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                    The national food safety standard food additive diacetyl tartaric single and double glyceride
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  Basic data             |  Standard ID  |          GB 25539-2010 (GB25539-2010) |               |  Description (Translated English)  |          The national food safety standard food additive diacetyl tartaric single and double glyceride |               |  Sector / Industry  |          National Standard |               |  Classification of Chinese Standard  |          X42 |               |  Classification of International Standard  |          67.220.20 |               |  Word Count Estimation  |          10,170 |               |  Date of Issue  |          2010-12-21 |               |  Date of Implementation  |          2011-02-21 |               |  Quoted Standard  |          GB/T 9741; GB 5009.12 |               |  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 diacetyl tartaric anhydride with mono-, di fatty acid glycerides prepared by the reaction of the food additive diacetyl tartaric acid mono-and diglycerides.  |         
  GB 25539-2010: The national food safety standard food additive diacetyl tartaric single and double glyceride ---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.  
The national food safety standard food additive diacetyl tartaric single and double glyceride
National Food Safety Standard
Food additive diacetyl tartaric acid esters Mono
Issued on. 2010-12-21
2011-02-21 implementation
National Standards of People's Republic of China
People's Republic of China Ministry of Health issued
Foreword
Appendix A of this standard is a normative appendix.
National Food Safety Standard
Food additive diacetyl tartaric acid esters Mono
1 Scope
This standard applies to the diacetyl tartaric acid anhydride and mono-, di- fatty acid esters prepared by the reaction of a food additive diacetyl tartaric acid alone
Di-glycerides.
2 Normative references
The standard file referenced in the application of this standard is essential. For cited documents with dates, only the date of
Version applies to this standard. For undated references, the latest edition (including any amendments) applies to this standard.
3 Technical requirements
3.1 Sensory requirements. comply with Table 1.
Table 1 Sensory requirements
Project requires test methods
Color light yellow or milky proper amount of sample is placed in a clean, dry white porcelain dish or beaker
, Under natural light, observe its color and texture,
Its taste and olfactory.
Smell of acetic acid taste
Organized state at room temperature, liquid, paste or waxy solid (flakes or powder)
3.2 Physical indicators. to comply with Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Total tartaric, w /% 10 ~ 40 in Appendix A A.3
Total glycerol, w /% 11 ~ 28 in Appendix A A.4
Total acetic acid, w /% 8 ~ 32 in Appendix A A.5
Free glycerol, w /% ≤ 2.0 A.6 in Appendix A
Residue on ignition, w /% ≤ 0.5 GB/T 9741a
Lead (Pb)/(mg/kg) ≤ 2 GB 5009.12
Acid value (in dollars KOH)/(mg/g) in line with claims A.7 in Appendix A
Saponification value (in dollars KOH)/(mg/g) in line with claims A.8 in Appendix A
a sample is weighed sample of about 5 g.
Appendix A
(Normative)
Testing method
A.1 General Provisions
Unless otherwise indicated in the analysis using only recognized as analytical reagents and GB/T 6682-2008 specified in the water. In the analysis
Standard titration solution, impurities measured by standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601, GB/T
602, the provisions of preparation GB/T 603's. This solution was used in the test does not indicate what is formulated with solvent, it refers to an aqueous solution.
A.2 Identification Test
A.2.1 Reagents and materials
a) ethanol.
b) Lead acetate test solution. Weigh 9.5g crystalline lead acetate [Pb (C2H3O2) 2 · 3H2O], dissolved in freshly boiled cooled water, and set the volume
To 100mL.
A.2.2 Determination
Weigh 0.5g sample was dissolved in 10mL of ethanol, a solution of lead acetate test solution should produce a white flocculent precipitate is almost insoluble in water.
A.3 Determination of Total tartaric acid
A.3.1 Reagents and materials
a) trichloromethane (chloroform).
b) tartaric acid.
c) acetic acid.
d) sodium metavanadate solution. 50g/L.
e) Potassium hydroxide solution. 0.5mol/L.
f) phosphoric acid. 14.
g) phenolphthalein indicator solution. 10g/L.
A.3.2 Instruments and Equipment
a) spectrophotometer equipped with a 520nm filter or a photoelectric colorimeter.
b) a length of 65cm or more air-cooled condenser.
A.3.3 Analysis step
A.3.3.1 Drawing standard curve
It weighs about 0.1g of tartaric acid (accurate to 0.001g), dissolved in water and dilute to 100mL, and mix. Imbibe 0 mL, 3.0 mL,
4.0 mL, 5.0 mL, 6.0mL of the solution, were placed in 25mL colorimetric tube, then add water volume to 10mL. To each ratio
Color tube was added 4.0mL freshly prepared solution of sodium metavanadate and 1.0mL of acetic acid. The blank absorbance is set to zero, the above measurement
Tartaric acid solution absorbance at a wavelength of 520nm (Note. In the determination of these solutions within 10min after color development).
Data obtained, the absorbance for the vertical axis, corresponding to the quality of tartaric acid (in mg) as abscissa, the standard curve.
A.3.3.2 Preparation of test solution
Weigh approximately 4g sample (accurate to 0.001 g of), was transferred to a 250 mL Erlenmeyer flask was added 80mL concentration of 0.5mol/L
Potassium hydroxide solution and phenolphthalein indicator solution 0.5mL. A length of 65cm or more air-cooled condenser connected to the Erlenmeyer flask, and then
The mixture was placed on a hot plate heated for about 2.5h. Hot phosphoric acid solution was added until Congo red was significantly acidic. reconnect
Air-cooled condenser and heated to liquefy the fatty acid and becomes clear. After the mixture was cooled, a small amount of added water and chloroform, the mixture was transferred
To a 250mL separating funnel -1, free fatty acids extracted with chloroform, each with 25mL, 3 times in a row. The extract was set out
At another -2 separating funnel, washed with water separating funnel - 2 of the liquid extracts, each with 25mL, 3 times in a row, and the washings
Into the aqueous phase containing layer separating funnel -1. Transfer separating funnel -1 all aqueous layer into a 250mL beaker, steam bath groove
On heating to remove traces of chloroform, and then by a pickled precision filter paper into a 500mL flask, diluted with water and set
To volume (this is the solution 1). Imbibe 25mL solution 1, placed in a 100mL volumetric flask, diluted with water and set the volume to
Scale (this is the solution 2). Leave the remaining solution 1, used to determine the total glycerol content.
A.3.3.3 Determination
Imbibe 10mL solution prepared in A.3.3.2 analysis step 2, placed in a 25mL than the color tube, and then follow
A.3.3.1 "standard curve" analysis steps, from "to each colorimetric tube was added 4.0mL" continue the procedure to give
The absorbance of the sample solution. Tartaric acid solution obtained quality 2 according to the standard curve.
A.3.4 Calculation Results
Total tartaric acid content X1 according to formula (A.1) Calculated.
1 ×× = m
mX% (A.1)
Where.
Total tartaric acid content X1──,%;
m── standard curve and the absorbance of the sample solution, and seek a solution of tartaric acid 2 mass, in milligrams (mg);
20── dilution;
M1── quality of the sample, in milligrams (mg).
The results parallel arithmetic mean of the measurement results shall prevail. Twice in repeatability conditions independent determination of no difference in the results
Greater than 1%.
A.4 Determination of total glycerol
A.4.1 Reagents and materials
a) glacial acetic acid.
b) periodic acid solution. 2.7g of periodic acid (H5IO6) was dissolved in 50mL of water, 950mL of glacial acetic acid was added, mixed well, and this solution to avoid the need
Light save.
c) potassium iodide solution. 150g/L.
d) sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1 mol/L.
e) Starch indicator solution. 10g/L.
A.4.2 Analysis step
Imbibe analysis step 5mL total solution A.3.3.2 Determination of tartaric acid prepared in Example 1, this is a 5mL sample solution
Solution, the sample was transferred into a 250mL glass-stoppered Erlenmeyer flask or iodine bottle. 15mL of glacial acetic acid was added to the flask and 25mL periodate
Was added and the mixture was shaken for 1min ~ 2min, standing 15min, then a solution of potassium iodide was added 15mL and 15mL water, shake well and quiet
Set 1min, titration with sodium thiosulfate standard titration of free iodine, using starch indicator solution as an indicator. Instead of the sample liquid into the water
Line blank titration. Blank corrected by volume is 5mL titration solution 1 sample contained tartaric acid and glycerin consumption required thiosulfate
Milliliters of sodium sulfate standard titration solution (V0-V2). Tartaric acid based on the total content of the test (A.3) determined tartaric acid content
The number of milliliters of the sample solution titration of sodium thiosulfate standard titration consumption required tartrate solution (V1).
After the blank with the calculated volume of the sample solution in tartaric acid consumption required corrected sodium thiosulfate standard titration solution milliliters of
Number of milliliters of difference, that is, the sample solution required glycerin consumption of sodium thiosulfate standard titration solution. Glycerin quality will be divided by the sample solution
The quality of the sample corresponds, total glycerol content can be obtained.
A.4.3 Calculation Results
The total glycerol content X2 according to formula (A.2) Calculated.
10003.23) (
2 ××× - = m
cVVVX% (A.2)
Where.
X2── total glycerol content,%;
Volume V0── blank titration consumption of sodium thiosulfate standard titration solution, in milliliters (mL);
V2── sample droplet volume consumption of sodium thiosulfate standard titration solution, in milliliters (mL);
Volume of the sample was calculated in V1── sodium thiosulfate standard titration solution of tartaric acid consumption required, in milliliters
(ML of);
C2── actual concentration of sodium thiosulfate standard titration solution, expressed in moles per liter (mol/L);
23.03── consumption 1mL 1.0 mol/L sodium thiosulfate standard titration solution is equivalent to 23.03mg glycerol;
m2── sample solution (5mL solution 1) corresponding to the mass of the sample, in milligrams (mg).
The results parallel arithmetic mean of the measurement results shall prevail. Twice in repeatability conditions independent determination of no difference in the results
Greater than 1%.
A.5 Determination of total acid
A.5.1 Reagents and materials
a) perchloric acid solution. about 4mol/L.
b) phenolphthalein indicator solution. 10g/L.
c) sodium hydroxide standard solution. c (NaOH) = 0.5mol/L.
A.5.2 Instruments and Equipment
As shown in Figure A.1 assembled a modified Hortvet-Sellier distillation equipment, the use of a sufficiently large (approximately 38 mm × 203mm)
Sellier within the tube and large distillation trap.
Figure A.1 improved Hortvet-Sellier distillation apparatus
A.5.3 Analysis step
Weigh about 4g sample (accurate to 0.001g), was transferred to a distillation apparatus of the inner tube, and the inner tube is inserted into an outer bottle, bottle outside
In just about 300mL heated to boiling hot water. The sample was added to a concentration of about 10mL 4mol/perchloric acid L solution. The inner tube
Well connected by distillation to a water-cooled condenser, distillation by heating the outer bottle, 100mL distillate collected in 20min ~ 25min.
Several 100mL distillate collected, adding phenolphthalein indicator solution in each test solution (100mL distillate) with sodium hydroxide standard solution
Titration. Distillation continued until 100mL distillate collected just less than 0.5mL standard solution of sodium hydroxide to neutralize up.
(Note. Do not evaporated.)
A.5.4 Results Settlement
Total acetic acid content X3 according to formula (A.3) Calculated.
10006.60
3 ××× = m
cVX% (A.3)
Where.
X3── total acetic acid content,%;
V3── continuous consumption of the total volume of sodium hydroxide titration standard solution, in milliliters (mL);
The actual concentration c3── standard solution of sodium hydroxide, in units of moles per liter (mol/L);
60.06── consumption 1mL 1.0 mol/L sodium hydroxide standard solution is equivalent to 60.06mg acetic acid;
M3── quality of the sample, in milligrams (mg).
The results parallel arithmetic mean of the measurement results shall prevail. Twice in repeatability conditions independent determination of no difference in the results
Greater than 2%.
A.6 Determination of free glycerol
A.6.1 Reagents and materials
a) glacial acetic acid.
b) trichloromethane (chloroform).
c) periodic acid solution. dissolve 2.7 g of periodic acid in a mixture of 50 mL of water and 950 mL of acetic acid, stored in the dark in a clean glass with stopper
Glass bottle.
d) potassium iodide solution. 150g/L.
e) sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1 mol/L.
f) Starch indicator solution. 10 g/L.
A.6.2 Analysis step
A.6.2.1 sample pretreatment
First sample melted (its melting temperature does not exceed 10 ℃) and mixed thoroughly. Weigh 0.2 g ~ 1.0g sample (accurate to 0.000
1 g), into a 100 mL beaker, add chloroform to dissolve 25 mL. The solution was transferred to a separatory funnel, and the other with 25 mL of chloroform shower
Wash the beaker and then with 25 mL water wash, wash all were transferred to a separatory funnel. Gasser closed strongly shaken 30 s ~ 60 s, then
After allowing to stand stratification of chloroform and the aqueous phase (such as the formation of milky, it can ice breaking acetate 1mL ~ 2 mL). The aqueous layer was transferred to 500 mL
Iodine bottle, and then were extracted with 25 mL aqueous solution of chloroform twice. The aqueous solution was extracted after concentrated into the same bottle for the determination of iodine
Content of free glycerol.
A.6.2.2 Determination
After sample preparation, 500 mL of water containing iodine bottle after extraction phase, add 20.0 mL periodic acid solution, and with 75 mL of water
Instead of the sample do two blank test, allowed to stand 30 min ~ 90 min. In each of the iodine bottle each added 15 mL potassium iodide solution, then place
1 min ~ 5 min, add 100 mL of water, sodium thiosulfate standard titration solution was titrated with a magnetic stirrer to titration
Maintaining the solution mixed thoroughly, then to fade iodine brown, add 2 mL of starch indicator solution and continue to drop until the blue fade.
A.6.3 Calculation Results
Free glycerol content X4 according to formula (A.4) Calculated.
30.2) (
cVVX ×× - = (A.4)
Where.
X4── free glycerol content,%;
Volume V0── blank titration consumption of sodium thiosulfate standard titration solution, in milliliters (mL);
Volume V4── sample titration consumption of sodium thiosulfate standard titration solution, in milliliters (mL);
C4── actual concentration of sodium thiosulfate standard titration solution, expressed in moles per liter (mol/L);
2.30── conversion factor, glycerin molecular weight divided by 40;
m4── sample mass, in grams (g).
The results parallel arithmetic mean of the measurement results shall prevail. Twice in repeatability conditions independent determination of no difference in the results
Greater than 0.2%.
A.7 Determination of acid value
A.7.1 Reagents and materials
a) 95% ethanol.
b) potassium hydroxide - ethanol standard titration solution. c (KOH) = 0.1 mol/L.
c) phenolphthalein indicator solution. 10g/L.
A.7.2 Analysis step
Weigh about 0.6 g sample (accurate to 0.001 g), placed in a conical flask, 50 mL neutral ethanol, heated to dissolve the sample,
After cooling, add 2 to 3 drops of phenolphthalein indicator solution with 0.1 mol/L potassium hydroxide - ethanol standard titration solution titration to reddish, and dimension
30s who do not fade as the end point.
A.7.3 Calculation Results
X5 acid value according to equation (A.5) Calculated.
1.56
cVX ×× = (A.5)
Where.
X5── acid value in units of milligrams per gram (mg/g) (in dollars KOH);
Potassium hydroxide V5── titration consumption - ethanol standard titration solution volume in milliliters (mL);
c5── potassium hydroxide - ethanol concentration standard titration solution, expressed in moles per liter (mol/L);
56.1── numerical molar mass of potassium hydroxide in grams per mole (g/mol);
m5── sample mass, in grams (g).
The results parallel arithmetic mean of the measurement results shall prevail (to one decimal place). Two independently under the same condition
The difference between the measurement result is not greater than 2 mg/g.
A.8 Determination of saponification value
A.8.1 Reagents and materials
a) 95% ethanol.
b) potassium hydroxide - ethanol standard titration solution. c (KOH) = 0.5 mol/L.
c) hydrochloric acid standard titration solution. c (HCl) = 0.5 mol/L.
d) phenolphthalein indicator solution. 10g/L.
A.8.2 Analysis step
Weigh about 0.7 g sample (accurate to 0.001 g), placed in 250mL grinding mouth Erlenmeyer flask, add 25 mL of potassium hydroxide - ethanol standard
Quasi-titration solution, connected to a condenser, at (85 ± 2) ℃ water bath was heated to reflux for 1h. Coolish rinsed with 5mL ethanol condenser.
Remove the conical flask, add 3 drops of phenolphthalein indicator solution with 0.5 mol/L hydrochloric acid standard titrant titration until the solution is red just disappeared
end. At the same time make a blank test.
A.8.3 Calculation Results
Saponification value X6 according to formula (A.6) Calculated.
1.56) (
cVVX ×× - = (A.6)
Where.
X6── saponification value, in milligrams per gram (mg/g) (in dollars KOH);
Hydrochloric acid standard titration solution volume consumed V0── blank, in milliliters (mL);
Hydrochloric acid standard titration solution volume V6── sample consumed in milliliters (mL);
C6── actual concentration of hydrochloric acid standard titration solution, expressed in moles per liter (mol/L);
56.1── numerical molar mass of potassium hydroxide in grams per mole (g/mol);
m6── sample mass, in grams (g).
The results parallel arithmetic mean of the measurement results shall prevail (to one decimal place). Twice under repeated condition alone
Li measurement result is not greater than the difference between the 1 mg/g.
   
   
  
  
    
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