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GB 25562-2010 English PDF

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GB 25562-2010: The national food safety standards of food additives tetrasodium pyrophosphate, potassium
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GB 25562-2010399 Add to Cart 3 days The national food safety standards of food additives tetrasodium pyrophosphate, potassium Obsolete

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Basic data

Standard ID: GB 25562-2010 (GB25562-2010)
Description (Translated English): The national food safety standards of food additives tetrasodium pyrophosphate, potassium
Sector / Industry: National Standard
Classification of Chinese Standard: X42
Classification of International Standard: 67.220.20
Word Count Estimation: 10,174
Date of Issue: 2010-12-21
Date of Implementation: 2011-02-21
Regulation (derived from): Ministry of Health Bulletin No. 19 of 2010
Issuing agency(ies): Ministry of Health of the People's Republic of China
Summary: This Chinese standard applies to thermal phosphoric acid and potassium hydroxide for raw materials for food additives potassium pyrophosphate four.

GB 25562-2010: The national food safety standards of food additives tetrasodium pyrophosphate, potassium


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The national food safety standards of food additives tetrasodium pyrophosphate, potassium National Food Safety Standard Food Additives four potassium pyrophosphate Issued on. 2010-12-21 2011-02-21 implementation National Standards of People's Republic of China People's Republic of China Ministry of Health issued

Foreword

Appendix A of this standard is a normative appendix. National Food Safety Standard Food Additives four potassium pyrophosphate

1 Scope

This standard applies to thermal phosphoric acid and potassium hydroxide as raw materials obtained food additive potassium tetrasodium pyrophosphate.

2 Normative references

The standard file referenced in the application of this standard is essential. For dated references, only the dated edition of fitness For this standard. For undated references, the latest edition (including any amendments) applies to this standard.

3 formula and relative molecular mass

Formula 3.1 K4P2O7 3.2 relative molecular mass 330.34 (according to 2007 international relative atomic mass) 4. Technical Requirements 4.1 Sensory requirements. comply with Table 1. Table 1 Sensory requirements Project requires test methods Color White take appropriate sample is placed in 50mL beaker was observed under natural light Color and texture. State organization powders or granules 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Tetrapotassium pyrophosphate, w /% ≥ 95.0 Appendix A A.4 Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.5 Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.6 Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.7 Fluorides (as F) // (mg/kg) ≤ 10 Appendix A A.8 Water-insoluble, w /% ≤ 0.1 A.9 in Appendix A pH (10g/L solution) 10.5 ± 0.5 A.10 Appendix A Loss on ignition, w /% ≤ 0.5 Appendix A A.11 Note. The LOI index of factory inspection targets.

Appendix A

(Normative) Testing method A.1 Warning Reagents used in this test method are toxic or corrosive, the operation must be careful as water rushed immediately on contact with skin Wash, severe cases should immediately heal. A.2 General Provisions This standard reagents and water, did not indicate when the other requirements, refer to three analytical reagent water and GB/T 6682-2008 stipulated. 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 requiring HG/T 3696.3 of preparation. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 ammonia. A.3.1.2 hydrochloric acid. A.3.1.3 nitrate. A.3.1.4 acetic acid solution. 11. A.3.1.5 silver nitrate solution. 17g/L. A.3.2 Analysis step A.3.2.1 Identification of potassium ions Take a small sample of about 0.1g, add 10 mL of water to dissolve. Platinum wire ring dipped in hydrochloric acid, in a colorless flame to burn. And then dipped in a flame test solution On combustion, the flame should be observed under cobalt glass purple. A.3.2.2 Identification of pyrophosphate Sample solution A.3.2.2.1. 0.1g sample was dissolved in 100mL the nitric acid solution; A.3.2.2.2 Test solution A. in 30mL Quimociac added dropwise 0.5mL sample solution; A.3.2.2.3 Test solution B. The remaining sample solution was heated at 95 ℃ 10min, take 0.5mL of this solution was added dropwise 30mL Quimociac solution; A.3.2.2.4 determination. Test solution B immediately formed yellow precipitate A test solution does not appear. A.4 Determination of potassium tetrasodium pyrophosphate A.4.1 Method summary Tetrapotassium pyrophosphate with hydrochloric acid, potassium dihydrogen pyrophosphate, adding zinc sulfate, zinc pyrophosphate generate sulfuric acid and precipitation by acid-base titration Determination of sulfuric acid generated. Reaction is as follows. K4P2O7 2HCl = K2H2P2O7 2KCl K2H2P2O7 2ZnSO4 = Zn2P2O7 K2SO4 H2SO4 H2SO4 2NaOH = Na2SO4 2H2O A.4.2 Reagents and materials A.4.2.1 hydrochloric acid solution. 120. A.4.2.2 hydrochloric acid solution. 1100. A.4.2.3 zinc sulfate solution. 125g/L; Weigh 125g of zinc sulfate dissolved in water and diluted to 1 000mL, with the acidity of the sulfuric acid solution (1500) or sodium hydroxide standard titration solution Solution (A.4.2.5) and the solution was adjusted to pH 3.8. A.4.2.4 anhydrous sodium pyrophosphate (pyrophosphate recrystallized three times); a) of anhydrous sodium pyrophosphate as an industrial method for preparing the starting material. The first crystallization. Weigh 30g of industrial anhydrous sodium pyrophosphate, placed in 400mL beaker, add 100mL water dissolved by heating with constant speed Quantity filter paper. The filtrate was cooled in a cold water bath, crystalline precipitation, the solution was decanted, washed with a small amount of water and crystallized twice. Second crystallization. the first crystallization with a small amount of water dissolved by heating in a cold water bath cooling, precipitated crystals were decanted solution. Third Crystallization. the second crystallization method according to the first crystallization recrystallization once. b) reagent sodium pyrophosphate decahydrate method of preparing a raw material. Weigh 80 g of sodium pyrophosphate decahydrate reagent, according to a) in the first and second crystallization operations. The above recrystallization pyrophosphate into a porcelain crucible, burning to constant mass at 400 ℃. A.4.2.5 sodium hydroxide standard titration solution. c (NaOH) = 0.1 mol/L. Calibration. Weigh about 0.5g of anhydrous sodium pyrophosphate, accurate to 0.000 2g, placed in 250mL beaker, add 50mL water to dissolve. In the pH meter On, stirring slowly adding the appropriate concentration of hydrochloric acid solution (A.4.2.1 or A.4.2.2) until the pH value of 3.8, zinc sulfate solution was added 50mL It was stirred for 5min. Standard titration with sodium hydroxide solution to titrate the pH value close to 3.6 under stirring stop titration, the solution was stirred for 2min Balance, continue titration, when every drop of sodium hydroxide standard titration solution was stirred to 30s, to a pH of 3.8 for the end. 0.1 mol per ml/L sodium hydroxide standard titration solution of sodium pyrophosphate equivalent mass (ρ), in grams per milliliter (g/mL) according to formula (A.1) Calculated. m = ρ (A.1) Where. m-- weighed anhydrous sodium pyrophosphate quality value in units of grams (g); Numerical V-- titration consumed sodium hydroxide standard titration solution volume in milliliters (mL). A.4.3 Instruments and Equipment A.4.3.1 pH meter. Indexing is 0.02. A.4.3.2 magnetic stirrer. A.4.4 Analysis step A.4.4.1 Preparation of test solution Weigh about 5g samples, accurate to 0.000 2g, placed in 250mL beaker, add water to dissolve 50mL, transferred to a 500mL volumetric flask with water Dilute to the mark. A.4.4.2 Determination With pipette 50mL test solution was placed in 250mL beaker, add 40mL water, the following press A.4.2.5 from "stirring slowly add the appropriate When the concentration of hydrochloric acid solution (A.4.2.1 or A.4.2.2) until the solution pH to 3.8 "to the" end to a pH of 3.8 for the "far into the Line operation. A.4.5 Calculation Results Tetrasodium pyrophosphate, potassium content of tetrapotassium pyrophosphate (K4P2O7) mass fraction w1 and its value is expressed in%, according to formula (A.2) Calculated. ) 500/50 ( 242.1 1 ×× × = Vw ρ (A.2) Where. ρ-- per milliliter of sodium hydroxide standard titration solution equivalent to the number of grams of anhydrous sodium pyrophosphate, in grams per milliliter (g/mL); Numerical V-- titration solution of sodium hydroxide standard titration solution consumption volume in milliliters (mL); m-- sample mass value in grams (g); 1.242-- anhydrous sodium pyrophosphate, tetrapotassium pyrophosphate in terms of coefficient. 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 0.3%. A.5 Determination of Arsenic Weigh 0.50g ± 0.01g sample was placed in 100mL beaker, add 20mL of water and 10mL of hydrochloric acid solution (11), heating dissolved, the whole Unit was transferred to measure arsenic bottle, add water to a total volume of about 40mL, according to GB/T 5009.76-2003 Chapter 11 in the second predetermined operation. Limits formulated solution. Pipette 1.50mL arsenic standard solution [1mL solution containing arsenic (As) 0.001mg], and treated in the same sample at the same time. A.6 Determination of Heavy Metals Weigh about 5g samples, accurate to 0.01g, placed in 100mL beaker, add 80mL water, heating dissolved moved 100mL flask, Dilute with water to volume, and mix. Speed dry filter paper filter with two layers Discard the first 20mL solution Pipette 20.00mL test solution was placed in 50mL Colorimetric tube. Add 1 drop of phenolphthalein indicator solution (10g/L), with sodium hydroxide solution (40g/L) was adjusted to neutral solution, add water to a total volume of about 30mL, according to GB/T 5009.74-2003 Chapter 6 operation. Color than standard solution preparation. Pipette 1.00mL lead standard solution [ImL solution of lead (Pb) 0.010mg], and treated in the same sample simultaneously. A.7 Determination of Lead A.7.1 Reagents and materials A.7.1.1 hydrochloric acid. A.7.1.2 nitrate. A.7.1.3 chloroform. A.7.1.4 sodium hydroxide solution. 40g/L. A.7.1.5 Pyrrolidine dithiocarbamate (The APDC) solution. 20g/L. Filtered before use. A.7.1.6 Lead standard solution. 1 mL solution containing lead (Pb) 0.010mg; Pipette Pipette 1.00mL lead standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark. A.7.1.7 test water line with two water GB/T 6682-2008 stipulated. A.7.2 Instruments and Equipment Atomic absorption spectrophotometer. A.7.3 Analysis step A.7.3.1 Preparation of test solution It weighs about 10g sample, accurate to 0.01g, placed in 150mL beaker. Add 30mL of water and a minimum amount of hydrochloric acid to dissolve the sample, excess 1mL Hydrochloric acid to ensure that the sample is dissolved. Heated to boiling for a few minutes, cooled, diluted to 100mL, pH of the solution adjusted with sodium hydroxide solution to 1.0 to 1.5, The solution was transferred to quantitatively 250mL separatory funnel, diluted to about 200mL. Add 2mL Pyrrolidine dithiocarbamate (The APDC) Solution, and mixed. Chloroform extracted twice, each added 20 mL, 50mL collect the extract in a clean beaker, steam bath and evaporated to near dryness, Add 3mL nitric acid heated nearly dry. Then add 0.5mL nitric acid and 10mL water, heated to the remaining 3 mL ~ 5mL. Transferred to a 10mL volumetric flask Diluted with water to the mark. A.7.3.2 Preparation of the blank test solution Take 30 mL water were placed in a 150 mL beaker, add 1 mL of hydrochloric acid. The following operation is the same in A.7.3.1 "boil a few minutes heating, cooling, Diluted to 100 mL transferred to a 10 mL volumetric flask, dilute with water to the mark. " A.7.3.3 Preparation of standard solutions Pipette 2.00 mL of lead standard solution was placed in a 150 mL beaker, add 1 mL of hydrochloric acid. The following operation is the same A.7.3.1 in "a few heated to boiling Diluted minutes, cooled with water to 100 mL transferred to a 10 mL volumetric flask, dilute with water to the mark. " A.7.3.4 Determination A.7.3.4.1 instrument conditions. resonance line of 283.3 nm; slit 0.7 nm; air - acetylene flame. A.7.3.4.2 Determination. The test solution, standard solution to import atomic absorption spectrophotometer, zero blank test solution, the test solution The absorption value can not be higher than the standard solution absorbance. A.8 Determination of fluoride A.8.1 Reagents and materials A.8.1.1 hydrochloric acid solution. 1 + 4. A.8.1.2 nitric acid solution. 1 + 15. A.8.1.3 sodium hydroxide solution. 100g/L. A.8.1.4 buffer solution. dissolve 270g of sodium citrate dihydrate (Na3C6H5O7 · 2H2O) and 24g of citric acid (C6H5O7 • 2H2O) in 800 mL of water, Then diluted with water to 1000mL, shake. A.8.1.5 fluoride standard solution. 1mL solution of fluorine (F) 0.010 mg; Pipette Pipette 1mL fluoride standard solution according to HG/T 3696.2 prepared, placed in 100mL volumetric flask, dilute to the mark, Shake well. This ready to use solution that is equipped. A.8.1.6 bromocresol green indicator solution. 1g/L. A.8.2 Instruments and Equipment A.8.2.1 fluoride ion selective electrode. A.8.2.2 saturated calomel electrode; A.8.2.3 potentiometer. A.8.3 Analysis step A.8.3.1 draw the curve Pipette 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL fluoride standard solution were placed in 50 mL capacity Flask, add 1mL hydrochloric acid solution, 5 drops of buffer solution, 2 drops of bromocresol green indicator solution. Adjusted with sodium hydroxide solution to a blue solution, and then Nitric acid solution to adjust the solution yellow. Add 20 mL buffer solution diluted with water to the mark. The fluoride ion selective electrode and calomel electrode and the potentiometer negative and a positive terminal coupled to the electrode insert filled with water 50 mL polyethylene plastic beaker, pre Thermal instrumentation, on a magnetic stirrer with constant stirring, to read the value of the equilibrium potential, the replacement of 2 to 3 times after water reached electrode specified in the instructions After the potential value to the standard working solution and the potential of the sample solution was measured. The standard working solution into a clean, dry 50 mL beaker placed on a magnetic stirrer, stirring into inserted fluorine ion selective Electrode and a saturated calomel electrode, a stirring moment, the zero adjustment potentiometer, record potential value at equilibrium. In logarithm of the concentration of fluoride ions is a cross-sit Standard, the corresponding potential value of the vertical axis, draw the working curve. A.8.3.2 Determination It weighs about 3 g samples, accurate to 0.000 2g. Placed in 50 mL volumetric flask, add 10 mL of water, following in A.8.3.1 self "plus 1mL hydrochloric acid solution "to" record potential value equilibrium "stop. Isolated corresponding fluoride content from the working curve values, seeking opposition Number of fluoride ions to obtain mass. A.8.4 Calculation Results Fluoride content of fluorine (F) mass fraction w2 and its value in mg/kg according to formula (A.3) Calculated. 2 10- × = m w (A.3) Where. Numerical m1-- test solution fluoride ion mass, in milligrams (mg); m-- sample mass value in grams (g). 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 greater than 2 mg/kg. A.9 Determination of insoluble matter A.9.1 Instruments and Equipment A.9.1.1 sintered glass crucible. filter plate pore size of 5μm ~ 15μm. A.9.1.2 electric oven. the temperature can be controlled at 105 ℃ ± 2 ℃. A.9.2 Analysis step It weighs about 20g sample, accurate to 0.01g, placed in 500mL beaker, add 400mL water dissolved, previously at 105 ℃ ± 2 ℃ Dried to a constant mass of glass sand filter crucible. The residue was washed with hot water until neutral (with a precision pH test paper). The glass crucible placed in sand 105 ℃ ± 2 ℃ in electric oven, and dried to a constant mass. A.9.3 Calculation Results Water-insoluble mass fraction w3 and its value is expressed in%, according to formula (A.4) Calculated. 0213 × - = m mm w (A.4) Where. Numerical quality m1-- glass crucible sand and water-insoluble material in grams (g); Numerical m2-- sintered glass crucible mass in grams (g); m-- sample mass value in grams (g). 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 0.001%. A.10 pH measurement of A.10.1 instruments and equipment pH meter. Indexing is 0.02. A.10.2 Analysis steps Weigh 1.00g ± 0.01g sample was dissolved in 100mL of water, with a pH meter pH. A.11 Determination of loss on ignition A.11.1 instruments and equipment High temperature furnace. the temperature can be controlled at 800 ℃ ± 25 ℃. A.11.2 Analysis steps To advance with burning at 800 ℃ ± 25 ℃ constant quality porcelain crucible Weigh about 10g sample to the nearest 0.01g. It will be filled with samples of porcelain crucible Placed in 800 ℃ ± 25 ℃ high temperature furnace burning 30min, after the removal, placed in a desiccator to cool and weigh. A.11.3 Calculation Results LOI mass fraction w4 and its value is expressed in%, according to formula (A.5) Calculated. 0214 × - = m mm w (A.5) Where. Numerical m1-- porcelain crucible and the sample mass, expressed in grams (g); Numerical m2-- porcelain crucible and the sample after burning mass in grams (g); m-- sample mass value in grams (g). 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%.
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