GB 24568-2009 English PDFUS$399.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 24568-2009: Calcium hydrogen phosphate for tooth-paste industry Status: Valid
Basic dataStandard ID: GB 24568-2009 (GB24568-2009)Description (Translated English): Calcium hydrogen phosphate for tooth-paste industry Sector / Industry: National Standard Classification of Chinese Standard: G12 Classification of International Standard: 71.060.50 Word Count Estimation: 17,197 Date of Issue: 2009-10-30 Date of Implementation: 2010-06-01 Quoted Standard: GB/T 191-2008; GB/T 3049-2006; GB/T 6003.1-1997; GB/T 6678; GB/T 6682-2008; GB/T 7917.2-1987; GB/T 7918.2; GB/T 7918.3; GB/T 7918.4; GB/T 7918.5; GB/T 8170; GB/T 9086-2007; HG/T 3696.2; HG/T 3696.3; HG/T 3696.1 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 toothpaste industry with DCP requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage. This standard applies to industrial use toothpaste DCP. The product is mainly used as toothpaste friction agent. GB 24568-2009: Calcium hydrogen phosphate 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.Calcium hydrogen phosphate for tooth-paste industry ICS 71.060.50 G12 National Standards of People's Republic of China Industrial toothpaste DCP 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 ForewordThis standard Chapters 4 and 7 chapters are mandatory, others 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. CNOOC Tianjin Chemical Research Institute, Yunnan days Technology Co., Ltd., Hubei Xingfa Chemical Group shares have Ltd., Yunnan Province Chemical Research Institute, Lianyungang Debang Fine Chemical Co., Ltd. Drafters of this standard. Li Guangming, Guo Yongxin, Long Ping, Xiong Ping, Huangqian Jun, Liu Zhen. This standard is the first release. Industrial toothpaste DCP1 ScopeThis standard specifies the toothpaste industry with calcium hydrogen phosphate (also known as. calcium hydrogen phosphate dihydrate toothpaste, toothpaste or toothpaste dicalcium phosphate dihydrate Dicalcium) requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage. This standard applies to industrial use toothpaste DCP. The products are mainly used as toothpaste friction agent.2 Normative referencesThe 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 research in accordance with this standard agreement Study 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 3049-2006 industrial chemical products used in the general method of determination of iron content 1,10 Philippines spectrophotometry method (ISO 6685. 1982, IDT) GB/T 6003.1-1997 Test sieves of metal wire cloth GB/T 6678 General Principles for Sampling Chemical Products GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD) GB/T 7917.2-1987 Standard Test Method cosmetics health chemical arsenic Total number of bacteria GB/T 7918.2 Cosmetics Standard methods of microbiological assay GB/T 7918.3 Cosmetics Standard methods of microbiological faecal coliforms GB/T 7918.4 Cosmetics Standard methods of microbiological Pseudomonas aeruginosa GB/T 7918.5 Cosmetics Standard methods of microbiological Staphylococcus aureus GB/T 8170 repair value expressed about the rules and limit values and judgment GB/T 9086-2007 standard for white color and photometry 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 analysis3 formula and relative molecular massFormula. CaHPO4 · 2H2O Molecular weight. 172.09 (according to 2007 international relative atomic mass)4 Requirements4.1 Appearance. white powder. 4.2 Toothpaste industrial DCP is divided into two models. Ⅰ type --- fluorine stable calcium hydrogen phosphate; Ⅱ type --- Normal DCP. 4.3 DCP toothpaste industry should meet the requirements of Table 1. Table 1 Requirements project index Fluorine stable common type Calcium oxide (CaO), /% 31.4 ~ 32.9 Phosphorus pentoxide (P2O5), /% 40.7 ~ 42.5 Whiteness (Wg)/degree ≥ 93 pH (20% suspension) of 6.8 to 8.1 Fineness (< 45μm), /% ≥ 99.0 Product water absorption capacity of 20g/mL 5.0 ~ 6.5 Apparent density, ρ/(g/cm 3) 0.80 to 1.00 Stability tests by Fluoride Stability Test by Test - Loss on ignition, /% 25.0 to 26.5 60 ℃ Loss on drying, /% ≤ 0.6 Heavy metals (Pb), /% ≤ 0.002 Arsenic (As), /% ≤ 0.0003 Iron (Fe), /% ≤ 0.01 Fluoro (F), /% ≤ 0.005 Chloride (Cl dollars), /% ≤ 0.03 Carbonate by testing Sulfate, /% ≤ 0.5 Sulfide by test Hydrochloric acid insoluble matter, /% ≤ 0.2 Cfu/(a / g) ≤ 200 Fecal Coliform Not Detected Pseudomonas aeruginosa can not be detected Staphylococcus aureus not detected Molds and the total number of yeast/(a / g) ≤ 2005 Test methods5.1 Safety Tips Reagents used in this test method are toxic or corrosive, be careful when operating! As splashed on the skin or eyes should stand That is rinsed with water, severe cases should be treated immediately. 5.2 General Provisions This standard reagents and water, did not indicate when the other requirements, refer to three analytical reagent and GB/T 6682-2008 specified in water. Used in the test standard titration solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according to HG/T 3696.1, HG/T 3696.2, the provisions prepared HG/T 3696.3 of. 5.3 Visual inspection In natural light, determined by visual appearance. 5.4 Determination of calcium oxide content 5.4.1 Method summary In the test solution, adding an excess of disodium edetate solution, complexes with calcium to acid chrome blue K- naphthol green B as indicator solution, With zinc sulfate heptahydrate standard titration solution titrate excess of disodium edetate solution. 5.4.2 Reagents 5.4.2.1 hydrochloric acid solution. 1 + 4; 5.4.2.2 ammonia - ammonium chloride buffer solution A. pH≈10; 5.4.2.3 disodium edetate solution. Ba (EDTA) ≈0.05mol/L; 5.4.2.4 zinc sulfate heptahydrate standard titration solution. Ba (ZnSO4 · 7H2O) ≈0.05mol/L; Preparation. Weigh 15g of zinc sulfate heptahydrate, dissolved in water, diluted with water to 1000mL, shake. Calibration. Pipette Pipette 25mL zinc sulfate heptahydrate standard titration solution prepared, placed in a conical flask, add 10mL ammonia - chloride Ammonium buffer solution A and 75mL water, add about 0.02g chrome black T indicator, using 0.05mol/EDTA standard titration solution to titrate L Solution from purple to pure blue, and keep the 30s does not fade, is the end. At the same time a blank test. Zinc sulfate standard titration solution concentration heptahydrate (Ba) according to equation (1). Ba = (Vp 1- V0) Ba 1 (1) Where. Value Vp 1 --- titration consumed disodium edetate (EDTA) standard titration solution volume in milliliters (mL); V0 value standard titration solution volume consumed in the blank test --- disodium edetate (EDTA), milliliters (ML of); Ba 1 --- disodium edetate (EDTA) Standard Solution accurate value in units of moles per liter (mol/L); Pipette value Vp --- zinc sulfate heptahydrate standard titration solution volume in milliliters (mL). 5.4.2.5 Acid chrome blue K- naphthol green B mixed indicator solution (KB indicator solution). 5.4.3 Analysis of step Weigh about 0.4g samples, accurate to 0.0002g, placed in a beaker of 100mL, 12mL of hydrochloric acid was added to dissolve the solution, transferred to a 250mL volumetric flask, dilute to the mark, shake. Pipette 25mL of this solution in 250mL conical flask, with a pipette 25.00mL edetate disodium solution, 50 mL of water and 10mL of ammonia - ammonium chloride buffer solution A, was added 4 drops of placing 5min KB indicator solution with zinc sulfate heptahydrate standard titration solution titration until the solution changed from blue to purple, the purple does not disappear in the 30s is in the final point. While doing the blank test. In addition to the blank test without the sample, the addition of reagents and other operations of the kind and amount (other than the standard titration solution) with the same Test. 5.4.4 Calculation Results Calcium oxide content of calcium oxide (CaO) mass fraction of 1 meter, expressed in%, according to equation (2). 1 = [(Vp 0- Vp)/1000] Ba M 100 (2) Where. Numerical zinc sulfate heptahydrate standard titration solution volume Vp --- titration solution consumed in milliliters (mL); Numerical zinc sulfate heptahydrate standard titration solution volume V0 --- blank test consumed in milliliters (mL); Accurate Ba --- zinc sulfate heptahydrate standard titration solution concentration value in units of moles per liter (mol/L); --- The M value of calcium oxide (CaO) molar mass of the units of grams per mole (g/mol) (M = 56.08). Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results is not more than 0.2% absolute difference. 5.5 Determination of phosphorus pentoxide content 5.5.1 Method summary Is generated in the entire sample solution acidic hydrolysis of orthophosphate, is added after the solution Quimociac quinoline phosphomolybdate precipitate was filtered, washed, dried Dry, weighed. 5.5.2 Reagents 5.5.2.1 hydrochloric acid solution. 1 + 1; 5.5.2.2 nitric acid solution. 1 + 1; 5.5.2.3 Quimociac solution (ie, citric acid sodium molybdate solution); Press HG/T 3696.3 requirements formulated Quimociac solution. 5.5.3 Instruments 5.5.3.1 sintered glass crucible. pore size of 5μm ~ 15μm; 5.5.3.2 electric oven. the temperature can be controlled at 180 ℃ ± 5 ℃ or 250 ℃ ± 10 ℃. 5.5.4 Analysis of step 5.5.4.1 Preparation of test solution Weigh about 0.5g sample, accurate to 0.0002g, placed in 100mL beaker, add 5mL hydrochloric acid solution was dissolved and transferred to 250mL Volumetric flask, dilute to the mark, shake. 5.5.4.2 Determination Pipette pipette 25mL above test solution was placed in a beaker of 250mL, 10mL of nitric acid solution was added, water was added to a total volume of about 100mL. Cover the surface of the dish, slow boil 5min, added 50mL Quimociac solution was incubated 30s (plus reagent and heating can not be Open flame, add reagents or heating can not be stirred, so as not to generate a clot). Cooled to room temperature, the cooling process was stirred for 3 to 4 times. With advance 180 ℃ ± 5 ℃ or 250 ℃ ± 10 ℃ dried to a constant mass of sand glass crucible filtration of the supernatant, the precipitate was washed by decantation with 5-6 Times, each time with water to about 20mL. The precipitate was transferred to a sintered glass crucible, continue washing with water 3 to 4 times. The glass sand crucible together with precipitation Placed in 180 ℃ ± 5 ℃ the electric oven to bake for 45min or 250 ℃ ± 10 ℃ drying 15min, remove the coolish, placed in the dryer Cool to room temperature, weighing, accurate to 0.0002g. 5.5.5 Calculation Results Phosphorus pentoxide content of phosphorus pentoxide (P2O5) mass fraction 2 and its value is expressed in%, according to equation (3) Calculated. 2 = 100 (3) Where. 0.03207 --- Quinoline phosphomolybdate mass in terms of the quality factor of phosphorus pentoxide. Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results is not more than 0.2% absolute difference. 5.6.1 instruments and equipment 5.6.1.1 whiteness meter. with a standard whiteness plate and work whiteness plate, dividing the value of 0.2 degrees; 5.6.1.2 standard whiteness plate. meet the standard white powder or matte white ceramic standard GB/T 9086-2007 specified; 5.6.1.3 working standard whiteness plate. in line with GB/T 9086-2007 the provisions of glossy white ceramic standard plate. 5.6.2 Analysis of step Regularly calibrated with standard whiteness plate calibration working standard whiteness plate. Working standard whiteness plate meter to adjust the white working condition, The sample was evenly placed in a powder dish and the sample surface than powder dish about 2cm. With a smooth glass plate coated on the surface of the specimen, the pressure Tight sample, and rotate a little, you remove the glass; or pressure injector with constant pressure powder sample. Horizontally observe the specimen surface, should not without irregularities Ping, trace anomalies and defects. The sample pan is placed instruments on stage, measured whiteness, read standard to 0.1 degrees; the instrument will sample dish turntable at 90 °, measured whiteness, read Associate to 0.1 degrees; then rotate 90 °, measured whiteness, read standard to 0.1 degrees. Three readings result poor shall not exceed 0.5 degrees. Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results of absolute difference is not more than 1 degree. 5.7.1 Reagents Carbon dioxide-free water. 5.7.2 Instruments 5.7.2.1 pH meter. Indexing is 0.1pH units, with a glass electrode and a saturated calomel electrode; 5.7.2.2 magnetic stirrer and stir. 5.7.3 Analysis of step Weigh 10g sample accurately to 0.1g, placed in 100mL beaker, add 40mL carbon dioxide-free water, stir 15min After the pH was measured with pH meter test solutions. 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 0.2pH units. 5.8 Determination of fineness 5.8.1 instruments and equipment 5.8.1.1 Test sieves. meet GB/T 6003.1-1997 prescribed R40/3 series, the pore size of 45μm; 5.8.1.2 electric oven. the temperature can be controlled at 60 ℃ ± 2 ℃. 5.8.2 Analysis of step Weigh about 10g sample, accurate to 0.01g, has been placed at 60 ℃ ± 2 ℃ in electric oven baked to constant quality test sieves The test sieve with tap water samples to test sieve effluent water is clear so far. The test sieve together with the sieve residue together placed 60 ℃ ± 2 ℃ in electric oven, and bake 2h. 5.8.3 Calculation Results Fineness mass fraction 3 and its value is expressed in%, according to equation (4) Calculated. (4) Where. Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results is not more than 0.2% absolute difference. 5.9 Determination of water absorption 5.9.1 Method summary Dropping water on the sample and shaken to form unbreakable spherical water at this time is the amount of water absorbed dropping. 5.9.2 instruments and equipment 5.9.2.1 Pharmaceutical enamel cup. 250mL; 5.9.2.2 medicine with a stainless steel spatula. 5.9.3 Analysis of step Weigh 20g ± 0.01g sample was placed in a dry 250mL medicine enamel cup, each with burette dropping 3 to 4 drops of water again Like uniform absorption, and pharmaceutical with a stainless steel spatula stirring to form a (or several) sphere, the sphere is not broken end. The elimination Water absorption of the sample consumption milliliters of water is measured. The entire analysis process takes no more than 20min. Take the arithmetic mean of the parallel determination results of the measurement results. Two parallel determination results is not more than the absolute difference 0.5mL. Determination of 5.10 Apparent density 5.10.1 Method summary Will be equipped with a certain amount of the sample graduated cylinder landed 50 times, calculate the apparent density of the volume occupied by the powder. 5.10.2 instruments and equipment 5.10.2.1 cylinder. 250mL; 5.10.2.2 Landing Box. 220mm × 130mm × 130mm, the top aperture 55mm. 5.10.3 analysis step After mixing the 40g sample placed in 250mL graduated cylinder with rubber-stoppered bottle, the whereabouts of 50, down from 220mm. Every 2s Lifting once (by stopwatch control time). Doing a circular motion to lift the cylinder, an angle of about 10 ° of rotation of the cylinder, do not shake, flat Slow free-fall. This is done so that the powder in the cylinder can have a flat, easy to read volume. 5.10.4 Calculation Results The apparent density (ρ) in mass per unit volume represented by formula (5) Calculated. ρ = (5) Where. Vp --- sample value of the share volume in milliliters (mL). Stability Test 5.11 5.11.1 Method summary With glycerin solution sample into a paste, boiled, cooled and paste observe whether changes to determine their stability. 5.11.2 Reagent Glycerol solution. 17 + 3. 5.11.3 instruments and equipment Enamel cup. 50mL. 5.11.4 analysis step Weigh about 25g sample, accurate to 0.1g, placed in enamel cup, slowly adding glycerol solution with a glass rod stirring constantly, so that the sample Was a viscous paste-like. When a glass rod stroke paste, paste grooves formed can slowly flat together, rush to the bubble surface layer, cover filter paper and glass Sheet, placed in a boiling water bath and boiled for 30min, then, still, cool to room temperature. With a glass rod in the paste paddle observed phenomena, and Compared to heating does not occur before significant change is through tests. Fluoride Stability Test 5.12 5.12.1 Method summary The sample was dispersed in a mixture of sodium monofluorophosphate, uniformly mixed to prepare a suspension, heating the quenched on a boiling water bath for 1h, centrifuged Away, supernatant was measured soluble fluorine. 5.12.2 Reagent 5.12.2.1 monofluorophosphate mixture; They were weighed 500g glycerol and 500g water, accurate to 0.1g, stir, slowly add 14.61g sodium monofluorophosphate (purity ≥93%), sodium monofluorophosphate and stirred until completely dissolved, the solution was placed in a plastic storage vial. 5.12.2.2 perchloric acid solution. 46mL/L; 5.12.2.3 ionic strength buffer; Plastic flask was added about 300mL 500mL water, 30g of ammonium acetate added 4gCDTA (trans-1,2-cyclohexanediamine tetraacetic Acetic acid) and 100g of sodium nitrate, diluted with water to the mark. 5.12.2.4 fluoride standard solution. 1mL solution containing fluorine (F) 0.10mg; Pipette 10mL fluoride standard solution according to HG/T 3696.2 requirements formulated, placed in 100mL volumetric flask, dilute to the mark with water Degree, shake. 5.12.3 instruments and equipment 5.12.3.1 constant temperature water bath; 5.12.3.2 tube. 25mm × 150mm, heat-resistant glass; 5.12.3.3 tube. 17mm × 10mm, made of polypropylene; 5.12.3.4 centrifuge. 3000r/min ~ 5000r/min; 5.12.3.5 Digital pH/ion concentration meter. 5.12.4 analysis step 5.12.4.1 draw the curve Pipette Pipette 1.0mL, 5.0mL, 10.0mL fluoride standard solution were placed in 100mL plastic flask, the first two Bottles plus 9.0mL and 5.0mL water, then add 6.7mL each bottle perchloric acid solution and diluted with ionic strength buffer solution to the mark Degree, shake. Determination of fluoride ion selective electrode to fluoride content of value as the horizontal, the corresponding potential value of the vertical axis, draw the work curve. 5.12.4.2 Determination Weigh 24g ± 0.01g sample was placed in a test tube heat, add 26g monofluorophosphate mixture, stir with a plastic stirring rod, And the tube stoppered with rubber, the tube was placed in a water bath (the temperature was kept 100 ℃), pay attention to the water bath level remains above the suspension level 20mm or more, and heating was continued for 60min. Placed immediately after removing the ice bath and stirring rod with a plastic test tube mixture, 5min After the tube was removed from the ice bath, the tube suspension poured into centrifuge tubes, centrifuged at speed 3000r/min centrifugal 15min. Pipette the supernatant after centrifugation 5mL, 50mL was added to a polypropylene flask, diluted with water to the mark. 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