GB 1886.64-2015 English PDF

Delivery: 2 working-hours manually (Sales@ChineseStandard.net)
Need delivered in 3-second? USA-Site: GB 1886.64-2015
Get Quotation: Click GB 1886.64-2015 (Self-service in 1-minute)
Historical versions (Master-website): GB 1886.64-2015
Preview True-PDF (Reload/Scroll-down if blank)

GB 1886.64-2015: National Food Safety Standard -- Food Additives -- Caramel color
GB 1886.64-2015
GB
NATIONAL STANDARD OF THE
PEOPLE?€?S REPUBLIC OF CHINA
National food safety standard ?€? Food additives ?€? Caramel
color
ISSUED ON: NOVEMBER 13, 2015
IMPLEMENTED ON: MAY 13, 2016
Issued by: National Health and Family Planning Commission of the People?€?s
Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Terms and definitions ... 4
3 Technical requirements ... 4
Appendix A Test methods ... 6
National food safety standard ?€? Food additives ?€? Caramel
color
1 Scope
This Standard applies to the food additive caramel color made from sucrose, starch
syrup, xylose mother liquor, etc. using plain caramel, caustic sulfite caramel, ammonia
caramel or sulfite ammonia caramel.
2 Terms and definitions
2.1 plain caramel color
It is made using carbohydrates as the main raw material, with or without the addition
of acid (base), and without the use of ammonia compounds and sulfites.
2.2 caustic sulfite caramel color
It is made using carbohydrates as the main raw material, in the presence of sulfite, with
or without the addition of acid (base), and without the use of ammonia compounds.
2.3 ammonia caramel color
It is made using carbohydrates as the main raw material, in the presence of ammonia
compounds, with or without the addition of acid (base), and without the use of sulfites.
2.4 sulfite ammonia caramel color
It is made using carbohydrates as the main raw material, in the presence of ammonia
compounds and sulfites, with or without the addition of acid (base).
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall be in accordance with Table 1.
Appendix A
Test methods
A.1 General
Unless otherwise specified in this Standard, the purity of the reagents used shall be
analytically pure. The standard titration solutions, standard solutions for impurity
determination, preparations and products used shall be prepared in accordance with the
provisions of GB/T 601, GB/T 602 and GB/T 603. The test water shall comply with the
provisions of Grade 3 water in GB/T 6682. The solutions used in the test shall refer to
aqueous solutions unless the solvent used is specified.
A.2 Determination of absorbance E0.1% 1 cm (610 nm)
A.2.1 Instruments and apparatuses
Spectrophotometer.
A.2.2 Analysis steps
Weigh about 0.5 g of the sample, accurate to 0.002 g; dissolve it in water; transfer it to
a 500 mL volumetric flask; add water to dilute it to the mark; shake it well. If the
solution is turbid, centrifuge it to obtain the sample solution. Place this sample solution
in a 1 cm colorimetric dish; use water as a blank control; use a spectrophotometer to
measure its absorbance at 610 nm (it is recommended to control the absorbance at 0.2
~ 0.8, otherwise, adjust the sample solution concentration and measure the absorbance
again).
A.2.3 Result calculation
Calculate the absorbance E0.1% 1 cm (610 nm) according to Formula (A.1):
Where:
A ?€? absorbance of the sample being measured;
c ?€? concentration of the sample solution being measured, in grams per milliliter (g/mL);
1 000 ?€? concentration conversion coefficient.
The test result is based on the arithmetic mean of the parallel determination results. The
ratio of the absolute difference between two independent determination results obtained
under repeatability conditions and the arithmetic mean shall not exceed 5%.
A ?€? built-in adapter;
B ?€? separating funnel;
C ?€? round bottom flask;
D ?€? gas internal pipe;
E ?€? condenser;
F ?€? connecting ball (see Figure A.2 for the structure of component F);
G ?€? receiver.
Figure A.1 ?€? Diagram of sulfur dioxide determination device
The device in Figure A.1 is used to selectively transfer sulfur dioxide from the sample
to the 3% hydrogen peroxide solution in a boiling hydrochloric acid aqueous solution.
This device is easier to connect than a conventional device. Since the height of the 3%
hydrogen peroxide solution is above the ball tip, the back pressure in the device is
difficult to avoid, and component F can reduce the back pressure to the lowest possible
level, thereby reducing the possibility of sulfur dioxide loss due to leakage.
Component D in Figure A.1 needs to be equipped with a hose connection. If
polyethylene and quartz tubes are used, they shall be pre-boiled before use in this
procedure.
Connect the entire device according to the requirements of Figure A.1. Except for the
connection between the separating funnel and the flask, the sealing surfaces of all other
connectors shall be coated with a thin layer of piston lubricant. All connectors shall be
clamped tightly to ensure sealing during analysis. The volume of the separating funnel
B shall be greater than or equal to 100 mL. It must be equipped with a built-in adapter
A with a hose connector to ensure that a certain pressure is maintained above the internal
solution. (It is not recommended to use a constant pressure titration funnel because the
condensed water may contain sulfur dioxide and adhere to the inner wall of the funnel
or the wall of the tube). The round bottom flask C, with a volume of 1 000 mL, is
provided with 3 24/40 mm conical interfaces. The gas internal pipe D shall be of
sufficient length to ensure that the introduced nitrogen can reach 2.5 cm from the bottom
of the flask. The jacket length of the condenser E shall be 300 mm. The connecting ball
F is a custom-made glass part according to the requirements of Figure A.2, with the
same size as the 50 mL measuring barrel. The 3% hydrogen peroxide solution is placed
in a receiver G, which has an inner diameter of 2.5 cm and a length of 18 cm.
connection is completed, the nitrogen flow through the 3% hydrogen peroxide solution
shall be restored immediately, and the connection shall be checked to ensure it is sealed.
The rubber ball above the separating funnel is equipped with a valve to ensure that there
is sufficient pressure above the hydrochloric acid solution. Open the separating funnel
valve to allow the hydrochloric acid solution to flow into the flask. Continue to ensure
that there is sufficient pressure above the solution. If necessary, the valve can be
temporarily closed to replenish the pressure. To prevent sulfur dioxide from escaping
into the separating funnel, the valve shall be closed before the last few milliliters flow
out of the separating funnel.
Connect the power supply for heating, and control the heating rate so that the reflux
liquid is 80 ~ 90 drops per minute. After distillation for 105 minutes, cool the contents
in the 1 000 mL flask at the above reflux rate. Transfer the contents in receiver G.
A.4.4.4 Titration
Add 3 drops of methyl red indicator solution and use standard titration solution to titrate
the above solution to the yellow end point; ensure that it does not fade within 20 seconds.
A.4.5 Result calculation
Calculate the mass fraction w2 of sulfur dioxide (as SO2) according to Formula (A.3):
Where:
M ?€? molar mass of sulfur dioxide, in grams per mole (g/mol), [M (SO2) = 64.06];
V ?€? volume of the sodium hydroxide standard titration solution consumed in the
titration, in milliliters (mL);
c ?€? concentration of the sodium hydroxide standard titration solution, in moles per liter
(mol/L);
0.1 ?€? conversion coefficient;
2 ?€? conversion coefficient;
m ?€? mass of the sample added to the 1 000 mL flask, in grams (g);
1 000 ?€? conversion coefficient;
A610 ?€? absorbance of the sample at 610 nm.
A.5.5.1 Preparation of 4-methylimidazole standard stock solution
Accurately weigh 50 mg of 4-methylimidazole standard; place it in a 50 mL volumetric
flask; use acetone to dilute to the mark; mix well; refrigerate for later use.
A.5.5.2 Preparation of 4-methylimidazole standard solution
Take 1.0 mL, 1.5 mL, 2.0 mL, 2.5 mL, 3.0 mL, 3.5 mL, 4.0 mL and 5.0 mL of 4-
methylimidazole standard stock solution; respectively place them in 10 mL volumetric
flasks; use acetone to dilute to the mark; mix well; prepare 4-methylimidazole standard
solutions with concentrations of 100 ??g/mL, 150 ??g/mL, 200 ??g/mL, 250 ??g/mL, 300
??g/mL, 350 ??g/mL, 400 ??g/mL and 500 ??g/mL, respectively. Keep refrigerated and use
within 1 month.
A.5.5.3 Preparation of sample solution
Weigh 10.0 g of the sample; place it in a 250 mL beaker; add 5 mL of sodium hydroxide
solution; shake well. Add 20.0 g of diatomaceous earth to the beaker; use a stainless-
steel spatula to stir thoroughly until a semi-dry, uniform mixture is formed.
Insert fine glass wool at the bottom of a 300 mm ?? 22 mm (inner diameter)
chromatographic column with a polytetrafluoroethylene stopper; transfer the mixture
quantitatively to the chromatographic column. The column layer is about 150 mm high.
Place a little glass wool on the top of the column. Use dichloromethane to wash the
sample beaker; open the stopper; pour the washing solution into the column. When
dichloromethane flows through the chromatographic column to the stopper, close the
stopper and let dichloromethane stay in the column layer for 5 minutes. Open the
stopper again and let dichloromethane pass through the column at a flow rate of 5
mL/min. Collect 200 mL of eluent in a 300 mL round-bottom flask; place it on a rotary
evaporator; maintain the water bath temperature at 35 ??? and the pressure at 350 mm ~
390 mm Hg to evaporate most of the solvent in the eluent and concentrate it to about 1
mL. During the concentration process, pay attention to the flask to prevent boiling. Use
a pipette to quantitatively transfer the concentrate to a 5 mL volumetric flask; use
acetone to wash the flask several times (about 0.7 mL each time); transfer all the
washings to a 5 mL volumetric flask; use acetone to dilute to the mark; mix well; set
aside.
A.5.5.4 Determination
Adjust the gas chromatograph to the operating conditions shown in Table A.1. After the
instrument is stable, perform chromatographic analysis on the 4-methylimidazole
standard solution and sample solution of different concentrations; quantify by the
external standard method.
A.6 Determination of total sulfur (as S)
A.6.1 Reagents and materials
A.6.1.1 Magnesium oxide.
A.6.1.2 Magnesium nitrate [Mg(NO3)2??6H2O].
A.6.1.3 Sucrose.
A.6.1.4 Nitric acid.
A.6.1.5 Hydrochloric acid solution: 1+1.
A.6.1.6 Barium chloride solution: mass fraction 10%.
A.6.2 Analysis steps
Select the largest porcelain crucible that matches the high-temperature furnace (to
prevent splashing of the reaction); add 1 g ~ 3 g of magnesium oxide or an equivalent
amount of magnesium nitrate [Mg(NO3)2??6H2O] (6.4 g ~ 19.2 g), 1 g of sucrose, and
50 mL of nitric acid. Weigh an appropriate amount of sample (5 g, if total sulfur content
??? 2.5%; 1 g, if total sulfur content > 2.5%), accurate to 0.01 g; add it to the porcelain
crucible. Evaporate in a steam bath to a paste; then, carbonize on an electric furnace
until smokeless; then, put it in a high-temperature furnace; heat to 525 ???; maintain the
temperature for 4 h ~ 5 h; cool. Dissolve the sample in 100 mL of water; use
hydrochloric acid solution to neutralize it to pH7; add 2 mL of hydrochloric acid
solution; filter the solution into a beaker; heat to boiling; slowly add 20 mL of barium
chloride solution to the hot solution while stirring; boil for 5 min; leave it overnight.
Filter it through the ash-free filter paper; transfer all the precipitate to the filter paper;
use hot water to thoroughly wash the filter paper and precipitate. Then, put the filter
paper and precipitate into a tongs pan that has been weighed in a high-temperature
furnace at 800 ??? in advance; keep it in an oven at 105 ??? for 1 hour; take it out. Use
an electric furnace to heat slowly until it is carbonized. Then, ash it in a high-
temperature furnace at 800 ??? for 1 hour; cool it; and weigh it. Perform a blank test in
the same way.
A.6.3 Result calculation
Calculate the mass fraction w3 of total sulfur (as S) according to Formula (A.4):
Where:
mS ?€? residual mass of barium sulfate after burning, in grams (g);
mB ?€? residual mass obtained from the blank test after burning, in grams (g);
0.137 ?€? coefficient for converting barium sulfate to sulfur;