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GB 4481.1-2010 English PDF

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GB 4481.1-2010: National food safety standards of food additives tartrazine
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GB 4481.1: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusPDF
GB 4481.1-2010English559 Add to Cart 5 days [Need to translate] National food safety standards of food additives tartrazine Valid GB 4481.1-2010
GB 4481.1-1999English559 Add to Cart 4 days [Need to translate] Food additive--Tartrazine Obsolete GB 4481.1-1999
GB 4481.1-1994EnglishRFQ ASK 3 days [Need to translate] Food additive-Tartrazine Obsolete GB 4481.1-1994
GB 4481-1984English319 Add to Cart 3 days [Need to translate] Food additive--Tartrazine Obsolete GB 4481-1984

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Basic data

Standard ID GB 4481.1-2010 (GB4481.1-2010)
Description (Translated English) National food safety standards of food additives tartrazine
Sector / Industry National Standard
Classification of Chinese Standard X42
Classification of International Standard 67.220.20
Word Count Estimation 24,251
Date of Issue 2010-12-21
Date of Implementation 2011-02-21
Older Standard (superseded by this standard) GB 4481.1-1999
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 diazotization of sulfanilic acid with a 1 (4' sulfo-phenyl) -3 carboxy methyl (ethyl) ester -5 pyrazolone even merge hydrolysis or sulfanilic acid diazotization with a 1 (4' sulfo-phenyl) -3 carboxy-5 pyrazolone coupling and prepared food additive tartrazine.

GB 4481.1-2010: National food safety standards of food additives tartrazine

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National food safety standards of food additives tartrazine National Food Safety Standard Food Additives Tartrazine 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

This standard replaces GB 4481.1-1999 "food additive tartrazine." This standard compared with GB 4481.1-1999, the main changes are as follows. - Added safety tips; - Canceled ≥60.0% quality specifications, will modify the index ≥85.0% ≥87.0%; - Loss on drying, chloride and sulfate aggregates by the ≤15.0% revised to ≤13.0%, and revised the detection method; - Water insoluble ≤0.30% by the index revised to ≤0.20%; - Modify the discrimination test methods; - Colorimetric method allows parallel determination by the difference revised to ≤2.0% ≤1.0%; - Added unsulfonated primary aromatic amine (aniline meter) indicators and detection methods; - Increases sulfanilic acid, 1- (4'-sulfonic acid) -3-carboxy-5-pyrazolone disodium salt, 1- (4-phenyl sulfonate) 3-carboxylic acid methyl (ethyl) ester-5-pyrazolone sodium salt, 4,4 '- (imino diazo) and other diphenyl sulfonate disodium salt of unreacted Intermediate and indicators and detection methods byproducts; - Arsenic (As) is modified by chemical detection methods limit law atomic absorption spectrometry; - Cancel the heavy metals (Pb) quality specifications; - Increase the lead (Pb) indicator and detection methods; - An increase of mercury (Hg) indicators and detection methods. The Standard Appendix A, Appendix B and Appendix C are normative appendices, Appendix D is an informative annex. This standard replaces the standards previously issued as follows. --GB 4481.1-1984, GB 4481.1-1999. National Food Safety Standard Food Additives Tartrazine

1 Scope

This standard applies to the rear of the amino acid diazotization with 1- (4'-sulfonic acid phenyl) -3-carboxy-methyl (ethyl) ester -5- pyrazolone coupling After hydrolysis or by the merger of the amino acid diazotization with 1- (4'-sulfonic acid) -3-carboxy-5-pyrazolone coupling in the system of food additives Additives tartrazine.

2 Normative references

The standard file referenced in the application of this standard is essential. For cited documents with dates, only the date of Version applies to this standard. For undated references, the latest edition (including any amendments) applies to this standard. 3 chemical name, structural formula, molecular formula, relative molecular mass 3.1 Chemical Name. 1- (4'-sulfonate-phenyl) -3-carboxy-4- (4'-sulfophenylazo) -5-pyrazolone trisodium salt 3.2 Structure. N = NNaO3S NO COONa SO3Na Formula 3.3 C16H9N4Na3O9S2 3.4 relative molecular mass 534.36 (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 orange or bright orange by visual assessment under natural light. State organization powders or granules 4.2 Physical indicators. to comply with Table 2. Table 2. Physical and chemical indicators Item Index Test Method Lemon yellow, w /% ≥ 87.0 Appendix A A.4 Loss on drying, chloride (based on NaCl) and sulfate (NaSO4 in dollars) of the total, w /% ≤ 13.0 Appendix A A.5 Water-insoluble, w /% ≤ 0.20 A.6 in Appendix A Amino benzene sulfonate, w /% ≤ 0.20 Appendix A A.7 1- (4'-sulfonic acid) -3-carboxy-5-pyrazolone disodium salt, w /% ≤ 0.20 Appendix A A.8 1- (4'-sulfonate-phenyl) -3-carboxylic acid, methyl (ethyl) ester-5-pyrazolone sodium salt, w /% ≤ 0.10 A.9 Appendix A 4,4 '- (diazo imino) two acid disodium salt, w /% ≤ 0.05 A.10 Appendix A Unsulfonated primary aromatic amine (aniline dollars), w /% ≤ 0.01 Appendix A A.11 Deputy dye, w /% ≤ 1.0 Appendix A A.12 Arsenic (AS)/(mg/kg) ≤ 1.0 Appendix A A.13 Lead (Pb)/(mg/kg) ≤ 10.0 Appendix A A.14 Mercury (Hg)/(mg/kg) ≤ 1.0 A.15 Appendix A

Appendix A

(Normative) Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive, according to the relevant provisions of the operation, the operation need to be careful. If splashed on the skin should immediately wash with water, severe cases should be treated immediately. When using a volatile acid, to be carried out in a fume hood. A.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 water. Standard test solution required impurity standard solution, preparations and products at the time did not indicate other provisions, according to GB/T 601, GB/T 602, GB/T 603 regulations formulated and calibration. A.3 Identification Test A.3.1 Reagents and materials A.3.1.1 sulfuric acid. A.3.1.2 ammonium acetate solution. 1.5g/L. A.3.2 Instruments and Equipment A.3.2.1 Spectrophotometer. A.3.2.2 cuvette. 10mm. A.3.3 Identification method It should meet the following conditions. A.3.3.1 Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL of water was yellow clear solution. A.3.3.2 Weigh about 0.1g sample (accurate to 0.01g), sulfuric acid 10mL was yellow after, take this solution 2 drops to 3 drops of water was added 5mL yellow. A.3.3.3 Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL ammonium acetate solution of this solution 1mL, plus ammonium acetate solution Liquid distribution to 100mL, the maximum absorption wavelength of the solution was 428 nm ± 2nm. A.4 Determination of lemon A.4.1 Titanium trichloride titration (Arbitration Act) A.4.1.1 Method summary In acidic medium, lemon yellow azo group is reductive decomposition of titanium trichloride, titanium trichloride consumption according to standard titration solution, Calculate the content. A.4.1.2 Reagents and materials A.4.1.2.1 sodium bitartrate; A.4.1.2.2 titanium trichloride standard titration solution. c (TiCl3) = 0.1mol/L (now with the existing, method of preparation see Appendix B); A.4.1.2.3 cylinders loaded carbon dioxide. A.4.1.3 instruments and equipment A-- conical flask (a 500 mL); B-- Brown burette (50mL); C-- under glass bottle package black paper (2000mL); D-- containing 100g/L solution of ammonium carbonate and 100g/L ferrous sulfate solution container of an equivalent mixture (5000mL); E-- piston; F-- bottles; G-- washing bottle filled with water. Figure A.1 apparatus of FIG titanium trichloride titration A.4.1.4 analysis step Weigh about 0.5g sample (accurate to 0.0001g), placed in 500mL Erlenmeyer flask was dissolved in 50mL boiling water and cooled to room temperature Added 15g sodium hydrogen tartrate and 150mL boiling water, after shaking dissolved, according to Figure A.1 installed equipment, with carbon dioxide in the subsurface While boiled with titanium trichloride standard titration solution titration end point so that the inherent color disappeared. A.4.1.5 Calculation Results Lemon mass fraction 1w its value is expressed in%, according to formula (A.1) Calculated. 0) 4 /) (1000/( 1 × = m MVcw (A.1) Where. c - accurate titanium trichloride standard titration solution concentration value in units of moles per liter (mol/L); V - accurate value of the sample consumed titration of titanium trichloride standard titration solution volume in milliliters (mL); M - molar mass of lemon value in units of grams per mole (g/mol) [M (C16H9N4Na3O9S2) = 534.36]; m1 - mass value of the sample in grams (g). The results represent a decimal. The absolute difference between the parallel determination results is not more than 1.0% (mass fraction), the arithmetic mean value as a measurement result. A.4.2 Colorimetric method A.4.2.1 Method summary A sample with a known amount of lemon standards were dissolved in water, dilute to volume with ammonium acetate solution, the maximum absorption wavelength At its absorbance values were measured to calculate its content. A.4.2.2 Reagents and materials A.4.2.2.1 ammonium acetate solution. 1.5g/L. A.4.2.2.2 lemon standards. ≥87.0% (mass fraction, measured according to A.4.1). A.4.2.3 instruments and equipment A.4.2.3.1 spectrophotometer. A.4.2.3.2 cuvette. 10mm. A.4.2.4 lemon preparation of standard solution Weigh about 0.25g lemon standards (accurate to 0.0001g), was dissolved in an appropriate amount of water, transferred to 1000mL volumetric flask, dilute with water Release to the mark. Draw 10mL, transferred to 500mL volumetric flask, add ammonium acetate solution was diluted to the mark, shake well and set aside. A.4.2.5 lemon preparation of the sample solution A.4.2.4 weighing and methods of operation with standard solution preparation. A.4.2.6 analysis step The lemon standard solution and the sample solution were placed 10mm lemon yellow cuvettes, with the maximum absorption wavelength using a spectrophotometer Meter measuring their absorbance values with ammonium acetate solution as the reference solution. A.4.2.7 Calculation Results Lemon mass fraction 1w its value is expressed in%, according to formula (A.2) Calculated. 1 wmA Amw × = (A.2) Where. A - absorbance values lemon sample solution; Numerical m0-- lemon standard mass in grams (g); Absorbance values A0-- lemon standard solution; Sample quality m-- value in units of grams (g); w0-- lemon standard mass fraction%. The results represent a decimal. The absolute difference between the parallel determination results is not more than 1.0% (mass fraction), the arithmetic mean value as a measurement result. A.5 Determination of loss on drying, chloride (based on NaCl) and sulfate (Na2S04 in dollars) of the total A.5.1 Determination of loss on drying A.5.1.1 analysis step Weigh about 2g sample (accurate to 0.001g), has been placed in the weighing bottle at 135 ℃ ± 2 ℃ oven temperature is constant at 135 ℃ ± 2 ℃ Thermostatic oven drying to constant weight. A.5.1.2 Calculation Results Loss on drying mass fraction to 2w and its value is expressed in%, according to formula (A.3) Calculated. 2 × - = m mmw (A.3) Where. Numerical m2-- sample before drying mass in grams (g); m3-- sample dried to a constant mass values, expressed in grams (g). The results represent a decimal. The absolute difference between the parallel determination results is not more than 0.2% (mass fraction), the arithmetic mean value as a measurement result. A.5.2 chloride (as NaCl) Determination A.5.2.1 Reagents and materials A.5.2.1.1 nitrobenzene. A.5.2.1.2 activated carbon; 767 needle. A.5.2.1.3 nitric acid solution. 11. A.5.2.1.4 silver nitrate solution. c (AgNO3) = 0.1mol/L. A.5.2.1.5 ammonium ferric sulfate solution. Preparation method. Weigh about 14g of ammonium ferric sulfate, dissolved in 100mL of water, filter, add 10mL of nitric acid, stored in a brown bottle; A.5.2.1.6 ammonium thiocyanate standard titration solution. c (NH4CNS) = 0.1mol/L. A.5.2.2 preparation of the sample solution Weigh about 2g sample (accurate to 0.001g), was dissolved in 150mL of water, add about 15g of activated carbon, a moderate boil 2 min ~ 3min, plus The nitric acid solution 1mL, continue to shake evenly placed 30min (during shaking from time to time). Filtered through a dry filter paper. Such as colored filtrate is then Add 5g of activated carbon, occasionally shaking place 1h, then dried filter paper (such as color still replace the activated carbon Repeat until the filtrate colorless). 10mL each wash with water three times activated carbon, and the filtrate combined move 200mL volumetric flask, add water to the mark. For chloride and sulfur Determination of salt content. A.5.2.3 analysis step Pipette 50mL sample solution, placed in 500mL conical flask, add 10mL 2mL nitric acid solution and silver nitrate solution (chloride content more To add more) and 5mL nitrobenzene, shake vigorously to silver chloride condensation, ammonium ferric sulfate is added 1mL solution with ammonium thiocyanate standard titration Titrate the excess silver nitrate to the end and keep 1min, at the same time in the same way to make a blank test. A.5.2.4 Calculation Results Chloride (as NaCl) mass fraction 3w and its value is expressed in%, according to formula (A.4) Calculated. ) 200/50 ( ] 1000 /) [( 3 × - = m MVVcw (A.4) Where. c1 - accurate ammonium thiocyanate standard titration solution concentration value in units of moles per liter (mol/L); V1 - accurate value of consumption of titration blank solution of ammonium thiocyanate standard titration solution volume in milliliters (mL); V0 - accurate value of the sample solution was titrated with ammonium thiocyanate standard titration solution consumed volume in milliliters (mL); M1 - the value of the molar mass of sodium chloride, in units of grams per mole (g/mol) [M1 (NaCl) = 58.4]; Sample quality m4-- value in units of grams (g). The results represent a decimal. Parallel determination results of absolute difference is not more than 0.3% (mass fraction), the arithmetic mean value as a measurement result. A.5.3 Sulfate (Na2S04 meter) measurement A.5.3.1 Reagents and materials A.5.3.1.1 sodium hydroxide solution. 2g/L; A.5.3.1.2 hydrochloric acid solution. 11999; A.5.3.1.3 barium chloride standard titration solution. c (1/2BaCl2) = 0.l mol/L (preparation see Appendix C); A.5.3.1.4 phenolphthalein indicator solution. 10g/L; A.5.3.1.5 Rose sodium indicator solution. Weigh 0.lg red roses, sodium dissolved in 10mL of water (using now). A.5.3.2 analysis step Draw 25mL sample solution (A.5.2.2), placed in 250mL conical flask, add 1 drop of phenolphthalein indicator solution, a solution of sodium hydroxide solution Pink, then a solution of hydrochloric acid solution to the pink color disappeared, shake, dissolved in constant shaking drops of barium chloride standard titration solution Set in red roses sodium indicator solution for outward indicator solution, and the reaction liquid indicator solution on filter paper presents the intersection of rose red spots and kept 2min Do not fade as the end point. At the same time in the same manner as a blank test. A.5.3.3 Calculation Results Sulfate (Na2SO4 meter) mass fraction 4w and its value is expressed in%, according to formula (A.5) Calculated. ) 200/25 ( ) 2 /] (1000 /) [( 4 × - = m MVVcw (A.5) Where. c2 - accurate barium chloride standard titration solution concentration value in units of moles per liter (mol/L); The exact value of the sample solution V2-- titration consumption of barium chloride standard titration solution volume in milliliters (mL); Accurate value of V3-- titrate blank solution consumed barium chloride standard titration solution volume in milliliters (mL); M2 - the value of the molar mass of sodium sulfate, units of grams per mole (g/mol) [M2 (Na2SO4) = 142.04]; m4 - mass of the sample value in units of grams (g). The results represent a decimal. The absolute difference between the parallel determination results is not more than 0.2% (mass fraction), the arithmetic mean value as a measurement result. Results A.5.4 Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) the total amount of calculation Total loss on drying and chloride (based on NaCl) and sulfate (Na2SO4 to count) to the mass fraction 5w and its value is expressed in% According to the formula (A.6) Calculated. 4325 wwww = (A.6) Where. 2w - drying loss mass fraction%; 3w - chloride (as NaCl) mass fraction%; 4w - Sulfate (Na2SO4 meter) mass fraction%. The results represent a decimal. A.6 Determination of insoluble matter A.6.1 Instruments and Equipment A.6.1.1 sand core glass crucible. G4, a pore size of 5μm ~ 15μm. A.6.1.2 oven thermostat. A.6.2 Analysis step Weigh about 3g sample (accurate to 0.001g), placed in 500mL beaker, add 50 ℃ ~ 60 ℃ hot water 250mL, dissolved, Has been used in 135 ℃ ± 2 ℃ drying to constant glass sand core crucible filtered and washed thoroughly with hot water to wash colorless liquid at 135 ℃ ± 2 ℃ constant Constant temperature oven to bake. A.6.3 Calculation Results Water insoluble mass fraction 6w and its value is expressed in%, according to formula (A.7) calculated as follows. 6 × = m mw (A.7) Where. m6 - Numerical dried water insoluble mass in grams (g); m5 - the value of the sample mass, in grams (g). The results represent two decimal. The absolute difference between parallel determination results is not more than 0.05% (mass fraction), the arithmetic mean value as a measurement result. A.7 determination of amino benzene sulfonate A.7.1 Method summary By reverse-phase liquid chromatography and quantified by external standard method, the calculation of the mass fraction of amino benzene sulfonate. A.7.2 Reagents and materials A.7.2.1 methanol. A.7.2.2 amino benzene sulfonate. A.7.2.3 ammonium acetate solution. 2g/L. A.7.3 Instruments and Equipment A.7.3.1 HPLC. infusion pump - flow range of 0.1 mL/min ~ 5.0mL/min, the flow rate in this range stability ± 1%; detector - multi-wavelength UV spectrophotometric detector or equivalent in performance to UV spectrophotometric detector. A.7.3.2 Column. length 150mm, an inner diameter of 4.6mm stainless steel column, stationary phase C18, particle size 5μm. A.7.3.3 chromatography workstation or integrator. A.7.3.4 ultrasonic generator. A.7.3.5 loop. 20μL. A.7.3.6 micro syringe. 20μL ~ 100μL. A.7.4 Chromatography conditions A.7.4.1 detection wavelength. 254nm. A.7.4.2 Column temperature. 40 ℃; A.7.4.3 Mobile phase. A, a solution of ammonium acetate; B, methanol; Concentration gradient. 40min linear gradient from A (95) than B (5) to A (50) than B (50); A.7.4.4 Flow. 1mL/min; A.7.4.5 Injection volume. 20μL. According to the different instruments, choose the best analytical conditions corresponding flow after shaking degassed by ultrasonic generator. Preparation of the sample solution A.7.5 Weigh 0.1g sample (accurate to 0.0001g), add a solution of ammonium acetate dissolved, diluted to 100mL, this is the sample solution. A.7.6 preparation of standard solution Weigh 0.01g (accurate to 0.0001g) was placed in a vacuum dryer amino benzene sulfonate, ammonium acetate solution is dried after 24h Dissolved, diluted to 100mL. Draw the above solution 10mL, add ammonium acetate solution was diluted to Pipette 2.5mL, 2.0mL 100mL later, 1.0mL of this solution, and then ammonium acetate solution was diluted to volume to 100mL, as a series of standard solution. A.7.7 Analysis step In the chromatographic conditions specified in A.7.4, respectively draw a sample solution and each series of standard solution is injected using a micro syringe and filled Chromatography detection loop until the last component of the outflow is completed, the results processing. Determination series of standard solution of sulfanilamide Sodium peak area of the standard curve plotted. Determination of the sample solution for amino benzene sulfonate peak area, based on the calculation of the standard curve Amino benzene sulfonate content. Chromatogram in Appendix D. A.8 1- (4'- sulfonic acid) -3-carboxy-5 Determination pyrazolone Disodium A.8.1 Method summary By reverse-phase liquid chromatography and quantified by external standard method to calculate the 1- (4'-sulfonic acid) -3-carboxy-5-pyrazolone disodium salt Mass fraction. A.8.2 Reagents and materials A.8.2.1 1- (4'- sulfonic acid) -3-carboxy-5-pyrazolone disodium salt. A.8.2.2 rest with A.7.2. A.8.3 Instruments and Equipment With A.7.3. Preparation of the sample solution A.8.4 With A.7.5. A.8.5 preparation of standard solution Weigh about 0.01g (accurate to 0.0001g) was placed 1- (4'-sulfonic acid phenyl) vacuum drier 24h after the 3-carboxy -5- Pyrazolone disodium salt, ammonium acetate was dissolved and diluted to volume to 100mL. Draw the above solution 10mL, add ammonium acetate solution Dilution constant volume to 100mL. Pipette 2.5mL, 2.0mL, 1.0mL, then ammonium acetate solution was diluted accurately set the volume to 100mL, as Standard solution for the series. A.8.6 Chromatography conditions With A.7.4. A.8.7 Analysis step In the chromatographic conditions specified in A 8.6, respectively, and each series draw sample solution standard solution is injected using a micro syringe and filled Chromatography detection loop until the last component of the outflow is completed, the results processing. Determination series of standard solution of 1- (4'-sulfonic acid ) -3-Carboxy-5-pyrazolone disodium salt peak areas plotted standard curve. Determination of sample solution of 1- (4'-phenyl sulfonate) -3- Carboxy-5-pyrazolone disodium salt peak area, calculated from standard curves of 1- (4'-sulfonic acid) -3-carboxy-5-pyrazolone two Sodium salt content. Chromatogram in Appendix D. A.9 1- (4'- sulfonic acid) -3-carboxylic acid A was measured (B) an ester-5-pyrazolone sodium salt A.9.1 Method summary By reverse-phase liquid chromatography and quantified by external standard method to calculate the 1- (4'-sulfonic acid phenyl) -3-carboxylic acid, methyl (ethyl) ester-5-pyrazole Imidazolidinone salt mass fraction. A.9.2 Reagents and materials A.9.2.1 1- (4'- sulfonate-phenyl) methyl 3-carboxylic acid (B) an ester-5-pyrazolone sodium salt. A.9.2.2 rest with A.7.2. A.9.3 Instruments and Equipment With A.7.3. Preparation of the sample solution A.9.4 With A.7.5. A.9.5 preparation of standard solution Weigh about 0.01g (accurate to 0.0001g) was placed 1- (4'-sulfonic acid phenyl) vacuum drier 24h after 3-carboxylic acid Methyl (ethyl) ester-5-pyrazolone sodium, ammonium acetate was dissolved and diluted to volume to 100mL. 10mL draw the above solution, add Ammonium acetate, dilute to volume Pipette 10.0mL, 5.0mL, 2.0mL, 1.0mL 100mL later, and then diluted with ammonium acetate solution Constant volume to 100mL, as a series of standard solution. A.9.6 Chromatography conditions With A.7.4. A.9.7 Analysis step In the chromatographic conditions specified in A.9.6, respectively draw a sample solution and each series of standard solution is injected using a micro syringe and filled Chromatography detection loop until the last component of the outflow is completed, the results processing. Determination series of standard solution of 1- (4'-sulfonic acid Yl-phenyl) -3-carboxylic acid, methyl (ethyl) ester-5-pyrazolone sodium salt peak area plotted standard curve. Determination of sample solution of 1- (4'- Sulfonic acid group-phenyl) -3-carboxylic acid, methyl (ethyl) ester-5-pyrazolone sodium salt of peak area, calculated from a standard curve of 1- (4'-phenyl sulfonate) 3-carboxylic acid methyl (ethyl) ester-5-pyrazolone sodium salt content. Chromatogram in Appendix D. A.10 4,4 '- (diazo imino) Determination of titanium acid disodium salt A.10.1 Method summary By reverse-phase liquid chromatography and quantified by external standard method to calculate the 4,4 '- (diazo imino) quality two sub-acid disodium salt number. A.10.2 reagents and materials A.10.2.1 4,4 '- (diazo imino) two acid disodium salt. A.10.2.2 rest with A.7.2. A.10.3 instruments and equipment With A.7.3. A.10.4 preparation of the sample solution With A.7.5. A.10.5 preparation of standard solution Weigh about 0.01g (accurate to 0.0001g) has placed 4,4 'vacuum drier after 24h - (diazo imino) diphenyl sulfonamide Disodium salt, ammonium acetate was dissolved and diluted to volume to 100mL. Draw 10mL above solution, add a solution of ammonium acetate, and dilute Yung were drawn to 100mL after 10.0mL, 5.0mL, 2.0mL, 1.0mL, then ammonium acetate solution is diluted to volume to 100mL, as Standard solution for the series. A.10.6 chromatographic conditions A.10.6.1 detection wavelength. 358nm. A.10.6.2 other with A.7.4. A.10.7 Analysis steps In the chromatographic conditions A.10.6 provisions were drawn and each series of sample solution standard solution is injected using a micro syringe and filled Full loop chromatography detection until the last component of the outflow is completed, the results processing. Determination of standard solutions of 4,4 '- (weight Imino nitrogen) two acid disodium salt peak area of the standard curve plotted. Determination of sample solution of 4,4 '- (diazo imino) diphenyl Acid, disodium salt peak area, calculated from standard curves of 4,4 '- (imino diazonium) content of the two acid disodium salt. Chromatogram Mitsuke Record D. A.11 unsulfonated primary aromatic amine (aniline meter) measurement A.11.1 Method summary The sample is extracted with ethyl acetate unsulfonated primary aromatic amine component, the extract and the standard solution were treated with aniline diazotization Measured after each generate dye absorbance to be compared with the judgment. A.11.2 reagents and materials A.11.2.1...

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