GB 1886.235-2016_English: PDF (GB1886.235-2016)
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Food safety national standard -- Food additive -- Citric acid
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GB 1886.235-2016
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Standards related to: GB 1886.235-2016
| Standard ID | GB 1886.235-2016 (GB1886.235-2016) | | Description (Translated English) | Food safety national standard -- Food additive -- Citric acid | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 20,253 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-01-01 | | Older Standard (superseded by this standard) | GB 1987-2007 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 | GB 1886.235-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Food Additives - citric acid
食品添加剂 柠檬酸
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. JANUARY 1, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Molecular formulas, structural formulas, and relative molecular mass ... 4
3 Technical requirements ... 4
Appendix A Inspection methods ... 6
National Food Safety Standard -
Food Additives - citric acid
1 Scope
This Standard is applicable to the food additives citric acid prepared by
fermentation of starchy or sugary raw materials.
2 Molecular formulas, structural formulas, and
relative molecular mass
2.1 Molecular formulas
Citric acid anhydrous. C6H8O7
Citric acid monohydrate. C6H8O7·H2O
2.2 Structural formulas
Citric acid anhydrous Citric acid monohydrate
2.3 Relative molecular mass
Citric acid anhydrous. 192.13 (according to the 2013 international relative
atomic mass)
Citric acid monohydrate. 210.14 (according to the 2013 international relative
atomic mass)
3 Technical requirements
3.1 Sensory requirements
Appendix A
Inspection methods
A.1 Safety instruction
Some of the reagents used in the inspection methods of this Standard are toxic
or corrosive. During operation, it shall take appropriate safety and protective
measures.
A.2 General provisions
Unless otherwise specified, the purity of the reagents used in this Standard
shall be analytically pure. The standard titration solution, standard solution 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 conform to the provisions of Grade III water in GB/T 6682. The
solution used in the test, when it is not indicated which solvent is used, refers
to aqueous solution.
A.3 Identification test
A.3.1 Reagents and materials
A.3.1.1 Ethyl alcohol.
A.3.1.2 Diethyl ether.
A.3.1.3 Sulfuric acid solution. MEASURE and TAKE 29 mL of sulfuric acid;
slowly INJECT it into approximately 700 mL of water; COOL and DILUTE to
1000 mL.
A.3.1.4 Mercury sulfate solution. WEIGH 5 g of mercury oxide; ADD 40 mL of
water; slowly ADD 20 mL of sulfuric acid; STIR while adding; and ADD 40 mL
of water to dissolve it.
A.3.1.5 Potassium permanganate solution. c(ଵହ KMnO4)=0.1 mol/L.
A.3.1.6 Sodium hydroxide solution. 50 g/L.
A.3.1.7 Pyridine-acetic anhydride solution. MIX pyridine and acetic anhydride
at 3.1 volume ratio.
A.3.2 Analytical procedures
A.3.2.1 The test piece is freely soluble in water, soluble in ethyl alcohol, slightly
soluble in diethyl ether.
A.3.2.2 TAKE an appropriate amount of test piece in 25 mL enamel; IGNITE, it
slowly decomposes; but caramel odor shall not be produced.
A.3.2.3 WEIGH 50 mg of the test piece; after dissolving it in water, DILUTE to
10 mL. PIPETTE 2 mL in 25 mL colorimetric tube; USE sodium hydroxide
solution to adjust to neutral; ADD 1 drop of sulfuric acid solution and HEAT to
boiling; ADD 1 drop of potassium permanganate solution; SHAKE well, purple
fades; and ADD 1 drop of mercury sulfate solution, white precipitate is produced.
A.3.2.4 WEIGH 5 mg of the test piece in 25 mL colorimetric tube; ADD about 5
mL of pyridine-acetic anhydride solution; SHAKE, and a yellow to red or purple
red solution is generated.
A.4 Determination of citric acid content
A.4.1 Method summary
In an aqueous medium, USE phenolphthalein as the indicator solution, and
USE the standard titration solution of sodium hydroxide to titrate citric acid
solution. According to the amount of the standard titration solution of sodium
hydroxide consumed, the content of citric acid is calculated.
A.4.2 Reagents and materials
A.4.2.1 Standard titration solution of sodium hydroxide. c(NaOH)=0.5 mol/L.
A.4.2.2 Phenolphthalein indicator solution. 10 g/L.
A.4.2.3 Carbon dioxide-free water.
A.4.3 Analytical procedures
WEIGH 1 g of the test piece, accurate to 0.0001 g; PLACE it in a 150 mL conical
flask; ADD 50 mL of carbon dioxide-free water to dissolve; ADD 3 drops of
phenolphthalein indicator solution; and USE standard titration solution of
sodium hydroxide to titrate to pink as the end-point. At the same time,
CONDUCT blank test.
A.4.4 Result calculation
The mass fraction w1 of citric acid content (calculated in citric acid anhydrous)
in citric acid monohydrate is calculated according to the equation (A.1). The
mass fraction w2 of citric acid content in citric acid anhydrous is calculated
according to the equation (A.2).
A.8.1 Method summary
Under acidic conditions, the sulfate ion in citric acid solution and barium chloride
solution generate barium sulfate precipitation. COMPARE it with the standard
solution treated in the same method; and PERFORM a limit test.
A.8.2 Reagents and materials
A.8.2.1 Hydrochloric acid solution. 6 mol/L. PIPETTE 54 mL of hydrochloric acid;
DILUTE to 100 mL.
A.8.2.2 Barium chloride solution. 250 g/L.
A.8.2.3 Acetic acid solution. MEASURE and TAKE 298 mL of acetic acid;
DILUTE to 1000 mL.
A.8.2.4 Ethyl alcohol solution. MEASURE and TAKE 300 mL of absolute ethyl
alcohol; USE water to dilute to 1000 mL.
A.8.2.5 Standard stock solution of sulfate. c(SO4) = 0.1 g/L.
A.8.2.6 Standard solution I of sulfate. c(SO4) = 0.01 g/L. PIPETTE 10 mL of
standard stock solution of sulfate; USE ethyl alcohol solution to dilute to 100
mL.
A.8.2.7 Standard solution II of sulfate. c(SO4) = 0.015 g/L. PIPETTE 15 mL of
standard stock solution of sulfate; USE ethyl alcohol solution to dilute to 100
mL.
A.8.3 Analytical procedures
WEIGH 1 g of test piece, accurate to 0.01 g; PLACE it in a 50 mL colorimetric
tube with stopper; ADD 15 mL of water to dissolve; ADD 1 mL of barium chloride
solution, and 1 mL of standard solution of sulfate; SHAKE, LET it stand for 1
min; ADD 1 mL of hydrochloric acid solution and 0.5 mL of acetic acid solution;
SHAKE well, LET it stand for 5 min. PIPETTE 10 mL of standard solution of
sulfate in a 50 mL colorimetric tube with stopper; ADD 5 mL of water; and
starting from “ADD 1 mL of barium chloride solution”, TREAT it the same way
as the test piece. The turbidity of the test piece tube shall not be deeper than
that of the standard tube.
Note. Standard solution I of sulfate for citric acid anhydrous; standard solution II of sulfate
for citric acid monohydrate.
A.9 Determination of chloride
A.9.1 Method summary
A.10.2.5 Standard solution of oxalic acid. 0.01 g/L. WEIGH 0.175 g of oxalic
acid (C2H2O4·2H2O); USE water to dissolve and dilute to 500 mL. PIPETTE 4
mL of this solution; and USE water to dilute to 100 mL.
A.10.3 Analytical procedures
WEIGH 0.4 g (accurate to 0.01 g) of the test piece in a 25mL colorimetric tube
with stopper; ADD 4 mL of water, 3 mL of hydrochloric acid, and 1 g of zinc
granule; BOIL it for 1 min; PLACE it for 2 min; TRANSFER it into a test tube
containing 0.25 mL of phenylhydrazine hydrochloride solution; HEAT to boiling;
quickly COOL; POUR into a 25 mL colorimetric tube with stopper; ADD 0.25 mL
of equal volume of hydrochloric acid and potassium ferricyanide solution;
SHAKE; and PLACE for 30 min. TAKE 4 mL of standard solution of oxalic acid;
and starting from “3 mL of hydrochloric acid and 1 g of zinc granule”, TREAT it
the same way as the test piece. The pink generated in the test piece tube shall
not be deeper than that in the standard tube.
A.11 Determination of calcium salt
A.11.1 Method summary
In acetic acid medium, trace calcium ions and oxalate ions form insoluble
calcium oxalate suspensions. COMPARE it with the standard solution treated
in the same method; and PERFORM a limit test.
A.11.2 Reagents and materials
A.11.2.1 Acetic acid solution. 2 mol/L. MEASURE and TAKE 118 mL of glacial
acetic acid; USE water to dilute to 1000 mL.
A.11.2.2 Ammonium oxalate solution. 40 g/L.
A.11.2.3 Standard solution of calcium. c(Ca)=0.01 g/L. WEIGH 2.5 g of the
calcium carbonate which is baked at 105 °C ~ 110 °C to a constant mass; ADD
12 mL of 6 mol/L acetic acid (MEASURE and TAKE 354 mL of glacial acetic
acid; USE water to dilute to 1000 mL) to dissolve; ADD water to dilute to 1000
mL. PIPETTE 1 mL of this solution; and ADD water to dilute to 100 mL.
A.11.3 Analytical procedures
WEIGH 0.5 g (accurate to 0.01 g) of the test piece; PLACE it in a 25 mL
colorimetric tube; ADD 15 mL of water to dissolve; ADD 1 mL of ammonium
oxalate solution and 1 mL of acetic acid solution; SHAKE, PLACE it for 15 min.
TAKE 10 mL of standard solution of calcium in a 25 mL colorimetric tube; ADD
5 mL of water; and starting from “ADD 1 mL of ammonium oxalate solution”,
TREAT it the same way as the test piece. The turbidity of the test piece tube
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