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GB 24567-2009: Sodium monofluorophosphate for tooth-paste industry
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Sodium monofluorophosphate for tooth-paste industry
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GB 24567-2009
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Basic data | Standard ID | GB 24567-2009 (GB24567-2009) | | Description (Translated English) | Sodium monofluorophosphate for tooth-paste industry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G12 | | Classification of International Standard | 71.060.50 | | Word Count Estimation | 11,170 | | Date of Issue | 2009-10-30 | | Date of Implementation | 2010-06-01 | | Quoted Standard | GB/T 191-2008; GB/T 610-2008; GB/T 6678; GB/T 6682-2008; HG/T 3696.1; HG/T 3696.2; HG/T 3696.3 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2009 (No. 152 overall) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard specifies the use of sodium monofluorophosphate toothpaste industry requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage. This standard applies to industrial use sodium monofluorophosphate toothpaste. The product is used as anti-caries toothpaste processing agents, desensitizing additives in fungicides and preservatives. | GB 24567-2009: Sodium monofluorophosphate for tooth-paste industry---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Sodium monofluorophosphate for tooth-paste industry
ICS 71.060.50
G12
National Standards of People's Republic of China
Toothpaste industrial monofluorophosphate
Posted 2009-10-30
2010-06-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
The standard Chapter 4 and Chapter 7 are mandatory content, the rest are recommended.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee chemical inorganic chemicals Club (SAC/TC63/SC1) centralized.
This standard was drafted. Institute of Physical and Chemical Engineering of Nuclear Industry China Nuclear New Technology Development Company, CNOOC Tianjin Chemical Research & Design Institute.
The main drafters of this standard. Li Guangming, Zhou Hongyan, Gao Jian, Fan Wenjun.
This standard is the first release.
Toothpaste industrial monofluorophosphate
1 Scope
This standard specifies the toothpaste industry monofluorophosphate requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage.
This standard applies to industrial use toothpaste monofluorophosphate. The product is used as an anti-caries agents in toothpaste processing, desensitizing additive, also used for sterilization
And preservatives.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
GB/T 191-2008 Packaging - Pictorial signs (ISO 780.1997, MOD)
GB/T 610-2008 General method for determination of arsenic chemical reagents
GB/T 6678 General Principles for Sampling Chemical Products
GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD)
Preparation of standard titration solution of HG/T 3696.1 inorganic chemical products, chemical analysis
Preparation of HG/T 3696.2 inorganic chemical products, chemical analysis of impurity standard solution
Preparations of HG/T 3696.3 inorganic chemical products, chemical analysis
3 formula and relative molecular mass
Molecular formula. Na2PO3F
Molecular weight. 143.95 (according to 2007 international relative atomic mass)
4 Requirements
4.1 Appearance. white powder.
4.2 Toothpaste industrial monofluorophosphate should meet the requirements of Table 1.
Table 1 Requirements
Item Index
Sodium monofluorophosphate (in Na2PO3F dollars), /% ≥ 95.0
Of combined fluorine (as F), /% ≥ 12.54
Free fluorine (as F), /% ≤ 0.68
Total Fluoride (as F), /% ≥ 13.0
Arsenic (As), /% ≤ 0.0002
Heavy metals (Pb), /% ≤ 0.002
Lead (Pb), /% ≤ 0.0002
Water-insoluble, /% ≤ 0.15
pH value (20g/L solution) 6.5-8.0
Loss on drying, /% ≤ 0.2
5 Test methods
5.1 Safety Tips
Reagents used in this test method are toxic or corrosive, be careful when operating! Such as water splashed on the skin should immediately
Flushing, severe cases should be treated immediately.
5.2 General Provisions
This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in
water. Test with the standard titration solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according
HG/T 3696.1, HG/T 3696.2, HG/T 3696.3 regulations in preparation.
5.3 Visual inspection
In natural light, determined by visual appearance.
5.4 Determination of the content of sodium monofluorophosphate
Monofluorophosphate content of sodium monofluorophosphate (Na2PO3F) mass fraction of 1 meter, expressed in%, according to equation (1).
A = 7.5772 (1)
Where.
2 --- combined with fluorine content, expressed in%;
7.577 --- fluorine converted into sodium monofluorophosphate coefficients.
5.5 Determination of fluorine content in combination
Combined with a fluorine content of fluorine (F) mass fraction 2 and its value is expressed in%, according to equation (2).
2 = 4-3 (2)
Where.
3 --- free fluoride content, expressed in%;
4 --- total fluorine content, the value expressed in%.
5.6 Determination of free fluorine content
5.6.1 Method summary
Sample in acid medium to fluoride ion selective electrode as indicator electrode, a saturated calomel electrode as the reference electrode, measurement test solution
Liquid fluoride concentration.
5.6.2 Reagents and materials
5.6.2.1 sodium nitrate solution. 30g/L;
5.6.2.2 nitric acid solution. 1 + 150;
5.6.2.3 hexamethylenetetramine solution. 50g/L;
5.6.2.4 fluoro standard solution. 1mL solution containing fluorine (F) 1mg;
Refining. two water in a plastic beaker with GB/T 6682-2008 predetermined dissolving sodium fluoride, make a saturated solution. Removed by filtration
Insoluble materials, the filtrate was added ethanol to precipitate sodium fluoride. The resulting crystals were filtered and washed with absolute ethanol and crystallized placed 105 ℃ ~
Electric oven 110 ℃, the drying to constant mass.
Weigh 0.2210g NaF (refined) (accurate to 0.0002g), dissolved in water, all transferred to 100mL volumetric flask, dilute with water
Release to the mark. Store in plastic bottle.
5.6.2.5 fluoro standard solution. 1mL solution containing fluorine (F) 0.1mg;
Pipette Pipette 10mL fluoro standard solution (5.6.2.4), placed in 100mL flask, diluted with water to the mark. Storage
Plastic bottle.
5.6.2.6 fluoro standard solution. 1mL solution containing fluorine (F) 0.01mg.
Pipette Pipette 10mL fluoro standard solution (5.6.2.5) into 100mL volumetric flask, dilute to the mark, shake. Storage
In a plastic bottle (the solution is valid for 10d).
5.6.3 instruments and equipment
5.6.3.1 digital ion meter or pH meter. Accuracy ± 0.5%;
5.6.3.2 fluoride ion selective electrode;
5.6.3.3 calomel electrode;
5.6.3.4 magnetic stirrer.
5.6.4 Analysis of step
5.6.4.1 Preparation of test solution
Weigh about 0.2g sample, accurate to 0.0002g, set 50mL volumetric flask, add 5mL dissolved in water, were added with a pipette
5mL diluted sodium nitrate solution and 5mL hexamethylenetetramine solution, plus 5mL nitric acid solution, add water to the mark.
5.6.4.2 Preparation of the calibration standard solution with fluorine
Each pipette Pipette 25mL fluoro standard solution (5.6.2.5) and fluorine standard solution (5.6.2.6), were placed in two 50mL capacity
Bottle with pipette add 5mL nitrate solution and 5mL hexamethylenetetramine solution, 5mL nitric acid solution was added to adjust the pH of the solution
To 5-6, dilute to the mark. They were transferred to two drying plastic bottles.
5.6.4.3 Determination
Open digital ion meter, connect the electrode, press the mode key "MODE" until "CONC" mode indication, adjust the instrument temperature
Room temperature. According to double standards into law, carried out by the above calibration slope calibration and positioning fluoro standard solution.
The test solution was poured into a plastic beaker, under stirring after equilibrium 4min, was measured.
5.6.5 Calculation Results
Free fluorine content of fluorine (F) the mass fraction of 3 and its value is expressed in%, according to equation (3) Calculated.
3 = ρ × Vp × 10
-3
(3)
Where.
ρ --- Numerical test solution was measured fluoride ion concentration, in milligrams per milliliter (mg/mL);
Numerical volume Vp --- test solution, in milliliters (mL);
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.01%.
5.7 Determination of total fluorine content
5.7.1 Method summary
The test solution was pre-hexamethyldisilazane by perchloric acid saturated ether acidification, the formation of a hydrophobic fluorine-trimethyl silane, diffusion is a basic solution
Absorption, hydrolysis of F ions in the absorbing solution to the fluoride ion selective electrode as measuring electrode, a saturated calomel electrode as the reference electrode, measured
Test fluoride ion concentration in the solution.
5.7.2 Reagents
5.7.2.1 sodium hydroxide solution. 4g/L;
5.7.2.2 nitric acid solution. 1 + 150;
5.7.2.3 perchlorate hexamethyldisilazane ether saturated solution;
The 100mL perchloric acid solution (1 + 3.3) poured into a 175mL separating funnel, add 50mL hexamethyl ether by vigorous shaking
After placing stratification, the lower is the perchlorate hexamethyldisilazane saturated ether solution.
5.7.2.4 hexamethylenetetramine solution. 15g/L.
5.7.3 instruments and equipment
5.7.3.1 digital ion meter or pH meter. Accuracy ± 0.5%;
5.7.3.2 fluoride ion selective electrode;
5.7.3.3 calomel electrode;
5.7.3.4 magnetic stirrer;
5.7.3.5 diffusion chamber. made of teflon or polypropylene round (see Figure 1).
a) Diffusion cover. 110mm × 20mm;
b) diffusion chamber. 110mm × 60mm;
c) absorption cell. L × S × H = 75mm × 50mm × 35mm.
1 --- diffusion cover;
2 --- diffusion chamber;
3 --- absorption cell.
Figure 1 diffusion chamber
5.7.4 Analysis of step
5.7.4.1 Preparation of test solution
Weigh about 0.2g sample, accurate to 0.0002g, placed in 100mL beaker, dissolved in water, all transferred to 250mL volumetric flask
Diluted with water to the mark.
Pipette pipette 5mL test solution was placed in the left side of the diffusion chamber (inclined 30o diffuser plate should be placed into three compartments). Pipette
Pipette tube 5mL sodium hydroxide solution was placed in the middle chamber diffusion chamber. Take about 13mL of perchloric acid hexamethyl ether saturated solution was placed diffusion
Box on the right. The interface diffusion chamber vacuum grease or Vaseline smeared with reclosable lid sealed. The diffusion box placed on the swing meter shaking 2h (again
Place 24h).
5.7.4.2 Determination
Open digital ion meter, connect the electrode, press the mode key "MODE" until "CONC" mode indication, adjust the instrument temperature
Room temperature. According to double standards into law, carry out calibration and positioning slope calibration with fluoride standard solution (5.6.4.2).
The diffusion box is opened, the middle chamber with a pipette add 5mL hexamethylenetetramine buffer and 5mL nitric acid solution to adjust the pH of the solution
To 5-6, after stirring state balance 4min, were measured.
5.7.5 Calculation Results
The total fluorine content of fluorine (F) the mass fraction of 4 and its value is expressed in%, according to equation (4) Calculated.
4 = ρ × Vp × 10
-3
× 100 (4)
Where.
ρ --- Numerical test solution was measured fluoride ion concentration, in milligrams per milliliter (mg/mL);
Vp --- diffusion chamber value of the total volume of liquid in the intermediate chamber, in milliliters (mL);
Vp 1 --- numerical diffusion box test solution volume in milliliters (mL);
2 --- value Vp of the total volume of the test solution, in milliliters (mL of);
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.2%.
5.8 Determination of Arsenic
5.8.1 Method summary
With GB/T 610-2008 4.1.1.
5.8.2 Reagents
With GB/T 610-2008 in Chapter 3.
Arsenic standard solution. 1mL solution containing arsenic (As) 0.001mg.
Pipette Pipette 1mL arsenic standard solution according to HG/T 3696.2 prepared, placed in 1000mL volumetric flask, dilute to the mark with water
Degree, shake.
5.8.3 Instruments
With GB/T 610-2008 in 4.1.2.
5.8.4 Analysis of step
Weigh accurately 1.0g ± 0.001g sample placed in 100mL beaker, add 50mL water, the following press GB/T 610-2008 in
4.1.3 "plus 6mL hydrochloride" operation. The test solution was the color can not be deeper than the standard.
Standard with a pipette of 2mL arsenic standard solution, and treated in the same sample at the same time.
5.9 Determination of Heavy Metal Content
5.9.1 Method summary
In acidic medium, heavy metal ions in the sample with sodium sulfide and generated brown by comparison with standard color solution, to determine a sample
The content of heavy metals.
5.9.2 Reagents
5.9.2.1 nitrate solution. 1 + 1;
5.9.2.2 ammonia solution. 2 + 3;
5.9.2.3 glacial acetic acid. 2 + 1;
5.9.2.4 sodium sulfide solution;
5.9.2.5 Lead standard solution. 1mL solution containing lead (Pb) 0.01mg.
Pipette Pipette 1mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark with water
Degree, shake.
5.9.3 Analysis of step
5.9.3.1 Preparation of test solution
Weigh accurately 1.0g ± 0.01g sample was placed in 100mL beaker, add 10mL water and 0.5mL nitric acid solution, aqueous ammonia solution
Adjusted to pH≈5 (precision strip test).
5.9.3.2 Determination
The test solution was fully transferred to 50mL colorimetric tube, add 0.5mL acetic acid solution, add water to about 50mL, add 3 drops of vulcanization
Soda solution, shake, in the dark place 10min, compared with the lead standard colorimetric solution.
Standard colorimetric solution with a pipette of 2mL lead standard solution, and treated in the same sample at the same time.
5.10 Determination of lead content
5.10.1 Method summary
After the sample is dissolved in dilute acid, into the atomic absorption spectrophotometer (graphite furnace), and after electrothermal atomic absorption 283.3nm resonance line,
In a certain concentration range, the absorption values of lead content in line with Lambert - Beer law, compared with standard series quantitation.
5.10.2 Reagent
5.10.2.1 nitric acid;
5.10.2.2 nitrate solution. 1 + 5;
5.10.2.3 nitric acid solution. 3 + 97;
5.10.2.4 nitric acid - perchloric acid mixture. Vp (HNO3). Vp (HclO4) = 4.1;
5.10.2.5 Lead standard solution. 1mL solution containing lead (Pb) 0.01mg;
Pipette Pipette 1mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark with water
Degree, shake.
5.10.2.6 Lead standard solution.
Pipette 1.00mL, 2.00mL, 4.00mL lead standard solution (5.10.2.5) were placed in 100mL flask, add nitric acid solution
(5.10.2.3) diluted to the mark. Per ml solution of lead (Pb) were 0.0001mg, 0.0002mg, 0.0004mg.
5.10.2.7 water; meet GB/T 6682-2008 the provisions of secondary water.
5.10.3 instruments and equipment
5.10.3.1 The glassware is required to nitric acid solution (5.10.2.2) soaked overnight with water repeatedly washed with deionized water will Xian
clean;
5.10.3.2 atomic absorption spectrophotometer (with furnace and lead hollow cathode lamp).
5.10.4 analysis step
5.10.4.1 Preparation of test solution
Weigh the sample 1.0g, set 10mL volumetric flask, add water and 0.2mL nitric acid - perchloric acid mixture, diluted with water to the mark,
Shake well.
Preparation 5.10.4.2 blank test solution
But without addition of the sample, the preparation of the test solution and other operations at the same time in the same manner.
5.10.4.3 Determination
According to their instrument performance to an optimal state.
Draw standard curve. Pipette formulated above lead standard solution injected into the furnace, measured obtaining absorbance values obtained absorbance and concentration
Relationship linear regression equation.
Sample assay. Pipette test solution and the blank test solution injected into the graphite furnace, obtaining the measured absorbance values, substituting one yuan line standard series
Regression equation obtained sample solution of lead content.
5.10.5 Calculation Results
Lead in lead (Pb) mass fraction 5 and its value is expressed in%, according to equation (5) Calculated.
5 =
(Ba Ba 1- 0) × Vp × 10-6
(5)
Where.
Numerical test solution Ba 1 --- lead concentration in micrograms per milliliter (μg/mL);
Ba 0 --- numerical test blank solution lead concentration in micrograms per milliliter (μg/mL);
Numerical volume Vp --- test solution, in milliliters (mL);
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.0001%.
5.11 Determination of Water-insoluble content
5.11.1 Method summary
Samples were dissolved in water, sintered glass crucible by the insolubles were filtered off, residue was washed with water, dried and the mass balance that can be used insolubles.
5.11.2 instruments and equipment
5.11.2.1 sintered glass crucible. filter plate pore size of 5μm ~ 15μm;
5.11.2.2 electric oven. temperature can be controlled at 105 ℃ ± 2 ℃.
5.11.3 analysis step
It weighs about 10g sample, accurate to 0.0002g, placed in 100mL beaker, add 30mL water 60 ℃ ~ 70 ℃ dissolved with stirring.
Has been used in 105 ℃ ± 2 ℃ electric oven drying to constant quality glass crucible sand filtration, washed with hot water insolubles, each with 20mL
Water, washed five times, placed in 105 ℃ ± 2 ℃ in electric oven, and dried to a constant mass.
5.11.4 Calculation Results
Water-insoluble mass fraction 6 and its value is expressed in%, according to equation (6) Calculated.
(6)
Where.
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.01%.
5.12.1 Method summary
The glass electrode and a reference electrode immersed in the test solution, constitute a galvanic cell potential and pH of the solution is related by measuring the original
The potential of the battery can be derived pH of the solution.
5.12.2 instruments and equipment
.( PH meter with a glass electrode, calomel electrode or composite electrode) accuracy 0.1pH units.
5.12.3 analysis step
Weigh accurately 2.0g ± 0.01g sample was placed in 150mL beaker, add 100mL water dissolved, it has been corrected acidimeter
pH value of the solution.
Determination of loss on drying of 5.13
5.13.1 Method summary
Drying the sample at a certain temperature in order to reduce the quality of the sample to calculate the drying loss.
5.13.2 Instruments
Electric oven. temperature can be controlled at 105 ℃ ± 2 ℃.
5.13.3 analysis step
Use has been dried to a constant mass of 105 ℃ ± 2 ℃ weighing bottle Weigh about 5g samples, accurate to 0.0002g, placed in 105 ℃ ±
2 ℃ electric oven, and dried to a constant mass.
5.13.4 Calculation Results
Drying loss mass fraction 7 and its value is expressed in%, according to equation (7) Calculated.
(7)
Where.
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.01%.
6 Inspection rules
6.1 standard indicators for the projects listed in the type test and factory inspection items items.
6.1.1 Type inspection
Book GB 24567-2009
All indicators project requirements prescribed for type test project, under normal circumstances, at least once every three months the type test. Have
When one of the following conditions must be type tested.
a) update key production process;
b) The main raw material change;
c) Discontinued resumed production;
d) are quite different and the last type inspection;
Provisions e) contract.
6.1.2 factory inspection
Monofluorophosphate requirements prescribed in combination fluorine, fluorine-free, total fluorine, pH and total loss on drying factory inspection items for the six indicators,
Batch should be tested.
6.2 Manufacturer of the same material, the same basic production conditions, continuous production or the same team produced toothpaste industrial monofluorophosphate
One batch, each batch of products shall not exceed 5t.
6.3 determine the sampling units according to GB/T 6678 provisions. Sampling, the sampler from the bag to a central vertical insertion depth of the material layer
3/4 of the sampling. The sample was taken out of the mix, with a quartering reduced to less than 500g. The samples were packed in two clean, dry density
Sealed containers, seal and label, indicating the manufacturer's name, product name, batch number, date of sampling and sampling by name. One for test
Use, and a second copy for future reference, save time is determined by the manufacturer according to the actual situation.
6.4 Toothpaste industrial monofluorophosphate by the manufacturer's quality supervision and inspection department inspection in accordance with this standard, the manufacturer shall ensure that
All manufactured products are in line with the requirements of this standard.
6.5 If the test results do not meet the requirements of this standard indicators should be twice the amount of packaging from re-sampling retest, retest results even with
When an indicator does not meet the requirements of this standard, the entire batch of products to be ineligible.
7 signs, labels
7.1 Industrial toothpaste on monofluorophosphate containers should be fixed and clear signs, including. manufacturer's name and address, product name, net
Content, batch number or production date, shelf life, and this standard number GB/T 191-2008 stipulated "afraid of the rain" signs.
7.2 each batch of toothpaste industrial monofluorophosphate should be accompanied by a certificate of quality, including. manufacturer's name and address, product name, net
Proof of content, batch number or production date, shelf life, quality of products conforming to this standard and this standard number.
8 packaging, transportation, storage
8.1 Toothpaste industrial applications monofluorophosphate double polyethylene film bags for packaging, packaging for paper-plastic bag. Net weight
25kg. Heat inside the bag; outer bag should be firmly sewn. Users have special requirements, supply and demand consultation.
8.2 Industrial monofluorophosphate dentifrice during transport to prevent rain, packaging can not be damaged.
8.3 Toothpaste industrial monofluorophosphate be stored in dry and ventilated warehouse, and the need to have a cushion to prevent moisture.
8.4 Toothpaste industrial monofluorophosphate in line with the standard packaging, transportation, storage conditions, from the date of production of a usable life of 18 months.
Overdue should re-examine whether the requirements of this standard.
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