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