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GB 25548-2010 English PDF

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GB 25548-2010: National food safety standards of food additives calcium propionate
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Basic data

Standard ID GB 25548-2010 (GB25548-2010)
Description (Translated English) National food safety standards of food additives calcium propionate
Sector / Industry National Standard
Classification of Chinese Standard X42
Classification of International Standard 67.220.20
Word Count Estimation 10,129
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 propionic acid and calcium hydroxide (or calcium carbonate) as raw material, and in, refining, drying food additive calcium propionate.

GB 25548-2010: National food safety standards of food additives calcium propionate

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

Foreword

Appendix A of this standard is a normative appendix. National standards for food safety Food additives calcium propionate

1 Scope

This standard applies to propionic acid and calcium hydroxide (or calcium carbonate) as raw materials, by the neutralization, refining, drying the food additive calcium propionate.

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 molecular formula, structural formula and relative molecular mass 3.1 Molecular formula C6H10CaO4 · nH2O (n = 0,1) 3.2 Structural formula H3 3.3 Relative molecular mass 186.22 (anhydrous) (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 and tissue state White crystals, granules or crystalline powder Odorless or slightly propionic Take appropriate laboratory samples, placed in a clean, dry white porcelain dish, in nature Under the 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 Calcium propionate (based on C6H10CaO4, dry basis), w /% ≥ 99.0 Appendix A, A.4 Water insoluble matter, w /% ≤ 0.30 Appendix A, A.5 The free acid or free base test was passed in Test Annex A, A.6 Dry reduction, w /% ≤ 9.5 Appendix A A.7 Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.8 Heavy metals (Pb)/(mg/kg) ≤ 10 Appendix A A.9 Fluoride (in F)/(mg/kg) ≤ 30 Appendix A. A.10 Iron (Fe)/(mg/kg) ≤ 50 Appendix A A.11

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 A.3.1 Reagents and materials A.3.1.1 hydrochloric acid solution. 1 3. A.3.1.2 Sulfuric acid solution. 1 9. A.3.1.3 Ammonium oxalate solution. 40 g/L. A.3.1.4 Acetic acid solution. 1 20. A.3.2 Analysis steps A.3.2.1 Identification of propionic acid Weigh 0.5g of laboratory samples, accurate to 0.01g, placed in a 100mL beaker containing 5mL water, stirring dissolved, add 5mL sulfur Acid solution, heating, there should be a special odor generated. A.3.2.2 Identification of calcium salts Weigh 0.5g of laboratory samples, accurate to 0.01g, placed in a 100mL beaker with 5mL water, stir dissolved, add ammonium oxalate Solution, which produces a white precipitate. Separation of precipitation, add acetic acid solution, precipitation does not dissolve; plus hydrochloric acid solution, can be completely dissolved. Dilute the sample with hydrochloric acid moistened platinum wire and red in a colorless flame. A.4 Determination of calcium propionate A.4.1 Methodological Summary To the calcium reagent sodium carboxylate as an indicator, under alkaline conditions with ethylenediamine tetraacetic acid disodium (EDTA) standard titration solution titration drying test Aqueous solution, according to the consumption of ethylenediamine tetraacetic acid disodium (EDTA) standard titration solution volume, calculated to C6H10CaO4 propionic acid Calcium content. A.4.2 Reagents and materials A.4.2.1 Sodium hydroxide solution. 100 g/L. A.4.2.2 Ethylenediamine tetraacetic acid disodium (EDTA) standard titration solution. c (EDTA) = 0.05 mol/L. A.4.2.3 calcium reagent sodium carboxylate indicator. Weigh 0.5g calcium reagent sodium carboxylate, add 50g potassium sulfate grinding, mixing. A.4.3 Analysis steps Weigh about 1gA.7.1 dry matter A, accurate to 0.0002g, soluble in water, into the 100mL volumetric flask, diluted to the mark. the amount Take (25 ± 0.02) mL of the sample solution, add 75 mL of water, titrate the solution with ethylenediaminetetraacetic acid disodium standard titration to near end 15mL sodium hydroxide solution, put 1min, add 0.1g calcium reagent sodium carboxylate indicator, with ethylenediamine tetraacetic acid disodium standard titration solution drops Set to red completely disappear to appear blue for the end. A.4.4 Calculation of results The mass fraction w1 of calcium propionate (calculated as C6H10CaO4 on a dry basis) is expressed in%, calculated according to the formula (A.1) w1 = (V/1000) cM m x 25/100 x 100% (A.1) Where. V - Ethylenediamine tetraacetic acid Disodium standard titration solution (A.4.2.2) Volume in milliliters (mL); c - Ethylenediamine tetraacetic acid disodium standard titration solution concentration of the exact value in moles per liter (mol/L); m - the mass of the sample, in grams (g); M - the value of the molar mass of calcium propionate in grams per mole (g/mol) (M = 186.2). 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 water insoluble content A.5.1 Instruments and equipment Glass filter. filter plate diameter 5μm ~ 15μm. A.5.2 Analysis steps Weigh 10.0g of laboratory samples, accurate to 0.01g, add 100mL water, stir and place for 1h, with a constant quality of glass Filtered filter, washed with water 30mL filter residue, dried at (180 ± 2) ℃ 4h, after cooling and weighing. A.5.3 Calculation of results The mass fraction of water insoluble matter w2, the value in%, calculated according to formula (A.2). w2 = m1 m2 × 100% (A.2) Where. m1 --- the value of the quality of residue, in grams (g); m2 --- the mass of the sample, in grams (g). 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 0.02%. A.6 Free acid or free base test A.6.1 Reagents and materials A.6.1.1 sodium hydroxide standard titration solution. c (NaOH) = 0.1mol/L. A.6.1.2 Standard titration solution for hydrochloric acid. c (HCl) = 0.1 mol/L. A.6.1.3 phenolphthalein indicator solution. 10g/L. A.6.2 Analysis steps Weigh 2.0g laboratory samples, accurate to 0.01g, dissolved in 20mL without carbon dioxide water, add 2 drops of phenolphthalein indicator solution, if the solution was red (0.3 ± 0.02) mL hydrochloric acid standard titration solution, the solution should be colorless; if the solution was colorless, add (0.6 ± 0.02) mL of sodium hydroxide Standard titration solution, the solution should be pink. A.7 Determination of dry reduction A.7.1 Analysis steps Weigh about 1g of laboratory samples, accurate to 0.0002g, placed in the pre-(120 ± 2) ℃ dry to the constant quality of the weighing bottle, shop Into the layer below 5mm. In the (120 ± 2) ℃ constant temperature drying oven for 2h, placed in a dryer for 30min cooling. Retention Department The dried product (this is dry matter A) is used for the determination of calcium propionate content. A.7.2 Result calculation The mass fraction of dry weight w3, expressed in%, is calculated according to formula (A.3). w3 = m-m1 m x 100% (A.3) Where. m - the mass of the sample before drying, in grams (g); m1 --- the quality of the sample after drying, in grams (g). 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.8 Determination of arsenic According to GB/T 5009.76 arsenic spot method. Weigh 0.25g laboratory samples, accurate to 0.01g, add water 5mL dissolved. (0.75 ± 0.02) mL of arsenic (As) standard solution (equivalent to 0.75 μgAs) with a pipette. At the same time the same treatment. A.9 Determination of heavy metals A.9.1 Reagents and materials A.9.1.1 Acetic acid solution. 1 19. A.9.1.2 sodium sulfide solution. Weigh 5g sodium sulfide, with 10mL water and 30mL glycerol mixed solution dissolved. Will be half the volume of that The solution was saturated with hydrogen sulfide while cooling, and the remaining half was added to the mixture. In the shade filled with vials, sealed closed preservation. Valid for three months after preparation. A.9.2 Analysis steps Weigh 2.0g laboratory samples, accurate to 0.01g, placed in 50mL colorimetric tube, add 40mL water dissolved, add 2mL acetic acid dissolved Liquid, add water to 50mL, add 2 drops of sodium sulfide solution, placed in the dark for 5min. The color should not be deeper than the standard colorimetric solution. Preparation of Standard Colorimetric Solution. Take (2 ± 0.02) mL of lead (Pb) standard solution (0.01 mg/mL) and treat the same sample at the same time as the sample. A.10 Determination of fluoride A.10.1 Reagents and materials A.10.1.1 perchloric acid. A.10.1.2 Acetone. A.10.1.3 Perchloric acid solution. 1 100. A.10.1.4 Sodium hydroxide solution. 40 g/L. A.10.1.5 Sodium hydroxide solution. 4 g/L. A.10.1.6 Acetic acid solution. 1 16. A.10.1.7 Silver nitrate solution. 17 g/L. A.10.1.8 phenolphthalein indicator solution. 10g/L. A.10.1.9 Alizarin Ammonia Complex Solution. Weigh 0.04g alizarin ammonia complexing agent, add a little sodium hydroxide solution (A.10.1.5) dissolved to The perchloric acid solution was neutralized to orange-red (but not milky) and diluted to.200 mL with water. A.10.1.10 lanthanum perchlorate solution. Weigh 0.04g lanthanum oxide, add 0.25mL perchloric acid, dissolve warm, diluted with water to 50mL. A.10.1.11 Acetic acid-sodium acetate buffer solution. Weigh 11.0 g of anhydrous sodium acetate, add 30 mL of glacial acetic acid, 170 mL of water and shake to dissolve. A.10.1.12 Compound reagent. 60.0mL alizarin complex solution and 6.0mL lanthanum perchlorate solution, 20.0mL acetic acid-sodium acetate The buffer solution was diluted with water to.200 mL. A.10.1.13 Fluoride (F) Standard solution. 0.01 mg/mL. A.10.2 Analysis steps Weigh 5.0g of laboratory samples, accurate to 0.01g, placed in 125mL with branching distillation bottle, add a few pieces of glass beads, slowly joined 10mL perchloric acid solution, 10mL water, 3 ~ 5 drops of silver nitrate solution, distillation bottle with a double hole rubber stopper, a hole into the.200 ℃ thermometer Branch, thermometer mercury ball should be inserted into the test solution, the other hole with a split funnel, then a capillary, capillary into the liquid surface. Branch pipe cold Condenser, condenser outlet end of a glass elbow, glass elbow into the water containing 10mL, sodium hydroxide solution (A.10.1.4) a few drops and phenolphthalein Indicator 1 drop of 100mL volumetric flask under the surface. Heating distillation, with a separatory funnel drop water control, keep the test solution temperature at 135 ℃ ~ 140 ° C, and the distillation is stopped when the distillate is about 80 mL. The distillate was neutralized with sodium hydroxide solution (A.10.1.4) to light red After neutralization with acetic acid solution to colorless, diluted with water to the mark, shake. Measure the amount of 10mL placed in 50mL colorimetric tube, add 5mL compound test Agent, 6mL acetone, add water to 50mL, shake, room temperature for 25min. Compared with the standard colorimetric solution, the blue and purple shall not be deeper than the standard Quasi-colorimetric solution. Standard colorimetric solution preparation. take (1.5 ± 0.02) mL fluoride (F) standard solution, the same sample with the same treatment. A.11 Determination of iron A.11.1 Reagents and materials A.11.1.1 Hydrochloric acid. A.11.1.2 ammonium persulfate. A.11.1.3 Ammonium thiocyanate solution. 250 g/L. A.11.1.4 iron (Fe) standard solution. 0.01 mg/mL. A.11.2 Analysis steps Weigh 0.5g of laboratory samples, accurate to 0.01g, dissolved in 40mL water, add 2mL hydrochloric acid, 40mg ammonium persulfate and 5mL Ammonium thiocyanate solution, shake, this is the sample solution. Preparation of standard colorimetric solution. (2.5 ± 0.02) mL of iron (Fe) standard solution, add water to 40mL, and sample the same treatment. Specimen solution is red not deep in the standard colorimetric solution, that is, through the test.

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