, cool to room temperature, and use the supernatant to analyze the free fluorine and soluble fluorine concentrations, and the suspension to analyze the total fluorine concentration. 5.9.4 Plotting of standard curve
Accurately pipette 0.5, 1.0, 1.5, 2.0, 2.5 ml of fluoride ion standard solution into five 50 ml volumetric flasks, pipette 5 ml of citrate buffer into each, dilute to scale with deionized water, then transfer into 50 ml plastic beakers one by one, measure the potential value E under magnetic stirring, record and plot the E-logc (c is concentration) standard curve. 5.9.5 Determination of free fluoride
Pipette 10 ml of supernatant into a 50 ml volumetric flask, add 5 ml of citrate buffer, dilute to scale with deionized water, transfer into 50 ml plastic beakers, measure its potential value under magnetic stirring, find its corresponding fluoride content on the standard curve, and calculate the free 298
fluorine concentration.
5.9.6 Determination of soluble fluorine
GB 8372--2001
Pipette 0.5 ml of supernatant and transfer it to a 2 ml microcentrifuge tube. Add 0.7 ml of 4 mol/L hydrochloric acid. Cover the tube and place it in a 50°C water bath for 10 min. Transfer it to a 50 ml volumetric flask and add 0.7 mL of 4 mol/L sodium hydroxide to neutralize it. Add 5 mL of citrate buffer and dilute to the mark with deionized water. Transfer it to a 50 mL plastic beaker and measure its potential value under magnetic stirring. Find the corresponding fluorine content on the standard curve and calculate the soluble fluorine concentration. 5.9.7 Determination of total fluorine content
5.9.7.1 Apply vaseline to the junction of the diffusion box and the box cover, and place it in an inclined position in advance (as shown in Figure 2) to form three small chambers separated from each other. Pipette 0.5mL of the suspension into the left chamber of the diffusion box, add 5mL of 0.4mol/L perchloric acid and shake it, put 0.5mL of 2mol/L potassium hydroxide into the middle chamber, and move 5mL of saturated perchloric acid solution of hexamethyldisiloxane into the right chamber. Cover and seal the diffusion box, mix the solutions in the left and right chambers thoroughly, and let it stand for more than 7h.
//////////////
Figure 2 Diffusion box placement diagram
Note: Diffusion box manufacturing material: polystyrene. 5.9.7.2 Open the diffusion box, take out the solution in the intermediate chamber, transfer the solution into a 50mL volumetric flask, add 0.25mL 4mol/L hydrochloric acid to neutralize, add 5mL citrate buffer, dilute to the mark with deionized water, transfer into a 50mL plastic beaker, measure its potential value under magnetic stirring, find its corresponding fluorine content on the standard curve, and calculate the total fluorine concentration. 5.9.8 Calculation formula
Free fluorine = antilogc × (50/10) × (100/m) Soluble fluorine = antilogc × (50/0.5) × (100/m) Total fluorine = antilogc X (50/0.5) × (100/m) Where: anti logc - the logarithm of the fluorine content found on the standard curve; - the mass of the sample, g.
Finally, convert the above calculation result (mg/kg) into a percentage concentration. (1)
(2)
5.9.9 In 5.9.7.1, "absorb 0.5mL of suspension" can also be used as 0.2g~~0.3g toothpaste is replaced by a small amount of deionized water, and the calculation formula is:
Total fluoride = antilogc × (50/m)
5.9.10 Allowable difference
The allowable difference of two parallel determination results is ±5%. 5.10 Total bacteria
Test according to GB/T7918.2.
5.11 Fecal coliform group
Test according to GB/T7918.3.
5.12 Pseudomonas aeruginosa
Test according to GB/T7918.4.
. (4)
5.13 Staphylococcus aureus
Test according to GB/T7918.5.
5.14 Heavy metal content (in terms of lead)
GB 8372—2001
This method is an arbitration test method. Non-arbitration tests can also use the method described in Appendix A (suggested Appendix). 5.14.1 Toothpaste based on calcium carbonate and calcium hydrogen phosphate 5.14.1.1 Reagents and instruments
a) Nitric acid: analytical grade;
b) 5 mol/L nitric acid solution: take 158 mL of analytical grade nitric acid and dilute it to 500 mL with water; c) 0.2 mol/L nitric acid solution: take 6.3 mL of analytical grade nitric acid and dilute it to 500 mL with water; d) 0.01 mol/L nitric acid solution: take 25.00 mL of 0.2 mol/L nitric acid, Dilute to 500mL with water; e) Hydrogen peroxide solution: analytical grade, content 30%; f) Ammonia water: analytical grade, nitrogen content 25%~28%; g) 1% ammonium hydroxide solution: take 4mL of ammonia water and dilute to 100mL with water; h) 10% ammonium sulfamate solution: weigh 10g of analytical grade ammonium sulfamate, dissolve in water and dilute to 100mlL; i) 2% APDC solution: APDC is an atomic absorption analytical reagent (ammoniumPgrroline dithiocarbamate tetrahydropyrroleammonium dithiocarbamate), weigh 500mg of APDC, dissolve in 25mL of water, the solution needs to be placed in a brown bottle, stored in the refrigerator, and re-prepared after a week; j) Lead standard stock solution: contains 1mg/mL lead; k) Lead standard solution: aspirate 10.0mL of lead stock solution in a 100mL volumetric flask, and dilute to the scale (containing 100μg/mL lead) with 0.01mol/L nitric acid solution. Use 0.01mol/L nitric acid solution to dilute again, so that the lead content is: 1μg/mL, 3μg/mL, 5μg/mL standard solution;
1) Chloroform: analytical grade;
m) Hg2+ solution: weigh 0.537g of mercuric oxide in a small beaker, add 1mL of nitric acid to dissolve it, add about 50mL of water, filter, and wash the beaker and funnel with a little water. Add water to about 480mL, adjust the pH to 1.6 with 5mol/L and 0.2mol/L nitric acid solutions, and add water to 500mL. The solution contains 1000μg/mL of Hg2+;
n) pH meter, 1 set, calibrated with pH=4.00 buffer;o) Atomic absorption spectrophotometer, 1 set, instrument conditions: wavelength 283.3nm. 5.14.1.2 Sample preparation and determination
Take any sample toothpaste, weigh 2.00g of toothpaste from it and put it in a 150ml conical flask, add 5ml of water and 5ml of nitric acid, heat with low heat and shake until the toothpaste dissolves. Let it cool slightly, add 1.5ml of 30% hydrogen peroxide solution, shake, and heat with low heat until the hydrogen peroxide is completely decomposed. If red-brown nitrogen dioxide smoke is produced, immediately add 2mL of 10% ammonium sulfamate solution and heat until the solution is slightly boiling, quickly add water to 50mL, cool it quickly, add 3mL of nitrogen water and cool it to room temperature, then transfer the solution into a 100mL beaker and wash the conical flask twice with 10mL of water. Use ammonia water and 1% ammonium hydroxide solution to adjust the pH to 1.1~~1.2. At this time, the solution will be slightly turbid; filter it into a 125mL separatory funnel and wash the beaker and funnel with 5mL of water. Add 1 mL of 2% APDC solution to the solution, shake well and place for about 3 minutes, add 10 mL of trichloromethane, shake for 2 minutes, transfer the trichloromethane to another separatory funnel after separation, and repeat the extraction with 10 mL of trichloromethane, and combine the extracts. Add 10.0 mL of Hg2+ solution, shake for 2 minutes, and take the upper aqueous phase for flame atomic absorption determination after separation. At the same time, use 0.01 mol/L nitric acid solution as a blank to determine the absorption of the lead standard series of 1 μg/ml, 3 μg/ml, and 5 μg/ml. Draw a standard curve with lead concentration as the horizontal axis and lead absorption as the vertical axis.
5.14.2 Toothpaste with aluminum hydroxide and silicon dioxide as the matrix 5.14.2.1 Reagents and instruments
a) Nitric acid: analytical grade;
b) 5 mol/L nitric acid solution: take 158 mL of analytical grade nitric acid and dilute it to 500 mL with water; c) 0.2 mol/L nitric acid solution: take 6.3 mL of analytical grade nitric acid and dilute it to 500 mL with water; d) 0.01 mol/L nitric acid solution: take 25.00 mL of 0.2 mol/L nitric acid and dilute it to 500 mL with water; 300
e) Sulfuric acid: analytical grade;
f) Hydrogen peroxide solution: analytical grade, content 30%; g) Ammonia water: analytical grade, ammonia content 25%~28%, GB 8372—2001
h) 1% ammonium hydroxide solution: take 4ml of ammonia water and dilute to 100mL with water; i) 10% ammonium sulfamate solution: weigh 10g of analytically pure ammonium sulfamate, dissolve in water and dilute to 100mL; j) 2% APDC solution: APDC is an atomic absorption analytical reagent (ammonium pyrroline dithiocarbamate tetrahydropyrrole ammonium dithiocarbamate), weigh 500mg of APDC, dissolve in 25mL of water. The solution should be stored in a brown bottle, stored in a refrigerator, and reconstituted after two weeks; k) Lead standard stock solution: containing 1mg/ml of lead; 1) Lead standard solution: aspirate 10.0mL of lead stock solution in a 100mL volumetric flask, and dilute to the mark with 0.01mol/L nitric acid solution (containing 100μg/mL of lead). Use 0.01mol/L nitric acid solution to dilute again, so that the lead content is: 1μg/mL, 3μg/mL, 5ug/ml standard solution;
m) Chloroform: analytical grade;
n) Hg2+ solution: weigh 0.537 parts of mercuric oxide in a small beaker, add 1mL of nitric acid to dissolve it, add about 50mL of water, filter, and wash the beaker and funnel with a little water. Add water to about 480mL, adjust the pH to 1.6 with 5mol/L and 0.2mol/L nitric acid solutions, and add water to 500mL. The solution contains 1000ug/mL of Hg2+;
o) pH meter, 1 set, calibrated with pH=4.00 buffer;p) Atomic absorption spectrophotometer, 1 set, instrument conditions: wavelength 283.3nm. 5.14.2.2 Sample preparation and determination
5.14.2.2.1 Aluminum hydroxide toothpaste: Take any one tube of sample toothpaste, weigh 2.0 g of it and put it into a 250 mL conical flask, add 15 mL of nitric acid and 1 mL of sulfuric acid, heat until reddish brown nitrogen dioxide gas is produced, remove the tube, cool slightly, add 2 mL of hydrogen peroxide solution, shake, cool to room temperature, add 10 mL~15 mL of water and 1 mL of hydrogen peroxide solution, boil for 5 min~6 min, and shake continuously to remove hydrogen peroxide, add 2 mL of 10% ammonium sulfamate solution, cool slightly, remove the tube, quickly add water to 60 mL, and quickly cool to room temperature. After adjusting the solution pH to 1.0, transfer it into a 125mL separatory funnel, add 1mL of 2% APDC solution and 10mL of chloroform, shake for 2min, transfer chloroform into another separatory funnel after separation, and repeat extraction with 10mL of chloroform, combine the extracts, add 10.0mL of Hg2+ solution, shake for 2min, and take the upper aqueous phase for flame atomic absorption determination after separation. At the same time, use 0.01moi/L nitric acid solution as blank to determine the absorption of the lead standard series of 1μg/ml, 3μg/mL, and 5μg/mL, and draw a standard curve with lead concentration as the horizontal axis and lead absorption as the vertical axis. 5.14.2.2.2 Silica toothpaste: Take any one tube of sample toothpaste, weigh 2.0g of it and put it in a 250mL conical flask, add 5mL of water and 5mL of nitric acid, heat it over low heat until the paste dissolves, cool it slightly, add 1.5mL of hydrogen peroxide solution, shake it, heat it over low heat until reddish brown nitrogen dioxide gas is generated, immediately add 2mL of 10% aminosulfonic acid solution, remove it while it is slightly hot, add 20mL of water, cool it to room temperature, filter it with two layers of filter paper, wash the inner wall of the conical flask and the Buchner funnel and the precipitate with 15mL of water several times, transfer the filtrate into a 100mL beaker, wash the filter bottle twice with 10mL of water, adjust the pH to 1.2, and except for adding 5.0mL of Hg2+ solution for back extraction, the rest of the following operations are carried out according to the aluminum hydroxide toothpaste complex extraction and determination. 5.14.3 Allowable difference
The allowable difference between two parallel determination results is ±5%. 5.15 Arsenic content
Test according to the arsenic spot method of GB/T7917.2.
5.16 Net content
5.16.1 Calibrate the rack balance (accuracy is 0.01g) and adjust the zero point. 5.16.2 Randomly extract 10 tubes of sample toothpaste, place them on the rack balance and weigh their mass, and record it as m1. 5.16.3 Randomly extract 10 empty hoses of sample toothpaste (with caps), place them on the rack balance and weigh their mass, and record it as m2. 5. 16. 4 Calculate
Net content = (m, -mz)/10
and compare with the marked net content.
(5)
6 Inspection rules
6.1 Inspection classification
6.1.1 Type inspection
GB 8372—2001
Toothpaste type inspection includes all items in the standard and shall be conducted at least once a quarter during normal production. Type inspection shall also be conducted in any of the following circumstances.
a) When there are major changes in raw material process or formula that may affect product performance; b) When the product is resumed after a long period of suspension; c) When the factory inspection results are significantly different from the last type inspection; d) When the national quality supervision agency proposes a type inspection requirement. 6.1.2 Factory inspection
Products must be inspected by the manufacturer and issued a certificate of conformity before they can be shipped. The factory inspection items are the physical and chemical indicators, sensory indicators, net content and packaging appearance requirements specified in Chapter 4. 6.2 Batch grouping, sampling and judgment rules
6.2.1 Toothpaste is delivered in batches. Products with the same process conditions, varieties, specifications and production dates are considered as a batch. The consignee can also consider the products delivered at one time as a batch.
6.2.2 Sampling
The sample is determined in boxes according to the batch size and Table 2. Table 2
Batch, number of boxes
>500～1000
Sampling, number of boxes
Randomly select box samples at the delivery location or toothpaste finished product warehouse. When accepting the packaging quality, check all small packages in the box and conduct inspection according to 4.3.2. The total qualified judgment rate is 10%. Then randomly select two medium boxes from each box, and then take out the same number of sticks from each medium box, so that the total number of samples is not less than 40 sticks.
6.2.3 If the inspection fails, samples can be taken from two boxes of samples and the unqualified items can be re-inspected. If the re-inspection results are still unqualified, the batch of products will be judged to be unqualified.
6.2.4 If the delivery parties disagree with the inspection results, they can request arbitration inspection, and the arbitration results will be the final basis. 7 Marking, packaging, transportation, storage
7.1 Marking
7.1.1 The sales packaging should have the following markings:
a) Product name and trademark;
b) Net content;
c) Manufacturer name and address;
d) Standard number adopted;
e) Shelf life, production date or limited use date; f) Fragrance.
7.1.2 The large package should have the following signs:
a) Product name;
b) Manufacturer name and address;
c) Packing quantity and gross weight;
d) Date of manufacture;
GB 8372--2001
e) Packing box specifications [length (mm)) × width (mm) × height (mm)]; f) "moisture-proof", "handle with care", "prevent inversion" and other words. 7.2 Packaging and packaging type
Under the condition that the product quality is not damaged, the product packaging form and packaging materials shall be determined by the enterprise. The box should be filled with no gaps and the product certificate should be placed.
7.3 Transportation
The products must be loaded and unloaded with care and stacked according to the arrows on the boxes to avoid violent movement, collision and sun and rain. 7.4 Storage
7.4.1 It should be stored in a ventilated and dry warehouse with a temperature not higher than 40℃, not near water sources and heating. When stacking, it must be 20cm from the ground and 50cm from the wall. There should be a passage in the middle. Stack according to the arrows on the boxes. It must not be stacked upside down. The stacking height should not exceed 2.5m. 7.4.2 Shelf life
The date should be marked on the visible surface. There are two marking methods: a) The shelf life must be marked with the production date, marked in the order of year and month, and cannot be reversed. The year must be 4 digits, such as 2000; b) Restricted use date and production batch number;
The shelf life is determined by the enterprise, but it cannot exceed five years at most. 303
A1 Instruments and reagents
GB 8372—2001
Appendix A
(Suggested Appendix)
Determination of lead content by direct sampling in graphite furnace
A1.1 Atomic absorption spectrometer (with CXR90 graphite furnace). Mainframe conditions:
Wavelength: 283.3nm, lamp current 3.5mA, slit 1.0, background subtraction with an oxygen lamp. Graphite furnace determination conditions are shown in Table A1.
Atomization
A1.2 A 10μL microinjector.
A1.3 A magnetic stirrer.
A1.4 A thousandth balance.
A1.5 A 50mL pipette.
A1.6 Several 100mL beakers.
A1.7 1:1 nitric acid (superior grade).
Temperature, ℃
90~120
Holding time, s
Heating rate, C/s
A1.8 Lead standard stock solution: Weigh 0.1598g of lead nitrate, dissolve it with an appropriate amount of 1:1 nitric acid, and dilute it to 1000mL with distilled water. The concentration of the solution is 100 μg/mL.
A1.9 Dilution: Take an appropriate amount of agar, ammonium dihydrogen phosphate, and release agent and dilute it to a certain volume with distilled water. A2 Sample treatment
Take 1 tube of sample toothpaste, weigh 2.00g of toothpaste from it and place it in a 100mL beaker, add 50mL of diluent and 1.0mL of 1:1 nitric acid, and stir on a magnetic stirrer until it becomes a uniform solution (about 20 min). A3 Sample determination
While the sample is being stirred on a magnetic stirrer, use a microinjector to draw 10uL (do not draw in bubbles), immediately inject it into the graphite tube, start the graphite furnace switch, measure the sample, and record the absorption value. Perform a blank test at the same time. A4 Drawing of the standard curve
According to the absorption value of the sample, prepare 35 lead standard solutions of corresponding concentrations, measure their absorption values, subtract the blank absorption value, and draw a concentration and absorption value curve.
A5 Result calculation
Subtract the blank absorption value from the sample absorption value, check the standard curve to get the corresponding concentration, and multiply it by the dilution multiple to get the lead content (mg/kg) in the sample toothpaste.
Where: X-lead content in toothpaste, ng/kg; 30.4
X=K·c
（A1）2. The total qualified rate is 10%. Then, two boxes are randomly selected from each box, and then the same number of sticks are taken from each box, so that the total number of samples is not less than 40 sticks.
6.2.3 If the inspection fails, samples can be taken from two boxes of samples and the unqualified items can be re-inspected. If the re-inspection result is still unqualified, the batch of products will be judged to be unqualified.
6.2.4 If the delivery parties have objections to the inspection results, they can request arbitration inspection, and the arbitration result shall be the final basis. 7 Marking, packaging, transportation and storage
7.1 Marking
7.1.1 The sales packaging shall have the following markings:
a) Product name and trademark;
b) Net content;
c) Manufacturer name and address;
d) Standard number adopted;
e) Shelf life, production date or limited use date; f) Fragrance.
7.1.2 The large package should have the following signs:
a) Product name;
b) Manufacturer name and address;
c) Packing quantity and gross weight;
d) Date of manufacture;
GB 8372--2001
e) Packing box specifications [length (mm)) × width (mm) × height (mm)]; f) "moisture-proof", "handle with care", "prevent inversion" and other words. 7.2 Packaging and packaging type
Under the condition that the product quality is not damaged, the product packaging form and packaging materials shall be determined by the enterprise. The box should be filled with no gaps and the product certificate should be placed.
7.3 Transportation
The products must be loaded and unloaded with care and stacked according to the arrows on the boxes to avoid violent movement, collision and sun and rain. 7.4 Storage
7.4.1 It should be stored in a ventilated and dry warehouse with a temperature not higher than 40℃, not near water sources and heating. When stacking, it must be 20cm from the ground and 50cm from the wall. There should be a passage in the middle. Stack according to the arrows on the boxes. It must not be stacked upside down. The stacking height should not exceed 2.5m. 7.4.2 Shelf life
The date should be marked on the visible surface. There are two marking methods: a) The shelf life must be marked with the production date, marked in the order of year and month, and cannot be reversed. The year must be 4 digits, such as 2000; b) Restricted use date and production batch number;
The shelf life is determined by the enterprise, but it cannot exceed five years at most. 303
A1 Instruments and reagents
GB 8372—2001
Appendix A
(Suggested Appendix)
Determination of lead content by direct sampling in graphite furnace
A1.1 Atomic absorption spectrometer (with CXR90 graphite furnace). Mainframe conditions:
Wavelength: 283.3nm, lamp current 3.5mA, slit 1.0, background subtraction with an oxygen lamp. Graphite furnace determination conditions are shown in Table A1.
Atomization
A1.2 A 10μL microinjector.
A1.3 A magnetic stirrer.
A1.4 A thousandth balance.
A1.5 A 50mL pipette.
A1.6 Several 100mL beakers.
A1.7 1:1 nitric acid (superior grade).
Temperature, ℃
90~120
Holding time, s
Heating rate, C/s
A1.8 Lead standard stock solution: Weigh 0.1598g of lead nitrate, dissolve it with an appropriate amount of 1:1 nitric acid, and dilute it to 1000mL with distilled water. The concentration of the solution is 100 μg/mL.
A1.9 Dilution: Take an appropriate amount of agar, ammonium dihydrogen phosphate, and release agent and dilute it to a certain volume with distilled water. A2 Sample treatment
Take 1 tube of sample toothpaste, weigh 2.00g of toothpaste from it and place it in a 100mL beaker, add 50mL of diluent and 1.0mL of 1:1 nitric acid, and stir on a magnetic stirrer until it becomes a uniform solution (about 20 min). A3 Sample determination
While the sample is being stirred on a magnetic stirrer, use a microinjector to draw 10uL (do not draw in bubbles), immediately inject it into the graphite tube, start the graphite furnace switch, measure the sample, and record the absorption value. Perform a blank test at the same time. A4 Drawing of the standard curve
According to the absorption value of the sample, prepare 35 lead standard solutions of corresponding concentrations, measure their absorption values, subtract the blank absorption value, and draw a concentration and absorption value curve.
A5 Result calculation
Subtract the blank absorption value from the sample absorption value, check the standard curve to get the corresponding concentration, and multiply it by the dilution factor to get the lead content (mg/kg) in the sample toothpaste.
Where: X-lead content in toothpaste, ng/kg; 30.4
X=K·c
（A1）2. The total qualified rate is 10%. Then, two boxes are randomly selected from each box, and then the same number of sticks are taken from each box, so that the total number of samples is not less than 40 sticks.
6.2.3 If the inspection fails, samples can be taken from two boxes of samples and the unqualified items can be re-inspected. If the re-inspection result is still unqualified, the batch of products will be judged to be unqualified.
6.2.4 If the delivery parties have objections to the inspection results, they can request arbitration inspection, and the arbitration result shall be the final basis. 7 Marking, packaging, transportation and storage
7.1 Marking
7.1.1 The sales packaging shall have the following markings:
a) Product name and trademark; bzxZ.net
b) Net content;
c) Manufacturer name and address;
d) Standard number adopted;
e) Shelf life, production date or limited use date; f) Fragrance.
7.1.2 The large package should have the following signs:
a) Product name;
b) Manufacturer name and address;
c) Packing quantity and gross weight;
d) Date of manufacture;
GB 8372--2001
e) Packing box specifications [length (mm)) × width (mm) × height (mm)]; f) "moisture-proof", "handle with care", "prevent inversion" and other words. 7.2 Packaging and packaging type
Under the condition that the product quality is not damaged, the product packaging form and packaging materials shall be determined by the enterprise. The box should be filled with no gaps and the product certificate should be placed.
7.3 Transportation
The products must be loaded and unloaded with care and stacked according to the arrows on the boxes to avoid violent movement, collision and sun and rain. 7.4 Storage
7.4.1 It should be stored in a ventilated and dry warehouse with a temperature not higher than 40℃, not near water sources and heating. When stacking, it must be 20cm from the ground and 50cm from the wall. There should be a passage in the middle. Stack according to the arrows on the boxes. It must not be stacked upside down. The stacking height should not exceed 2.5m. 7.4.2 Shelf life
The date should be marked on the visible surface. There are two marking methods: a) The shelf life must be marked with the production date, marked in the order of year and month, and cannot be reversed. The year must be 4 digits, such as 2000; b) Restricted use date and production batch number;
The shelf life is determined by the enterprise, but it cannot exceed five years at most. 303
A1 Instruments and reagents
GB 8372—2001
Appendix A
(Suggested Appendix)
Determination of lead content by direct sampling in graphite furnace
A1.1 Atomic absorption spectrometer (with CXR90 graphite furnace). Mainframe conditions:
Wavelength: 283.3nm, lamp current 3.5mA, slit 1.0, background subtraction with an oxygen lamp. Graphite furnace determination conditions are shown in Table A1.
Atomization
A1.2 A 10μL microinjector.
A1.3 A magnetic stirrer.
A1.4 A thousandth balance.
A1.5 A 50mL pipette.
A1.6 Several 100mL beakers.
A1.7 1:1 nitric acid (superior grade).
Temperature, ℃
90~120
Holding time, s
Heating rate, C/s
A1.8 Lead standard stock solution: Weigh 0.1598g of lead nitrate, dissolve it with an appropriate amount of 1:1 nitric acid, and dilute it to 1000mL with distilled water. The concentration of the solution is 100 μg/mL.
A1.9 Dilution: Take an appropriate amount of agar, ammonium dihydrogen phosphate, and release agent and dilute it to a certain volume with distilled water. A2 Sample treatment
Take 1 tube of sample toothpaste, weigh 2.00g of toothpaste from it and place it in a 100mL beaker, add 50mL of diluent and 1.0mL of 1:1 nitric acid, and stir on a magnetic stirrer until it becomes a uniform solution (about 20 min). A3 Sample determination
While the sample is being stirred on a magnetic stirrer, use a microinjector to draw 10uL (do not draw in bubbles), immediately inject it into the graphite tube, start the graphite furnace switch, measure the sample, and record the absorption value. Perform a blank test at the same time. A4 Drawing of the standard curve
According to the absorption value of the sample, prepare 35 lead standard solutions of corresponding concentrations, measure their absorption values, subtract the blank absorption value, and draw a concentration and absorption value curve.
A5 Result calculation
Subtract the blank absorption value from the sample absorption value, check the standard curve to get the corresponding concentration, and multiply it by the dilution factor to get the lead content (mg/kg) in the sample toothpaste.
Where: X-lead content in toothpaste, ng/kg; 30.4
X=K·c
（A1）0mL1:1 nitric acid, stir on a magnetic stirrer until it becomes a uniform solution (about 20 min). A3 Sample determination
While the sample is stirred on a magnetic stirrer, use a microinjector to draw 10uL (do not draw in bubbles), immediately inject it into the graphite tube, start the graphite furnace switch, measure the sample, and record the absorption value. Perform a blank test at the same time. A4 Drawing of the standard curve
According to the absorption value of the sample, prepare 35 lead standard solutions of corresponding concentrations, measure their absorption values, subtract the blank absorption value, and draw a concentration and absorption value curve.
A5 Result calculation
Subtract the blank absorption value from the sample absorption value, check the standard curve to get the corresponding concentration, and multiply it by the dilution multiple, which is the lead content in the sample toothpaste (mg/kg).
Where: X-lead content in toothpaste, ng/kg; 30.4
X=K·c
（A1）0mL1:1 nitric acid, stir on a magnetic stirrer until it becomes a uniform solution (about 20 min). A3 Sample determination
While the sample is stirred on a magnetic stirrer, use a microinjector to draw 10uL (do not draw in bubbles), immediately inject it into the graphite tube, start the graphite furnace switch, measure the sample, and record the absorption value. Perform a blank test at the same time. A4 Drawing of the standard curve
According to the absorption value of the sample, prepare 35 lead standard solutions of corresponding concentrations, measure their absorption values, subtract the blank absorption value, and draw a concentration and absorption value curve.
A5 Result calculation
Subtract the blank absorption value from the sample absorption value, check the standard curve to get the corresponding concentration, and multiply it by the dilution multiple, which is the lead content in the sample toothpaste (mg/kg).
Where: X-lead content in toothpaste, ng/kg; 30.4
X=K·c
（A1）
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