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GB 1886.21-2016: Food additive -- Calcium lactate
Status: Valid
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Food additive -- Calcium lactate
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GB 1886.21-2016
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Basic data | Standard ID | GB 1886.21-2016 (GB1886.21-2016) | | Description (Translated English) | Food additive -- Calcium lactate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Word Count Estimation | 11,172 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-01-01 | | Older Standard (superseded by this standard) | GB 6226-2005 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | GB 1886.21-2016: Food additive -- Calcium lactate---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 safety national standard - Food additive - Calcium lactate)
National Standards of People's Republic of China
National Food Safety Standard
Food Additives Calcium Lactate
Issued on.2016-08-31
2017-01-01 implementation
People's Republic of China
National Health and Family Planning Commission released
Foreword
This standard replaces GB 6226-2005 "food additive calcium lactate."
This standard compared with GB 6226-2005, the main changes are as follows.
--- Standard name was changed to "national food safety standards for food additives calcium lactate."
National Food Safety Standard
Food Additives Calcium Lactate
1 Scope
This standard applies to starch, sugar feedstock inoculated with lactic acid bacteria fermented extract obtained directly and lactic acid and calcium hydroxide (or carbonate
Calcium) synthetically produced food additive calcium lactate.
2 chemical name, molecular formula, molecular mass and structural formula
2.1 Chemical Name
α- hydroxy calcium propionate
Formula 2.2
C6H10CaO6 · nH2O (n = 0 ~ 5)
2.3 formula
OH
H3C COO-
êê
úú
Ca2 · nH2O
2.4 relative molecular mass
218.22 (anhydrous) (according to 2007 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall comply with the requirements of Table 1.
Table 1 Sensory requirements
Project requires test methods
Color White
Status crystalline powder or granules
Odour odorless or slight specific odor
Take the right amount of sample is placed in a clean, dry white porcelain dish, under natural light, Views
Police state and its color and smell its odor
3.2 Physical and Chemical Indicators
Physical and chemical indicators should be consistent with the provisions of Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Calcium lactate (C6H10CaO6) content (dry basis), w /% 98.0 ~ 101.0 Appendix A A.4
Loss on drying, w /%
Pentahydrate 22.0 to 27.0
Trihydrate 15.0 to 20.0
Monohydrate 5.0-8.0
Anhydrous ≤ 3.0
Appendix A A.5
Dissolved in water by testing A.6 in Appendix A
Free acid and free base by testing in A.7 in Appendix A
Volatile fatty acids by test A.8 in Appendix A
Chloride (Cl dollars), w /% ≤ 0.05 A.9 in Appendix A
Sulfate (SO4 dollars), w /% ≤ 0.075 Appendix A A.10
Fluorides (as F), w /% ≤ 0.0015 Appendix A A.11
Magnesium and alkali metal, w /% ≤ 1.0 Appendix A A.12
Iron (Fe), w /% ≤ 0.005 Appendix A A.13
Arsenic (As)/(mg/kg) ≤ 2.0 GB 5009.76
Lead (Pb)/(mg/kg) ≤ 10.0 GB 5009.75
Heavy metals (Pb)/(mg/kg) ≤ 20 GB 5009.74
Appendix A
Testing method
A.1 Warning
Some test procedures prescribed test method can lead to dangerous situations. The operator shall take appropriate safety and health practices.
A.2 General Provisions
This standard reagents and water in the absence of other specified requirements, refer to the three water analytical reagent and GB/T 6682 regulations. test
In the standard titration solution, impurity measurement standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601,
GB/T 602 and GB/T 603 provisions prepared. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution.
A.3 Identification Test
A.3.1 Reagents and materials
A.3.1.1 sulfuric acid.
A.3.1.2 potassium permanganate solution. 3.2g/L.
A.3.1.3 ammonium oxalate solution. 40g/L.
A.3.1.4 acetic acid solution. 120.
A.3.1.5 hydrochloric acid solution. 13.
A.3.2 Identification method
A.3.2.1 Identification of lactate
Take about 0.5g sample was dissolved in 10mL water, a solution of sulfuric acid to make it acidic, add appropriate amount of potassium permanganate solution is heated, which produce acetaldehyde
odor.
A.3.2.2 Identification of calcium
A.3.2.2.1 taking about 0.5g sample was dissolved in 10mL water, a solution of ammonium oxalate solution, namely a white precipitate. The precipitate was isolated, in acetic acid was added
Solution, insoluble precipitate, hydrochloric acid solution was added, the precipitate was completely dissolved.
A.3.2.2.2 wetted with hydrochloric acid after the platinum wire dipped samples, red yellow colorless flame.
A.4 Determination of calcium lactate (C6H10CaO6) content (dry basis) of
A.4.1 Method summary
Under basic conditions to the sample (in terms of dry goods) the volume of consumption of complexing agent disodium edetate standard titration solution to calculate the milk
Calcium content, calcium reagent color change indicator to determine carboxylate end of the titration.
A.4.2 Reagents and materials
A.4.2.1 hydrochloric acid solution. 14.
A.4.2.2 sodium hydroxide solution. 100g/L.
A.4.2.3 disodium EDTA standard titration solution. c (EDTA) = 0.05mol/L.
A.4.2.4 calcium carboxylate indicator reagent. Weigh 0.1g of calcium reagent carboxylic acid sodium salt, sodium chloride plus 10g grinding dried at about 110 ℃,
Mix well.
A.4.3 Analysis step
Weigh about 0.3g samples, accurate to 0.0002g, was dissolved in 2mL of hydrochloric acid solution was added 50mL of water, was added dropwise with stirring
15mL disodium EDTA standard titration solution, plus 5mL sodium hydroxide solution and 0.1g calcium indicator reagent carboxylate with acetic
Diamine tetra acetic acid disodium standard titration solution titrated to a solution blue color as the end point.
A.4.4 Calculation Results
Calcium lactate (C6H10CaO6) content (dry basis) of the mass fraction w1, according to equation (A.1) Calculated.
w1 =
V1
1000 × c1 × M1
m1 × (1-w2) ×
100% (A.1)
Where.
V1 --- sample consumption volume of disodium EDTA standard titration solution, in milliliters (mL);
1000 --- conversion factor;
Concentration c1 --- disodium edetate standard titration solution, expressed in moles per liter (mol/L);
Molar mass M1 --- calcium lactate, in units of grams per mole (g/mol), [M1 (C6H10CaO6) = 218.2];
M1 --- the quality of the sample, in grams (g);
w2 --- A.5.2 Loss on drying mass fraction,%.
Take two parallel determination results of the arithmetic average of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.3%.
A.5 Determination of loss on drying
A.5.1 Analysis step
Weigh about 1.5g sample, accurate to 0.0002g, placed in a pre dried to a constant mass of 120 ℃ ± 2 ℃ weighing bottle, paved
Layer of 3mm or less. At 120 ℃ ± 2 ℃ constant temperature drying oven 4h, placed in a desiccator to cool 30min weighing.
A.5.2 Calculation Results
Loss on drying mass fraction w2, according to equation (A.2) Calculated.
w2 =
m2-m3
m2 ×
100% (A.2)
Where.
M2 --- dried before the mass of the sample, in grams (g);
Quality, unit m3 --- after drying the sample in grams (g).
Take two parallel determination results of the arithmetic average of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.1%.
A.6 Determination of water soluble
A.6.1 Method summary
The sample is dissolved in water, and to compare the standard turbidity solution.
A.6.2 Reagents and materials
A.6.2.1 nitric acid solution. 12.
A.6.2.2 dextrin solution. 20g/L.
A.6.2.3 silver nitrate solution. 17g/L.
A.6.2.4 turbidity standard solution. chlorine (Cl) 0.01mg/mL. Measure 14.10mLc (HCl) = 0.1mol/L hydrochloric acid standard solution, set
In 50mL volumetric flask, diluted with water to the mark. The solution was weighed 10.00mL placed 1000mL volumetric flask, dilute with water to
Scale.
A.6.3 Analysis step
Weigh 1.0g sample accurate to 0.01g, placed in 25mL colorimetric tube, add 20mL of water on a water bath heated to dissolve, as the sample
Solution; other single 25mL colorimetric tube, was added 0.20mL turbidity standard solution, add water to 20mL, add 1mL nitric acid solution, 0.2mL
Dextrin solution and silver nitrate solution 1mL, shake, dark place 15min, as a standard turbidity solution.
In the absence of direct sunlight, axial and lateral visual observation, the turbidity of the sample solution is not greater than the standard nephelometric turbidity of the solution.
A.7 Determination of free acid and free base
A.7.1 Reagents and materials
A.7.1.1 carbon dioxide-free water.
A.7.1.2 sodium hydroxide standard solution. c (NaOH) = 0.1mol/L.
A.7.1.3 phenolphthalein indicator solution. 10g/L.
A.7.2 Analysis step
Weigh 1.0g sample, accurate to 0.01g, was dissolved in 20mL of carbon dioxide-free water, add 2 drops of phenolphthalein indicator solution, there should be produced a pink
Health; add 0.5mL standard solution of sodium hydroxide, should be pink.
A.8 Determination of volatile fatty acids
A.8.1 Reagents and materials
sulfuric acid.
A.8.2 Analysis step
Weigh about 0.5g sample accurate to 0.01g, in a dry evaporating dish, add 1mL of sulfuric acid, stirred and heated on a water bath, there should be
Fatty odor escape.
A.9 chloride (Cl) Determination
A.9.1 Reagents and materials
A.9.1.1 nitric acid solution. 19.
A.9.1.2 silver nitrate solution. 17g/L.
A.9.1.3 chloride (Cl) standard solution. 0.01mg/mL.
A.9.2 Analysis step
Weigh 1.0g sample (accurate to 0.01g), add water 40mL dissolved, the solution was adjusted to neutral with a solution of nitric acid, diluted with water to
50mL, shaking, filtered, and the filtrate was retained. The filtrate 5.0mL, as a sample solution, placed in 50mL Nessler colorimetric tube, add 10mL nitrate
Acid solution, add water to a volume of about 40mL, add 1.0mL silver nitrate solution, dilute with water to 50mL, shake, dark place for 5min, black
Under the background color, the axial observation, the sample solution turbidity was no larger than a standard turbidity solution.
Turbidity standard solution. Pipette 5.00mL chloride (Cl) standard solution, placed in 50mL colorimetric tube. At the same time with the same sample solution
deal with.
A.10 Sulfate (SO4 meter) measurement
A.10.1 reagents and materials
A.10.1.1 hydrochloric acid solution. 13.
A.10.1.2 barium chloride solution. 250g/L.
A.10.1.3 potassium sulfate standard solution. 0.1mg/mL.
A.10.2 Analysis steps
Weigh 1.0g sample (accurate to 0.01g), a 50mL Nessler colorimetric tube, add water 40mL dissolved, the solution was adjusted with hydrochloric acid solution
Solution to neutral, shaking, diluted hydrochloric acid solution 2mL, 5mL plus barium chloride solution with water to 50mL, shake, place 10min, black
Background, seen in the axial sample solution turbidity was no larger than a standard turbidity solution.
Turbidity standard solution. Measure 7.5mL potassium sulfate standard solution, placed in 50mL colorimetric tube. And the sample solution while the same treatment.
A.11 fluoride (as F) measurement
A.11.1 Method summary
In perchloric acid medium, by steam distillation sample isolated from fluorine, fluorine and Alizarin and lanthanum nitrate mixture formed blue
Color complex. The color of the sample solution and standard colorimetric solution for comparison.
A.11.2 reagents and materials
A.11.2.1 perchloric acid.
A.11.2.2 acetone.
A.11.2.3 silver nitrate solution. 17g/L.
A.11.2.4 sodium hydroxide solution. 4g/L.
A.11.2.5 sodium hydroxide solution. 40g/L.
A.11.2.6 hydrochloric acid solution. 110.
A.11.2.7 Alizarin solution. Weigh 0.193g Alizarin, add a small amount of water and sodium hydroxide solution (40g/L) make
Was dissolved, add 0.13g of sodium acetate, with acetic acid solution (116) was adjusted to pH 5.0 (pH paper with a precision inspection, red), diluted with water
To 500mL, stored in a brown bottle, set in the refrigerator (6 ℃ ~ 8 ℃) saved, precipitation should be reconstituted.
A.11.2.8 buffer solution (pH≈4.7). Weigh 44g of sodium acetate dissolved in 400mL of water, add 22mL glacial acetic acid, acetic acid and then slowly ice
PH was adjusted to 4.7, and then diluted with water to 500mL.
A.11.2.9 lanthanum nitrate solution. Weigh 0.271g lanthanum nitrate, dissolved in a small amount of acetic acid solution (116), add water to about 450mL, with 25g/L
Sodium acetate solution adjusted to pH 5.0 (with a precision pH test paper), and then diluted with water to 500mL, built-in refrigerator, after mildew should
Reassortment.
A.11.2.10 fluoride standard solution. 0.01mg/mL. With water before use fluoride standard solution 0.1mg/mL dilution from.
A.11.2.11 phenolphthalein indicator solution. 10g/L.
A.11.3 instruments and equipment
Measuring fluorine distillation apparatus is shown in Figure A.1.
A.11.4 Analysis steps
Weigh 2.00g sample, accurate to 0.01g, placed in 250mL three-necked flask (see Figure A.1), add a few grains of glass beads, was slowly added
10mL of perchloric acid, with about 8mL water rinse bottle wall, add 4 drops to 6 drops of silver nitrate solution, the thermometer on the cork should Mesa and thermometer
The mercury bulb is inserted in the sample solution, connect the steam generator and straight condenser, a condenser connected to the ends of the glass pipe, and bend
10mL tube is inserted containing sodium hydroxide solution (A.11.2.4) and 2 drops of phenolphthalein indicator solution of 250mL volumetric flask. Steam generator
Adding 500mL of water was added dropwise a solution of sodium hydroxide (A.11.2.5) and the solution was made alkaline. Open the screw clamp and heated to near boiling. Close screw clamp, will
Steam introduced into three-neck flask, three-neck flask while heating, adjusting the amount of water vapor entering, after the temperature rise is maintained at 135 ℃ ~
Between 140 ℃. If the flask solution fade, supplemented with an appropriate amount of sodium hydroxide solution (A.11.2.4) until the distillate of about 200mL, stop
Distillation stop, shake. With sodium hydroxide solution (A.11.2.4) or a hydrochloric acid solution was adjusted to pH 7.0 (pH paper with a precision test), then more
2 drops of hydrochloric acid solution was diluted with water to the mark, shake, as a sample solution. Pipette 25.00mL sample solution, placed in 50mL colorimetric tube, add
5mL Alizarin solution and 3mL buffer solution and mix. Slowly add lanthanum nitrate solution 5mL, shake, plus 10mL propionate
Ketones, water was added to 50mL, room temperature for 20min, compared with the standard colorimetric solution, the color may not be deeper than the standard colorimetric solution.
Standard colorimetric solution is a fluoride standard solution Pipette 0.30mL placed 50mL colorimetric tube, add 25mL water, add 5mL Qian
Su aminoxatyl complexing agent solution and 3mL buffer solution and mix. 5mL solution of lanthanum nitrate was slowly added, shaken, plus 10mL of acetone, water was added
To 50mL, room temperature for 20min.
Explanation.
1 --- steam generator (1000mL flask);
2 --- φ5mm security management;
3 --- φ5mm glass;
4,13,14 --- rubber stopper;
5 --- tee and screw clamp;
6 --- 200 ℃ thermometer;
7 --- 250mL three-necked flask;
8,10 --- glass bends;
9 --- 500mm straight condenser;
11 --- 250mL flask;
12 --- or electric heating mantle.
Figure A.1 measuring fluorine distillation apparatus schematic
A.12 Determination of magnesium and alkali metals
A.12.1 Method summary
Sample of calcium and oxalic acid under acidic conditions form insoluble calcium oxalate precipitation, filtration, the filtrate magnesium sulfate and the alkali metal and heating raw
To sulphate, taken with hot water, then filtered and the filtrate evaporated to dryness, after burning quantification.
A.12.2 reagents and materials
A.12.2.1 hydrochloric acid.
A.12.2.2 sulfuric acid.
A.12.2.3 ammonia.
A.12.2.4 oxalic acid solution. 150g/L.
A.12.2.5 methyl red indicator solution. 1g/L.
A.12.3 Analysis steps
Weigh 1.0g sample accurate to 0.01g, add 40mL water, add 1mL hydrochloric acid, boil 1min, quickly add 40mL solution of oxalic acid
And 2 drops of methyl red indicator solution, neutralized with ammonia solution until just yellow and cooled to room temperature. Transferred to 100mL volumetric flask, dilute to the mark
Degree, shake overnight. Dry filter paper, take 50mL clear filtrate, placed in the evaporating dish, add 1mL of sulfuric acid, evaporated on a water bath
To near dryness on a hot plate heated to sulfuric acid vapor Yat do. The residue was 25mL of water, heated to 80 ℃ leaching, filtration, the filtrate was kept in advance
800 ℃ ± 25 ℃ dried to constant mass crucible, on a hot plate heated to dryness, burning to constant mass at 800 ℃ ± 25 ℃. Residue
Quality must not be greater than 5.0mg.
A.13 Determination of iron (Fe) of
A.13.1 reagents and materials
A.13.1.1 ammonium persulfate.
A.13.1.2 hydrochloric acid solution. 13.
A.13.1.3 ammonium thiocyanate solution. 300g/L.
A.13.1.4 iron (Fe) standard solution. 0.1mg/mL. Before use the preparation to 0.01mg/mL ammonium ferric sulfate standard solution.
A.13.1.5 standard colorimetric solution. Take 2.5mL of iron (Fe) standard solution (0.01mg/mL), placed in 50mL Nessler colorimetric tube, add
4mL hydrochloric acid solution with ammonium sulfate 50mg before, after 35mL diluted with water, add 3mL ammonium thiocyanate solution was diluted with water to 50mL
Nessler colorimetric tube.
A.13.2 Analysis steps
Weigh 0.5g sample accurate to 0.01g, add 25mL water, placed in a water bath heated to dissolve, after cooling the sample solution, add 4mL salt
Acid solution with ammonium sulfate 50mg before, after dilution with water to 35mL, add 3mL ammonium thiocyanate solution, dilute with water to 50mL colorimetric Nessler
tube. The sample solution was the color can not be deeper than the standard colorimetric solution.
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