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GB 29220-2012: National food safety standards -- Food additives -- Sorbitan monostearate (Span 65)
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National food safety standards -- Food additives -- Sorbitan monostearate (Span 65)
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Basic data
Standard ID: GB 29220-2012 (GB29220-2012)
Description (Translated English): National food safety standards -- Food additives -- Sorbitan monostearate (Span 65)
Sector / Industry: National Standard
Classification of Chinese Standard: X40
Classification of International Standard: 67.220.20
Word Count Estimation: 9,991
Regulation (derived from): Ministry of Health Bulletin 2012 No. 23
Issuing agency(ies): Ministry of Health of the People's Republic of China
Summary: This Chinese standard applies to sorbitan stearic acid as raw materials, by esterification reaction of a food additive sorbitan monostearate (Span 65).
GB 29220-2012: National food safety standards -- Food additives -- Sorbitan monostearate (Span 65)
---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 .Food points.Sorbitan monostearate (Span 65)
National Standards of People's Republic of China
National standards for food safety
Food additives sorbitan tristearate
(Span 65)
2012-12-25 release
2013-01-25 Implementation
Issued by the Ministry of Health of the People's Republic of China
National standards for food safety
Food additives sorbitan tristearate
(Span 65)
1 Scope
This standard applies to stearic acid and sorbitan as raw materials, the esterification reaction of the food additive sorbitan tristearate
(Span 65).
2 Chemical name
Sorbitan tristearate
3 technical requirements
3.1 sensory requirements
Shall comply with the provisions of Table 1.
Table 1 sensory requirements
The project requires a test method
Color is yellow to white at room temperature
State at room temperature for the waxy solid
Take the appropriate amount of sample, placed in a clean, dry white porcelain dish, in the self
Under the light visual observation of color and state
3.2 Physical and chemical indicators
Shall comply with the provisions of Table 2.
Table 2 Physical and chemical indicators
Item Index Test Method
Fatty acids, w /% 85 ~ 92 Appendix A, A.4
Polyols, w /% 14 ~ 21 Appendix A, A.5
Acid value (in KOH)/(mg/g) ≤ 15 Appendix A A.6
Saponification value (in KOH)/(mg/g) 176 to 188 Appendix A A.7
Hydroxyl value (in KOH)/(mg/g) 66 to 80 Appendix A A.8
Moisture, w /% ≤ 1.5 Appendix A, A.9
Burning residue, w /% ≤ 0.50 GB/T 7531a
Table 2 (continued)
Item Index Test Method
Lead (Pb)/(mg/kg) ≤ 2 GB 5009.12
Freezing point/℃ 47 ~ 50 Appendix A. A.10
a The burning temperature is 850 ℃ ± 25 ℃.
Appendix A
Testing method
A.1 Warning
The test procedure specifies that some of the test procedures may lead to dangerous conditions and that the operator 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. The solution used in the test method refers to the aqueous solution when the solvent is not specified.
A.3 Identification test
A.3.1 Determination of fatty acid value
A.3.1.1 Reagents and materials
A.3.1.1.1 anhydrous ethanol.
A.3.1.1.2 sodium hydroxide standard titration solution. c (NaOH) = 0.5mol/L.
A.3.1.1.3 phenolphthalein indicator solution. 10g/L.
A.3.1.2 Analysis steps
Weigh about 3gA.4.3.2 in the coagulation D, accurate to 0.001g, placed in a conical flask, add 50mL of anhydrous ethanol dissolved, must
To be heated. Add 5 drops of phenolphthalein indicator solution, titration with sodium hydroxide titration solution to the solution was pink, keep 30s does not fade for
end.
A.3.1.3 Calculation of results
The fatty acid value w1 is expressed in milligrams per gram (mg/g) in terms of potassium hydroxide (KOH) and is calculated according to formula (A.1)
w1 =
V1 × c × M
(A.1)
Where.
V1 --- sodium hydroxide standard titration solution volume of the value in milliliters (mL);
c - the exact value of sodium hydroxide standard titration solution concentration in moles per liter (mol/L);
m - the mass of the sample, in grams (g);
M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109].
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 greater than 0.5 (mg/g).
A.3.1.4 Judgment of results
The recovered fatty acid value should be 190mg/g ~ 220mg/g.
A.3.2 Polyol color test
A.3.2.1 Reagents and materials
A.3.2.1.1 Sulfuric acid.
A.3.2.1.2 Catechol solution. 100g/L, is now available.
A.3.2.2 Analysis steps
Take A.5.2 in the viscous material E about 2g, add 2mL catechol solution, mix; add 5mL sulfuric acid mix, should be red or red
brown.
A.4 Determination of Fatty Acids
A.4.1 Methodological Summary
The samples were hydrolyzed by saponification, and the fatty acids and polyols formed after acidification were separated by repeated extraction and concentrated to obtain a recovered fat
The quality of the acid is calculated and the mass fraction of the fatty acids is calculated.
A.4.2 Reagents and materials
A.4.2.1 Potassium hydroxide.
A.4.2.2 Ethanol (95%).
A.4.2.3 petroleum ether.
A.4.2.4 Sulfuric acid solution. 1 2.
A.4.3 Analysis steps
A.4.3.1 Saponification. Weigh about 25g of sample, accurate to 0.01g. Placed in a 500 mL flask, 250 mL of ethanol (95%) and
7.5g potassium hydroxide. Connect the condenser and place it in a water bath for 2h. The saponified product was transferred to a 800 mL beaker, ca.
The flask was washed with water and transferred to the beaker. Place the beaker on the water bath and evaporate until the alcohol evaporates. The volume of the solution is adjusted with hot water
To about 250 mL, as solution A.
A.4.3.2 Acidification, Extraction Separation. Add sulfuric acid solution to Solution A with heating and stirring to precipitate the coagulum and add an excess of about 10%
The sulfuric acid solution is cooled and layered. The supernatant was transferred to a 250 mL beaker which had a constant mass at 80 ° C and three times with 20 mL
Hot water washing, cooling the lotion and the lower solution after the merger in a 500mL separatory funnel, 3 times with 100mL petroleum ether extraction,
Floor. The lower layer B solution was transferred to a 800 mL beaker; the combined petroleum ether extract was added to a second 500 mL separatory funnel,
Water washing. The lower layer of water solution and solution B into solution C, retained for the determination of polyol content; transfer of the upper layer of petroleum ether extract in the Sheng solidification
In a beaker, concentrated on a water bath to 100 mL, dried at 80 ° C until the mass was constant, and the recovered coagulum D was obtained as the quality of the fatty acid
the amount. The coagulated substance D after weighing was used for the determination of the fatty acid value.
A.4.4 Calculation of results
The mass fraction of fatty acids w2 is calculated according to formula (A.2)
w2 =
m2-m1
m x 100%
(A.2)
Where.
m1 --- 250mL beaker mass value in grams (g);
m2 --- 250mL beaker plus the value of the quality of coagulation D, in grams (g);
m - 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 should not exceed 1%.
A.5 Determination of polyol
A.5.1 Reagents and materials
A.5.1.1 anhydrous ethanol.
A.5.1.2 Potassium hydroxide solution. 100 g/L.
A.5.2 Analysis steps
The solution C to pH 7 obtained in A.4.3.2 was neutralized with potassium hydroxide solution (tested with pH paper). Place the solution in a water bath
Evaporated to white crystals. The polyol in the residue was then extracted twice with 150 mL of hot ethanol and the combined extracts were washed with G4
Glass funnel (filter plate pore size 5μm ~ 15μm) filter, anhydrous ethanol washing. The filtrate was transferred to another 800 mL beaker and placed on a water bath
Concentrated to about 100 mL. And transferred to a pre-dried at 80 ° C to a constant volume of 250 mL beaker and continue to evaporate to a viscous shape. in
Dried at 80 ° C until the mass was constant, and the mass of the viscous material E was recovered as the polyol. After weighing the viscous material E is used as a polyol color
test.
A.5.3 Calculation of results
The mass fraction w3 of the polyol is calculated according to formula (A.3)
w3 =
m4-m3
m x 100%
(A.3)
Where.
m3 --- 250mL beaker quality, in grams (g);
m4 --- 250mL beaker plus viscous material E in grams (g);
m --- A.4.4 The mass of the sample in grams, 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 should not exceed 1%.
A.6 Determination of acid value (in KOH)
A.6.1 Reagents and materials
A.6.1.1 isopropanol.
A.6.1.2 Toluene.
A.6.1.3 sodium hydroxide standard titration solution. c (NaOH) = 0.1mol/L.
A.6.1.4 phenolphthalein indicator solution. 10g/L.
A.6.2 Analysis steps
Weigh about 2.5g sample, accurate to 0.0002g, placed in a conical flask, add isopropyl alcohol and toluene 40mL, heated to dissolve.
Add 5 drops of phenolphthalein indicator solution, titration with sodium hydroxide titration solution to the solution was pink, keep 30s does not fade for the end.
A.6.3 Calculation of results
The acid value w4, expressed in potassium hydroxide (KOH), is expressed in milligrams per gram (mg/g) and calculated as in formula (A.4)
w4 =
V2 × c × M
(A.4)
Where.
V2 --- sodium hydroxide standard titration solution volume of the value in milliliters (mL);
c - the exact value of sodium hydroxide standard titration solution concentration in moles per liter (mol/L);
m - the mass of the sample, in grams (g);
M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109].
The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations should not be greater than 0.2 mg/g.
A.7 Determination of saponification value (in KOH)
A.7.1 Reagents and materials
A.7.1.1 anhydrous ethanol.
A.7.1.2 Potassium hydroxide ethanol solution. 40 g/L.
A.7.1.3 hydrochloric acid standard titration solution. c (HCl) = 0.5mol/L.
A.7.1.4 phenolphthalein indicator solution. 10g/L.
A.7.2 Analysis steps
Weigh about 2g sample, accurate to 0.0002g, placed in 250mL mill vial flask, add 25mL ± 0.02mL potassium hydroxide
Ethanol solution, connected to the condenser tube, refluxed in a boiling water bath for 1h, slightly cold with 10mL anhydrous ethanol leaching condensate tube, remove the conical flask, add
5 drops of phenolphthalein indicator solution, titrated with hydrochloric acid standard titration solution to the red just disappeared, heating the test solution to boiling. If there is pink, then
Continued titration to red disappears is the end point.
At the same time as the measurement, the same amount of reagent solution was used as a blank test in the same procedure as in the measurement.
A.7.3 Calculation of results
The saponification value w5, expressed in potassium hydroxide (KOH), is expressed in milligrams per gram (mg/g), calculated as in formula (A.5)
w5 =
(V0 - V3) × c × M
(A.5)
Where.
V0 --- sample consumption of hydrochloric acid standard titration solution volume value in milliliters (mL);
V3 --- blank test consumption of hydrochloric acid standard titration solution volume value, the unit is ml (mL);
c - the exact value of the standard titration solution for hydrochloric acid, in moles per liter (mol/L);
m - the mass of the sample, in grams (g);
M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109].
The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations should not be greater than 1 mg/g.
A.8 Determination of hydroxyl value (in KOH)
A.8.1 Reagents and materials
A.8.1.1 Pyridine. neutralized with hydrochloric acid solution (1 110) using phenolphthalein as an indicator.
A.8.1.2 n-butanol. phenol phenol as the indicator, with potassium hydroxide ethanol standard titration solution and.
A.8.1.3 Acetylating agent. Acetic anhydride and pyridine were mixed in 1 3 and stored in a brown bottle.
A.8.1.4 Potassium hydroxide ethanol standard titration solution. c (KOH) = 0.5mol/L.
A.8.1.5 phenolphthalein indicator solution. 10g/L.
A.8.2 Analysis steps
Approximately 1.2 g of the sample was weighed to 0.0002 g, placed in a 250 mL Erlenmeyer flask, and 5 mL of 0.02 mL of acetylation
Agent, connected to the condenser, heated in the water bath reflux 1h. Add 10 mL of water from the top of the condenser to the conical flask and continue heating for 10 min
After cooling to room temperature. Rinse the condenser with 15 mL of n-butanol, remove the condenser, and rinse the wall with 10 mL of n-butanol. Add 8 drops of phenol
Phthalate indicator solution, titration with potassium hydroxide ethanol titration solution to the solution was pink is the end point.
At the same time as the measurement, the same amount of reagent solution was used as a blank test in the same procedure as in the measurement.
To correct the free acid, weigh about 10g of the sample, accurate to 0.01g. Placed in a conical flask, add 30mL of pyridine, add 5 drops of phenolphthalein
Indicator solution, titrated with potassium hydroxide ethanol titration solution to the solution was pink.
A.8.3 Result calculation
The hydroxyl value w6, expressed in potassium hydroxide (KOH), is expressed in milligrams per gram (mg/g) and is calculated as in formula (A.6)
w6 =
(V0 - V4) × c × M
V5 × c × M
m5
(A.6)
Where.
V4 --- sample consumption of potassium hydroxide ethanol standard titration solution volume value in milliliters (mL);
V0 --- blank test consumption of potassium hydroxide ethanol standard titration solution volume value, the unit is ml (mL);
V5 --- corrected free acid consumption of potassium hydroxide ethanol standard titration solution volume value in milliliters (mL);
c - potassium hydroxide ethanol standard titration solution concentration of the exact value in moles per liter (mol/L);
m - value of the mass of the sample when measured by the hydroxyl value, in grams (g);
m5 --- corrected free acid determination of the sample quality of the value of the unit in grams (g);
M - the molar mass of potassium hydroxide in grams per mole (g/mol) [M = 56.109].
The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations should not be greater than 4 mg/g.
A.9 Determination of moisture
Weigh about 0.6g of sample, accurate to 0.0002g. Placed in a 25mL beaker, add a small amount of trichloromethane heated and dissolved and transferred to
25mL volumetric flask, rinse the beaker several times with chloroform, into the volumetric flask, diluted to the scale. Measure 5 mL ± 0.02 mL
Sample solution, according to GB/T 6283 in the direct electricity method.
The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations should not be greater than 0.05%.
A.10 Determination of freezing point
A.10.1 Instruments and equipment
Glass tube. length 100mm, diameter 25mm, wall thickness 1mm.
A.10.2 Analysis steps
Add about 5g of sample to the glass tube, slowly heat the sample to dissolve, and make the temperature slightly higher than the freezing point of 15 ℃ ~ 20 ℃, the glass tube
Placed in a transparent glass bottle (length 150mm, diameter 70mm), with a covered lid to cover the glass bottle, the standard thermometer placed in the melting test
Like, stirring. If you need to cool, slowly stir until the thermometer mercury column rises for 30s the same, stop stirring the thermometer in the sample
, Observe the mercury column to rise, read the maximum temperature of the mercury column to rise for the freezing point.
......
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