GB 22557-2008 English PDFUS$229.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 22557-2008: Food additive -- Sodium iron (Ⅲ) ethylenediaminetetraacetate, trihydrate Status: Valid
Basic dataStandard ID: GB 22557-2008 (GB22557-2008)Description (Translated English): Food additive -- Sodium iron (��) ethylenediaminetetraacetate, trihydrate Sector / Industry: National Standard Classification of Chinese Standard: X42 Classification of International Standard: 67.220.20 Word Count Estimation: 10,142 Date of Issue: 2008-12-03 Date of Implementation: 2009-06-01 Quoted Standard: GB/T 601; GB/T 602; GB/T 603; GB/T 5009.12; GB/T 5009.76; GB/T 6682; General Administration of Quality Supervision, Inspection and Quarantine of Decree No. 75 of prepackaged goods metrological supervision and management approach Adopted Standard: JECFA 53-1999, NEQ Regulation (derived from): Announcement of Newly Approved National Standards No. 19 of 2008 (No. 132 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 food additive sodium iron EDTA technical requirements, test methods, inspection rules, marking, packaging, transportation, storage and shelf life. This standard applies to trivalent iron machine with EDTA sodium salt as raw food additive reaction of sodium iron EDTA, the product as iron fortifier use. GB 22557-2008: Food additive -- Sodium iron (Ⅲ) ethylenediaminetetraacetate, trihydrate---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.Food additive.Sodium iron (Ⅲ) ethylenediaminetetraacetate, trihydrate ICS 67.220.20 X42 National Standards of People's Republic of China Food additive sodium iron EDTA Published 2008-12-03 2009-06-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China issued Foreword4.2 This standard is mandatory, the rest are recommended. This standard and the Codex Alimentarius Commission (CODEX) "sodium iron EDTA" (in English) [JECFA 53rd (1999)] of It is not equivalent. Appendix A of this standard is normative. This standard by the National Standardization Technical Committee on Food Additives and centralized. This standard was drafted. Beijing VITA nutrition and health care products companies. The main drafters. Huo Junsheng, Yu Bo, Huang Jian, Sun Jing. Food additive sodium iron EDTA Range 1 This standard specifies the food additive sodium iron EDTA (of NaFeEDTA) technical requirements, test methods, inspection rules, standard Chi, packaging, transportation, storage and shelf life. This standard applies to ferric salts and sodium ethylenediaminetetraacetic acid as a raw material of food additives produced by the reaction of iron ethylenediaminetetraacetic acid Sodium, the product is used as an iron nutrition enhancer.2 Normative referencesTerms of the following documents become provisions of this standard by reference in this standard. For dated reference documents, all later Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to agreements based on this standard Whether the latest versions of these documents. For undated references, the latest version applies to this standard. Preparation GB/T 601 standard titration solution Chemicals GB/T 602 Chemicals determination of impurities in the prepared standard solution (GB/T 602-2002, ISO 6353-1. 1982, NEQ) with GB/T 603 Test Methods Chemicals Preparations of articles (GB/T 603-2002, ISO 6353-1 with. 1982, NEQ) Determination of lead in food GB/T 5009.12 Determination of arsenic in food additives 5009.76 GB/T GB/T 6682 for analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD) The State Administration of Quality Supervision, Inspection and Quarantine Decree No. 75 of prepackaged goods metrological supervision and management measures 3 Product Chemical name, molecular formula, structural formula and relative molecular mass 3.1 Chemical Name. sodium iron EDTA. 3.2 Molecular formula. C10H12FeN2NaO8 · 3H2O. 3.3 Structure. 3.4 molecular weight. 421.09 (according to 2005 international relative atomic mass). 4. Technical Requirements 4.1 Appearance. pale yellow powder, soluble in water. Food additive EDTA 4.2 sodium iron shall meet the technical requirements shown in Table 1. Table 1 Technical Requirements Item Index Iron (Fe) mass fraction/12.5 to 13.5% Ethylenediaminetetraacetic acid mass fraction /% 70.5 65.5 - The pH (10g/L solution) 3.5 to 5.5 TABLE 1 (cont.) Item Index Mass fraction of water insoluble /% ≤ 0.1 The mass fraction of nitrilotriacetic acid /% ≤ 0.1 Lead (Pb) content/(mg/kg) ≤ 1 Arsenic (As) content/(mg/kg) ≤ 15 Test methods5.1 Warning Some test procedure specified test methods can lead to dangerous situations. The operator shall take appropriate safety and health practices. 5.2 General Provisions Unless otherwise stated, use only confirmed in the analysis of analytical grade reagents and GB/T 6682 provisions tertiary water. When in the test methods standard titration solution, standard solution, the determination of impurities, products and preparations, in the absence of other requirements specified use, are by GB/T 601, GB/T 602 and GB /603 Preparation of predetermined T. 5.3 Identification Test 5.3.1 Reagents 5.3.1.1 ammonium thiocyanate solution. 8g/L. 5.3.1.2 hydrochloric acid solution (10%). 5.3.2 Identification of 5.3.2.1 Color Reaction. 50mg sample was weighed to the nearest 0.1 mg, into 10mL glass test tube, was added 5mL of water dissolved, The ammonium thiocyanate solution 1.0mL, solution color change should not occur. Was added 0.5 mL of hydrochloric acid solution, mixing the solution presented deep red. 5.3.2.2 UV absorption. Weigh the sample to the nearest 0.1 mg, add water formulated as 20μg/mL solution, using an ultraviolet spectrophotometer Fixed, maximum absorption at a wavelength of 256nm ± 2nm. 5.4 Determination of the iron content 5.4.1 Principle The oxidation-reduction titration iodometry. Ethylenediaminetetraacetic acid sodium iron under strongly acidic conditions, is liberated with an excess of potassium iodide given Fe3 + And the amount of reaction product precipitated I2, I2 standard sodium thiosulfate titration solution and then precipitated titration. Fe3 + + 2I- = Fe2 + + I2 I2 + 2S2O32- = 2I- + S2O62- 5.4.2 Reagents 5.4.2.1 potassium iodide. 5.4.2.2 hydrochloric acid. 5.4.2.3 sodium thiosulfate standard titration solution. Ba (Na2S2O3) = 0.1mol/L. 5.4.2.4 starch indicator solution. 10g/L. 5.4.3 Analysis of step Weigh about 0.5g samples, accurate to 0.0002g, 40mL water with iodine dissolved in a flask, 3g ± 0.0002g iodide Potassium, 20 mL hydrochloric acid, shake, cork seal, is placed in the dark for about 5min, stopper cap from the plug and rinsed with a small amount of water, dropwise with sodium thiosulfate standard Solution was titrated to fixed near the end, was added 2.0mL starch indicator solution and continue the titration to the disappearance of the blue end point. While determination, titrated without sample blank solution was titrated with standard sodium thiosulfate. 5.4.4 calculation results An iron content, expressed in% value, calculated according to formula (1). 1 = Qiao Qiao 1- 2 1000 × 1 × M1 Ba 100 (1) Where. Qiao consumption sample 1 --- sodium thiosulfate standard titration solution (5.4.2.3) the value of the volume in milliliters (mL); Qiao consumption blank 2 --- sodium thiosulfate standard titration solution (5.4.2.3) the value of the volume in milliliters (mL); Ba 1 --- sodium thiosulfate standard solution concentration titration accurate value, in units of moles per liter (mol/L); Numerical molar mass Ml --- iron units of grams per mole (M1 = 55.85) (g/mol); 5.4.5 allows poor Under the repeated twice to obtain absolute difference between the measurement results should not exceed 2% of the arithmetic mean, taking two parallel geodesic The arithmetic average of a predetermined measurement result. 5.5 Determination of the content of ethylenediamine tetraacetic acid 5.5.1 Principle Complexometric titration. Triethanolamine after masking of Fe3 + at pH 12.5 ~ 13 alkaline solution, Ca2 + titration NaFeEDTA, and wherein the EDTA form a stable complex, Ca2 + and then with a hydroxy naphthol blue (hydroxynaphtholblue) excess Indicator combined into complexes, the titration end point is wine red. EDTA content is calculated by Ca2 + consumed titrant. 5.5.2 Reagents 5.5.2.1 acetate monohydrate. 5.5.2.2 EDTA. standard reagents. 5.5.2.3 hydroxy naphthol blue. indicator, by hydroxy naphthol blue. NaCl = 1.100 formulated by mixing milled. 5.5.2.4 sodium hydroxide solution. 500g/L. Sodium hydroxide 50g, dissolved in water and dilute to 100mL. 5.5.2.5 triethanolamine. 5.5.3 Determination 5.5.3.1 0.25mol/L calcium acetate monohydrate calibration titration solution. Weigh 44.0g of analytically pure calcium acetate monohydrate, accurate to 0.0002g, into 1L volumetric flask, and dissolved in water to volume. Weigh 2.0g ~ 2.1g of ethylenediaminetetraacetic acid, 0.0002g precision, set Into a 250mL Erlenmeyer flask, 150 mL water was added, then sodium hydroxide solution to dissolve and the pH adjusted to 11 ~ 12. Join 30mg Hydroxy naphthol blue indicator, titrated with a titration of calcium acetate monohydrate, and the solution changed from blue to red, is the end. Molar concentration of the calcium acetate monohydrate titration solution Ba 2, the value in mol/L expressed by the formula (2). Ba 2 = Qiao 3 × M2 (2) Where. Qiao 3 --- consumption value titration calibrated with a solution of calcium acetate monohydrate volume in milliliters (mL); --- M2 molar mass values of ethylenediaminetetraacetic acid, in units of grams per mole (g/mol) (M2 = 292.24). 5.5.3.2 titrations. Weigh about 0.8g ~ 1.0g sample in duplicate, accurate to 0.0002g, into a 250mL Erlenmeyer flask, add 75mL of distilled water. With triethanolamine and the solution was adjusted to pH 9.0. Sodium hydroxide solution and then adjusted the pH of the sample solution 12.5 to 13.0, the solution became colorless, clear. Was added 30mg hydroxy naphthol blue indicator, calibrated drops with calcium acetate monohydrate Set, the solution from blue to red is the titration end point. 5.5.4 computing Ethylenediaminetetraacetic acid content of 2, expressed in%, (3) is calculated according to the formula. 2 = Qiao Ba 4 × 2 × M2 100 (3) Where. 4 --- Qiao consumption value titration sample solution volume solution of calcium acetate monohydrate in milliliters (mL); 5.5.5 allowable difference Under the repeated twice to obtain absolute difference between the measurement results should not exceed 2% of the arithmetic mean, taking two parallel geodesic The arithmetic average of a predetermined measurement result. Weighed amount of sample, the concentration of aqueous solution formulated as 100 + 1, measured using a pH meter at room temperature. 5.7 Determination of insoluble matter 5.7.1 Determination 5g samples were weighed to the nearest 0.0002g, placed in 250mL beaker, 100mL of water was added with stirring to dissolve. The quantitative filter paper put Diameter fritted funnel into 3.5cm ~ 4.0cm in deionized water against the filter paper by vacuum filtration fritted funnel. In an oven at 175 ℃ After 15min remove dried, placed in a desiccator to cool to room temperature, the recording accurately weighed, is connected to the vacuum filter apparatus. The sample solution Was slowly poured into a fritted funnel, the entire sample solution was filtered under reduced pressure, washed with deionized water three times 10mL above. Sand core funnel After drying 110 ℃ IH, cooled to room temperature and placed in a desiccator, weighed and recorded. Calculated mass fraction of water-insoluble. 5.7.2 computing Ω3 mass fraction of water-insoluble, values are expressed in%, calculated according to formula (4). ω3 = (4) Where. 5.8 Determination of the content of three amino acid Nitrilotriacetic acid abbreviation. NTA, Formula. C6H9NO6, molecular weight. 191.14. Inspection method specified in Appendix A. 5.9 Determination of lead content Inspection method according to GB/T 5009.12 provisions. Determination of arsenic content of 5.10 Inspection method according to GB/T 5009.76 provisions.6 Inspection Rules6.1 Batch To determine the lot number of the product in accordance with its respective rules by the quality inspection departments of production units, the final mixing and there is uniformity of quality of production Product batch. 6.2 Sampling rules Randomly selected samples from each batch, each batch of 3% of the number of extracted sample packages, each consisting of not less than three packages, each package Samples taken not less than 100g, the extracted sample is rapidly mixed, dispensed into two clean, dry bottle and attach a label on the bottle, marked Manufacturer name, product name, production date, batch number and date of sampling bottle for examination, a bottle sealed retained for future reference. 6.3 factory inspection 6.3.1 factory inspection items Including sensory requirements, iron, EDTA, pH value, water insoluble. 6.3.2 release requirements Each batch of products must be specified in this standard test method by the factory inspection department, before leaving the factory after passing inspection. 6.4 Type inspection All items specified in Chapter 4 are type test items. Type inspection once every six months, or when one of the following occurs When tested. --- large change material, the process occurs; --- after long shutdown to resume production; --- factory inspection results with the usual record is quite different; --- When the national health or quality supervision and inspection agencies or user request. 6.5 determine the rules When tested on all the technical requirements, test results if an index does not meet this standard, it should be doubled sampling, unqualified items Head re-examination, if any one still review the results do not meet the standard requirements, the lot is determined to be defective. Within the warranty period, when the two sides dispute between supply and demand on product quality by mutual agreement or arbitration commission review unit, according to the standards set by the Test methods for arbitration. 7 signs, packaging, transportation, storage and shelf life 7.1 marks Firm should be clearly marked on the product packaging containers, including. product name, manufacturer name, address, health permits, Production license number, lot number or production date, net content, shelf life, and labeled "food additive" or "nutritional supplements" words. 7.2 Packaging Packaging materials and containers shall be approved by the state, and in accordance with appropriate hygiene standards of food packaging materials, ethylene diamine tetra-acetic acid Sodium iron should be stored in a sealed container protected from light. Packaging net weight deviation should be consistent with the State General Administration of Quality Supervision, Inspection and Quarantine of the first 75 orders. 7.3 Transport Carry goods should not be mixed with toxic and hazardous substances and contamination during transport to avoid the rain and sun and so on. 7.4 Storage Airiness product, clean, dry place, can not coexist with toxic, hazardous and corrosive substances and the like. 7.5 Shelf Life The product from the production date, in conformity with the above storage conditions, the intact original packaging, shelf life should not be less than 24 months.Appendix A(Normative) Determination of nitrilotriacetic acid A. 1 reagent This reagent not traveled the method designator, were of analytical grade (the AR), ultrapure water was used (18.2MΩ · cm). A. 1.1 Methanol. HPLC grade. A. 1.2 to 25% (mass concentration) of tetrabutyl ammonium hydroxide solution in methanol (TBAOH). A. Blank solution of ammonium hydroxide 1.3. 0.5mL was diluted with water to 10 mL ammonium hydroxide. A. 1.4 copper nitrate solution (10g/L). Weigh 10.0g copper nitrate, dissolved in water and dilute 1000mL. A. 1.5 1mol/L phosphoric acid. phosphoric acid diluted with 6.25mL water to 100mL. A. 1.6 nitrilotriacetic acid standard stock solution. Weigh 100mg nitrilotriacetic acid, accurate to 0.0002g, moved 10mL volumetric flask, add 0.5mL of ammonium hydroxide was diluted and mixed with water to the mark. A. 1.7 nitrilotriacetic acid standard solution. Weigh 1.00g sample, accurate to 0.0002g, moved to a 100mL volumetric flask. Added 100μL Standard stock solution, dilute to the mark with a copper nitrate solution, shake. Ultrasonic treatment to give a standard solution. A. 2 equipment and instruments A. 2.1 commonly used laboratory equipment. A. 2.2 HPLC. a UV detector. A. 2.3 pH meter. A. Step 3 analysis A. 3.1 Sample Processing 1g samples were weighed to the nearest 0.0002g, into a 100mL volumetric flask, add 100μL blank solution of ammonium hydroxide, nitric acid Copper solution was diluted to the mark. Ultrasonic treatment, to obtain a test solution. A. Chromatographic conditions 3.2 Reference Precolumn. C85μm, 4.6mm × 10mm. Mobile phase. Add 10mL of 25% tetrabutylammonium hydroxide solution in methanol and 200mL water, then with 1mol/L phosphoric acid was adjusted to pH 7.5 ± 0.1. The solution was transferred to 1000mL volumetric flask, diluted with 90mL of methanol with water to the mark with 0.45μm or less Porosity membrane filter filtering, degassing. Analysis Column. C85μm, 4.6mm × 150mm. UV detection wavelength. 244nm. Injection volume. 20μL. Flow rate. 2.0mL/min. A. 3.3 Sample Analysis They were injected into the same volume of standard solution (approximately 20 L) and the test solution, the test corresponding to the maximum peak. When nitrilotriacetic acid reservations Between 3.5min, sodium ethylenediaminetetraacetic acid iron 11.9min. All experimental solution prior to injection were analyzed with 0.45μm micropore filter Membrane filtration. Under the experimental conditions, it was injected into the test solution and standard solution were measured. Each sample was repeated 3 times and averaged. Injecting recording peak of standard solution after three operations as a guide, the relative standard deviation of not more than 2.0%, nitrilotriacetic acid and ethylene Resolution between the amine Sodium Iron is greater than 4.0. A. Calculated Nitrilotriacetic acid mass fraction of [omega], values are expressed in%, calculated according to formula (A.1). ω = A2 × 100 (A1-A2) × 1000 (A.1) Where. A2 --- copper test solution nitrilotriacetic acid chromatographic peak area, unit million seconds millivolts (Wan mV · s); A1 --- standard solution nitrilotriacetic acid copper average peak area millivolts unit million seconds (ten thousand mV · s). Detection limit. used for the determination of sodium edetate iron nitrilotriacetic acid lowest detection limit of 20mg/kg. ...... |
