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GB 25546-2010 English PDF

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GB 25546-2010: National food safety standards of food additives fumarate
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
GB 25546-2010	English	229	Add to Cart	3 days [Need to translate]	National food safety standards of food additives fumarate	Valid	GB 25546-2010

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Basic data

Standard ID	GB 25546-2010 (GB25546-2010)
Description (Translated English)	National food safety standards of food additives fumarate
Sector / Industry	National Standard
Classification of Chinese Standard	X42
Classification of International Standard	67.220.20
Word Count Estimation	10,193
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 maleic acid as raw material by isomerization, crystallization, drying and prepared food additives fumaric acid.

GB 25546-2010: National food safety standards of food additives fumarate

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National food safety standards of food additives fumarate National Standards of People's Republic of China National standards for food safety Food additives fumaric acid 2010-12-21 release 2011-02-21 Implementation Issued by the Ministry of Health of the People's Republic of China

Foreword

Appendix A, Appendix B and Appendix C of this standard are normative appendices. National standards for food safety Food additives fumaric acid

1 Scope

This standard is suitable for the use of maleic acid as raw materials by isomerization, crystallization, drying and the preparation of food additives fumaric acid.

2 normative reference documents

The documents cited in this standard are indispensable for the application of this standard. Any reference to the date of the document, only the date of the edition This applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard. 3 Chemical name, molecular formula, structural formula and relative molecular mass 3.1 Chemical name Fumaric acid 3.2 Molecular formula C4H4O4 3.3 Structural formula 3.4 Relative molecular mass 116.07 (according to.2007 international relative atomic mass)

4 technical requirements

4.1 sensory requirements. should be consistent with the provisions of Table 1. Table 1 sensory requirements The project requires a test method Color white Smell sour Organizational state Crystalline powder or crystalline particles Take appropriate laboratory samples, placed in clean, dry white porcelain Intraday, in the natural light, visual observation, smell the smell 4.2 Physical and chemical indicators. should be consistent with the provisions of Table 2. Table 2 Physical and chemical indicators Item Index Test Method Fumaric acid (based on C4H4O4, dry basis), w /% 99.5 to 100.5 Appendix A, A.4 Arsenic (As)/(mg/kg) ≤ 2 Appendix A A.5 Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.6 Residue on ignition, w /% ≤ 0.1 Appendix A A.7 Maleic acid, w /% ≤ 0.10 Appendix A, A.8 Moisture, w /% ≤ 0.5 Appendix A A.9

Appendix A

(Normative appendix) Testing method A.1 Warning Some of the test procedures specified in the test method may result in a hazardous situation. Operators should take appropriate safety and protective measures. A.2 General provisions Unless otherwise stated, only the reagents identified as analytical reagents and the tertiary water specified in GB/T 6682-2008 are used in the analysis. Standard titration solution used in the test method, standard solution for the determination of impurities, preparations and articles, in the absence of other requirements, GB/T 601, GB/T 602 and GB/T 603. A.3 Identification test Weigh about 1mg of laboratory samples and 100mg potassium bromide, research into uniform powder, into the former, after pressing into the film with infrared The spectra of the fumaric acid are shown in Figure B.1. The spectra of the fumaric acid are shown in Figure B.1. A.4 Determination of fumaric acid A.4.1 Methodological Summary The aqueous solution of the sample was titrated with the standard solution of sodium hydroxide with phenolphthalein as the indicator, and the amount of the solution was titrated according to the standard of sodium hydroxide. The total acid content of C4H4O4 dry basis is fumaric acid content. A.4.2 Reagents and materials A.4.2.1 Sodium hydroxide standard titration solution. c (NaOH) = 0.5 mol/L. A.4.2.2 phenolphthalein indicator solution. 10g/L. A.4.3 Analysis steps A.4.3.1 Weigh 1.0g of laboratory samples, accurate to 0.0002g, into the 250mL Erlenmeyer flask, add 100mL of water, dissolved by heating, After cooling, add 3 drops of phenolphthalein indicator solution, titration with sodium hydroxide standard solution to the reddish, keep 30s do not fade for the end. A.4.3.2 At the same time as the determination, the same amount of reagent solution was used as a blank test in the same procedure as for the measurement. A.4.4 Calculation of results The mass fraction w1 of fumaric acid (based on C4H4O4, dry basis) is expressed in%, calculated according to formula (A.1) w1 = [(V-V0)/1000] cM (1-w3) m × 100% (A.1) Where. V --- sample consumption of sodium hydroxide standard titration solution (A.4.2.1) volume of the value in milliliters (mL); V0 --- blank test consumption of sodium hydroxide standard titration solution (A.4.2.1) volume of the value in milliliters (mL); c - the exact value of sodium hydroxide standard titration solution concentration in moles per liter (mol/L); m - the mass of the sample, in grams (g); w3 --- A.9 measured moisture,%; M - fumaric acid (1/2C4H4O4) in grams per mole (g/mol) (M = 58.04). The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.2%. A.5 Determination of arsenic A.5.1 Weigh 1.0g of laboratory samples, accurate to 0.01g, sample treatment by GB/T 5009.76 wet digestion. Use absorption Liquid B, the limited test. A.5.2 Preparation of limited standard solution. Remove (2 ± 0.02) mL of arsenic (As) standard solution (equivalent to 2.0 μgAs) with pipettes, At the same time the same treatment. A.5.3 Other according to GB/T 5009.76 in the diethylamino dithiocarbamate colorimetric method. A.6 Determination of lead A.6.1 Colorimetric method (arbitration law) According to GB/T 5009.75. The sample treatment was carried out by dry digestion. Before use, 1mg/mL lead (Pb) standard solution dilute Release 5 μg/mL lead (Pb) standard solution. (25 ± 0.02) mL sample solution (equivalent to 2.5 g of laboratory sample) at the time of measurement (1 ± 0.02) mL lead (Pb) standard solution (equivalent to 5μgPb), placed in 125mL separatory funnel, lead standard solution plus 1% Nitric acid solution to 25 mL. A.6.2 Atomic Absorption Spectrometry Specimen treatment according to GB/T 5009.75 dry digestion. Others are carried out according to GB 5009.12. A.7 Determination of burning residue Weigh about 2g of laboratory samples, accurate to 0.0001g, burning temperature (800 ± 25) ℃. Other according to GB/T 9741. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.01%. A.8 Determination of maleic acid A.8.1 Methodological Summary The components of the sample solution were separated by high performance liquid chromatography under the selected working conditions, and the samples were separated by UV absorption Detection, with external standard method to calculate the sample of maleic acid content. A.8.2 Reagents and materials A.8.2.1 Maleic acid. mass fraction ≥99.0%. A.8.2.2 Sodium hydroxide solution. 20 g/L. A.8.2.3 Phosphoric acid solution. Take phosphoric acid (excellent grade reagent) (1 ± 0.02) mL In 1000mL volumetric flask, add 100mL methanol (HPLC grade reagent) (according to the column to adjust the amount of added), diluted with water to the mark, and then filtered through the 0.45μm filter. A.8.3 Instruments and equipment A.8.3.1 High Performance Liquid Chromatography System (HPLC) A.8.3.1.1 High pressure pump. no pulse, can keep the flow rate from 0.1mL/min ~ 10.0mL/min. A.8.3.1.2 Dosing ring. 5 μL. A.8.3.1.3 UV detector. variable wavelength. A.8.3.1.4 Data processing systems. Chromatographic workstations or data processors. A.8.3.2 Filtration system The filter system uses a cellulose ester membrane filter with a pore size of 0.45 μm (for pretreatment of the mobile phase). A.8.3.3 Filtration systems The filtration system uses a cellulose ester membrane filter with a pore size of 0.45 m (for pretreatment of the sample). A.8.3.4 injector Autosampler or microinjector, 50 [mu] L or 100 [mu] L. A.8.4 Chromatographic analysis conditions Recommended column and typical operating conditions are shown in Table A.1. Maleic Acid Determination Typical High Performance Liquid Chromatogram See Appendix C, The relative retention times for each component are given in Table C.1 in Appendix C. Other columns that can achieve the same degree of separation and chromatographic operating conditions can be use. Table A.1 Columns and Typical Chromatographic Operating Conditions Column column length 250mm, column diameter 4.6mm, silica gel as the matrix, the surface bonding C8 functional non-polar packing column Column temperature 15 ℃ ~ 60 ℃, control accuracy ± 1 ℃ Mobile phase phosphoric acid solution Flow rate/(mL/min) 1.0 Detector detection wavelength/nm 214 Injection volume/μL 5 A.8.5 Analysis steps A.8.5.1 Preparation of standard solution of maleic acid Weigh 50mg maleic acid, accurate to 0.0002g, dissolved in the amount of water (if necessary, add a small amount of sodium hydroxide solution), transferred to 250mL volumetric flask, diluted with phosphoric acid solution to the scale. Remove the above solution (1 ± 0.02) mL, placed in 100mL volumetric flask, diluted with phosphoric acid solution to the mark, shake, by 0.45μm filter Filter, and then degassed by ultrasonic treatment. A.8.5.2 Preparation of sample solution Weigh 0.1g of laboratory samples, accurate to 0.0002g, placed in 50mL volumetric flask, the mobile phase diluted to the mark, shake, by 0.45μm Filter filter, and then by ultrasonic degassing treatment. A.8.5.3 Determination According to high-performance liquid chromatography procedures to start preheating, adjust the temperature and flow to achieve the conditions of analysis and baseline smooth, with a micro-injector Take the standard sample solution 5μL, injection (or automatic injection), record the maleic acid peak area A2. Take the sample solution with a micro-injector 5μL, injection (or automatic injection), record the resulting measured material peak area A1. A.8.6 Calculation of results Maleic acid mass fraction w2, the value in%, calculated according to formula (A.2). w2 = A1 × m2A2 × m × 100% (A.2) Where. A1 --- peak area of the substance to be tested in the sample solution; A2 - peak area of maleic acid in standard sample solution; m2 - the amount of maleic acid injected in the standard sample solution in micrograms (μg); m - the amount of sample injected in micrograms (μg). A.9 Determination of moisture A.9.1 Dry reduction method Weigh about 5g of laboratory samples, accurate to 0.0002g. Others according to GB/T 6284. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.05%. A.9.2 Karl Fischer Act (Arbitration Act) Weigh 0.5g ~ 1.0g laboratory samples, accurate to 0.0002g. Other according to GB/T 6283. The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.05%.

Appendix B

(Normative appendix) Fumaric acid infrared standard spectra Figure B.1 shows the fumaric acid infrared standard spectra. Figure B.1 Fumaric acid infrared standard spectra Appendix C. (Normative appendix) Maleic acid was used to determine the typical high performance liquid chromatograms and the relative retention times of the components Figure C.1 shows typical high performance liquid chromatograms for the determination of maleic acid. 1 --- maleic acid; 2 --- fumaric acid. Figure C.1 Typical determination of maleic acid for high performance liquid chromatography Table C.1 shows the relative retention times for each component. Table C.1 Relative Retention Time for Each Component Peak sequence name relative retention time 1 maleic acid 0.77 2 fumaric acid 1

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