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MINISTRY OF HEALTH
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THE SOCIALIST REPUBLIC OF VIETNAM
Independence - Freedom - Happiness
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No. 44/2010/TT-BYT
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Hanoi, December 22, 2010
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CIRCULAR
PROMULGATING
NATIONAL TECHNICAL REGULATIONS ON FOOD ADDITIVES
THE MINISTER OF HEALTH
Pursuant to the Law on Standards and Technical Regulations dated
June 29, 2006 and Government's Decree No. 127/2007/ND-CP dated August 01, 2007 elaborating
some Articles of the Law on Standards and Technical Regulations;
Pursuant to the Ordinance on Food Safety dated August 07, 2003 and Government’s
Decree No. 163/2004/ND-CP dated September 07, 2004 elaborating some Articles of
the Ordinance on Food Safety;
Pursuant to the Government’s Decree No. 188/2007/ND-CP dated December 27, 2007
defining functions, tasks, powers and organizational structure of the Ministry
of Health;
At the request of the Director General of the Vietnam Food Administration, the
Director General of the Science and Education Department, the Director General
of the Department of Legal Affairs,
HEREBY PRESCRIBES:
Article 1. Promulgated together
with this Circular are National technical regulations on food additives,
including:
1. QCVN 4-12:2010/BYT -
National technical regulation on food additives - Preservatives;
2. QCVN 4-13:2010/BYT -
National technical regulation on food additives - Stabilizers;
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4. QCVN 4-15:2010/BYT -
National technical regulation on food additives - Flour treatment agents;
5. QCVN 4-16:2010/BYT -
National technical regulation on food additives - Bulking agents;
6. QCVN 4-17:2010/BYT -
National technical regulation on food additives - Propellants;
Article 2. This Circular comes into
force from July 01, 2011.
Article 3. Director General of Vietnam Food Administration,
heads of units owned by the Ministry of Health, heads of units affiliated to
the Ministry of Health, Directors of Departments of Health of provinces and
central-affiliated cities and relevant organizations and individuals are
responsible for the implementation of this Circular./.
PP. THE MINISTER
THE DEPUTY MINISTER
Trinh Quan Huan
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NATIONAL TECHNICAL REGULATION
QCVN 4-12:2010/BYT
NATIONAL
TECHNICAL REGULATION ON FOOD ADDITIVE - PRESERVATIVE
FOREWORD
QCVN 4- :2010/BYT is
developed by the Drafting Board for National technical regulation on food
additives and food processing aids, submitted by the Vietnam Food
Administration for approval and promulgated together with the Circular No.
44/2010/TT-BYT dated December 22, 2010 of the Minister of Health.
NATIONAL TECHNICAL REGULATION ON FOOD ADDITIVE - PRESERVATIVE
I. GENERAL
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This National technical
regulation (hereinafter referred to as “the Regulation”) provides for
specifications and regulatory requirements for quality, hygiene and safety of
preservatives used as food additives.
2. Regulated entities
This Regulation applies
to:
2.1. Importers,
exporters, producers, traders and users of preservatives used as food additives
(hereinafter referred to as “entities”).
2.2. Relevant regulatory
bodies.
3. Interpretation of
terms and acronyms:
3.1. “preservative”
refers to a food additive used for the purpose of extending the shelf life of a
product by preventing microbial spoilage.
3.2. JECFA monograph
1 - Vol. 4 (JECFA monographs 1 - Combined compendium of food additive
specifications; Joint FAO/WHO expert committee on food additives; Volume 4 -
Analytical methods, test procedures and laboratory solutions used by and
referenced in the food additive specifications; FAO, 2006) is developed by
JECFA and was published by FAO in 2006.
3.3. “C.A.S number”
(Chemical Abstracts Service) refers to registry numbers of chemical substances
identified by the American Chemical Society.
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3.5. “ADI” stands
for Acceptable daily intake.
3.6. “INS” stands
for international numbering system.
II. SPECIFICATIONS,
TESTS AND SAMPLING
1. Specifications and
tests for flavour enhancers specified in the annexes to this Regulation:
1.1.
Annex 1:
Specifications and
tests for acid sorbic
1.2.
Annex 2:
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1.3.
Annex 3:
Specifications and
tests for calcium sorbate
1.4.
Annex 4:
Specifications and
tests for benzoic acid
1.5.
Annex 5:
Specifications and
tests for sodium benzoate
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Annex 6:
Specifications and
tests for potassium benzoate
1.7.
Annex 7:
Specifications and
tests for calcium benzoate
1.8.
Annex 8:
Specifications and
tests for ethyl p-hydroxybenzoate
1.9
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Specifications and
tests for methyl p-hydroxybenzoate
1.10
Annex 10:
Specifications and
tests for sulfur dioxide
1.11
Annex 11:
Specifications and
tests for sodium sulfite
1.12
Annex 12:
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1.13
Annex 13:
Specifications and
tests for sodium metabisulfite
1.14
Annex 14:
Specifications and
tests for potassium metabisulfite
1.15
Annex 15:
Specifications and
tests for potassium sulfite
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Annex 16:
Specifications and
tests for nisin
1.17
Annex 17:
Specifications and
tests for hexamethylene tertramine
1.18
Annex 18:
Specifications and
tests for dimethyl dicarbonate
1.19
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Specifications and
tests for propionic acid
1.20
Annex 20:
Specifications and
tests for sodium propionate
1.21
Annex 21:
Specifications and
tests for sodium hyposulfite
2. Specifications and
tests for sodium nitrate and potassium nitrate used as preservatives are
specified in QCVN 4-5 :2010/BYT promulgated together with the Circular No.
22/2010/TT-BYT dated May 20, 2010 of the Minister of Health.
3. Specifications
specified in this Regulation are tested under JECFA monograph 1 - Vol. 4,
except for some specific tests described in the annexes. The tests provided in
this Regulation are optional. Other equivalent tests may be used.
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III. REGULATORY
REQUIREMENTS
1. Declaration of
conformity
1.1. Conformity of
preservatives shall be declared in accordance with the regulations set out in
this Regulation.
1.2. Methods and
procedures for declaration of conformity shall comply with the Regulation on
certification and declaration of conformity with regulations and standards
under the Decision No. 24/2007/QĐ-BKHCN dated September 28, 2007 of the
Minister of Science and Technology and regulations of laws.
2. Inspection of
preservatives
The quality, hygiene and
safety of flavour enhancers must be inspected in accordance with the
regulations of law.
IV. RESPONSIBILITIES OF
ENTITIES
1. Entities must declare
conformity according to the specifications mentioned in this Regulation,
register their declarations of conformity at the Vietnam Food Administration
and ensure the quality, hygiene and safety as declared.
2. Entities are only
entitled to import, export, produce, sell and use flavour enhancers as declared
after their completion of registration of declarations of conformity and their
compliance with regulations of law on quality, hygiene, safety and labeling.
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1. The Vietnam Food
Administration shall preside over and cooperate with competent authorities
concerned to provide guidance on and organize the implementation of this
Regulation.
2. The Vietnam Food
Administration shall, according to its managerial duties, suggest amendments to
this Regulation to the Ministry of Health.
3. In the cases where
any of the international guidelines for tests and regulations of law referred
to in this Regulation is amended or replaced, the newest one shall apply.
ANNEX 1
SPECIFICATIONS
AND TESTS FOR ACID SORBIC
1. Synonyms
Sorbic acid
INS 200
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2. Definition
Chemical names
Acid sorbic; acid
2,4-hexadienoic; acid 2-propenylacrylic
C.A.S. number
110-44-1
Chemical formula
C6H8O2
Structural formula
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Formula weight
112.12
3. Description
Colourless needles or
white free flowing powder, having a slight characteristic odour.
4. Functional uses
Antimicrobial
preservative, fungistatic agent
5. Specifications
5.1. Identification
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Slightly soluble in
water, soluble in ethanol.
Melting range
Between 132 and 135oC
(the melting apparatus should be preheated to 125º before introducing the
sample).
Spectrophotometry
A 1 in 400,000
solution in isopropanol solution shows absorbance maximum at 254±2 nm
Test for double bond
Passes test.
5.2. Purity
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Not more than 0.5%.
Sulfated ash
Not more than 0.2%.
Aldehydes
Not more than 0.1% (as
formaldehyde).
Lead
Not more than 2 mg/kg.
5.3. C6H8O2 content
Not less than 99.0%
calculated on the anhydrous basis.
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6.1. Identification
Test for double bond
Shake about 0.02 g of
the sample with 1 ml bromine TS; the colour disappears
6.2. Purity
Water
- Karl Fischer Method.
- Tested according to JECFA monograph 1 - Vol.4.
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- Test 2 g of the
sample.
- Tested according to
method I, JECFA monograph 1 - Vol.4.
Aldehydes
To 1 ml of a saturated
aqueous solution of the sample, add 0.5 ml of Schiff's reagent TS and allow
to stand for 10-15 min. Compare the colour with that produced by 1 ml of
formaldehyde solution (containing 2 µg) with the same amount of Schiff's
reagent under the same conditions. The colour of the test solution should not
be more intense than that of the formaldehyde solution.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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Dissolve about 0.25 g
of the sample, accurately weighed, in 50 ml of anhydrous methanol previously
neutralized with 0.1 N sodium hydroxide, add phenolphthalein TS, and titrate
with 0.1 N sodium hydroxide to the first pink colour which persists for at
least 30 sec.
Each ml of 0.1 N
sodium hydroxide is equivalent to 11.21 mg of C6H8O2.
ANNEX 2
SPECIFICATIONS
AND TESTS FOR POTASSIUM SORBATE
1. Synonyms
Potassium sorbate
INS 202
ADI = 0 – 25 mg/kg bw
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Chemical names
Potassium sorbate,
potassium salt of trans, trans-2,4-hexadienoic acid
C.A.S. number
24634-16-5
Chemical formula
C6H7KO2
Structural formula
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150.22
3. Description
White or
yellowish-white crystals or crystalline powder or granules.
4. Functional uses
Preservative
5. Specifications
5.1. Identification
Solubility
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Test for potassium
Passes test.
Melting range of
sorbic acid derived from the sample
132-135oC.
Test for unsaturation
Passes test.
5.2. Purity
Loss on drying
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Acidity or alkalinity
Not more than about 1%
(as sorbic acid or potassium carbonate).
Aldehydes
Not more than 0.1% (as
formaldehyde).
Lead
Not more than 2 mg/kg.
5.3. C6H7KO2 content
Not less than 98% and
not more than 102% at the dried basis.
6. Tests
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Test for potassium
Tested according to
JECFA monograph 1 - Vol.4.
Melting range of
sorbic acid derived from the sample
Acidify a solution of
the sample with dilute hydrochloric acid TS. Collect the precipitated sorbic
acid on a filter paper, wash free of chloride with water and dry under vacuum
over sulfuric acid.
Test for unsaturation
To 2 ml of a 1 in 10
solution of the sample, add a few drops of bromine TS. The colour of the
bromine disappears.
6.2. Purity
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Tested according to
JECFA monograph 1 - Vol. 4. (105º, 3 h).
Acidity or alkalinity
Dissolve 1.1 g of the
sample in 20 ml of water and add 3 drops of phenolphthalein TS. If the
solution is colourless, titrate with 0.1 N sodium hydroxide to a pink colour
that persists for 15 sec. Not more than 1.1 ml should be required.
If the solution is
pink in colour titrate with 0.1 N hydrochloric acid. Not more than 0.8 ml
should be required to discharge the pink colour.
Aldehydes
Prepare a 0.3%
solution of the sample, adjust the pH to 4 with 1N HCl and filter. To 5 ml of
the filtrate add 2.5 ml of Schiff's reagent TS and allow to stand for 10 - 15
min. Compare the colour with that produced by 5 ml of a control solution
containing 15 µg of formaldehyde instead of the sample. The colour of the
test solution should not be more intense than that of the control solution.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
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Weigh, to the nearest
0.1 mg, 0.25 g of the sample, previously dried at 105º for 3 h. Dissolve in
36 ml of glacial acetic acid and 4 ml acetic anhydride in a 250-ml
glass-stoppered flask, warming to effect solution. Cool to room temperature,
add 2 drops of crystal violet TS and titrate with 0.1 N perchloric acid in
glacial acetic acid to a blue-green end point which persists for at least 30
sec. Perform a blank determination and make any necessary correction.
Each ml of 0.1 N
perchloric acid is equivalent to 15.02 mg of C6H7KO2.
ANNEX 3
SPECIFICATIONS
AND TESTS FOR CALCIUM SORBATE
1. Synonyms
Calcium sorbate
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ADI = 0 - 25 mg/kg bw
2. Definition
Chemical names
Calcium sorbate;
calcium salt of trans, trans-2,4-hexadienoic acid.
C.A.S. number
7492-55-9
Chemical formula
C12H14CaO4
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Formula weight
262.32
3. Description
Fine white crystalline
powder not showing any change in colour after heating at 105oC for
90 min.
4. Functional uses
Preservative
5. Specifications
5.1. Identification
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Solubility
Soluble in water;
practically insoluble in ethanol.
Test for calcium
Passes test.
Melting range of
sorbic acid derived from the sample
132-135oC.
Test for unsaturation
Passes test.
5.2. Purity
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Loss on drying
Not more than 3%.
Fluoride
Not more than 10
mg/kg.
Aldehydes
Not more than 0.1% (as
formaldehyde).
Lead
Not more than 2 mg/kg.
5.3. C12H14CaO4
content
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6. Tests
6.1. Identification
Test for calcium
Tested according to
JECFA monograph 1 - Vol.4.
Melting range of
sorbic acid derived from the sample
Acidify a solution of
the sample with dilute hydrochloric acid TS. Collect the precipitated sorbic
acid on a filter paper, wash free of chloride with water and dry under vacuum
over sulfuric acid.
Test for unsaturation
To 2 ml of a 1 in 10
solution of the sample, add a few drops of bromine TS. The colour of the
bromine disappears.
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Loss on drying
Tested according to
JECFA monograph 1 - Vol. 4. (over sulfuric acid in vacuum, 4h).
Fluoride
Tested according to
method I, JECFA monograph 1 - Vol.4 (weigh 5 g of the sample to the nearest
mg and proceed as directed in the Fluoride Limit Test (Method I or III).
Aldehydes
Prepare a 0.3%
solution of the sample, adjust the pH to 4 with 1N HCl and filter. To 5 ml of
the filtrate add 2.5 ml of Schiff's reagent TS and allow to stand for 10 - 15
min. Compare the colour with that produced by 5 ml of a control solution
containing 15 µg of formaldehyde instead of the sample. The colour of the
test solution should not be more intense than that of the control solution.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
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6.3. Method of essay
Weigh to the nearest
mg, 0.25 g of the dried sample. Dissolve in 35 ml of glacial acetic acid and
4 ml of acetic anhydride in a 250-ml glass-stoppered flask, warming to effect
solution. Cool to room temperature, add 2 drops of crystal violet TS and
titrate with 0.1 N perchloric acid in glacial acetic acid to a blue-green end
point which persists for at least 30 sec. Perform a blank determination and
make any necessary correction.
Each ml of 0.1 N
perchloric acid is equivalent to 13.12 mg of C12H14CaO4.
ANNEX 4
SPECIFICATIONS
AND TESTS FOR BENZOIC ACID
1. Synonyms
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INS 210
ADI = 0 – 5 mg/kg bw
2. Definition
Chemical names
Benzoic acid,
benzenecarboxylic acid, phenylcarboxylic acid
C.A.S. number
65-85-10
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C7H6O2
Structural formula
Formula weight
122.12
3. Description
White crystalline
solid, usually in the form of scales or needles, having not more than a faint
characteristic odour.
4. Functional uses
Antimicrobial
preservative
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5.1. Identification
Solubility
Slightly soluble in
water, freely soluble in ethanol
Melting range
121oC -123oC
Test for benzoate
Passes test.
pH
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5.2. Purity
Loss on drying
Not more than 0.5%.
Sublimation test
Passes test (described
in “Tests”).
Sulfated ash
Not more than 0.05%.
Lead
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Readily carbonizable
substances
Passes test (described
in “Tests”).
Chlorinated organic
compounds
Not more than 0.07%
(as Cl2).
Readily oxidizable
substances
Passes test (described
in “Tests”).
5.3. C7H6O2 content
Not less than 99.5% on
the dried basis.
6. Tests
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Test for benzoate
- Tested according to
JECFA monograph 1 - Vol.4.
- Use 0.1 g of the
sample with 0.1 g of calcium carbonate and 5 ml of water.
6.2. Purity
Loss on drying
- Tested according to
JECFA monograph 1 - Vol.4.
- Over sulfuric acid,
3 h.
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Place a small amount
of the sample in a dry test tube. Wrap the test tube about 4 cm from the
bottom with moistened filter paper. Heat the test tube over a low flame.
Benzoic acid sublimes and crystals deposit in the colder part of the test
tube leaving no residue at the bottom.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
Readily carbonizable
substances
- Tested according to
JECFA monograph 1 - Vol.4.
- Dissolve 0.5 g of
the sample, weighed to the nearest mg, in 5 ml of sulfuric acid TS. The
colour produced should not be darker than a light pink (Matching Fluid Q).
Chlorinated organic
compounds
Test 0.25 g of the
sample dissolved in 10 ml of 0.1 N sodium hydroxide, using 0.5 ml of 0.01N
hydrochloric acid in the control.
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Add 1.5 ml of sulfuric
acid to 100 ml of water, heat to boiling and add 0.1N potassium permanganate
in drops, until the pink colour persists for 30 sec. Dissolve 1 g of the
sample, weighed to the nearest mg, in the heated solution, and titrate with
0.1N potassium permanganate to a pink colour that persists for 15 sec. Not
more than 0.5 ml should be required.
6.3. Method of essay
Weigh, to the nearest
mg, 2.5 g of the dried sample. Dissolve in 15 ml of warm ethanol previously
neutralized using phenol red TS as indicator. Add 20 ml of water and titrate
with 0.5N sodium hydroxide, using phenolphthalein TS as indicator.
Each ml 0.5N sodium
hydroxide is equivalent to 61.06 mg of C7H6O2.
ANNEX 5
SPECIFICATIONS
AND TESTS FOR SODIUM BENZOATE
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Sodium benzoate;
INS 211
ADI = 0 - 5 mg/kg bw
2. Definition
Chemical names
Benzoic acid,
benzenecarboxylic acid, phenylcarboxylic acid
C.A.S. number
532-32-1
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C7H5NaO2
Structural formula
Formula weight
144.11
3. Description
White, almost
odourless, crystalline powder, flakes or granules
4. Functional uses
Antimicrobial
preservative
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5.1. Identification
Solubility
Freely soluble in water,
sparingly soluble in ethanol.
Test for sodium
Passes test.
Test for benzoate
Passes test.
5.2. Purity
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Loss on drying
Not more than 1.5%.
Acidity or alkalinity
Passes test (described
in “Tests”).
Readily carbonizable
substances
Passes test (described
in “Tests”).
Chlorinated organic
compounds
Not more than 0.07%
(as Cl2).
Readily oxidizable
substances
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Lead
Not more than 2 mg/kg.
5.3. C7H5NaO2 content
Not less than 99.0%
calculated on the anhydrous basis.
6. Tests
6.1. Identification
Test for sodium
- Tested according to
JECFA monograph 1 - Vol.4.
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- Tested according to
JECFA monograph 1 - Vol.4.
- Use a 10% solution
of the sample
6.2. Purity
Loss on drying
- Tested according to JECFA
monograph 1 - Vol. 4.
- 105oC, 4
h.
Acidity or alkalinity
Dissolve 2 g of the
sample, weighed to the nearest mg, in 20 ml of freshly boiled water. Not more
than 0.5 ml of either 0.1N sodium hydroxide or 0.1N hydrochloric acid should
be required for neutralization, using phenolphthalein TS as indicator.
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Dissolve 0.5 g of the
sample, weighed to the nearest mg, in 5 ml of sulfuric acid TS. The colour
produced should not be darker than a light pink ("Matching Fluid
Q") (Tested according to JECFA monograph 1 - Vol. 4).
Chlorinated organic
compounds
- Tested according to
JECFA monograph 1 - Vol.4.
- Test 0.25 g of the
sample using 0.5 ml of 0.01N hydrochloric acid in the control.
Readily oxidizable
substances
Add 1.5 ml of sulfuric
acid to 100 ml of water, heat to boiling and add 0.1N potassium permanganate,
dropwise, until the pink colour persists for 30 sec. Dissolve 1 g of the
sample, weighed to the nearest mg, in the heated solution, and titrate with
0.1N potassium permanganate to a pink colour that persists for 15 sec. Not
more than 0.5 ml should be required.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
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Weigh, to the nearest
mg, 3 g of the sample previously dried for 4 h at 105oC and
transfer to a 250-ml Erlenmeyer flask. Add 50 ml of water to dissolve the
sample. Neutralize the solution, if necessary, with 0.1N hydrochloric acid,
using phenolphthalein TS as indicator. Add 50 ml of ether and a few drops of
bromophenol blue TS, and titrate with 0.5N hydrochloric acid, shaking the
flask constantly, until the colour of the indicator begins to change.
Transfer the lower aqueous layer to another flask. Wash the ethereal layer
with 10 ml of water, and add the washing and an additional 20 ml of ether to
the separated aqueous layer. Complete the titration with the 0.5N
hydrochloric acid, shaking constantly the flask.
Each ml of 0.5N
hydrochloric acid is equivalent to 72.05 mg of C7H5NaO2.
ANNEX 6
SPECIFICATIONS
AND TESTS FOR POTASIUM BENZOATE
1. Synonyms
Potasium benzoate;
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ADI=0 - 5 mg/kg bw
2. Definition
Chemical names
Potassium benzoate,
potassium salt of benzenecarboxylic acid, potassium salt of phenylcarboxylic
acid
C.A.S. number
582-25-2 (anhydrous)
Chemical formula
C7H5KO2.3H2O
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Formula weight
160.22 (anhydrous
C7H5KO2)
214.27 (trihydrate
C7H5KO2.3H2O)
3. Description
White crystalline
powder
4. Functional uses
Antimicrobial
preservative
5. Specifications
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Solubility
Freely soluble in
water, soluble in ethanol.
Test for potassium
Passes test.
Test for benzoate
Passes test.
5.2. Purity
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Not more than 26.5%.
Acidity or alkalinity
Passes test (described
in “Tests”).
Readily carbonizable
substances
Passes test (described
in “Tests”).
Chlorinated organic
compounds
Not more than 0.07%
(as Cl2).
Readily oxidizable
substances
Passes test (described
in “Tests”).
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Not more than 2 mg/kg.
5.3. C7H5KO2 content
Not less than 99.0%
calculated on the anhydrous basis.
6. Tests
6.1. Identification
Test for potassium
- Tested according to
JECFA monograph 1 - Vol. 4.
- Use a 10% solution
of the sample.
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- Tested according to
JECFA monograph 1 - Vol.4.
- Use a 10% solution
of the sample.
6.2. Purity
Loss on drying
- Tested according to
JECFA monograph 1 - Vol. 4.
- 105oC, 4
h.
Acidity or alkalinity
Dissolve 2 g of the
sample, weighed to the nearest mg, in 20 ml of freshly boiled water. Not more
than 0.5 ml of either 0.1N sodium hydroxide or 0.1N hydrochloric acid should
be required for neutralization, using phenolphthalein TS as indicator.
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- Tested according to
JECFA monograph 1 - Vol. 4.
- Dissolve 0.5 g of
the sample, weighed to the nearest mg, in 5 ml of sulfuric acid TS. The
colour produced should not be darker than a light pink (Matching Fluid Q).
Chlorinated organic
compounds
- Tested according to
JECFA monograph 1 - Vol. 4.
- Test 0.25 g of the
sample using 0.5 ml of 0.01N hydrochloric acid in the control.
Readily oxidizable
substances
Add 1.5 ml of sulfuric
acid to 100 ml of water, heat to boiling and add 0.1N potassium permanganate,
dropwise, until the pink colour persists for 30 sec. Dissolve 1 g of the
sample, weighed to the nearest mg, in the heated solution, and titrate with
0.1N potassium permanganate to a pink colour that persists for 15 sec. Not
more than 0.5 ml should be required.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
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6.3. Method of essay
Weigh to the nearest
0.1 mg, 2.5 to 3 g of the dried sample, and transfer to a 250-ml Erlenmeyer
flask. Add 50 ml of water to dissolve the sample. Neutralize the solution, if
necessary, with 0.1N hydrochloric acid, using phenolphthalein TS as
indicator. Add 50 ml of ether and a few drops of bromophenol blue TS, and
titrate with 0.5N hydrochloric acid, shaking the flask constantly, until the
colour of the indicator begins to change. Transfer the lower aqueous layer to
another flask. Wash the ethereal layer with 10 ml of water, and add the
washing and an additional 20 ml of ether to the separated aqueous layer.
Complete the titration with the 0.5N hydrochloric acid, shaking constantly
the flask.
Each ml of 0.5N
hydrochloric acid is equivalent to 80.11 mg of C7H5KO2.
ANNEX 7
SPECIFICATIONS
AND TESTS FOR CALCIUM BENZOATE
1. Synonyms
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INS 213
ADI = 0 - 5 mg/kg bw
2. Definition
Chemical names
Calcium benzoate
C.A.S. number
2090-05-3
Chemical formula
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Monohydrate:
C14H10CaO4.H2O
Trihydrate:
C14H10CaO4.3H2O
Structural formula
Anhydrous
Formula weight
Anhydrous: 282.31
Monohydrate: 300.32
Trihydrate: 336.36
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White or colourless
crystals, or white powder.
4. Functional uses
Antimicrobial
preservative
5. Specifications
5.1. Identification
Solubility
Sparingly soluble in
water
Test for calcium
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Test for benzoate
Passes test.
5.2. Purity
Loss on drying
Not more than 17.5%.
Water insoluble matter
Not more than 0.3%.
Acidity or alkalinity
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Fluoride
Not more than 10
mg/kg.
Lead
Not more than 2 mg/kg.
Chlorinated organic
compounds
Not more than 0.07%
(as Cl2).
Readily oxidizable
substances
Passes test (described
in “Tests”).
5.3. C14H10CaO4
content
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6. Tests
6.1. Identification
Test for calcium
Tested according to
JECFA monograph 1 - Vol.4.
Test for benzoate
Tested according to
JECFA monograph 1 - Vol. 4.
6.2. Purity
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- Tested according to
JECFA monograph 1 - Vol. 4.
- 105oC, 4
h.
Water insoluble matter
Dissolve 10 g of the
sample, weighed to the nearest mg, in 100 ml of hot water. Filter through a
Gooch crucible, tared to an accuracy of ±0.2 mg, and wash any residue with
hot water. Dry the crucible for 2 h at 105ºC. Cool, weigh and calculate as
percentage.
Acidity or alkalinity
Dissolve 2 g of the
sample, weighed to the nearest mg, in 20 ml of freshly boiled water. Not more
than 0.5 ml of either 0.1N sodium hydroxide or 0.1N hydrochloric acid should
be required for neutralization, using phenolphthalein TS as indicator.
Fluoride
- Tested according to
JECFA monograph 1 - Vol. 4, Method I or III.
- Weigh 5 g of the
sample to the nearest mg.
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- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
Chlorinated organic
compounds
Test 0.25 g of the
sample using 0.5 ml of 0.01N hydrochloric acid in the control.
Readily oxidizable
substances
Add 1.5 ml of sulfuric
acid to 100 ml of water, heat to boiling and add 0.1N potassium permanganate
in drops, until the pink colour persists for 15 sec. Dissolve 1 g of the
sample, weighed to the nearest mg, in the heated solution, and titrate with
0.1N potassium permanganate to a pink colour that persists for 15 sec. Not
more than 0.5 ml should be required.
6.3. Method of essay
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Each ml of 0.05M
disodium ethylenediamine tetraacetate is equivalent to 14.116 mg of
C14H10CaO4.
ANNEX 8
SPECIFICATIONS
AND TESTS FOR ETHYL p-HYDROXYBENZOATE
1. Synonyms
Ethyl p-oxybenzoate; Ethylparaben
INS 214
ADI= 0 – 10 mg/kg bw
2. Definition
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Chemical names
Ethyl
p-hydroxybenzoate, ethyl ester of p-hydroxybenzoic acid
C.A.S. number
120-47-8
Chemical formula
C9H10O3
Structural formula
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166.18
3. Description
Almost odourless,
small, colourless crystals or a white, crystalline powder.
4. Functional uses
Preservative
5. Specifications
5.1. Identification
Solubility
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Melting range
115oC -118oC.
Test for
p-hydroxybenzoate
Melting range of
p-hydroxybenzoic acid derived from the sample is 212- 217o.
5.2. Purity
Loss on drying
Not more than 0.5%.
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Not more than 0.05%.
Acidity
Passes test (described
in “Tests”).
p-Hydroxybenzoic acid
and salicylic acid
Passes test (described
in “Tests”).
Lead
Not more than 2 mg/kg.
5.3. C9H10O3 content
Not less than 99.0%
calculated on the anhydrous basis.
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6.1. Identification
Test for p-hydroxybenzoate
To 0.5 g of the sample
add 10 ml of sodium hydroxide TS. Boil for 30 min and concentrate to about 5
ml. Cool, acidify with dilute sulfuric acid TS, collect the precipitate on a
filter, and wash thoroughly with water. Dry in a desiccator over sulfuric
acid. Determine the melting range of phydroxybenzoic acid so obtained.
6.2. Purity
Loss on drying
- Tested according to
JECFA monograph 1 - Vol. 4.
- Not more than 0.5%
(80º, 2 h).
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- Tested according to
JECFA monograph 1 - Vol. 4, Method I.
- Test 2 g of the
sample.
Acidity
Heat 750 mg of the
sample with 15 ml of water at 80o for 1 min, cool, and filter. The filtrate
should be acid or neutral to litmus. To 10 ml of the filtrate add 0.2 ml of
0.1 N sodium hydroxide and 2 drops of methyl red TS. The solution should be
yellow without even a light cast of pink.
p-Hydroxybenzoic acid
and salicylic acid
Dissolve 0.5 g of the
sample, accurately weighed, in 30 ml of ether, add 20 ml of a 1 in 100 sodium
hydrogen carbonate solution, shake, and separate the water layer. Wash the
water layer with two 20 ml portions of ether, add 5 ml of dilute sulfuric
acid and 30 ml of ether, and shake. Separate the ether layer, and shake with
about 10 ml of water. Filter the ether
layer, and wash the vessel and the filter with a small amount of ether.
Combine the washings and the filtrate, evaporate ether on a water bath, and
dry the residue over sulfuric acid to constant weight. The weight of the
residue should not exceed 5 mg. Dissolve any residue in 25 ml of water, heat
to about 70o , filter, and add a few drops of dilute ferric chloride TS. No
violet to reddish violet colour should be produced.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
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Weigh, to the nearest
mg, 2 g of the dried sample and transfer into a flask. Add 40 ml of N sodium
hydroxide and rinse the sides of the flask with water. Cover with a watch
glass, boil gently for 1 h and cool. Add 5 drops of bromothymol blue TS and
titrate the excess sodium hydroxide with N sulfuric acid, comparing the
colour with a buffer solution (pH 6.5) containing the same proportion of
indicator. Perform a blank determination with the reagents and make any
necessary correction.
Each ml of N sodium
hydroxide is equivalent to 166.18 mg of C9H10O3.
ANNEX 9
SPECIFICATIONS
AND TESTS FOR METHYL p-HYDROXYBENZOATE
1. Synonyms
Methyl p-oxybenzoate; Methylparaben
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ADI = 0 - 10mg/kg bw
2. Definition
Chemical names
Methyl
p-hydroxybenzoate, methyl ester of p-hydroxybenzoic acid
C.A.S. number
99-76-3
Chemical formula
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Structural formula
Formula weight
152.15
3. Description
Almost odourless,
small, colourless crystals or a white, crystalline powder.
4. Functional uses
Preservative
5. Specifications
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Solubility
Slightly soluble in
water; freely soluble in ethanol and propylene glycol; soluble in ether.
Melting range
125oC -128oC.
Test for
p-hydroxybenzoate
Melting range of
p-hydroxybenzoic acid derived from the sample is 212- 217o.
5.2. Purity
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Not more than 0.5%.
Sulfated ash
Not more than 0.05%.
Acidity
Passes test (described
in “Tests”).
p-Hydroxybenzoic acid
and salicylic acid
Passes test (described
in “Tests”).
Lead
Not more than 2 mg/kg.
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Not less than 99.0%
calculated on the anhydrous basis.
6. Tests
6.1. Identification
Test for
p-hydroxybenzoate
To 0.5 g of the sample
add 10 ml of sodium hydroxide TS. Boil for 30 min and concentrate to about 5
ml. Cool, acidify with dilute sulfuric acid TS, collect the precipitate on a
filter, and wash thoroughly with water. Dry in a desiccator over sulfuric
acid. Determine the melting range of phydroxybenzoic acid so obtained.
6.2. Purity
Loss on drying
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- Over silica gel, 5
h.
Sulfated ash
Tested according to
JECFA monograph 1 - Vol. 4, Method I (Test 2 g of the sample).
Acidity
Heat 750 mg of the
sample with 15 ml of water at 80o for 1 min, cool, and filter. The filtrate
should be acid or neutral to litmus. To 10 ml of the filtrate add 0.2 ml of
0.1 N sodium hydroxide and 2 drops of methyl red TS. The solution should be
yellow without even a light cast of pink.
p-Hydroxybenzoic acid
and salicylic acid
Dissolve 0.5 g of the
sample, accurately weighed, in 30 ml of ether, add 20 ml of a 1 in 100 sodium
hydrogen carbonate solution, shake, and separate the water layer.
Wash the water layer
with two 20 ml portions of ether, add 5 ml of dilute sulfuric acid and 30 ml
of ether, and shake. Separate the ether layer, and shake with about 10 ml of
water.Filter the ether layer, and wash the vessel and the filter with a small
amount of ether. Combine the washings and the filtrate, evaporate ether on a
water bath, and dry the residue over sulfuric acid to constant weight. The
weight of the residue should not exceed 5 mg. Dissolve any residue in 25 ml
of water, heat to about 70o , filter, and add a few drops of dilute ferric
chloride TS. No violet to reddish violet colour should be produced.
Lead
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- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
6.3. Method of essay
Weigh, to the nearest
mg, 2 g of the dried sample and transfer into a flask. Add 40 ml of N sodium
hydroxide and rinse the sides of the flask with water. Cover with a watch
glass, boil gently for 1 h and cool. Add 5 drops of bromothymol blue TS and
titrate the excess sodium hydroxide with N sulfuric acid, comparing the
colour with a buffer solution TS (pH 6.5) containing the same proportion of
indicator. Perform a blank determination with the reagents and make any
necessary correction.
Each ml of N sodium
hydroxide is equivalent to 152.2 mg of C8H8O3.
ANNEX 10
SPECIFICATIONS
AND TESTS FOR SULFUR DIOXIDE
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INS 220
ADI = 0 - 0.7 mg/kg bw
2. Definition
C.A.S. number
7446-09-5
Structural formula
SO2
Formula weight
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3. Description
Colourless,
non-flammable gas, with strong, pungent, suffocating odour. Its vapour
density is 2.26 times that of air at atmospheric pressure and 0oC.
The specific gravity of the liquid is about 1.436 at 0o/4oC.
At 20o the solubility is about 10 g of SO2 per 100 g of solution.
It is normally supplied under pressure in containers in which it is present
in both liquid and gaseous phases.
Caution: Sulfur
dioxide gas is intensely irritating to the eyes, throat, and upper
respiratory system. Liquid sulfur dioxide may cause skin burns, which result
from the freezing effect of the liquid on tissue. Safety precautions to be
observed in handling of the material are specified in technical brochures
from liquid sulfur dioxide manufacturers, suppliers or organizations of gas
manufacturers or suppliers.
4. Functional uses
Preservative,
antibrowning agent, antioxidant.
5. Specifications
5.1. Identification
Solubility
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Test for sulfurous
substances
Passes test.
Oxidizing activity
Passes test.
5.2. Purity
Water
Not more than 0.05%.
Non-volatile residue
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Selenium
Not more than 20 mg/kg.
Lead
Not more than 5 mg/kg.
5.3. SO2 content
Not less than 99.9 %
SO2 by weight.
6. Tests
6.1. Identification
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The sample blackens
filter paper moistened with mercurous nitrate TS.
Oxidizing activity
Expose a filter paper,
treated with potassium iodate and starch TS, to the sample. A blue colour is
developed that fades on continued exposure.
6.2. Purity
Water
- Tested according to
JECFA monograph 1 - Vol. 4.
- Transfer about 50 ml
of liquid sulfur dioxide into a Karl Fischer titration jar, determine the
weight of the sample taken, and determine the water content by Karl Fischer
Method.
Non-volatile residue
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Selenium
- A 2.0-ml portion of
the Sample Solution meets the requirements of the Selenium Limit Test, Method
II.
- For sampling and
sample preparation, see “Tests”.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
6.3. Sampling
Samples of sulfur
dioxide may be safely withdrawn from a tank or transfer lines, either of
which should be equipped with a 1-cm nozzle and valve. Samples should be
taken in bombs constructed of 316 stainless steel, designed to withstand 7
MPa (1000 psig) and equipped with 316 stainless steel needle valves on both
ends. To draw a sample, the bomb is first flushed with dry air to remove any
sulfur dioxide, remaining from previous sample drawings, and then attached to
the tank or transfer lines with a solid pipe connection. A hose is connected
to the other end of the bomb and submerged in either a weak caustic solution
or water. Any gas in the bomb is discharged into the caustic or water by
first opening the valve at the pipe end, followed by slowly opening at the
valve at the hose end. When all of the gas is dispelled and liquid sulfur dioxide
begins to emerge into the solution, the valve at the hose end is blocked off. The other valves are then tightly closed, and the bomb is
detached from the pipe connecting it to the tank or transfer line
Approximately 15% of the liquid sulfur dioxide in the bomb is then discharged
into the water or caustic solution. The bomb is then
capped at its end and transferred to the laboratory for analysis.
Caution: The bomb
should never be stored with more than 85% of the total water capacity of the
bomb.
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Note: The tests in
which this solution is to be used will be accurate assuming a 144 g sample
has been taken; if not, the weight of sample actually taken must be
considered in the calculations.
6.4. Method of essay
Subtract from 100 the
percentages of non-volatile residue and of water, as determined herein, to
obtain the percentage of SO2.
ANNEX 11
SPECIFICATIONS
AND TESTS FOR SODIUM SULFITE
1. Synonyms
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INS 221
ADI=0 – 0.7 mg/kg bw
as SO2
2. Definition
Chemical names
Sodium sulfite
C.A.S. number
7757-83-7
Chemical formula
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Formula weight
126.04
3. Description
White powder with not
more than a faint odour of sulfur dioxide.
4. Functional uses
Antibrowning agent,
antioxidant, preservative
5. Specifications
5.1. Identification
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Freely soluble in
water; sparingly soluble in ethanol.
Test for sodium
Passes test.
Test for sulfite
Passes test.
5.2. Purity
pH
8.5 - 10.0 (1 in 10
soln).
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Not more than 0.1%.
Iron
Not more than 10
mg/kg.
Lead
Not more than 2 mg/kg.
Selenium
Not more than 5 mg/kg.
5.3. Na2SO3 content
Not less than 95.0%.
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6.1. Identification
Test for sodium
- Tested according to
JECFA monograph 1 - Vol. 4.
Test for sulfite
- Tested according to
JECFA monograph 1 - Vol. 4.
6.2. Purity
Thiosulfate
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Iron
- Tested according to
JECFA monograph 1 - Vol. 4.
- Use 0.5 ml of Iron
Standard Solution (5 µg Fe) in the control.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
Selenium
Reagents:
Hydrochloric acid,
hydrazinium sulfate, standard selenium solution (100 µg Se/ml)
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Weigh 2.0 ± 0.1 g of
sample and transfer to a 50-ml beaker. Add 10 ml water, 5 ml hydrochloric
acid and boil to remove SO2.
Into a second beaker,
weigh 1.0 ± 0.1 g of sample, add 0.05 ml standard selenium solution and
proceed as above.
To each beaker add 2 g
hydrazinium sulfate and warm to dissolve. Let stand for 5 min. Dilute the
contents of each beaker to 50 ml in a Nessler tube and compare the colour of
the two solutions. The sample should be less pink than the sample with the
added standard.
6.3. Method of essay
Weigh 250 mg of the
sample, add to 50.0 ml of 0.1 N iodine in a glassstoppered flask, and stopper
the flask. Allow to stand for 5 min, add 1 ml of hydrochloric acid and
titrate the excess iodine with 0.1 N sodium thiosulfate, adding starch TS as
the indicator.
Each ml of 0.1 N
iodine is equivalent to 6.302 mg of Na2SO3.
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SPECIFICATIONS
AND TESTS FOR SODIUM HYDROGEN SULFITE
1. Synonyms
Sodium hydrogen
sulfite;
INS 222
ADI =0 - 0,7 mg/kg bw
as SO2
2. Definition
Chemical names
Sodium hydrogen
sulfite, sodium bisulfite
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7631-90-5
Chemical formula
NaHSO3
Formula weight
104.06
3. Description
White crystals or
granular powder having an odour of sulfur dioxide.
4. Functional uses
Antibrowning agent,
antioxidant, preservative
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5.1. Identification
Solubility
Freely soluble in
water; sparingly soluble in ethanol
Test for sodium
Passes test.
Test for sulfite
Passes test.
5.2. Purity
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Water insolubles
Passes test (described
in “Tests”).
pH
2.5 - 4.5 (1 in 10
soln).
Iron
Not more than 10
mg/kg.
Lead
Not more than 2 mg/kg.
Selenium
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5.3. SO2 content
Not less than 58.5%
and not more than 67.4% of SO2
6. Tests
6.1. Identification
Test for sodium
Tested according to
JECFA monograph 1 - Vol. 4.
Test for sulfite
Tested according to
JECFA monograph 1 - Vol. 4.
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Water insolubles
Dissolve 20 g of the
sample in 200 ml of water. The solution should be clear with only a trace of
suspended matter.
Iron
- Tested according to
JECFA monograph 1 - Vol. 4.
- Use 0.5 ml of Iron
Standard Solution (5 µg Fe) in the control.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
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Reagents:
Hydrochloric acid,
hydrazinium sulfate, standard selenium solution (100 µg Se/ml)
Procedure:
Weigh 2.0 ± 0.1 g of
sample and transfer to a 50-ml beaker. Add 10 ml water, 5 ml hydrochloric
acid and boil to remove SO2.
Into a second beaker,
weigh 1.0 ± 0.1 g of sample, add 0.05 ml standard selenium solution and
proceed as above.
To each beaker add 2 g
hydrazinium sulfate and warm to dissolve. Let stand for 5 min. Let stand for
5 min. Dilute the contents of each beaker to 50 ml in a Nessler tube and
compare the colour of the two solutions. The sample should be less pink than
the sample with the added standard.
6.3. Method of essay
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Each ml of 0.1 N
iodine is equivalent to 3.203 mg of SO2.
ANNEX 13
SPECIFICATIONS
AND TESTS FOR SODIUM METABISULFITE
1. Synonyms
Sodium metabisulfite;
INS 223
ADI = 0 - 0.7mg/kg bw
as SO2
2. Definition
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Chemical names
Sodium disulfite,
disodium pentaoxodisulfate, disodium pyrosulfite
C.A.S. number
7681-57-4
Chemical formula
Na2S2O5
Formula weight
190.11
3. Description
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4. Functional uses
Antibrowning agent,
antioxidant, flour treatment agent, preservative
5. Specifications
5.1. Identification
Solubility
Freely soluble in
water; sparingly soluble in ethanol.
Test for sodium
Passes test.
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Passes test.
5.2. Purity
Water insolubles
Passes test (described
in “Tests”).
pH
4.0 - 4.5 (1 in 10
soln).
Thiosulfate
Not more than 0.1%.
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Not more than 10
mg/kg.
Lead
Not more than 2 mg/kg.
Selenium
Not more than 5 mg/kg.
5.3. Na2S2O5 content
Not less than 90.0%.
6. Tests
6.1. Identification
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Test for sodium
- Tested according to
JECFA monograph 1 - Vol. 4.
Test for sulfite
- Tested according to
JECFA monograph 1 - Vol. 4.
6.2. Purity
Water insolubles
Dissolve 20 g of the
sample in 200 ml of water. The solution should be
clear with only a trace of suspended matter.
Thiosulfate
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Iron
- Tested according to
JECFA monograph 1 - Vol. 4.
- Use 0.5 ml of Iron
Standard Solution (5 µg Fe) in the control.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
Selenium
Reagents:
Hydrochloric acid,
hydrazinium sulfate, standard selenium solution (100 µg Se/ml)
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Weigh 2.0 ± 0.1 g of
sample and transfer to a 50-ml beaker. Add 10ml ml water, 5 ml hydrochloric
acid and boil to remove SO2.
Into a second beaker,
weigh 1.0 ± 0.1 g of sample, add 0.05 ml standard selenium solution and
proceed as above.
To each beaker add 2 g
hydrazinium sulfate and warm to dissolve. Let stand for 5 min. Let stand for
5 min. Dilute the contents of each beaker to 50 ml in a Nessler tube and
compare the colour of the two solutions. The sample should be less pink than
the sample with the added standard.
6.3. Method of essay
Weigh 0.2 g of the
sample, to the nearest mg, add 50.0 ml of 0.1 N iodine in a glass-stoppered
flask, and stopper the flask. Allow to stand for 5 min, add 1 ml of
hydrochloric acid and titrate the excess iodine with 0.1 N sodium
thiosulfate, adding starch TS as the indicator.
Each ml of 0.1 N
iodine is equivalent to 4.753 mg of Na2S2O5.
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SPECIFICATIONS
AND TESTS FOR POTASSIUM METABISULFITE
1. Synonyms
Potassium
metabisulfite;
INS 224
ADI=0 - 0.7 mg/kg bw
as SO2
2. Definition
Chemical names
Potassium disulfite,
potassium pentaoxodisulfate, potassium pyrosulfite
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16731-55-8
Chemical formula
K2S2O5
Formula weight
222.33
3. Description
Colourless
free-flowing crystals, crystalline powder, or granules, usually having an
odour of sulfur dioxide.
4. Functional uses
Antibrowning agent,
antioxidant, preservative
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5.1. Identification
Solubility
Soluble in water;
insoluble in ethanol.
Test for potassium
Passes test.
Test for sulfite
Passes test.
5.2. Purity
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Water insolubles
Passes test (described
in “Tests”).
Thiosulfate
Not more than 0.1%.
Iron
Not more than 10
mg/kg.
Lead
Not more than 2 mg/kg.
Selenium
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5.3. K2S2O5 content
Not less than 90.0%.
6. Tests
6.1. Identification
Test for potassium
Passes test.
Test for sulfite
Passes test.
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Water insolubles
Dissolve 20 g of the
sample in 200 ml of water. The solution should be clear with only a trace of
suspended matter.
Thiosulfate
A 10% solution of the
sample should remain clear on acidification with sulfuric or hydrochloric
acid.
Iron
- Tested according to
JECFA monograph 1 - Vol. 4.
- Use 0.5 ml of Iron
Standard Solution (5 µg Fe) in the control.
Lead
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- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
Selenium
Reagents:
Hydrochloric acid,
hydrazinium sulfate, standard selenium solution (100 µg Se/ml)
Procedure:
Weigh 2.0 ± 0.1 g of
sample and transfer to a 50-ml beaker. Add 10 ml water, 5 ml hydrochloric
acid and boil to remove SO2.
Into a second beaker,
weigh 1.0 ± 0.1 g of sample, add 0.05 ml standard selenium solution and
proceed as above.
To each beaker add 2 g
hydrazinium sulfate and warm to dissolve. Let stand for 5 min. Let stand for
5 min. Dilute the contents of each beaker to 50 ml in a Nessler tube and
compare the colour of the two solutions. The sample should be less pink than
the sample with the added standard.
6.3. Method of essay
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Weigh 250 mg of the
sample, add to 50.0 ml of 0.1 N iodine in a glass stoppered flask, and
stopper the flask. Allow to stand for 5 min, add 1 ml of dilute hydrochloric
acid TS and titrate the excess iodine with 0.1 N sodium thiosulfate, using
starch TS as the indicator.
Each ml of 0.1 N
iodine is equivalent to 5.558 mg of K2S2O5.
ANNEX 15
SPECIFICATIONS
AND TESTS FOR POTASSIUM SULFITE
1. Synonyms
Potassium sulfite;
INS 225
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2. Definition
Chemical names
Potassium sulfite
C.A.S. number
10117-38-1
Chemical formula
K2SO3
Formula weight
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3. Description
White, odourless, granular powder.
4. Functional uses
Antibrowning agent,
antioxidant, preservative
5. Specifications
5.1. Identification
Solubility
Freely soluble in
water; slightly soluble in ethanol.
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Passes test.
Test for sulfite
Passes test.
5.2. Purity
Alkalinity
Between 0.25 and 0.45%
as K2CO3.
Iron
Not more than 10
mg/kg.
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Not more than 2 mg/kg.
Selenium
Not more than 5 mg/kg.
5.3. K2SO3 content
Not less than 90.0%.
6. Tests
6.1. Identification
Test for potassium
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Test for sulfite
Tested according to
JECFA monograph 1 - Vol. 4.
6.2. Purity
Alkalinity
Dissolve 1 g of the
sample in 20 ml of water and add 25 ml of 3% hydrogen peroxide, previously
neutralized to methyl red TS. Mix thoroughly, cool to room temperature, and
titrate with 0.02 N hydrochloric acid. Perform a blank
determination using 25 ml of neutralized hydrogen peroxide solution. Each ml
of 0.02 N hydrochloric acid is equivalent to 1.38 mg of K2CO3.
Iron
- Tested according to
JECFA monograph 1 - Vol. 4.
- Use 0.5 ml of Iron
Standard Solution (5 µg Fe) in the control.
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- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
Selenium
Reagents:
Hydrochloric acid,
hydrazinium sulfate, standard selenium solution (100 µg Se/ml)
Procedure:
Weigh 2.0 ± 0.1 g of
sample and transfer to a 50-ml beaker. Add 10 ml water, 5 ml hydrochloric
acid and boil to remove SO2.
Into a second beaker,
weigh 1.0 ± 0.1 g of sample, add 0.05 ml standard selenium solution and
proceed as above.
To each beaker add 2 g
hydrazinium sulfate and warm to dissolve. Let stand for 5 min. Let stand for
5 min. Dilute the contents of each beaker to 50 ml in a Nessler tube and
compare the colour of the two solutions. The sample should be less pink than
the sample with the added standard.
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Weigh accurately about
0.75 g of the sample and dissolve in a mixture of 100 ml of 0.1 N iodine and
5 ml of dilute hydrochloric acid TS. Titrate the excess iodine with 0.1 N
sodium thiosulfate, adding starch TS as the indicator.
Each ml of 0.1 N
iodine is equivalent to 7.912 mg of K2SO3.
ANNEX 16
SPECIFICATIONS
AND TESTS FOR NISIN
1. Synonyms
INS 234
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Nisin is a mixture of
closely related antimicrobial polypeptides produced by strains of Lactococcus
lactis subsp. lactis under appropriate fermentation conditions.
Nisin preparation
consists of nisin and sodium chloride with an activity of not less than 900
units per mg. Nisin preparation is stable at ambient temperatures and upon
heating under acid conditions (maximum stability at pH 3).
C.A.S. number
1414-45-5
Chemical formula
C143H230N42O37S7
Structural formula
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Dhb=dehydrobutyrine
Formula weight
Ca. 3354
3. Description
White to light brown
micronized powder
4. Functional uses
Antimicrobial
preservative
5. Specifications
5.1. Identification
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Solubility
Soluble in water and
insoluble in non-polar solvents
Differentiation from
other antimicrobial substances
Passes test.
5.2. Purity
Loss on drying
Not more than 3.0%
(105oC , 2 h)
Lead
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Microbiological
criteria
Salmonella species:
Absent in 25 g of sample
Total coliforms: Not
more than 30 per gram
Escherichia coli:
Absent in 25 g sample
5.3. Content
Not less than 900 IU
of nisin per milligram and not less than 50% sodium chloride
6. Tests
6.1. Identification
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- Stability to acid:
Suspend a 100-mg sample in 0.02 N hydrochloric acid as described in “Standard
stock solution” under Method of Assay. Boil this solution for 5 min.
Using the method of
assay described below, determine the nisin activity. No significant loss of
activity is noted following this heat treatment. The calculated nisin
concentration of the boiled sample is 100% +/- 5% of the assay value. Adjust
the pH of the nisin solution to 11.0 by adding 5N sodium hydroxide. Heat the
solution at 65° for 30 min, and then cool. Adjust the pH to 2.0 by adding
hydrochloric acid dropwise. Again determine the nisin concentration using the
assay method described below. Complete loss of the antimicrobial activity of
nisin is observed following this treatment.
- Tolerance of
Lactococcus lactis to high concentrations of nisin: Prepare cultures of
Lactococcus lactis (ATCC 11454, NCIMB 8586) in sterile skim m (<1% fat)
milk by incubating for 18 h at 30°. Prepare one or more flasks containing 100
ml of litmus milk, and sterilize at 121° for 15 min. Suspend 0.1 g of sample
in the sterilized litmus milk, and allow to stand at room temperature for 2
h. Add 0.1 ml of the L. lactis culture, and incubate at 30° for 24 h. L.
lactis will grow in this concentration of sample (about 1000 IU/ml); however,
it will not grow in similar concentrations of other antimicrobial substances.
This test will not differentiate nisin from subtilin.
6.2. Purity
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
6.2. Method of essay
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Determination of nisin
activity (Based on the method of Friedman and Epstein, J. Gen. Microbiol. 5:
830, 1951)
Preparation of the
test organism:
Lactococcus lactis
sbsp .cremoris (ATCC 14365, NCDO 495) is subcultured daily in sterile
separated milk by transferring one loopful to a McCartney bottle of litmus
milk and incubating at 30o. Prepare inoculated milk for the assay
by inoculating a suitable quantity of sterile skim milk with 2 percent of a
24 h culture, and place it in a water-bath at 30o for 90 min. Use
immediately.
Standard stock
solution:
Dissolve an accurately
weighed quantity of standard nisin in 0.02N hydrochloric acid to give a
solution containing 5 000 units/ml. Immediately before use, dilute the
solution further with 0.02N hydrochloric acid to give 50 units/ml. (NOTE:
Nisin preparation containing 2.5 % nisin, minimum potency of 10 6 IU/g,
obtainable from Sigma, St Louis, USA or Fluka, Buchs, Switzerland, may be
used for the Standard Stock Preparation, as well as, the preparation under
the name of Nisaplin, available from Danisco, Copenhagen, Dennmark).
Sample solution:
Weigh an amount of
sample sufficient to ensure that corresponding tubes of the sample and
standard series match, i.e. within close limits, the nisin content in the sample and standard is the same. Dilute the
sample solution in 0.02 N hydrochloric acid to give an estimated
concentration of 50 units of nisin per ml.
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Prepare a 0.0125%
solution of resazurin in water immediately before use.
Procedure:
Pipet graded volumes
(0.60, 0.55, 0.50, 0.45, 0.41, 0.38, 0.34, 0.31, 0.28, 0.26 ml) of the 50
unit per ml sample and standard solutions into rows of 10 dry 6-inches x
5/8-inch bacteriological test-tubes. Add 4.6 ml of the inoculated milk to
each by means of an automatic pipetting device. The addition of inoculated
milk is made in turn across each row of tubes containing the same nominal
concentration, not along each row of ten tubes. Place the tubes in a
water-bath at 30o for 15 min, then cool in an ice water bath while
adding 1 ml resazurin solution to each. The addition is made with an
automatic pipetting device, in the same order used for the addition of
inoculated milk. Thoroughly mix the contents of the tubes by shaking.
Continue incubation at 30o in a water-bath for a further 3-5 min.
Examine the tubes
under fluorescent light in a black matt-finish cabinet. The sample tube of
the highest concentration which shows the first clear difference in colour
(i.e. has changed from blue to mauve) is compared with tubes of the standard
row to find the nearest in colour. Make further matches at the next two lower
concentrations of the sample and standard. Interpolation of matches may be
made at half dilution steps. As the standard tubes contain known amounts of
nisin, calculate the concentration of nisin in the sample solution. Obtain
three readings of the solution and average them. Calculate the activity in
terms of IU per gram of preparation.
NaCl
Accurately weigh about
100 mg of sample, and transfer to a porcelain casserole. Add 100 ml water, 2
ml 2% dextrin soln, and 1 ml 0.1% dichlorofluoroscein soln. Mix, and titrate
with 0.1 N silver nitrate soln until the silver chloride flocculates and the
mixture acquires a faint pink colour.
Sodium chloride,%
(w/w):
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Where:
V is the volume of
silver nitrate solution consumed (ml)
N is the normality of
the silver nitrate solution
58.5 is the formula
weight of sodium chloride, and
W is the weight of the
sample (mg).
ANNEX 17
SPECIFICATIONS
AND TESTS FOR HEXAMETHYLENE TERTRAMINE
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Hexamethylenetertramine;
Hexamine; Methenamine
INS 239
ADI = 0 - 0.15 mg/kg
bw.
2. Definition
Chemical names
1,3,5,7-tetraazatricylo[3.3.1.13,7]-decan;
hexamethylen- tetramin
C.A.S. number
100-97-0
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C6H12N4
Structural formula
Formula weight
140.19
3. Description
Nearly odourless,
colourless lustrous crystals, or white crystalline powder.
4. Functional uses
Antimicrobial
preservative
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5.1. Identification
Solubility
Freely soluble in
water, soluble in ethanol.
Test for formaldehyde
Passes test.
Ammonium
Passes test.
5.2. Purity
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Loss on drying
Not more than 2.0%.
Sulfated ash
Not more than 0.05%.
Test for ammonia
Passes test (described
in “Tests”).
Lead
Not more than 2 mg/kg.
5.3. C6H12N4 content
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6. Tests
6.1. Identification
Test for formaldehyde
Heat a 1 in 10
solution of the sample with dilute sulfuric acid TS. Formaldehyde is
liberated, recognizable by its odour and by its darkening of paper moistened
with silver ammonium nitrate TS.
Ammonium
Tested according to
JECFA monograph 1 - Vol. 4.
6.2. Purity
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Tested according to
JECFA monograph 1 - Vol. 4. (over P2O5, 4 h).
Sulfated ash
Tested according to
JECFA monograph 1 - Vol. 4, Method I (Test 2 g of the sample).
Test for ammonia
Add 1 ml of Nessler's
reagent TS to 10 ml of a 5% solution of the sample. The mixture should not be
darker than a mixture of 1 ml of the reagent in 10 ml of water.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
6.3. Method of essay
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Weigh, to the nearest
0.1 mg, 1 g of the sample, previously dried for 4 h over phosphorus
pentoxide. Transfer into a beaker and add 40.00 ml of N sulfuric acid. Boil gently adding water from time to time, if necessary, until
the odour of formaldehyde is no longer perceptible. Cool, add 20 ml of water,
and methyl red TS and titrate the excess acid with N sodium hydroxide.
Each ml of N sulfuric
acid is equivalent to 35.05 mg of C6H12N4.
ANNEX 18
SPECIFICATIONS
AND TESTS FOR DIMETHYL DICARBONATE
1. Synonyms
Dimethyl dicarbonate;
DMDC, dimethyl pyrocarbonate
INS 242
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Chemical names
Dimethyl dicarbonate
C.A.S. number
004-525-33-1
Chemical formula
C4H6O5
Structural formula
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139.09
3. Description
Colourless liquid.
Caution: Corrosive to
eyes and skin and toxic by inhalation and ingestion; must be kept in a tightly sealed container to exclude moisture.
4. Functional uses
Preservative
5. Specifications
5.1. Identification
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Soluble in water with
decomposition; miscible with toluene.
Infrared absorption
The infrared spectrum
of the sample corresponds with the reference infrared spectrum below.
5.2. Purity
Dimethyl dicarbonate
Not more than 0.2%.
Lead
Not more than 2 mg/kg.
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Not less than 99.8%.
6. Tests
6.1. Purity
Dimethyl dicarbonate
Apparatus:
Gas chromatograph with
a flame ionization detector, equipped for capillary gas chromatography, and
inlet part for the "on column" technique (e.g., Carlo Erba
Fraktovap 4160, or Hewlett-Packard 5880 or 5792).
- Capillary: 50 m SE
30-D (internal diameter: 0,3 mm).
- Potentiometric
recorder, 1 mV.
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Operating conditions
Temperatures:
- Injection block:
Room temperature (approximately 25o)
- Detector: 200o.
- Capillary Tube:
Initial temperature 30o; Preliminary phase 5 min, Rate of ascent
40o/min; Final temperature 120o, Final phase 5 min.
Carrier gas:
- Preliminary
pressure: 3.0 bar (Helium)
- Capillary tubes:
Approx. 11 ml/min
- Make-up gas: 28
ml/min
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- Air: 300 ml/min
Recorder feed: 1
cm/min
Reagents:
Methylisobutylketone,
purest grade.
Procedure:
Accurately weigh about
10 g of the sample to the nearest mg (W1 mg) into a rolled rim vial. Add in a
quantity of dimethyl-isobutylketone (W2 mg), corresponding to the anticipated
dimethylcarbonate content. Seal the rolled rim vial, mix well and inject
0.002 ml.
Retention times:
dimethylcarbonate:
Approx. 2 min
methylisobutylketone:
Approx. 4.5 min
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Typical Chromatogram
in 7.2
Determine the peak
areas. Calculate the % of dimethyl carbonate from:
Where:
F1: peak area of
dimethylcarbonate
F2: peak area of the standard
K: a Correction Factor
for dimethylcarbonate
Remarks:
1. It should be noted
the DMDC is sensitive to moisture and heat.
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3. The correction
factor for dimethylcarbonate should be determined with corresponding test
solutions in DMDC which is to the greatest extent possible free of
dimethylcarbonate.
4. The specimen mixed
with the standard must be measured immediately
5. Hamilton syringes
with Metal needles can result in a partial decomposition of the DMDC.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- The selection of
sample size and method of sample preparation may be based on the principles
of the method described in JECFA monograph 1 -
Vol. 4, “Instrumental Methods.”
6.2. Method of essay
Introduce about 70 ml
of pure acetone into a 150-ml glass beaker. Using a disposable 2 ml syringe
weigh 1.0-1.3 g of the sample to an accuracy of ±0.1 mg into the glass
beaker. Pipette exactly 20 ml dibutyl amine solution (add chlorobenzene to
120 g dibutyl amine until the 1 L mark is reached) while stirring. Titrate
the solution potentiometrically with 1N hydrochloric acid. Run a blank test.
Calculate the % of
dimethyldicarbonate from:
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Where:
V1 = amount of
hydrochloric acid used for titration of the sample (ml)
V2 = amount of
hydrochloric acid used for titration of the blank (ml)
t = normality of
hydrochloric acid
W = weight of sample
(g)
7. Spectrum and chromatogram
7.1. Infrared spectrum
7.2. Typical chromatogram
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ANNEX 19
SPECIFICATIONS
AND TESTS FOR PROPIONIC ACID
1. Synonyms
Propionic acid;
propanoic acid; ethylformic acid; methylacetic
acid
INS 280
ADI “Not limited”
2. Definition
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Propionic acid
C.A.S. number
79-09-4
Chemical formula
C3H6O2
Structural formula
Formula weight
74.08
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An oily liquid with a
slightly pungent odour
4. Functional uses
Preservative,
antimould, antirope agent, flavouring agent
5. Specifications
5.1. Identification
Solubility
Miscible with water
and ethanol.
Specific gravity
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5.2. Purity
Distillation range
138.5 - 142.5o.
Non-volatile residue
Not more than 0.01%
when dried at 140o to constant weight
Formic acid
Not more than 0.1%.
Aldehydes
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Lead
Not more than 2 mg/kg.
5.3. C3H6O2 content
Not less than 99.5% on
dried basis.
6. Tests
6.1. Purity
Formic acid
Dissolve 15 g of
sodium hydroxide in 50 ml of water, cool, add 6 ml of bromine, stirring to
effect complete solution, and dilute to 2,000 ml with water. Transfer 25.0 ml
of this solution, into a 250 ml, glass-stoppered Erlenmeyer flask containing
100 ml of water, and add 10 ml of a 1 in 5 solution of sodium acetate and
10.0 ml of the sample. Allow to stand for 15 min, add 5 ml of a 1 in 4
solution of potassium iodide and 10 ml of hydrochloric acid, and titrate with
0.1 N sodium thiosulfate just to the disappearance of the brown
colour.Perform a blank determination. The difference between the volume of
0.1 N sodium thiosulfate required for the blank and that required for the
sample is not more than 4.4 ml.
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Transfer 10.0 ml of
the sample into a 250-ml glass-stoppered conical flask containing 50 ml of
water and 10.0 ml of a 1 in 8 solution of sodium bisulfite. Stopper the flask, and shake vigorously. Perform a blank
determination. Allow the mixture to stand for 30 min, then titrate with 0.1N
iodine to the same brownish yellow end-point obtained with a blank treated
with the same quantities of the same reagents. The difference between the
volume of 0.1N iodine required for the blank and that required for the sample
is not more than 7 ml.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
6.2. Method of essay
Mix 3 g of the sample,
weighed to the nearest 0.1 mg, with 50 ml of water in a 250-ml flask. Add
phenolphthalein TS, and titrate with 1N sodium hydroxide to the first
appearance of a faint pink end-point which persists for at least 30 sec.
Each ml of 1N sodium
hydroxide is equivalent to 74.08 mg of C3H6O2.
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ANNEX 20
SPECIFICATIONS
AND TESTS FOR SODIUM PROPIONATE
1. Synonyms
Sodium propionate;
Sodium propanoate;
INS 281
ADI “Not limited”
2. Definition
Chemical names
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C.A.S. number
137-40-6
Chemical formula
C3H5NaO2
Structural formula
Formula weight
96.06
3. Description
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4. Functional uses
Preservative,
antimould and antirope agent.
5. Specifications
5.1. Identification
Solubility
Freely soluble in
water, soluble in ethanol.
Test for sodium
Passes test.
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Passes test.
Test for alkali salt
of organic acid
Passes test.
5.2. Purity
Loss on drying
Not more than 4.0%.
pH
7.5 - 10.5 (1 in 10
soln).
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Not more than 0.1%.
Iron
Not more than 50.0
mg/kg.
Lead
Not more than 5 mg/kg.
5.3. C3H6NaO2 content
Not less than 99.0% on
the dried basis.
6. Tests
6.1. Identification
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Test for sodium
Tested according to
JECFA monograph 1 - Vol. 4.
Test for propionate
Warm the sample with
sulfuric acid. The propionic acid evolved may be recognized by its odour.
Test for alkali salt
of organic acid
Ignite the sample at a
relatively low temperature. The alkaline residue effervesces with acid.
6.2. Purity
Loss on drying
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Water-insoluble matter
Weigh 5 g of the
sample to the nearest mg, transfer into a 100-ml beaker and add 50 ml of
water. Stir until all the sample appears to be completely dissolved. Filter through a Gooch crucible, tared to an accuracy
of ± 0.2 mg. Rinse the beaker with 20 ml of water. Dry the crucible with its
contents in a 60º oven to constant weight. Cool in a desiccator, weigh, and
calculate as percentage.
Iron
- Tested according to
JECFA monograph 1 - Vol. 4.
- Test 0.5 g of the
sample as described in the Limit Test using 2.5 ml of Iron Standard Solution
(25 µg Fe) in the control.
Lead
- Tested according to
JECFA monograph 1 - Vol. 4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
6.3. Method of essay
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Weigh, to the nearest
mg, 3 g of the sample previously dried at 105º for 1 h, into a distillation
flask and add 200 ml of 50% phosphoric acid. Boil for 2 h and collect the
distillate. During distillation keep the volume in the flask at about 200 ml
by adding water using a dropping funnel. Titrate with 1N sodium hydroxide using phenolphthalein TS as indicator to the first appearance of
a faint pink end-point which persists for at least 30 sec.
Each ml of 1N sodium
hydroxide corresponds to 96.06 mg of C3H5NaO2.
ANNEX 21
SPECIFICATIONS
AND TESTS FOR SODIUM HYPOSULFITE
1. Synonyms
Sodium hyposulfite;
INS 539
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2. Definition
Chemical names
Sodium thiosulfate
C.A.S. number
7772-98-7
Chemical formula
Na2S2O3.5H2O
Formula weight
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3. Description
Colourless crystals or
coarse crystalline powder; deliquesces in moist air and effloresces in dry
air above 33o.
4. Functional uses
Antibrowning agent,
antioxidant, sequestrant
5. Specifications
5.1. Identification
Solubility
Very soluble in water;
insoluble in ethanol
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Passes test.
Test for sodium
Passes test.
Thiosulfate
Passes test.
5.2. Purity
Loss on drying
32-37% (40-45o
, 16 h, under vacuum).
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Not more than 10
mg/kg.
Selenium
Not more than 5 mg/kg.
Lead
Not more than 2 mg/kg.
5.3. Na2S2O3 content
Not less than 99.0% on
the dried basis.
6. Tests
6.1. Identification
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Reducing activity
To a 1 in 10 solution
of the sample add a few drops of iodine TS; the colour is discharged.
Test for sodium
Tested according to
JECFA monograph 1 - Vol. 4.
Thiosulfate
Tested according to
JECFA monograph 1 - Vol. 4.
6.2. Purity
Iron
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- Use 0.5 ml of Iron
Standard Solution (5 µg Fe) in the control.
Selenium
Reagents
Hydrochloric acid,
hydrazinium sulfate, standard selenium solution (100 µg Se/ml).
Procedure
Weigh 2 ± 0.1 g of
sample and transfer to a 50-ml beaker.
Into a second beaker,
weigh 1.0 ± 0.1 g of sample, add 0.05 ml standard selenium solution and
proceed as above.
To each beaker, add 10
ml water, 5 ml hydrochloric acid and boil to remove SO2; then add 2 g
hydrazinium sulfate and warm to dissolve. Dilute the contents of each beaker
to 50 ml in a Nessler tube and compare the colour of the two solutions. The
sample should be less pink than the sample with the added standard.
Lead
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- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol. 4,
“Instrumental Methods.”
6.3. Method of essay
Dissolve about 0.5 g
of the dried sample, accurately weighed, in 30 ml of water and titrate with
0.1 N iodine solution using starch TS as the indicator. Perform a blank
determination.
Each ml of 0.1 N
iodine is equivalent to 15.81 mg of Na2S2O3.
NATIONAL TECHNICAL REGULATION
QCVN 4-13:2010/BYT
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FOREWORD
QCVN 4- :2010/BYT is
developed by the Drafting Board for National technical regulation on food
additives and food processing aids, submitted by the Vietnam Food
Administration for approval and promulgated together with the Circular No.
44/2010/TT-BYT dated December 22, 2010 of the Minister of Health.
NATIONAL TECHNICAL REGULATION ON FOOD ADDITIVE - STABILIZER
I. GENERAL
1. Scope
This National technical
regulation (hereinafter referred to as “the Regulation”) provides for
specifications and regulatory requirements for quality, hygiene and safety of
stabilizers used as food additives.
2. Regulated entities
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2.1. Importers,
exporters, producers, traders and users of preservatives used as stabilizers
used as food additives (hereinafter referred to as “entities”).
2.2. Relevant regulatory
bodies.
3. Interpretation of
terms and acronyms:
3.1. “stabilizer” refers
to a food additive used for the purpose of maintaining the dispersion of two or
more ingredients in order to create uniformity of a product.
3.2. JECFA monograph 1 -
Vol. 4 (JECFA monographs 1 - Combined compendium of food additive
specifications; Joint FAO/WHO expert committee on food additives; Volume 4 -
Analytical methods, test procedures and laboratory solutions used by and
referenced in the food additive specifications; FAO, 2006) is developed by
JECFA and was published by FAO in 2006.
3.3. “C.A.S number”
(Chemical Abstracts Service) refers to registry numbers of chemical substances
identified by the American Chemical Society.
3.4. “TS” stands for
test solution.
3.5. “ADI” stands for
acceptable daily intake.
3.6. “MTDI” stands for
maximum tolerable daily intake.
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II. SPECIFICATIONS,
TESTS AND SAMPLING
1. Specifications and
tests for stabilizers are specified in the annexes to this Regulation as
follows:
1.1.
Annex 1:
Specifications and
tests for Polyvinylpyrrolidone
1.2.
Annex 2:
Specifications and
tests for calcium lactate
1.3.
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Specifications and
tests for potassium dihydrogen citrate
1.4.
Annex 4:
Specifications and
tests for disodium orthophosphate
1.5.
Annex 5:
Specifications and
tests for dispotasium orthophosphate
1.6.
Annex 6:
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1.7.
Annex 7:
Specifications and
tests for ammonium polyphosphate
1.8.
Annex 8:
Specifications and
tests for sodium hydrogen carbonate
1.9
Annex 9:
Specifications and
tests for potassium carbonate
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Annex 10:
Specifications and
tests for ammonium hydrogen carbonate
1.11
Annex 11:
Specifications and
tests for potassium chloride
1.12
Annex 12:
Specifications and
tests for monopotassium orthophosphate
2. Specifications and
tests for calcium lactate used as stabilizers are specified in QCVN 3-4
:2010/BYT promulgated together with the Circular No. 17/TT-BYT dated May 20,
2010 of the Minister of Health.
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4. Sampling adheres to
the guidelines in the Circular No. 16/2009/TT-BKHCN dated June 02, 2009 by the
Ministry of Science and Technology and relevant regulations of law.
III. REGULATORY
REQUIREMENTS
1. Declaration of
conformity
1.1. Stabilizers shall
be declared in accordance with the regulations set out in this Regulation.
1.2. Methods and
procedures for declaration of conformity shall comply with the Regulation on
certification and declaration of conformity with regulations and standards
under the Decision No. 24/2007/QĐ-BKHCN dated September 28, 2007 of the
Minister of Science and Technology and regulations of laws.
2. Inspection of
stabilizers
The quality, hygiene and
safety of stabilizers must be inspected in accordance with the regulations of
law.
IV. RESPONSIBILITIES OF
ENTITIES
1. Entities must declare
conformity according to the specifications mentioned in this Regulation,
register their declarations of conformity at the Vietnam Food Administration
and ensure the quality, hygiene and safety as declared.
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V. IMPLEMENTATION
1. The Vietnam Food
Administration shall preside over and cooperate with competent authorities
concerned to provide guidance on and organize the implementation of this
Regulation.
2. The Vietnam Food
Administration shall, according to its managerial duties, suggest amendments to
this Regulation to the Ministry of Health.
3. In the cases where
any of the international guidelines for tests and regulations of law referred
to in this Regulation is amended or replaced, the newest one shall apply.
ANNEX 1
SPECIFICATIONS
AND TESTS FOR POLYVINYLPYRROLIDONE
1. Synonyms
Povidone, PVP,
Polyvinylpyrrolidone
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ADI = 0-50 mg/kg
2. Definition
Chemical names
Polyvinylpyrolidone,
poly-[1-(2-oxo-1-pyrolidinyl)- ethylene]
C.A.S. number
9003-39-8
Chemical formula
(C6H9NO)n
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Formula weight
Lower molecular weight
range product: about 40000.
Higher molecular
weight range product: about 360000.
3. Description
White to tan powder;
supplied in two molecular weight forms; the molecular weight value is an
average molecular weight for the two forms.
4. Functional uses
Clarifying agent,
stabilizer, bodying agent, tableting adjunct, dispersing agent
5. Specifications
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Solubility
Soluble in water, in
ethanol and in chloroform; insoluble in ether
pH
3.0 - 7.0 (5% soln)
Precipitate formation
Passes test.
5.2. Purity
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Not more than 5%.
Relative viscosity
Between 1.188 and
1.325 for lower molecular weight product, and between 3.225 and 5.662 for higher
molecular weight product (See description under Tests).
Total ash
Not more than 0.02%.
Aldehydes
Not more than 0.2% (as
acetaldehyde)
Monomer content
Not more than 1% (as
vinylpyrrolidone) (see description under Tests)
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Not more than 1 mg/kg
(see description under Tests).
Lead
Not more than 2 mg/kg.
5.3. Nitrogen content
Not less than 12.2%
and not more than 13.0% of Nitrogen (N) on the anhydrous basis
6. Tests
6.1. Identification
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To 5 ml of a 1 in 50
solution of the sample add 5 ml of dilute hydrochloric acid TS, 5 ml of water
and 2 ml of 1 in 10 solution of potassium dichromate. A yellow precipitate
forms.
Add 5 ml of a 1 in 50
solution of the sample to 75 mg of cobalt nitrate and 0.3 g of ammonium thiocyanate
dissolved in 2 ml of water, mix and acidify with dilute hydrochloric acid TS.
A pale blue precipitate forms.
To 5 ml of a 1 in 50
solution of the sample add 1 ml of 25% hydrochloric acid and 5 ml of 5%
barium chloride solution and 1 ml of 5% phosphomolybdotungstic acid solution.
A voluminous white precipitate is formed which becomes gradually blue on
standing in daylight. (Note: The blue colouration on exposure to light
distinguishes polyvinylpyrrolidone from polyethylene oxide adducts which give
similar precipitates with the same reagents but which retain their white
colour in light).
6.2. Purity
Water
- Tested according to
JECFA monograph 1 - Vol.4.
- Karl Fischer Method.
Relative viscosity
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Transfer an accurately
weighed portion of the sample, equivalent to 1 g of anhydrous
polyvinylpyrrolidone, into a 250 ml conical flask, and calculate the amount
of water to be added to make a 1% solution. Allow the mixture to stand at
room temperature, with occasional swirling, until solution is complete, and
then allow to stand for 1 h. longer. Filter through a dry sintered-glass
filter funnel of coarse porosity, then pipet 10 ml of the filtrate into a
Cannon-Fenske viscometer, or equivalent, and place the viscometer in a water
bath maintained at 25±0.05oC. After allowing the sample solution
and pipet to warm in the water bath for 10 min., draw the solution by means
of very gentle suction up through the capillary until the meniscus is formed
from 3 to 4 mm above the upper etched mark. Release the vacuum, and, when the
meniscus reaches the upper etched mark, begin timing the flow through the
capillary. Record the exact time when the meniscus reaches the lower etched
mark, and calculate the flow time to the nearest 0.1 sec. Repeat this
operation until at least three readings are obtained. The readings must agree
within 0.3 sec.; if not, repeat the determination with additional 10 ml
portions of the sample solution after recleaning the viscosity pipet with
sulfuric acid-dichromate cleaning solution. Calculate the average flow time
for the sample solution, and then obtain the average flow time in similar
manner for 10 ml of filtered water for the same viscosity pipet. Calculate
the relative viscosity of the sample by dividing the average flow time for
the sample solution by that of the water sample.
Total ash
Test 10 g of the
sample.
Tested according to
JECFA monograph 1 - Vol.4
Aldehydes
Transfer about 10 g of
the sample, accurately weighed and dissolved in 300 ml of water, into a 1000
ml round-bottom flask containing 80 ml of 25% sulfuric acid, reflux for about
45 min. under a water-cooled condenser, and then distil about 100 ml into a
receiver containing 20 ml of 1 N hydroxylamine hydrochloride previously
adjusted to pH 3.1. Titrate the contents of the receiver with 0.1 N sodium
hydroxide to a pH of 3.1, using a pH meter. Perform a blank determination and
make any necessary correction.
Each ml of 0.1 N
sodium hydroxide is equivalent to 4.405 mg of C2H4O.
Monomer content
Dissolve about 4 g of
the sample, accurately weighed, in 30 ml of water in a 125 ml round-bottom
flask, add 0.5 g of sodium acetate, mix and begin titrating with 0.1 N
iodine. When the iodine colour no longer fades, add additional 3.0 ml of the
titrant, and allow the solution to stand for 5 to 10 min. Add starch TS, and
titrate the excess iodine with 0.1 N sodium thiosulfate. Perform a blank
determination, using the same volume of 0.1 N iodine, accurately measured, as
was used for the sample.
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Hydrazine
Transfer 2.5 g of the
sample into a 50-ml centrifuge tube, add 25 ml of a 1 in 20 solution of
salicylaldehyde in methanol, swirl, and heat in a water bath at 60oC
for 15 min. Allow to cool, add 2.0 ml of toluene, insert a stopper in the
tube, shake vigorously for 2 min, and centrifuge. On a suitable thin-layer
chromatographic plate, coated with a 0.25-mm layer of dimethylsilanized
chromatographic silica gel mixture, apply 10 µl of the clear upper toluene
layer in the centrifuge tube and 10 µl of a Standard solution of
salicylaldazine in toluene containing 9.38 µg per ml. Allow the spots to dry,
and develop the chromatogram in a solvent system of methanol and water (2:1)
until the solvent front has moved about three-fourths of the length of the
plate. Remove the plate from the developing chamber, mark the solvent front,
and allow the solvent to evaporate. Locate the spots on the plate by
examination under ultraviolet light at a wavelength of 365 nm:
salicylaldazine appears as a fluorescent spot having an Rf value of about
0.3, and the fluorescence of any salicylaldazine spot from the test specimen
is not more intense than that produced by the spot obtained from the Standard
solution (1 ppm of hydrazine).
Preparation of
Salicylaldazine Standard: Dissolve 300 mg of
hydrazine sulfate in 5 ml of a freshly prepared 20% (v/v) solution of
salicylaldehyde in isopropyl alcohol, mix, and allow to stand until a yellow
precipitate forms. Extract the mixture with two 15-ml portions of methylene
chloride. Combine the methylene chloride extracts, and dry over anhydrous
sodium sulfate. Decant the methylene chloride solution, and evaporate it to
dryness. Recrystallize the residue of salicyclaldazine from a mixture of warm
toluene and methanol (60:40) with cooling; filter and dry the crystals in vacuum. The crystals have a melting range of 213o
C to 214o C.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Determine as directed
under Nitrogen Determination in Volume 4, using about 1 g of the sample,
accurately weighed.
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SPECIFICATIONS
AND TESTS FOR CALCIUM LACTATE
1. Synonyms
INS 327
ADI “Not limited”
2. Definition
Chemical names
Calcium dilactate,
calcium dilactate hydrate, 2-Hydroxypropanoic acid calcium salt
C.A.S. number
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Chemical formula
C6H10CaO6.xH2O (x = 0
- 5)
Structural formula
Formula weight
218.22 (anhydrous)
3. Description
White to cream
coloured, almost odourless, crystalline powder or granules. The pentahydrate
is somewhat efflorescent.
4. Functional uses
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5. Specifications
5.1. Identification
Solubility
Soluble in water;
insoluble in ethanol.
Lactate
Passes test.
Test for calcium
Passes test.
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Loss on drying
Not more than 30%
pH
6.0-8.0 (1 in 20
soln).
Acidity
Passes test (described
in “Tests”).
Magnesium and alkali
salts
Not more than 1%.
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Not more than 30
mg/kg.
Lead
Not more than 2 mg/kg.
5.3. C6H10CaO6 content
Not less than 98.0% on
the dried basis.
6. Tests
6.1. Identification
Lactate
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Test for calcium
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Loss on drying
- Tested according to
JECFA monograph 1 - Vol.4.
- 120o, 4
h.
Acidity
Dissolve 1 g of the
sample in 20 ml of water, add 3 drops of phenolphthalein TS, and titrate with
0.1 N sodium hydroxide. Not more than 0.5 ml should be required.
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Dissolve 1 g of the
sample in 40 ml of water, add 0.5 g of ammonium chloride, boil, and add about
20 ml of ammonium oxalate TS. Heat the solution on a water bath for 1 h,
cool, add water to 100 ml, and filter. To 50 ml of the filtrate, add 0.5 ml
of sulfuric acid, evaporate to dryness, and ignite to constant weight. Cool,
weigh and calculate as percentage. The weight of the residue should not
exceed 5 mg.
Fluoride
- Tested according to
JECFA monograph 1 - Vol.4.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Dissolve about 350 mg
of previously dried sample, accurately weighed, in 150 ml of water containing
2 ml of dilute hydrochloric acid TS. While stirring, preferably with a
magnetic stirrer, add about 30 ml of 0.05 M disodium
ethylenediaminetetraacetate from a 50-ml buret. Then add 15 ml of sodium
hydroxide TS and 300 mg of hydroxy-naphthol blue indicator, and continue the
titration to a blue end-point.
Each ml of 0.05 M
disodium ethylenediaminetetraacetate is equivalent to 10.91 mg of C6H10CaO6.
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ANNEX 3
SPECIFICATIONS
AND TESTS FOR POTASSIUM DIHYDROGEN CITRATE
1. Synonyms
Monopotassium citrate,
potassium citrate monobasic
INS 332i
ADI “Not limited”
2. Definition
Chemical names
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C.A.S. number
866-83-1
Chemical formula
C6H7KO7
Structural formula
Formula weight
230.21
3. Description
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4. Functional uses
Buffering agent,
sequestrant, yeast food.
5. Specifications
5.1. Identification
Solubility
Freely soluble in
water; very slightly soluble in ethanol.
pH
3.5 - 3.9 (1 in 10
soln).
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Passes test.
Test for potassium
Passes test.
5.2. Purity
Loss on drying
Not more than 0.5%
(105º, 4 h).
Oxalate
Not more than 0.04%.
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Not more than 2 mg/kg.
5.3. C6H7NaO7 content
Not less than 99.0%
and not more than the equivalent of 101.0% on the dried basis.
6. Tests
6.1. Identification
Citrate
Tested according to
JECFA monograph 1 - Vol.4.
Test for potassium
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6.2. Purity
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Dissolve about 180 mg
of the dried sample, accurately weighed in 25 ml of water and titrate with
0.1 N sodium hydroxide (potentiometric end-point determination).
Each ml of 0.1 N
sodium hydroxide is equivalent to 11.511 mg of C6H7KO7.
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SPECIFICATIONS
AND TESTS FOR POTASSIUM DIHYDROGEN PHOSPHATE
1. Synonyms
Disodium hydrogen
phosphate; Disodium phosphate; Dibasic sodium phosphate; Disodium acid
phosphate; secondary sodium phosphate; Dinatri orthophosphate
INS 339ii
MTDI=70mg/kg bw as
phosphorus from all food sources
2. Definition
Chemical names
Disodium hydrogen
phosphate; disodium hydrogen orthophosphate; disodium hydrogen monophosphate;
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7558-79-4
Chemical formula
Anhydrous: Na2HPO4
Hydrated: Na2HPO4.xH2O
Formula weight
141.98 (anhydrous)
3. Description
Anhydrous: White,
hygroscopic, odourless powder.
Dihydrate: White
crystalline, odourless solid.
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Dodecahydrate: White,
efflorescent, odourless powder or crystals.
4. Functional uses
Emulsifier,
texturizer, buffer
5. Specifications
5.1. Identification
Solubility
Freely soluble in water;
insoluble in ethanol.
pH
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Test for sodium
Passes test.
Test for phosphate
Passes test.
Test for
orthophosphate
Passes test.
5.2. Purity
Loss on drying
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Dihydrate: Not more
than 22.0% (40oC, 3 h, then 105oC , 5 h)
Heptahydrate: Not more
than 50.0% (40oC , 3 h, then 105oC , 5 h)
Dodecahydrate: Not
more than 61.0% (40oC , 3 h, then 105oC , 5 h)
Water insoluble matter
Not more than 0.2%.
Fluoride
Not more than 50.0
mg/kg.
Arsenic
Not more than 3.0
mg/kg.
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Not more than 4.0
mg/kg.
5.3. Na2HPO4 content
Not less than 98.0% on
the dried basis.
6. Tests
6.1. Identification
Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Test for phosphate
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Test for
orthophosphate
Dissolve 0.1 g of the
sample in 10 ml water. Acidify slightly with dilute acetic acid TS, and add 1
ml of silver nitrate TS. A yellow precipitate is formed.
6.2. Purity
Fluoride
Tested according to
JECFA monograph 1 - Vol. Vol.4, Method I or III.
Arsenic
Tested according to
JECFA monograph 1 - Vol. Vol.4, Method II.
Lead
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- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Into a 250-ml beaker
transfer about 6.5 g of the dried sample accurately weighed. Add 50 ml of 1N
hydrochloric acid and 50 ml of water, and stir until the sample is completely
dissolved. Place the electrodes of a suitable pH meter in the solution and
titrate the excess acid with 1N sodium hydroxide to the inflection point
occurring at about pH 4. Record the buret reading and calculate the volume
(A) of 1N hydrochloric acid consumed by the sample. Continue the titration
with 1N sodium hydroxide until the inflection point occurring at about pH 8.8
is reached, record the buret reading, and calculate the volume (B) of 1N
sodium hydroxide required in the titration between the two inflection points
(pH 4 to pH 8.8).
When (A) is equal to,
or less than, (B), each ml of the volume (A) of 1N hydrochloric acid is
equivalent to 142.0 mg of Na2HPO4.
When (A) is greater
than (B), each ml of the volume 2(B) -(A) of 1N sodium hydroxide is
equivalent to 142.0 mg of Na2HPO4.
ANNEX 5
SPECIFICATIONS
AND TESTS FOR DIPOTASSIUM HYDROGEN PHOSPHATE
1. Synonyms
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INS 340ii
MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
Chemical names
Dipotassium
hydrogenphosphate; dipotassium hydrogen orthophosphate; dipotassium hydrogen
monophosphate
C.A.S. number
7758-11-4
Chemical formula
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Formula weight
174.18
3. Description
Colourless or white
granular powder, crystals or masses; deliquescent
4. Functional uses
Buffering agent,
sequestrant, yeast food
5. Specifications
5.1. Identification
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Freely soluble in
water; insoluble in ethanol.
pH
8.7-9.3 (1 in 100
soln).
Test for potassium
Passes test.
Test for phosphate
Passes test.
Test for
orthophosphate
Passes test.
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Loss on drying
Not more than 5% (105oC
, 4 h).
Water insoluble matter
Not more than 0.2%.
Fluoride
Not more than 10
mg/kg.
Arsenic
Not more than 3.0
mg/kg.
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Not more than 4.0 mg/kg.
5.3. K2HPO4 content
Not less than 98.0% on
the dried basis.
6. Tests
6.1. Identification
Test for potassium
Tested according to
JECFA monograph 1 - Vol.4.
Test for phosphate
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Test for
orthophosphate
Dissolve 0.1 g of the
sample in 10 ml water, acidify slightly with dilute acetic acid TS, and add 1
ml of silver nitrate TS. A yellow precipitate is formed.
6.2. Purity
Fluoride
Place 5 g of the
sample, 25 ml of water, 50 ml of perchloric acid, 5 drops of silver nitrate
solution (1 in 2), and a few glass beads in a 250-ml distilling flask
connected with a condenser and carrying a thermometer and a capillary tube,
both of which must extend into the liquid. Connect a small dropping funnel,
filled with water, or a steam generator, to the capillary tube. Support the
flask on an asbestos mat with a hole which exposes about one-third of the
flask to the flame. Distil into a 250-ml flask until the temperature reaches
135oC. Add water from the funnel or introduce steam through the
capillary to maintain the temperature between 135oC and 140oC.
Continue the distillation until 225-240 ml has been collected, then dilute to
250 ml with water, and mix. Place a 50-ml aliquot of this solution in a
100-ml Nessler tube. In another similar Nessler tube place 50 ml of water as
a control. Add to each tube 0.1 ml of a filtered solution of sodium
alizarinsulfonate (1 in 1000) and 1 ml of freshly prepared hydroxylamine
solution (1 in 4000), and mix well. Add, drop wise, and with stirring, 0.05 N
sodium hydroxide to the tube containing the distillate until its colour just
matches that of the control, which is faintly pink. Then add to each tube
exactly 1 ml of 0.1 N hydrochloric acid, and mix well. From a buret,
graduated in 0.05 ml, add slowly to the tube containing the distillate enough
thorium nitrate solution (1 in 4000) so that, after mixing, the colour of the
liquid just changes to a faint pink. Then add to each tube exactly 1 ml of
0.1 N hydrochloric acid, and mix well. Now add to the control sodium fluoride
TS (10 µg F per ml) from a buret to make the colours of the two tubes match
after dilution to the same volume. Mix well, and allow all air bubbles to
escape before making the final colour comparison. Check the end-point by
adding 1 or 2 drops of sodium fluoride TS to the control. A distinct change
in colour should take place. Note the volume of sodium fluoride added. The
volume of sodium fluoride TS required for the control solution should not
exceed 1 ml.
Arsenic
Tested according to
JECFA monograph 1 - Vol. Vol.4- Method II.
Lead
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- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Into a 250-ml beaker
transfer about 6.5 g of the dried sample, accurately weighed. Add 50 ml of 1
N hydrochloric acid and 50 ml of water, and stir until the sample is
completely dissolved. Place the electrodes of a suitable pH meter in the
solution and titrate the excess acid with 1N sodium hydroxide to the
inflection point occurring at about pH 4. Record the buret
reading and calculate the volume (A) of 1N hydrochloric acid consumed by the
sample. Continue the titration with 1N sodium hydroxide until the inflection
point occurring at about pH 8.8 is reached, record the buret reading, and
calculate the volume (B) of 1 N sodium hydroxide required in the titration
between the two inflection points (pH 4 to pH 8.8).
When (A) is equal to,
or less than, (B), each ml of the volume (A) of 1N hydrochloric acid is
equivalent to 174.2 mg of K2HPO4.
When (A) is greater
than (B), each ml of the volume 2(B) - (A) of 1N sodium hydroxide is
equivalent to 174.2 mg of K2HPO4.
ANNEX 6
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1. Synonyms
Calcium phosphate,
tribasic; precipitated calcium phosphate;
INS 341iii
MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
Consists of a variable
mixture of calcium phosphates having and approximate composition of
10CaO.3P2O5.H2O. The article of commerce can be specified further as to
titration value.
3. Description
White, odourless
powder which is stable in air.
4. Functional uses
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5. Specifications
5.1. Identification
Solubility
Practically insoluble
in water; insoluble in ethanol, soluble in dilute hydrochloric and nitric
acid.
Test for calcium
Passes test.
Test for phosphate
Passes test.
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Loss on ignition
Not more than 10%
after ignition at 825oC to constant weight.
Fluoride
Not more than 50
mg/kg.
Lead
Not more than 4 mg/kg.
5.3. Ca3(PO4)2 content
Not less than the
equivalent of 90% of Ca3(PO4)2, calculated on the ignited basis.
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6.1. Identification
Test for calcium
Dissolve about 100 mg
of the sample by warming with 5 ml of dilute hydrochloric acid TS and 5 ml of
water. Add 1 ml of ammonia TS, dropwise, with shaking, and then add 5 ml of
ammonium oxalate TS. A white precipitate is formed.
Test for phosphate
To a warm solution of
the sample in a slight excess of nitric acid add ammonium molybdate TS. A
yellow precipitate forms.
6.2. Purity
Fluoride
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Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Weigh 200 mg of the
sample to the nearest 0.1 mg and dissolve in a mixture of 25 ml of water and
10 ml of dilute nitric acid TS. Filter, if necessary, wash any precipitate,
add sufficient ammonia TS to the filtrate to produce a slight precipitate,
then dissolve the precipitate with the addition of 1 ml of dilute nitric acid
TS. Adjust the temperature to about 50o, add 75 ml of ammonium
molybdate TS, and maintain the temperature at about 50o for 30
min, stirring occasionally. Wash the precipitate once or twice with water by
decantation, using from 30 to 40 ml each time. Transfer the precipitate to a
filter, and wash with a 1 in 100 potassium nitrate solution until the last
washing is not acid to litmus paper. Transfer the precipitate and filter to
the precipitation vessel, add 40.0 ml of N sodium hydroxide, agitate until
the precipitate is dissolved, add 3 drops of phenolphthalein TS, and then
titrate the excess alkali with N sulfuric acid.
Each ml of N sodium
hydroxide corresponds to 6.743 mg of Ca3(PO4)2.
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SPECIFICATIONS
AND TESTS FOR AMMONIUM POLYPHOSPHATE
1. Synonyms
INS 452v
MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
Chemical names
Ammonium polyphosphate
C.A.S. number
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Chemical formula
Heterogeneous mixture
of ammonium salts of linear condensed polyphosphoric acids of general formula
Hn+2PnO3n+1
3. Description
Aqueous solution
4. Functional uses
Stabilizer,
sequestrant, emulsifier
5. Specifications
5.1. Identification
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Freely soluble in
water
pH
4.0 - 9.0 (1% soln)
Test for ammonium
Passes test.
Test for phosphate
Passes test.
5.2. Purity
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Not more than 8%
calculated as P2O5 content
Fluoride
Not more than 10 mg/kg
Arsenic
Not more than 3 mg/kg
Lead
Not more than 4 mg/kg.
5.3. Content
Not less than 55.0%
and not more than 75.0% on an anhydrous basis, calculated as P2O5
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6.1. Identification
Ammonium
Tested according to
JECFA monograph 1 - Vol.4.
Test for phosphate
- Test a solution
resulting from mixing 0.5 g of sample with 10 ml of nitric acid and 50 ml of
water, boiled for 30 min and cooled.
- Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
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Cyclic phosphate
Tested according to
JECFA monograph 1 - Vol.4.
Fluoride
Tested according to
JECFA monograph 1 - Vol.4.
Arsenic
Tested according to
JECFA monograph 1 - Vol.4.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
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Proceed as directed
under “Phosphate Determination as P2O5”, Method I, in Volume 4.
ANNEX 8
SPECIFICATIONS
AND TESTS FOR SODIUM HYDROGEN CARBONATE
1. Synonyms
Baking soda,
bicarbonate of soda, sodium bicarbonate
INS 500(ii)
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2. Definition
Chemical names
Sodium hydrogen
carbonate, sodium acid carbonate
C.A.S. number
144-55-8
Chemical formula
NaHCO3
Formula weight
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3. Description
Colourless, white,
crystalline masses or crystalline powder
4. Functional uses
Stabilizer, alkali,
raising agent, buffer, leavening agent
5. Specifications
5.1. Identification
Solubility
Soluble in water;
insoluble in ethanol.
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8.0 - 8.6 (1 in 100
soln of the sample in cold water without shaking)
Test for sodium
Passes test.
Test for carbonate
Passes test.
5.2. Purity
Loss on drying
Not more than 0.25%
(over silica gel, 4 h).
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Passes test (described
in “Tests”).
Ammonium salts
Passes test (described
in “Tests”).
Lead
Not more than 2 mg/kg.
5.3. NaHCO3 content
Not less than 99.0%
after drying
6. Tests
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Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Test for carbonate
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Water insoluble matter
1 g of the sample
dissolves completely in 20 ml of water and gives a clear solution.
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Heat 1 g of the sample
in a test tube. No odour of ammonia is detected.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Weigh accurately about
3 g of the dried sample, add methyl orange TS and titrate with 1 N sulfuric
acid.
Each ml of 1 N
sulfuric acid is equivalent to 84.01 mg of NaHCO3.
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ANNEX 9
SPECIFICATIONS
AND TESTS FOR POTASSIUM CARBONATE
1. Synonyms
INS 501(i)
ADI “Not limited”
2. Definition
Chemical names
Potassium carbonate,
potassium salt of carbonic acid
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584-08-7
Chemical formula
Anhydrous: K2CO3
Hydrated: K2CO3.1½H2O
Formula weight
138,21 (anhydrous)
3. Description
White, odourless, very
deliquescent powder. The hydrated form occurs as small, white, translucent
crystals or granules.
4. Functional uses
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5. Specifications
5.1. Identification
Solubility
Very soluble in water;
insoluble in ethanol.
Test for potassium
Passes test.
Test for carbonate
Passes test.
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Loss on drying
Anhydrous: Not more
than 5% (180o, 4 h)
Hydrated forms:
Between 10% and 18% (180o, 4 h)
Lead
Not more than 2 mg/kg.
5.3. K2CO3 content
Not less than 99.0%
after drying.
6. Tests
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Test for potassium
Tested according to
JECFA monograph 1 - Vol.4.
Test for carbonate
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
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6.3. Method of essay
Weigh accurately about
1 g of the dried sample. Dissolve carefully in 50 ml of 1 N sulfuric acid,
add methyl orange TS and titrate the excess acid with 1 N sodium hydroxide.
Each ml of 1 N
sulfuric acid is equivalent to 69.11 mg of K2CO3.
ANNEX 10
SPECIFICATIONS
AND TESTS FOR AMMONIUM HYDROGEN CARBONATE
1. Synonyms
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INS 503(ii)
ADI “Not limited”
2. Definition
Chemical names
Ammonium hydrogen
carbonate
C.A.S. number
1066-33-7
Chemical formula
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Structural formula
NH4HCO3
Formula weight
79.06
3. Description
White crystals or a
crystalline powder with a slight odour of ammonia.
4. Functional uses
Stabilizer, raising
agent.
5. Specifications
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Solubility
Freely soluble in
water, insoluble in ethanol
pH
About 8 (1 in 20
soln).
Test for carbonate
Passes test.
Ammonium
Passes test.
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When heated, it
volatilizes without charring and the vapour is alkaline to moist litmus.
5.2. Purity
Non-volatile residue
Not more than 500
mg/kg (Test 4 g of the sample in 10 ml of water)
Chlorides
Not more than 30 mg/kg
(see description under Tests).
Sulfates
Not more than 70 mg/kg
(see description under Tests).
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Not more than 2 mg/kg
(see description under Tests).
5.3. NH4CO3 content
Not less than 99.0%.
6. Tests
6.1. Identification
Test for carbonate
Tested according to
JECFA monograph 1 - Vol.4.
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Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Chlorides
- Tested according to
JECFA monograph 1 - Vol.4.
- Dissolve 500 mg of
the sample in 10 ml of hot water, add about 5 mg of sodium carbonate, and
evaporate to dryness on a steam bath. Test the residue as directed under the
Limit Test. Any turbidity produced does not exceed that shown in a control
containing 15 µg of chloride ion (Cl- ).
Sulfates
Dissolve 4 g of the
sample in 40 ml of water, add about 10mg of sodium carbonate and 1 ml of 30%
hydrogen peroxide, and evaporate the solution to dryness on a steam bath.
Treat the residue as directed under the Limit Test. Any turbidity produced
does not exceed that shown in a control containing 280 µg of sulfate ion (SO4
2-).
Lead
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- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Place about 10 ml of
water in a weighing bottle, tare the bottle and its contents, add about 2 g
of the sample and weigh accurately. Transfer the contents of the bottle to a
250-ml flask and slowly add, with mixing, 50 ml of 1 N sulfuric acid. When
solution has been effected, wash down the sides of the flask, add methyl
orange TS, and titrate the excess acid with 1 N sodium hydroxide.
Each ml of 1 N
sulfuric acid is equivalent to 79.06 mg of NH4HCO3.
ANNEX 11
SPECIFICATIONS
AND TESTS FOR POTASSIUM CHLORIDE
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Sylvite; Sylvine
INS 508
ADI “Not limited”
2. Definition
Chemical names
Potassium chloride
C.A.S. number
7447-40-7
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KCl
Formula weight
74.56
3. Description
Colourless, elongated,
prismatic, or cubital crystals, or white granular powder; odourless.
4. Functional uses
Stabilizer, seasoning
agent, gelling agent, yeast food
5. Specifications
5.1. Identification
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Solubility
Freely soluble in
water; insoluble in ethanol.
Test for chloride
Passes test.
Test for potassium
Passes test.
5.2. Purity
Loss on drying
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Acidity or alkalinity
Passes test (described
in “Tests”).
Iodide or bromide
Passes test (described
in “Tests”).
Test for sodium
Negative test
(described in “Tests”).
Lead
Not more than 2 mg/kg.
5.3. KCl content
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6. Tests
6.1. Identification
Chlorides
Tested according to
JECFA monograph 1 - Vol.4.
Potassium
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
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To a solution of 5 g
of the sample in 50 ml of recently boiled and cooled water add 3 drops of
phenolphthalein TS. No pink colour is produced. Then add 0.3 ml of 0.02 N
sodium hydroxide. A pink colour is
produced.
Iodide or bromide
Dissolve 2 g of the
sample in 6 ml of water, add 1 ml of chloroform, and then add, dropwise and
with constant agitation, 5 ml of a mixture of equal parts of chlorine TS and
water. The chloroform is free from even a transient violet or permanent
orange colour.
Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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Dissolve about 250 mg
of the dried sample, accurately weighed in 50 ml of water in a
glass-stoppered flask. Add, while agitating, 50 ml of 0.1 N silver nitrate, 3
ml of nitric acid, and 5 ml of nitrobenzene, shake vigorously, add 2 ml of
ferric ammonium sulfate TS, and titrate the excess silver nitrate with 0.1 N
ammonium thiocyanate.
Each ml of 0.1 N
silver nitrate is equivalent to 7.456 mg of KCl.
ANNEX 12
SPECIFICATIONS
AND TESTS FOR POTASSIUM DIHYDROGEN PHOSPHATE
1. Synonyms
Potassium dihydrogen
phosphate; Monobasic potassium phosphate; Monopotassium monophosphate;
Potassium acid phosphate; Potassium biphosphate
INS 340i
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2. Definition
Chemical names
Potassium
dihydrogenphosphate, monopotassium dihydrogenorthophosphate, monopotassium
dihydrogen monophosphate
C.A.S. number
7778-77-0
Chemical formula
KH2PO4
Formula weight
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3. Description
Odourless, colourless
crystals or white granular or crystalline powder
4. Functional uses
Stabilizer, buffer,
neutralizing agent, sequestrant, yeast food
5. Specifications
5.1. Identification
Solubility
Freely soluble in
water; insoluble in ethanol.
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4.2 - 4.7 (1 in 100
soln).
Test for potassium
Passes test.
Test for phosphate
Passes test.
Test for
orthophosphate
Passes test.
5.2. Purity
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Not more than 2% (105o,
4 h).
Water insoluble matter
Not more than 0.2%.
Fluoride
Not more than 10
mg/kg.
Arsenic
Not more than 3.0
mg/kg.
Lead
Not more than 4.0
mg/kg.
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Not less than 98.0% on
the dried basis.
6. Tests
6.1. Identification
Test for potassium
Tested according to
JECFA monograph 1 - Vol.4.
Test for phosphate
Tested according to
JECFA monograph 1 - Vol.4.
Test for
orthophosphate
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6.2. Purity
Fluoride
Place 5 g of the
sample, 25 ml of water, 50 ml of perchloric acid, 5 drops of silver nitrate
solution (1 in 2), and a few glass beads in a 250-ml distilling flask
connected with a condenser and carrying a thermometer and a capillary tube,
both of which must extend into the liquid.Support the flask on an asbestos
mat with a hole which exposes about one-third of the flask to the flame.
Distil into a 250-ml flask until the temperature reaches 135o. Add
water from the funnel or introduce steam through the capillary to maintain
the temperature between 135o and 140o. Continue the
distillation until 225-240 ml has been collected, then dilute to 250 ml with
water, and mix. Place a 50-ml aliquot of this solution in a 100-ml Nessler
tube. In another similar Nessler tube place 50 ml of water as a control. Add
to each tube 0.1 ml of a filtered solution of sodium alizarinsulfonate (1 in
1000) and 1 ml of freshly prepared hydroxylamine solution (1 in 4000), and
mix well. Add, dropwise, and with stirring, 0.05 N sodium hydroxide to the
tube containing the distillate until its colour just matches that of the
control, which is faintly pink. Then add to each tube exactly 1 ml of 0.1 N
hydrochloric acid, and mix well. From a buret, graduated in 0.05 ml, add
slowly to the tube containing the distillate enough thorium nitrate solution
(1 in 4000) so that, after mixing, the colour of the liquid just changes to a
faint pink. Then add to each tube exactly 1 ml of 0.1 N hydrochloric acid,
and mix well. Now add to the control sodium fluoride TS (10 µg F per ml) from
a buret to make the colours of the two tubes match after dilution to the same
volume. Mix well, and allow all air bubbles to escape before making the final
colour comparison. Check the end-point by adding 1 or 2 drops of sodium
fluoride TS to the control. A distinct change in colour should take place.
Note the volume of sodium fluoride added. A distinct change in colour should
take place. Note the volume of sodium fluoride added.
The volume of sodium
fluoride TS required for the control solution should not exceed 1 ml.
Arsenic
Tested according to
JECFA monograph 1 - Vol. Vol.4, Method II.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
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6.3. Method of essay
Transfer about 5 g of
the dried sample, accurately weighed, into a 250-ml beaker. Add 100 ml of
water and 5 ml of 1 N hydrochloric acid, and stir until the sample is
completely dissolved. Place the electrodes of a suitable pH meter in the
solution, and slowly titrate the excess acid, stirring constantly, with 1 N
sodium hydroxide to the inflection point occurring at about pH 4. Record the
buret reading, and calculate the volume (A), if any, of 1 N hydrochloric acid
consumed by the sample. Continue the titration with 1 N sodium hydroxide
until the inflection point occurring at about pH 8.8 is reached, record the
buret reading, and calculate the volume (B) of 1 N sodium hydroxide required
in the titration between the two inflection points (pH 4 and pH 8.8).
Each ml of the volume
(B) - (A) of 1 N sodium hydroxide is equivalent to 136.1 mg of KH2PO4.
ON FOOD ADDITIVE – PROPELLANT
Foreword
QCVN 4- :2010/BYT is
developed by the Drafting Board for National technical regulation on food
additives and food processing aids, submitted by the Vietnam Food Administration
for approval and promulgated together with the Circular No. 44/2010/TT-BYT
dated December 22, 2010 of the Minister of Health.
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I. GENERAL
1. Scope
This National technical
regulation (hereinafter referred to as “the Regulation”) provides for
specifications and regulatory requirements for quality, hygiene and safety of
sequestrants used as food additives.
2. Regulated entities
This Regulation applies
to:
2.1. Importers,
exporters, producers, traders and users of preservatives used as sequestrants
used as food additives (hereinafter referred to as “entities”).
2.2. Relevant regulatory
bodies.
3. Interpretation of
terms and acronyms:
3.1. “sequestrant”
refers to a food additive used for the purpose of controlling the availability
of a cation in food.
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3.3. “C.A.S number”
(Chemical Abstracts Service) refers to registry numbers of chemical substances
identified by the American Chemical Society.
3.4. “TS” stands for
test solution.
3.5. “ADI” stands for
acceptable daily intake.
3.6. “MTDI” stands for
maximum tolerable daily intake.
3.7. “INS” stands for
international numbering system.
II. SPECIFICATIONS,
TESTS AND SAMPLING
1. Specifications and
tests for sequestrants are specified in the annexes to this Regulation as
follows:
1.1.
Annex 1:
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1.2.
Annex 2:
Specifications and
tests for calcium disodium ethylenediaminetetraacetate
1.3.
Annex 3:
Specifications and
tests for disodium ethylenediaminetetraacetate
1.4.
Annex 4:
Specifications and
tests for tetrasodium diphosphate
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Annex 5:
Specifications and
tests for tetrapotassium diphosphate
1.6.
Annex 6:
Specifications and
tests for pentasodium triphosphate
1.7.
Annex 7:
Specifications and
tests for pentapotassium triphosphate
1.8.
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Specifications and
tests for sodium polyphosphate
1.9
Annex 9:
Specifications and
tests for potassium polyphosphate
1.10
Annex 10:
Specifications and
tests for sodium calcium polyphosphate
1.11
Annex 11:
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1.12
Annex 12:
Specifications and
tests for potassium gluconate
2. Specifications
specified in this Regulation are tested under JECFA monograph 1 - Vol. 4,
except for some specific tests described in the annexes. The tests provided in
this Regulation are optional. Other equivalent tests may be used.
3. Sampling adheres to
the guidelines in the Circular No. 16/2009/TT-BKHCN dated June 02, 2009 by the
Ministry of Science and Technology and relevant regulations of law.
III. REGULATORY
REQUIREMENTS
1. Declaration of
conformity
1.1. Sequestrants shall
be declared in accordance with the regulations set out in this Regulation.
1.2. Methods and
procedures for declaration of conformity shall comply with the Regulation on
certification and declaration of conformity with regulations and standards
under the Decision No. 24/2007/QĐ-BKHCN dated September 28, 2007 of the
Minister of Science and Technology and regulations of laws.
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The quality, hygiene and
safety of sequestrants must be inspected in accordance with the regulations of
law.
IV. RESPONSIBILITIES OF
ENTITIES
1. Entities must declare
conformity according to the specifications mentioned in this Regulation,
register their declarations of conformity at the Vietnam Food Administration
and ensure the quality, hygiene and safety as declared.
2. Entities are only
entitled to import, export, produce, sell and use sequestrants as declared
after their completion of registration of declarations of conformity and their
compliance with regulations of law on quality, hygiene, safety and labeling.
V. IMPLEMENTATION
1. The Vietnam Food
Administration shall preside over and cooperate with competent authorities
concerned to provide guidance on and organize the implementation of this
Regulation.
2. The Vietnam Food
Administration shall, according to its managerial duties, suggest amendments to
this Regulation to the Ministry of Health.
3. In the cases where
any of the international guidelines for tests and regulations of law referred
to in this Regulation is amended or replaced, the newest one shall apply.
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SPECIFICATIONS
AND TESTS FOR ISOPROPYL CITRATE
1. Synonyms
Isopropyl citrate
mixture
INS 384
ADI = 0 – 14 mg/kg bw
2. Definition
Chemical names
Citric acid mixed
ester of 2-propanol. The article of commerce, monoisopropyl citrate mixture,
is composed of approximately 38 parts by weight of isopropyl citrate in 62
pars by weight of mono- and diglycerides.
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where R is either
hydrogen or a isopropyl group. The major component of the 38 parts of
isopropyl citrate mixture is monoisopropyl citrate (approximately 25 parts),
the remainder being diisopropyl citrate (approximately 9 parts) and
triisopropyl citrate (approximately 4 parts).
Approximate
composition:
Monoisopropyl citrate
- 27 parts by weigh
Diisopropyl citrate -
9 parts by weight
Triisopropyl citrate -
2 parts by weight
3. Description
Oil miscible
semi-solid material. The commercial product, monoisopropyl citrate mixture,
is a viscous, colourless syrup exhibiting some crystallization upon standing,
and may be further specified as to saponification value, acid value, citric
acid and isopropyl content.
4. Functional uses
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5. Specifications
5.1. Identification
Solubility
Soluble in water and
ethanol.
Test for citrate
Passes test.
Test for isopropanol
Passes test.
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Acids other than citric
acid
Should be absent.
Alcohols other than
isopropanol
Should be absent.
Sulfated ash
Not more than 0.3%.
Lead
Not more than 2 mg/kg.
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6.1. Identification
Citrate
Reflux 3 g of sample
with 50 ml of sodium hydroxide TS for 1 h, and let stand to cool. This
solution is used for the following tests:
Neutralize the
solution with a (1 in 20) sulfuric acid solution, add an excess of mercuric
sulfate TS, heat to boil, and add potassium permanganate TS. The permanganate
colour of the solution disappears, and a white precipitate forms.
Neutralize the
solution with hydrochloric acid, add an excess of calcium chloride TS, and
boil. A white crystalline precipitate is formed which is insoluble in sodium
hydroxide TS, but soluble in dilute hydrochloric acid TS.
Test for isopropanol
Reflux 2 g of sample
with 50 ml of sodium hydroxide TS for 1 h. Distil off 20 ml. Place 8 g of
chromic oxide in a flask, add 15 ml water and 2 ml concentrated sulfuric
acid. Provide the flask with a reflux condenser and add 5 ml distillate
slowly through the condenser. Reflux for 30 min, then cool and distil off 2
ml. Add 3 ml water and 10 ml mercuric sulfate TS to the distillate. Heat in a
boiling water bath for 3 min. A white or yellow precipitate within 3 min
indicates the presence of isopropanol.
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Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
ANNEX 2
SPECIFICATIONS
AND TESTS FOR CALCIUM DISODIUM ETHYLENEDIAMINETETRAACETATE
1. Synonyms
Calcium disodium
ethylenediaminetetraacetate; calcium disodium EDTA; calcium disodium edetate
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ADI = 0 – 2.5 mg/kg bw
2. Definition
Chemical names
N,N'-1,2-Ethanediylbis[N-(carboxymethyl)-glycinate](4-)-
N,N',O,O',ON,ON]calciate(2-)disodium;
Calcium disodium
ethylenediaminetetraacetate;
Calcium disodium
(ethylene-dinitrilo)- tetraacetate.
C.A.S. number
662-33-9
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C10H12CaN2Na2O8.2H2O
Structural formula
Formula weight
410.31
3. Description
White, odourless
crystalline granules or a white to nearly white powder; slightly hygroscopic
4. Functional uses
Sequestrant,
preservative.
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5.1. Identification
Solubility
Freely soluble in
water; sparingly soluble in ethanol
Test for calcium
Passes test.
Test for sodium
Passes test.
Chelating activity to
metal ions
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5.2. Purity
pH
6.5 - 7.5 (1 in 100
soln)
Magnesium chelating
substances
Passes test (described
in “Tests”).
Lead
Not more than 2 mg/kg.
5.3. C10H12CaN2Na2O8
content
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6. Tests
6.1. Identification
Test for calcium
Tested according to
JECFA monograph 1 - Vol.4.
Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Chelating activity to
metal ions
To 5 ml of water in a
test tube add 2 drops of ammonium thiocyanate TS and 2 drops of ferric
chloride TS. A deep red solution develops. Add about 50 mg of the sample and
mix. The deep red colour disappears.
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Magnesium chelating
substances
Transfer 1 g of the
sample, accurately weighed, to a small beaker, and dissolve it in 5 ml of
water. Add 5 ml of buffer solution prepared by dissolving 67.5 g of ammonium
chloride in 200 ml of water, adding 570 ml of strong ammonia TS, and diluting
with water to 1000 ml. To the buffered solution add 5 drops of eriochrome
black TS, and titrate with 0.1 M magnesium acetate to the appearance of a
deep wine-red colour. Not more than 2.0 ml should be required.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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Each ml of 0.1 M
mercuric nitrate is equivalent to 37.43 mg of C10H12CaN2Na2O8.2H2O.
(*) Mercuric nitrate
solution:
Dissolve about 35 g of
mercuric nitrate Hg(NO3)2.H2O in a mixture of 5 ml of nitric acid and 500 ml
of water and dilute with water to 1000 ml. Standardize the solution as
follows: Transfer an accurately measured volume of about 20 ml of the
solution into an Erlenmeyer flask and add 2 ml of nitric acid and 2 ml of
ferric ammonium sulfuric TS. Cool to below 20o and titrate with 0.1 N
ammonium thiocyanate to the first appearance of a permanent brownish colour.
Calculate the molarity. (0.1 M=32.46g Hg(NO3)2/l).
ANNEX 3
SPECIFICATIONS
AND TESTS FOR DISODIUM ETHYLENEDIAMINETETRAACETATE
1. Synonyms
Disodium EDTA,
disodium edetate;
Disodium
ethylenediaminetetraacetate;
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ADI = 0 – 2.5 mg/kg bw
2. Definition
Chemical names
Disodium salt of
N,N'-1,2-Ethanediylbis[N-(carboxymethyl)glycine]; disodium dihydrogen
ethylenediaminetetraacetate; disodium dihydrogen
(ethylene-dinitrilo)-tetraacetate
C.A.S. number
139-33-3
Chemical formula
C10H14N2Na2O8 · 2H2O
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Formula weight
372.24
3. Description
White, odourless
crystalline granules or a white to nearly white powder
4. Functional uses
Sequestrant,
antioxidant synergist, preservative
5. Specifications
5.1. Identification
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Solubility
Freely soluble in
water, practically insoluble in ethanol.
Infrared absorption
The infrared spectrum
of the sample corresponds with that of a reference standard (a Reference
standard may be obtained from the U.S. Pharmacopeia, 12601 Twin Brook
Parkway, Rockville, Maryland 20852)
Test for sodium
Passes test.
Chelating activity to
metal ions
Passes test.
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pH
4.3 - 4.7 (1 in 100 soln)
Nitrilotriacetic acid
Passes test (described
in “Tests”).
Lead
Not more than 2 mg/kg.
5.3. C10H14N2Na2O8
content
Not less than 99.0%.
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6.1. Identification
Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Chelating activity to
metal ions
To 5 ml of water in a
test tube add 2 drops of ammonium to thiocyanate TS and 2 drops of ferric
chloride TS. A deep red solution develops. Add about 50 mg of the sample and
mix. The deep red colour disappears.
6.1. Purity
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Stock test solution
Transfer 10 g of the
sample into a 100-ml volumetric flask, dissolve in 40 ml of a (1 in 10)
potassium hydroxide solution, dilute to volume with water, and mix.
Diluted stock test
solution
Pipette 10 ml of the
"stock test solution" into a 100-ml volumetric flask, dilute to
volume with water, and mix.
Test preparation
Pipette 20 ml of the
"diluted stock test solution" into a 150-ml beaker, add 1 ml of a
(1 in 10) potassium hydroxide solution, 2 ml of a (1 in 10) ammonium nitrate
solution, and about 50 mg of eriochrome black T indicator, and titrate with a
(3 in 100) cadmium nitrate solution to a red endpoint. Record the volume, in
ml, of the titrant required as V, and discard the solution.
Pipette 20 ml of the
"diluted stock test solution" into a 100-ml volumetric flask, and
add the volume V of the (3 in 100) cadmium nitrate solution required in the
initial titration, plus 0.05 ml in excess. Add 1.5 ml of a (1 in 10)
potassium hydroxide solution, 10 ml of a (1 in 10) ammonium nitrate solution,
and 0.5 ml of methyl red TS, then dilute to volume with water and mix.
Stock standard
solution
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Dilute stock standard
solution
Pipette 1 ml of the
"stock standard solution" and 10 ml of the "stock test
solution" into a 100-ml volumetric flask, dilute to volume with water,
and mix.
Standard preparation
Proceed as directed under
"test preparation", using "diluted stock standard
solution" where "diluted stock test solution" is specified.
Polarographic test:
Rinse a polarographic cell with a portion of the "standard
preparation", then add a suitable volume to the cell, immerse it in a
constant-temperature bath maintained at 25 ± 0.5o , and de-aerate by bubbling
oxygen-free nitrogen through the solution
for 10 min. Insert the dropping mercury electrode of a suitable polarograph,
and record the polarogram from -0.6 to -1.2 volts at a sensitivity of 0.006
microampere per mm, using a saturated calomel electrode as the reference
electrode. In the same manner, obtain a polarogram for a portion of the
"test preparation". The diffusion current
observed with the "test preparation" is not greater than 10% of the
difference between the diffusion currents observed with the "standard
preparation" and the "test preparation", respectively. (Note:
An extra polarographic wave appearing ahead of the nitrilotriacetic acid-cadmium
complex wave is probably due to uncomplexed cadmium. This wave should be
ignored in measuring the diffusion current).
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.2. Method of essay
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Transfer about 5 g,
accurately weighed, of the sample, into a 250-ml volumetric flask, dissolve
in water, dilute to volume and mix, to give the assay preparation. Place
about 200 mg, accurately weighed, of reagent grade calcium carbonate of known
purity in a 400-ml beaker, add 10 ml of water and swirl to form a slurry. y.
Cover the beaker with a watch glass and introduce 2 ml of dilute hydrochloric
acid TS from a pipette inserted between the lip of the beaker and the edge of
the watch glass. Swirl the contents of the beaker to dissolve the calcium
carbonate. Wash down the outer surface of the pipette, the watch glass and
the sides of the beaker, and dilute to about 100 ml with water. While
stirring the solution, preferably with a magnetic stirrer, add about 30 ml of
the assay preparation from a 50- ml burette. Add 15 ml of sodium hydroxide
TS, 300 mg of hydroxynaphthol blue indicator and continue the titration with
the assay preparation to a blue end point. Calculate the percentage of
C10H14N2Na2O8.2H2O in the sample by the formula:
% sodium EDTA = 
where
mCaCO3 = the weight
in grams of calcium carbonate;
Vt = the volume in ml
of assay preparation; and
mt = the weight in
gram of the sample taken
ANNEX 4
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1. Synonyms
Sodium pyrophosphate,
tetrasodium diphosphate
INS 450iii
MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
Chemical names
Tetrasodium
diphosphate, tetrasodium pyrophosphate
C.A.S. number
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Chemical formula
Anhydrous: Na4P2O7
Decahydrate:
Na4P2O7.10H2O
Formula weight
Anhydrous: 265.94
Decahydrate: 446.09
3. Description
Colourless or white
crystals, or a white crystalline or granular powder; the decahydrate
effloresces slightly in dry air.
4. Functional uses
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5. Specifications
5.1. Identification
Solubility
Soluble in water;
insoluble in ethanol.
pH
9.9 - 10.8 (1 in 100
soln).
Test for sodium
Passes test.
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Passes test.
5.2. Purity
Loss on ignition
Not more than 0.5% for
anhydrous
38-42% for decahydrate
(105º, 4h then 550º,
30 min).
Water insoluble matter
Not more than 0.2%.
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Not more than 10
mg/kg.
Arsenic
Not more than 3.0
mg/kg.
Lead
Not more than 4.0
mg/kg.
5.3. Na4P2O7 content
Not less than 95.0% on
the dried basis.
6. Tests
6.1. Identification
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Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Test for phosphate
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Water insoluble matter
Dissolve 10 g of the
sample in 100 ml of hot water, and filter through a tared filtering crucible.
Wash the insoluble residue with hot water, dry at 105o for 2 h,
cool and weigh.
Fluoride
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Arsenic
Tested according to
JECFA monograph 1 - Vol..4, Method II.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Dissolve an accurately
weighed quantity of the sample, equivalent to about 500 mg of anhydrous
Na4P2O7, in 100 ml of water in a 400-ml beaker. Adjust the pH of the solution
to 3.8 with hydrochloric acid, using a pH meter, then add 50 ml of a 1 in 8
solution of zinc sulfate (125 g of ZnSO4.7H2O dissolved in water, diluted to
1000 ml, filtered, and adjusted to pH 3.8) and allow to stand for 2
min.Titrate the liberated acid with 0.1 N sodium hydroxide until a pH of 3.8
is again reached. After each addition of sodium hydroxide near the end-point,
time should be allowed for any precipitated zinc hydroxide to redissolve.
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ANNEX 5
SPECIFICATIONS
AND TESTS FOR TETRAPOTASSIUM DIPHOSPHATE
1. Synonyms
Tetrapotassium
diphosphate; Potassium pyrophosphate.
INS 450v
MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
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Tetrapotassium
diphosphate, tetrapotassium pyrophosphate, tetrapotassium salt of
diphosphoric acid
C.A.S. number
7320-34-5
Chemical formula
K4P2O7
Formula weight
330.34
3. Description
Colourless or white
crystals, or a white crystalline or granular powder, powder of granular
solid; hygroscopic
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Stabilizer,
emulsifier, sequestrant
5. Specifications
5.1. Identification
Solubility
Soluble in water;
insoluble in ethanol.
pH
10.0 - 10.7 (1 in 100
soln).
Test for potassium
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Test for phosphate
Passes test.
5.2. Purity
Loss on ignition
Not more than 2% (105o,
4 h; then 550o, 30 min)
Water insoluble matter
Not more than 0.2%.
Fluoride
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Arsenic
Not more than 3.0
mg/kg.
Lead
Not more than 4.0
mg/kg.
5.3. K4P2O7 content
Not less than 95% on
the ignited basis
6. Tests
6.1. Identification
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Tested according to
JECFA monograph 1 - Vol.4.
Test for phosphate
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Fluoride
Place 5 g of the
sample, 25 ml of water, 50 ml of perchloric acid, 5 drops of silver nitrate
solution (1 in 2), and a few glass beads in a 250-ml distilling flask
connected with a condenser and carrying a thermometer and capillary tube,
both of which must extend into the liquid.Connect a small dropping funnel,
filled with water, or a steam generator, to the capillary tube. Support the
flask on an asbestos mat with a hole which exposes about one-third of the
flask to the flame. Distil into a 250-ml flask until the temperature reaches
135o. Add water from the funnel or introduce steam through the
capillary to maintain the temperature between 135o and 140o.
Continue the distillation until 225-240 ml has been collected, then dilute to
250 ml with water, and mix.
Place a 50-ml aliquot
of this solution in a 100-ml Nessler tube. In another similar Nessler tube
place 50 ml of water as a control. Add to each tube 0.1 ml of a filtered
solution of sodium alizarinsulfonate (1 in 1000) and 1 ml of freshly prepared
hydroxylamine solution (1 in 4000), and mix well. Add, dropwise, and with
stirring, 0.05 N sodium hydroxide to the tube containing the distillate until
its colour just matches that of the control, which is faintly pink. Then add
to each tube exactly 1 ml of 0.1 N hydrochloric acid, and mix well. From a
buret, graduated in 0.05 ml, add slowly to the tube containing the distillate
enough thorium nitrate solution (1 in 4000) so that, after mixing, the colour
of the liquid just changes to a faint pink. Note the volume of the solution
added, add exactly the same volume to the control, and mix. Now add to the
control sodium fluoride TS (10 µg F per ml) from a buret to make the colours
of the two tubes match after dilution to the same volume. Mix well, and allow
all air bubbles to escape before making the final colour comparison. Check
the end-point by adding 1 or 2 drops of sodium fluoride TS to the control. A
distinct change in colour should take place. Note the volume of sodium
fluoride added.
The volume of sodium
fluoride TS required for the control solution should not exceed 1.0 ml.
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Tested according to
JECFA monograph 1 - Vol..4, Method II.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Dissolve about 600 mg
of the sample, accurately weighed, in 100 ml of water in 400-ml beaker, and
adjust the pH of the solution to exactly 3.8 with hydrochloric acid, using a
pH meter. Add 50 ml of a 1 in 8 solution of zinc sulfate (125 g of ZnSO4 ·
7H2O dissolved in water, diluted to 1000 ml, filtered, and adjusted to pH
3.8) and allow to stand for 2 min. Titrate the liberated acid with 0.1 N
sodium hydroxide until a pH of 3.8 is again reached. After each addition of
sodium hydroxide near the end-point, time should be allowed for any
precipitated zinc hydroxide to redissolve.
Each ml of 0.1 N
sodium hydroxide is equivalent to 16.52 mg of K4P2O7.
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ANNEX 6
SPECIFICATIONS
AND TESTS FOR PENTASODIUM TRIPHOSPHATE
1. Synonyms
Penta sodium
tripolyphosphate, sodium triphosphate,
sodium
tripolyphosphae, triphosphate;
INS 451i
2. Definition
Chemical names
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C.A.S. number
7758-29-4
Chemical formula
Na5O10P3.x H2O (x = 0
or 6)
Structural formula
Formula weight
Anhydrous: 367.86
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3. Description
White, slightly
hygroscopic granules or powder
4. Functional uses
Sequestrant,
texturizer.
5. Specifications
5.1. Identification
Solubility
Freely soluble in
water; insoluble in ethanol
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9.1 - 10.1 (1 % soln)
Test for phosphate
Passes test.
Test for sodium
Passes test.
5.2. Purity
Loss on drying
Anhydrous: not more
than 0.7% (105o, 1 h).
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Hexahydrate: not more
than 23.5% (60o, 1 h, followed by 105o, 4 h).
Water-insoluble matter
Not more than 0.1%.
Higher polyphosphates
Not detectable (see
description under Tests).
Fluoride
Not more than 50 mg/kg
(Method I or III)
Arsenic
Not more than 3 mg/kg
(Method II)
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Not more than 4.0
mg/kg.
5.3. Content
Anhydrous: not less
than 85.0% of Na5O10P3 and not less than 56.0% and not more than 58.0% of
P2O5
Hexahydrate: not less
than 65.0% of Na5O10P3 and not less than 43.0% and not more than 45.0% of
P2O5
6. Tests
6.1. Identification
Test for phosphate
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Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Higher polyphosphates
- Chromatographic
solvent: Mix 75 ml of isopropanol, 10 ml of water, 20 ml of 20%
trichloroacetic acid and 0.3 ml of 20% ammonia. Make fresh every week.
- Chromatographic
spray: Dissolve 1 g of ammonium molybdate in 85 ml of water, 10 ml of N
hydrochloric acid and 5 ml of 60% perchloric acid.
- Sample solution:
Dissolve 1 g of the sample in 50 ml of water.
- Reference solution:
Dissolve 1 g of a standard sample of pentasodium triphosphate in 50 ml of
water.
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- Procedure: Place
0.01 ml of the sample solution and 0.01 ml of reference solution on the
starting line of the chromatographic paper and allow to dry in a stream of
warm air. Use ascending chromatography at 18-20º until the solvent has
ascended about 25 cm from the starting line (12 - 15 h) Dry at 60° in an oven
and spray with the chromatographic spray. . Place the paper under an
ultraviolet lamp and irradiate until the phosphates are visible as blue spots
(about 2 min).
Three spots (one from
the monophosphate (Rf = 0.69), a second from the diphosphate (Rf = 0.44) and
the third from the triphosphate (Rf = 0.29) are observed, and no other spot
is observed.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Determination of
Na5O10P3:
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+ Potassium acetate
buffer (pH 5.0): Dissolve 78.5 g of potassium acetate in 1000 ml of water and adjust the pH of the solution to 5.0
with acetic acid. Add a few mg of mercuric iodide to inhibit mould growth.
+ 0.3 M Potassium
chloride: Dissolve 22.35 g of potassium chloride in water, add 5 ml of
potassium acetate buffer, dilute with water to 1000 ml, and mix. Add a few mg
of mercuric iodide.
+ 0.6 M Potassium
chloride: Dissolve 44.7 g of potassium chloride in water, add 5 ml of
potassium acetate buffer, dilute with water to 1000 ml, and mix. Add a few mg
of mercuric iodide.
+ - 1 M Potassium
chloride: Dissolve 74.5 g of potassium chloride in water, add 5 ml of
potassium acetate buffer, dilute to 1000 ml with water, and mix. Add a few mg
of mercuric iodide.
- Chromatographic
Column: Use a standard chromatographic column 20 to 40 cm length, 20 to 28 cm
inside diameter, with a sealed-in, coarse porosity fritted disk. If a stopcock
is not provided, attach a stopcock.
- Procedure: Close the
column stopcock, fill the space between the fritted disk and the stopcock
with water, and connect a vacuum line to the stopcock. Prepare a 1:1 water
slurry of Dowex F x 8, or equivalent, chloride form, 100-200 or 200-400 mesh,
styrenedivinylbenzene ion exchange resin, and decant off any fine particles
and any foam. Do this two or three times or until no more finely suspended
material or foaming is observed. Fill the column with the slurry, and open
the stopcock to allow the vacuum to pack the resin bed until the water level
is slightly above the top of the resin, then immediately close the stopcock.
Do not allow the liquid level to fall below the resin level at any time.
Repeat this procedure until the packed resin column is 15 cm above the
fritted disk. Place one circle of tightly fitting fibre filter paper on top
of the resin bed, then place a perforated polyethylene disk on top of the
paper. Alternatively, a loosely packed plug of glass wool may be placed on
top of the bed. Close the top of the column with a rubber stopper in which a
7.6 cm length of capillary tubing (1.5 mm i.d., 7 mm o.d.) has been inserted
through the centre, so that about 12 mm of the tubing extends through the
bottom of the stopper. Connect the top of the capillary tubing to the stem of
a 500-ml separator with flexible vinyl tubing, and clamp the separator to a
ring stand above the column. Wash the column by adding 100 ml of water to the
separator with all stopcocks closed. First open the separator stopcock, then
open the column stopcock. The rate of flow should be about 5 ml per min. When
the separator is empty, close the stopcock on the column then close the
separator stopcock.
Transfer about 500 mg
of the sample (a), accurately weighed, into a 250 ml volumetric flask,
dissolve and dilute to volume with water, and mix. Transfer 10 ml of this
solution into the separator, open both stopcocks and allow the solution to
drain into the column, rinsing the separator with 20 ml of water. Discard the
eluate. Add 370 ml of 0.3 M Potassium Chloride to the separator, and allow
this solution to pass through the column, discarding the eluate. Add 250 ml
of 0.6 M Potassium Chloride to the column, allow the solution to pass through
the column, and receive the eluate in a 400-ml beaker (To ensure a clean
column for the next run, pass 100 ml of 1 M Potassium Chloride through the
column, followed by 100 ml of water. Discard all washings.) To the beaker add
15 ml of nitric acid, mix, and boil for 15 to 20 min. Add
methyl orange TS, and neutralize the solution with stronger ammonia TS. Add 1
g of ammonium nitrate crystals, stir to dissolve, and cool. Add 15 ml of
ammonium molybdate TS, with stirring, and stir vigorously for 3 min or allow
to stand with occasional stirring for 10 to 15 min. Filter the contents of
the beaker with suction through a 6-7 mm paper pulp filter pad supported in a
25 mm porcelain disk. After the contents of the beaker have been transferred
to the filter, wash the beaker with five 10 ml portions of a 1% solution of
sodium or potassium nitrate, passing the washings through the filter, then
wash the filter with five 5-ml portions of the wash solution. Return the
filter pad and the precipitate to the beaker, wash the funnel thoroughly with
water into the beaker, and dilute to about 150 ml. Add 0.1 N sodium hydroxide
from a buret until the yellow precipitate is dissolved, then add 5 to 8 ml in
excess. Add phenolphthalein TS, and titrate the excess alkali with 0.1 N
nitric acid. Finally, titrate with 0.1 N sodium hydroxide to the first
appearance of the pink colour. The difference between the total volume of 0.1
N sodium hydroxide added and the volume of nitric acid required represents
the volume, V, in ml, of 0.1 N sodium hydroxide consumed by the
phosphomolybdate complex.
Calculate the Na5O10P3
content of the sample in % by the formula:
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a = the weight of the
sample (mg)
Determination of P2O5:
Accurately weigh about
20 mg of sample, and transfer to a porcelain casserole. Add 150 ml water and
20 ml concentrated nitric acid. Introduce anti-bumping granules, cover the
beaker with a watch glass and boil gently for 1 h. Cool to room temperature.
Quantitatively transfer the solution to a 500-ml volumetric flask, dilute
with water, mix well and dilute to the mark with water. Transfer 20.0 ml of
the solution to a plastic beaker, dilute to about 50 ml with water and place
the beaker in an automatic titrator equipped with a pH meter. Adjust the pH
of the solution to between 2.5 and 2.8 with 5 mol/l sodium hydroxide. Titrate
the solution with 0.5 mol/l sodium hydroxide. Record the consumed volumes at
the inflection points at about pH 4 (V1) and about pH 9 (V2).
Calculate the P2O5
content of the sample in % by the formula
% P2O5 = [(V2 –
V1)/2000] x f x 70,97 x (500/20) x (100/w)
= [(V2 – V1)/w] x f x
88,71
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where:
w = weight of the
sample (g)
f = factor of 0.5
mol/l sodium hydroxide (= actual molarity/0.5)
ANNEX 7
SPECIFICATIONS
AND TESTS FOR PENTAPOTASSIUM TRIPHOSPHATE
1. Synonyms
Penta potassium
tripolyphosphate, potassium triphosphate,
potassium
tripolyphosphate;
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MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
Chemical names
Pentapotassium
triphosphate, pentapotassium tripolyphosphate
C.A.S. number
13845-36-8
Chemical formula
K5O10P3
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448.42
3. Description
Hygroscopic white
granules or powder
4. Functional uses
Sequestrant,
texturizer
5. Specifications
5.1. Identification
Solubility
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pH
9.2 - 10.1 (1 in 100
soln)
Test for phosphate
Passes test.
Test for potassium
Passes test.
5.2. Purity
Water-insoluble matter
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Loss on ignition
Not more than 0.4%
after drying (105o, 4 h), followed by ignition at 550o
for 30 min.
P2O5
Not less than 46.5%
and not more than 48.0% (using about 1.5 g of the dried sample accurately
weighed).
Fluoride
Not more than 10 mg/kg
(see description under Tests)
Arsenic
Not more than 3 mg/kg
(Method II)
Lead
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5.3. K5O10P3 content
Not less than 85% of
K5O10P3 on the dried basis, the remainder being principally other potassium
phosphates.
6. Tests
6.1. Identification
Test for phosphate
Tested according to
JECFA monograph 1 - Vol.4.
Test for potassium
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6.2. Purity
Fluoride
Place 5 g of the
sample, 25 ml of water, 50 ml of perchloric acid, 5 drops of silver nitrate
solution (1 in 2), and a few glass beads in a 250-ml distilling flask
connected with a condenser and carrying a thermometer and a capillary tube,
both of which must extend into the liquid. Connect a small dropping funnel,
filled with water, or a steam generator to the capillary tube. Support the
flask on an asbestos mat with a hole which exposes about one-third of the
flask to the flame. Distil into a 250-ml flask until the temperature reaches
135o. Add water from the funnel or introduce steam through the
capillary to maintain the temperature between 135 and 140o.
Continue the distillation until 225-240 ml has been collected, then dilute to
250 ml with water, and mix. Place a 50-ml aliquot of this solution in a 100-
ml Nessler tube. In another similar Nessler tube place 50 ml of water as a
control. Add to each tube 0.1 ml of a filtered solution of sodium alizarinsulfonate
(1 in 1000) and 1 ml of freshly prepared hydroxylamine hydrochloride solution
(1 in 4000), and mix well. Add, dropwise, and with stirring, 0.05 N sodium
hydroxide to the tube containing the distillate until its colour just matches
that of the control, which is faintly pink. Then add to each tube exactly 1
ml of 0.01 N hydrochloric acid, and mix well. From a buret, graduated in 0.05
ml, add slowly to the tube containing the distillate enough thorium nitrate
solution (1 in 4000) so that, after mixing, the colour of the liquid just
changes to a faint pink. Note the volume of the solution added, add exactly
the same volume to the control, and mix. Now add to the control sodium
fluoride TS (10 µg, F per ml) from a buret to make the colours of the two
tubes match after dilution to the same volume. Mix well, and allow all air
bubbles to escape before making the final drops of sodium fluoride TS to the
control. A distant change in colour should take place. Note the volume of
sodium fluoride added. The volume of sodium fluoride TS required for the
control solution should not exceed 10 ml.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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Reagents and Solutions
- Potassium acetate
buffer (pH 5.0): Dissolve 78.5 g of potassium acetate in 1000 ml of water.
and adjust the pH of the solution to 5.0 with acetic acid. Add a few mg of
mercuric iodide to inhibit mould growth.
- 0.3 M Potassium
chloride: Dissolve 22.35 g of potassium chloride in water, add 5 ml of
potassium acetate buffer, dilute with water to 1000 ml, and mix. Add a few mg
of mercuric iodide.
- 0.6 M Potassium
chloride: Dissolve 44.7 g of potassium chloride in water, add 5 ml of
potassium acetate buffer, dilute with water to 1000 ml, and mix. Add a few mg
of mercuric iodide.
- 1 M Potassium
chloride: Dissolve 74.5 g of potassium chloride in water, add 5 ml of
potassium acetate buffer, dilute to 1000 ml with water, and mix. Add a few mg
of mercuric iodide.
Chromatographic
Column:
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Use a standard
chromatographic column 20 to 40 cm in length, 20 to 28 cm in inside diameter,
with a sealed-in, coarse porosity fritted disk. If a stopcock is not
provided, attach a stopcock.
Procedure:
Close the column
stopcock, fill the space between the fritted disk and the stopcock with water,
and connect a vacuum line to the stopcock. Prepare a 1:1 water slurry of
Dowex F x 8, or equivalent, chloride form, 100-200 or 200-400 mesh,
styrenedivinylbenzene ion exchange resin, and decant off any fine particles
and any foam. Do this two or three times or until no more finely suspended
material or foaming is observed. Fill the column with the slurry, and open
the stopcock to allow the vacuum to pack the resin bed until the water level
is slightly above the top of the resin, then immediately close the stopcock.
Do not allow the liquid level to fall below the resin level at any time.
Repeat this procedure until the packed resin column is 15 cm above the
fritted disk. Place one circle of tightly fitting fiber filter paper on top
of the resin bed, then place a perforated polyethylene disk on top of the
paper. Alternatively, a loosely packed plug of glass wool may be placed on
top of the bed. Close the top of the column with a rubber stopper in which a
7.6 cm length of capillary tubing (1.5 mm i.d., 7 mm 0.d.) has been inserted
through the centre, so that about 12 mm of the tubing extends through the
bottom of the stopper. Connect the top of the capillary tubing to the stem of
a 500 ml separator with flexible vinyl tubing, and clamp the separator to a
ring stand above the column. Wash the column by adding 100 ml of water to the
separator with all stopcocks closed. First open the separator stopcock, then
open the column stopcock. The rate of flow should be about 5 ml per min. When
the separator is empty, close the stopcock on the column then close the
separator stopcock.
Transfer about 500 mg
of the sample previously dried at 105º for 4 h and accurately weighed, into a
250 ml volumetric flask, dissolve and dilute to volume with water, and mix.
Transfer 10 ml of this solution into the separator, open both stopcocks and
allow the solution to drain into the column, rinsing the separator with 20 ml
of water. Discard the eluate. Add 370 ml of 0.3 M Potassium Chloride to the
separator, and allow this solution to pass through the column, discarding the
eluate. Add 250 ml of 0.6 M Potassium Chloride to the column, allow the
solution to pass through the column, and receive the eluate in a 400 ml
beaker. (To ensure a clean column for the next run,
pass 100 ml of 1 M Potassium Chloride through the column, followed by 100 ml
of water. Discard all washings). To the beaker add 15 ml of nitric acid, mix,
and boil for 15 to 20 min. Add methyl orange TS, and neutralize the solution
with stronger ammonia TS. Add 1 g of ammonium nitrate crystals, stir to
dissolve, and cool. Add 15 ml of ammonium molybdate TS, with stirring, and
stir vigorously for 3 min or allow to stand with occasional stirring for 10
to 15 min. Filter the contents of the beaker with suction through a 6-7 mm
paper pulp filter pad supported in a 25 mm porcelain disk. After the contents
of the beaker have been transferred to the filter, wash the
beaker with five 10 ml portions of a 1 in 100 solution of sodium or potassium
nitrate, passing the washings through the filter, then, wash the filter with
five 5-ml portions of the wash solution. Return the filter pad and the
precipitate to the beaker, wash the funnel thoroughly with water into the
beaker, and dilute to about 150 ml. Add 0.1 N sodium hydroxide from a buret
until the yellow precipitate is dissolved, then add 5 to 8 ml in excess. Add
phenolphthalein TS, and titrate the excess alkali with 0.1 N, nitric acid.
Finally, titrate with 0.1 N sodium hydroxide to the first appearance of the
pink colour. The difference between the total volume of 0.1 N sodium
hydroxide added and the volume of nitric acid required represents the volume,
V, in ml, of 0.1 N sodium hydroxide consumed by the phosphomolybdate complex.
Calculate the
quantity, in mg, of K5O10P3 in the sample taken by the formula 0.650 x 25V.
ANNEX 8
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1. Synonyms
Sodium
hexametaphosphate, sodium tetrapolyphosphate, Graham's salt
INS 452i
MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
Obtained by fusion and
subsequent chilling of sodium orthophosphates; a class of compounds
consisting of several amorphous, water-soluble polyphosphates composed of
linear chains of metaphosphate units.
Chemical names
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C.A.S. number
68915-31-1,
10124-56-8, 10361-03-2
Structural formula
Where x = 2 ; 4 ; 13 –
18, 20 – 100 or more
3. Description
Colourless or white,
transparent platelets, granules, or powders
4. Functional uses
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5. Specifications
5.1. Identification
Solubility
Very soluble in water
Test for sodium
A 1 in 20 solution
passes test
Test for
orthophosphate
Passes test.
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Loss on ignition
Not more than 1.0%.
Insoluble substances
Not more than 0.1%.
Fluoride
Not more than 10 mg/kg
(Method I or III)
Arsenic
Not more than 3 mg/kg
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Not more than 4 mg/kg.
5.3. P2O5 content
Not less than 60.0%
and not more than 71.0% of P2O5
6. Tests
6.1. Identification
Test for
orthophosphate
Dissolve 0.1 g of the
sample in 5 ml of hot dilute nitric acid TS. Warm on a steam bath for 10 min,
and cool.Neutralize to litmus with sodium hydroxide TS, and add silver
nitrate TS. A yellow precipitate is formed which is soluble in dilute nitric
acid TS.
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Insoluble substances
Dissolve about 10 g of
the sample, accurately weighed, in 100 ml of hot water, and filter through a
tared filtering crucible. Wash the insoluble residue with hot water, dry at
105o for 2 h, and weigh.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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ANNEX 9
SPECIFICATIONS
AND TESTS FOR POTASSIUM POLYPHOSPHATE
1. Synonyms
Potassium
metaphosphate;
MTDI = 70 mg/kg bw as
phosphorus from all food sources
INS 452ii
2. Definition
A heterogeneous
mixture of potassium salts of linear condensed polyphosphoric acids of general
formula Hn+2PnO3n+1 where "n" is not less than 2.
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Potassium
metaphosphate, potassium polymetaphosphate, potassium polyphosphate
C.A.S. number
7790-53-6
Chemical formula
Hn+2PnO3n+1
where n ≥ 2
3. Description
Odourless, colourless
or white glassy masses, fragments, crystals or powder
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Emulsifier,
moisture-retaining agent, sequestrant, texturizer
5. Specifications
5.1. Identification
Solubility
1 g dissolves in 100
ml of a 1 in 25 soln of sodium acetate
Gel formation
Passes test.
Test for potassium
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Test for phosphate
Passes test.
5.2. Purity
Loss on ignition
Not more than 2 %
after drying (105o, 4 h) followed by ignition at 550o for 30 min
Cyclic phosphate
Not more than 8.0%
Fluoride
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Arsenic
Not more than 3 mg/kg
(Method II)
Lead
Not more than 4 mg/kg.
5.3. P2O5 content
Not less than 53.5%
and not more than 61.5% of P2O5 on the ignited basis
6. Tests
6.1. Identification
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Gel formation
Finely powder about 1
g of the sample, and add it slowly to 100 ml of a 1 in 50 solution of sodium
chloride while stirring vigorously. A gelatinous mass is formed.
Test for potassium
Mix 0.5 g of the
sample with 10 ml of nitric acid and 50 ml of water, boil for about 30 min,
and cool. The resulting solution is used for the test.
Test for phosphate
Mix 0.5 g of the
sample with 10 ml of nitric acid and 50 ml of water, boil for about 30 min,
and cool. The resulting solution is used for the test.
6.2. Purity
Fluoride
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Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Mix about 300 mg of
the sample, accurately weighed, with 15 ml of nitric acid and 30 ml of water,
boil for 30 min, and dilute with water to about 100 ml. Heat at 60o
, add an excess of ammonium molybdate TS, and heat at 50o for 30
min. Filter, and wash the precipitate with dilute nitric acid (1 in 36 soln),
followed by potassium nitrate solution (1 in 100 soln) until the filtrate is
no longer acid to litmus. Dissolve the precipitate in 50 ml of 1 N sodium
hydroxide, add phenolphthalein TS, and titrate the excess sodium hydroxide
with 1 N sulfuric acid. Each ml of 1 N sodium hydroxide is equivalent to
3.086 mg of P2O5.
ANNEX 10
SPECIFICATIONS
AND TESTS FOR SODIUM CALCIUM POLYPHOSPHATE
1. Synonyms
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INS 452iii
MTDI = 70 mg/kg bw as
phosphorus from all food sources
2. Definition
Chemical names
Sodium calcium
polyphosphate
Chemical formula
(NaPO3)n_CaO where n
is typically 5
3. Description
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4. Functional uses
Sequestrant,
stabilizer, leavening agent, emulsifier, nutrient
5. Specifications
5.1. Identification
Test for sodium
Passes test.
Test for phosphate
Passes test.
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Passes test.
5.2. Purity
Fluoride
Not more than 10
mg/kg.
Arsenic
Not more than 3.0
mg/kg.
Lead
Not more than 4 mg/kg.
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Not less than 61% and
not more than 69 % expressed as P2 O5 on dried basis.
6. Tests
6.1. Identification
Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Test for phosphate
Tested according to
JECFA monograph 1 - Vol.4.
Test for calcium
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6.2. Purity
Fluoride
Tested according to
JECFA monograph 1 - Vol..4, Method 3; use an appropriate sample size and
appropriate volumes of standard solution for construction of the calibration
curve.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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Weigh accurately about
200 mg of the sample, dissolve in 25 ml of water and 10 ml of diluted nitric
acid TS and boil for 30 min. Filter if necessary,
and wash any precipitate, then dissolve the precipitate by the addition of 1
ml diluted nitric acid TS. Adjust the temperature to about 50o,
add 75 ml of ammonium molybdate TS, and maintain the temperature at about 50o
for 30 min, stirring occasionally. Allow to stand for 16 h or overnight at
room temperature. Decant the supernate, through a filter paper, wash the
precipitate once or twice with water by decantation using 30 to 40 ml each
time, and pour the washings through the same filter. Transfer the precipitate to the same filter, and wash with
potassium nitrate solution (1 in 100) until the filtrate is no longer acid to
litmus paper. Transfer the precipitate with filter paper to the
original precipitation vessel, add 50.0 ml of 1N sodium hydroxide, agitate
until the precipitate is dissolved, add 3 drops of phenolphthalein TS and
titrate the excess alkali with 1N sulfuric acid.
Each ml of 1N sodium
hydroxide consumed is equivalent to 3.088 mg of P2O5.
ANNEX 11
SPECIFICATIONS
AND TESTS FOR SODIUM GLUCONATE
1. Synonyms
Sodium gluconate
INS 576
ADI “Not limited”
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Chemical names
Sodium D-gluconate
C.A.S. number
527-07-1
Chemical formula
C6H11NaO7
Structural formula
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218.14
3. Description
White to tan, granular
to fine, crystalline powder.
4. Functional uses
Sequestrant, yeast
food
5. Specifications
5.1. Identification
Solubility
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Test for sodium
Passes test.
Test for gluconate
Passes test.
5.2. Purity
Reducing substances
Not more than 1.0%
calculated as D-glucose.)
Lead
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5.3. C6H11NaO7 content
Not less than 98.0%.
6. Tests
6.1. Identification
Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
Test for gluconate
Tested according to
JECFA monograph 1 - Vol.4.
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Reducing substances
Tested according to
JECFA monograph 1 - Vol.4 - Method I.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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Each ml of 0.1 N
perchloric acid is equivalent to 21.81 mg of C6H11NaO7.
ANNEX 12
SPECIFICATIONS
AND TESTS FOR POTASSIUM GLUCONATE
1. Synonyms
Potassium gluconate,
Potassium D-gluconate
INS 577
ADI “Not limited”
2. Definition
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Chemical names
Potassium D-gluconate
C.A.S. number
Anhydrous: 299-27-4
Monohydrate:
35398-15-3
Chemical formula
C6H11KO7
Structural formula
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Anhydrous: 234.25
Monohydrate: 252.26
3. Description
Odourless, free
flowing white to yellowish white, crystalline powder or granules.
4. Functional uses
Sequestrant, acidity
regulator, nutrient supplement, yeast food
5. Specifications
5.1. Identification
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Passes test.
Test for gluconate
Passes test.
5.2. Purity
Loss on drying
Anhydrous: Not more
than 3%
Monohydrate: Not less
than 6% and not more than 7.5%.
(105o, 4 h,
under vacuum).
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Not more than 1.0%
calculated as D-glucose.
Lead
Not more than 2 mg/kg.
5.3. C6H11KO7 content
Not less than 97.0%
and not more than 103.0% on dried basis.
6. Tests
6.1. Identification
Test for potassium
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Test for gluconate
Tested according to
JECFA monograph 1 - Vol.4.
6.2. Purity
Reducing substances
Tested according to
JECFA monograph 1 - Vol.4 - Method I.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the principles
of the method described in JECFA monograph 1 - Vol.4, “Instrumental Methods.”
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Transfer about 175 mg
of the sample, accurately weighed, into a clean, dry 200-ml Erlenmeyer flask,
add 75 ml of glacial acetic acid and dissolve by heating on a hot plate.
Cool, add quinaldine red TS, and titrate with 0.1 N perchloric acid in
glacial acetic acid, using a 10-ml microburet, to a colourless end point.
Each ml of 0.1 N
perchloric acid is equivalent to 23.42 mg of C6H11KO7.
ON FOOD ADDITIVE – FLOUR
TREATMENT AGENT
Foreword
QCVN 4- :2010/BYT is
developed by the Drafting Board for National technical regulation on food
additives and food processing aids, submitted by the Vietnam Food Administration
for approval and promulgated together with the Circular No. 44/2010/TT-BYT
dated December 22, 2010 of the Minister of Health.
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I. GENERAL
1. Scope
This National technical
regulation (hereinafter referred to as “the Regulation”) provides for
specifications and regulatory requirements for quality, hygiene and safety of
flour treatment agents used as food additives.
2. Regulated entities
This Regulation applies
to:
2.1. Importers,
exporters, producers, traders and users of preservatives used as flour
treatment agents used as food additives (hereinafter referred to as
“entities”).
2.2. Relevant regulatory
bodies.
3. Interpretation of
terms and acronyms:
3.1. “flour treatment
agent” refers to a food additive added to flour or dough to improve its baking
quality or color.
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3.3. “C.A.S number”
(Chemical Abstracts Service) refers to registry numbers of chemical substances
identified by the American Chemical Society.
3.4. “TS” stands for
test solution.
3.5. “ADI” stands for
acceptable daily intake.
3.6. “INS” stands for
international numbering system.
II. SPECIFICATIONS,
TESTS AND SAMPLING
1. Specifications and
tests for azodicarbonamide used as a flour treatment agent are specified in the
Annex to this Regulation.
2. Specifications
specified in this Regulation are tested under JECFA monograph 1 - Vol. 4,
except for some specific tests described in the Annex. The tests provided in
this Regulation are optional. Other equivalent tests may be used.
3. Sampling adheres to
the guidelines in the Circular No. 16/2009/TT-BKHCN dated June 02, 2009 by the
Ministry of Science and Technology and relevant regulations of law.
III. REGULATORY
REQUIREMENTS
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1.1. Flour treatment
agents shall be declared in accordance with the regulations set out in this
Regulation.
1.2. Methods and
procedures for declaration of conformity shall comply with the Regulation on
certification and declaration of conformity with regulations and standards
under the Decision No. 24/2007/QĐ-BKHCN dated September 28, 2007 of the
Minister of Science and Technology and regulations of laws.
2. Inspection of flour
treatment agents
The quality, hygiene and
safety of flour treatment agents must be inspected in accordance with the
regulations of law.
IV. RESPONSIBILITIES OF
ENTITIES
1. Entities must declare
conformity according to the specifications mentioned in this Regulation, register
their declarations of conformity at the Vietnam Food Administration and ensure
the quality, hygiene and safety as declared.
2. Entities are only
entitled to import, export, produce, sell and use flour treatment agents as
declared after their completion of registration of declarations of conformity
and their compliance with regulations of law on quality, hygiene, safety and
labeling.
V. IMPLEMENTATION
1. The Vietnam Food
Administration shall preside over and cooperate with competent authorities
concerned to provide guidance on and organize the implementation of this
Regulation.
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3. In the cases where
any of the international guidelines for tests and regulations of law referred
to in this Regulation is amended or replaced, the newest one shall apply.
ANNEX
SPECIFICATIONS
AND TESTS FOR AZODICARBONAMIDE
1. Synonyms
Azobisformamide;
INS 927a
2. Definition
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Azodicarbonamide,
azodicarboxylic acid diamide
C.A.S. number
123-77-3
Chemical formula
C2H4N4O2
Structural formula
Formula weight
116.08
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Yellow to orange-red,
odourless, crystalline powder
4. Functional uses
Flour treatment agent
5. Specifications
5.1. Identification
Solubility
Practically insoluble
in water and in ethanol; slightly soluble in dimethyl sulfoxide
Melting range
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Test for oxidation
Passes test
(liberates iodine from potassium iodide TS solution in the presence of 10%
sulfuric acid)
Test for carbon
dioxide
Passes test.
5.2. Purity
Loss on drying
Not more than 0.5% (50o,
2h in vacuo).
pH
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Sulfated ash
Not more than 0.15%
(Test 1.5 g of the sample (Method I))
Lead
Not more than 2 mg/kg.
5.3. Content
Not less than 98.6%;
not less than 47.2% and not more than 48.7% of N on the dried basis
6. Tests
6.1. Identification
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Test for carbon
dioxide
Heat about 10 mg of
the sample in a crucible. A drop of barium hydroxide solution held above the
sample by means of a glass rod becomes turbid.
6.2. Purity
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
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Titrimetric
method/azodicarbonamide:
Transfer about 225 mg
of the accurately weighed sample, previously dried in a vacuum oven at 50o
for 2 h, into a 250-ml glass-stoppered iodine flask. Add about 23 ml of
dimethyl sulfoxide to the flask, washing any adhered sample down with the
solvent, stopper the flask, and place about 2 ml of the solvent in the cup or
lip of the flask. Swirl occasionally until complete solution of the sample is
effected, and then loosen the stopper to drain the remainder of solvent into
the flask and to rinse down any dissolved sample into the solution. Add 5 g
of potassium iodide followed by 15 ml of water, immediately pipet 10 ml of
0.5 N hydrochloric acid into the flask, and stopper quickly. Swirl until the
potassium iodide dissolves, and allow to stand for 20-25 min protected from
light. Titrate the liberated iodine with 0.1 N sodium thiosulfate to the
disappearance of the yellow colour. Titrate with additional thiosulfate if
any yellow colour appears within 15 min. Perform a blank determination on a
solution consisting of 25 ml of dimethyl sulfoxide, 5 g of potassium iodide,
15 ml of water, and 5 ml of 0.5 N hydrochloric acid, and make any necessary
correction. Each ml of 0.1 N sodium thiosulfate is equivalent to 5.804 mg of
C2H4N4O2.
Kjeldahl method
(semimicro)/nitrogen:
Transfer about 50 mg
of the accurately weighed sample, previously dried in a vacuum oven at 50o
for 2 h, into a 100-ml Kjeldahl flask, add 3 ml of hydriodic acid (min. 57%)
and digest the mixture for 75 min adding sufficient water, when necessary, to
maintain the original volume. Increase the heat at the end of the digestion
period and continue heating until the volume is reduced by about one-half.
Cool to room temperature, add 1.5 g of potassium sulfate and 3 ml of water.
Carefully add 4.5 ml of concentrated sulfuric acid and heat until iodine
fumes are no longer evolved. Allow the mixture to cool, wash down the sides
of the flask with water, heat until charring occurs, and again cool to room
temperature. To the charred material add 40 mg of mercuric oxide, heat until
the colour of the solution is pale yellow, then cool, wash down the sides of
the flask with a few ml of water and digest the mixture for 3 h. Cool the digest,
add 20 ml ammonia-free water, 16 ml of a 50% sodium hydroxide solution and 5
ml of a 44% sodium thiosulfate solution. Connect the flask to a distillation
apparatus and distil, collecting the distillate in 10 ml of a 4% boric acid
solution. Add a few drops of methyl red-methylene blue TS to the distillate
and titrate with 0.05 N sulfuric acid. Perform a blank determination. Each ml
of 0.05 N sulfuric acid is equivalent to 0.7004 mg of N.
ON FOOD ADDITIVE - BULKING
AGENT
Foreword
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NATIONAL TECHNICAL REGULATION ON FOOD ADDITIVE – BULKING AGENT
I. GENERAL
1. Scope
This National technical
regulation (hereinafter referred to as “the Regulation”) provides for specifications
and regulatory requirements for quality, hygiene and safety of bulking agents
used as food additives.
2. Regulated entities
This Regulation applies
to:
2.1. Importers,
exporters, producers, traders and users of preservatives used as bulking agents
used as food additives (hereinafter referred to as “entities”).
2.2. Relevant regulatory
bodies.
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3.1. “bulking agent”
refers to a food additive added to a food
without contributing significantly to its available energy value.
3.2. JECFA monograph 1 -
Vol. 4 (JECFA monographs 1 - Combined compendium of food additive
specifications; Joint FAO/WHO expert committee on food additives; Volume 4 -
Analytical methods, test procedures and laboratory solutions used by and
referenced in the food additive specifications; FAO, 2006) is developed by
JECFA and was published by FAO in 2006.
3.3. “C.A.S number”
(Chemical Abstracts Service) refers to registry numbers of chemical substances
identified by the American Chemical Society.
3.4. “TS” stands for
test solution.
3.5. “ADI” stands for
acceptable daily intake.
3.6. “INS” stands for
international numbering system.
II. SPECIFICATIONS,
TESTS AND SAMPLING
1. Specifications and
tests for bulking agents are specified in the annexes to this Regulation as
follows:
1.1.
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Specifications and
tests for microcrystalline cellulose
1.2.
Annex 2:
Specifications and
tests for carnauba wax
1.3.
Annex 3:
Specifications and
tests for sodium alginate
2. Specifications
specified in this Regulation are tested under JECFA monograph 1 - Vol. 4,
except for some specific tests described in the annexes. The tests provided in
this Regulation are optional. Other equivalent tests may be used.
3. Sampling adheres to
the guidelines in the Circular No. 16/2009/TT-BKHCN dated June 02, 2009 by the
Ministry of Science and Technology and relevant regulations of law.
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1. Declaration of
conformity
1.1. Bulking agents
shall be declared in accordance with the regulations set out in this
Regulation.
1.2. Methods and
procedures for declaration of conformity shall comply with the Regulation on
certification and declaration of conformity with regulations and standards
under the Decision No. 24/2007/QĐ-BKHCN dated September 28, 2007 of the
Minister of Science and Technology and regulations of laws.
2. Inspection of bulking
agents
The quality, hygiene and
safety of bulking agents must be inspected in accordance with the regulations
of law.
IV. RESPONSIBILITIES OF
ENTITIES
1. Entities must declare
conformity according to the specifications mentioned in this Regulation,
register their declarations of conformity at the Vietnam Food Administration
and ensure the quality, hygiene and safety as declared.
2. Entities are only
entitled to import, export, produce, sell and use bulking agents as declared
after their completion of registration of declarations of conformity and their
compliance with regulations of law on quality, hygiene, safety and labeling.
V. IMPLEMENTATION
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2. The Vietnam Food
Administration shall, according to its managerial duties, suggest amendments to
this Regulation to the Ministry of Health.
3. In the cases where
any of the international guidelines for tests and regulations of law referred
to in this Regulation is amended or replaced, the newest one shall apply.
ANNEX 1
SPECIFICATIONS
AND TESTS FOR MICROCRYSTALLINE CELLULOSE
1. Synonyms
Mycrocrystalline
cellulose; Cellulose gel;
INS 460
ADI “Not limited”
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Purified, partially
depolymerized cellulose prepared by treating alphacellulose, obtained as a
pulp from fibrous plant material, with mineral acids. The degree of
polymerization is typically less than 400. Not more than 10% of the particles
have a diameter below 5 µm.
Chemical names
Cellulose
C.A.S. number
9004-34-6
Chemical formula
(C6H10O5)n
3. Description
Fine, white or almost
white, odourless, free flowing crystalline powder.
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Bulking agent,
emulsifier, stabilizer, anticaking agent, dispersing agent.
5. Specifications
5.1. Identification
Solubility
Insoluble in water,
ethanol, ether and dilute mineral acids. Slightly soluble in sodium hydroxide
solution.
Infrared absorption
The infrared
absorption spectrum of a potassium bromide dispersion of the sample
corresponds to the infrared spectrum below.
Test for suspensoid
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5.2. Purity
Loss on drying
Not more than 7.0%
(105o, 3 h).
pH
5.0 – 7.5
Water soluble
Not more than 0.24%.
Sulfated ash
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Starch
Not detectable.
Lead
Not more than 2 mg/kg.
5.3. Content
Not less than 97% of
carbohydrate calculated as cellulose on the dry basis.
6. Tests
6.1. Identification
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Mix 30 g of the sample
with 270 ml of water in a high-speed (18,000 rpm) blender for 5 min. Transfer
100 ml of the mixture to a 100-ml graduated cylinder, and allow to stand for
3 h. A white, opaque, bubble-free dispersion that forms a supernatant, is
obtained.
6.2. Purity
pH
Shake 5 g of the
sample with 40 ml of water for 20 min and centrifuge. Determine the pH of the
supernatant.
Water soluble
Shake 5 g of the
sample with approximately 80 ml of water for 10 min, filter through Whatman
No. 42 or equivalent filter paper into a tared beaker, wash residue with 20
ml of water and evaporate to dryness on a steam bath. Dry at 105o
for 1 h., cool, weigh and calculate as percentage.
Sulfated ash
Tested according to
JECFA monograph 1 - Vol. 4 - Method 1, (Test 10 g of the sample).
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To 20 ml of the
dispersion obtained in the identification test for starch, add a few drops of
iodine TS, and mix. No purplish to blue or blue colour should be obtained.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Method of essay
Transfer about 125 mg
of the sample, accurately weighed, to a 300 ml Erlenmeyer flask, using about
25 ml of water. Add 50.0 ml of 0.5N potassium dichromate and mix. Carefully
add 100 ml of sulfuric acid and heat to boiling. Remove from heat, allow to
stand at room temperature for 15 min and cool in a water bath. Transfer the
contents into a 250 ml volumetric flask, rinse flask with distilled water,
add rinsings to the volumetric flask and dilute with water almost to volume.
Allow the volumetric flask to reach room temperature (25o), then
make up to volume with water and mix. Titrate a 50.0 ml aliquot with 0.1N
ferrous ammonium sulfate using 2 or 3 drops of ortho-phenanthroline TS as the
indicator and record the volume required as S in ml. Perform a blank
determination and record the volume of 0.1N ferrous ammonium sulfate required
as B in ml. Calculate the percentage of cellulose in the sample by the
formula:
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W is the weight of
sample taken, in mg, corrected for loss on drying.
Infrared spectrum
Microcrystalline
cellulose
ANNEX 2
SPECIFICATIONS
AND TESTS FOR CARNAUBA WAX
1. Synonyms
INS 903
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2. Definition
The refined wax
obtained from the fronds of the Brazilian tropical palm tree Copernicia
cerifera (Arruda) Mart. [syn. C. purnifera (Muell.)]; a complex mixture of
several chemical compounds, predominantly esters, e.g.,
- aliphatic esters
(straight-chain acids with even-numbered carbon chains from C24 to C28 and
straight-chain alcohols with even-numbered carbon chains from C30 to C34).
- - alpha-hydroxy
esters (straight-chain hydroxy acids with even-numbered carbon chains from
C22 to C28, straight-chain acids with even-numbered carbon chains from C24 to
C28, straight-chain monohydric alcohols with evennumbered carbon chains from
C24 to C34 and dihydric alcohols with evennumbered carbon chains from C24 to
C34).
- cinnamic aliphatic
diesters (p-methoxycinnamic acid and dihydric alcohols with even-numbered
carbon chains from C24 to C34).
It also contains free
acids (straight-chain acids with even-numbered carbon chains from C24 to
C28), free alcohols (straight-chain alcohols with evennumbered carbon chains
from C30 to C34), hydrocarbons (straight-chain oddnumbered carbon chains from
C27 to C31) and resins.
C.A.S. number
8015-86-9
3. Description
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4. Functional uses
Glazing agent, bulking
agent, acidity regulator, carrier.
5. Specifications
5.1. Identification
Solubility
Insoluble in water;
partially soluble in boiling ethanol; soluble in ether.
Melting range
80oC - 86oC
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Acid value
Between 2 and 7.
Saponification value
Between 78 and 95.
Ester value
Between 71 and 93.
Subtract the Acid
value from the Saponification value to obtain the Ester value.
Sulfated ash
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Unsaponifiable matter
Between 50% and 55%.
Lead
Not more than 2 mg/kg.
6. Tests
6.1. Purity
Sulfated ash
Heat a 2-g sample in a
tared, open porcelain or platinum dish over an open flame. It volatilizes
without emitting an acrid odour. Ignite as described in procedure for Ash
(sulfated ash) Method I - JECFA monograph 1 - Vol.4).
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Weigh accurately about
5 g of the sample into a 250-ml flask, add a solution of 2 g of potassium
hydroxide in 40 ml ethanol, and boil gently under reflux for 1 h or until
saponification is complete. Transfer the content of the flask to a
glass-stoppered extraction cylinder (approximately 30 cm in length, 3.5 cm in
diameter and graduated at 40, 80 and 130 ml). Wash the flask with sufficient
alcohol to achieve a volume of 40 ml in the cylinder, and complete the
transfer with warm and then cold water until the total volume is 80 ml.
Finally wash the flask with a few ml of petroleum ether, add the washings to
the cylinder, cool the contents of the cylinder to room temperature and add
50 ml of petroleum ether. Insert the stopper and shake the cylinder
vigorously for at least 1 min, and allow both layers to become clear. Siphon
the upper ether layer as completely as possible without removing any of the
lower layer, collecting the ether fraction in a 500-ml separator. . Repeat extraction and siphoning at least six times with 50-ml
portions of petroleum ether, shaking vigorously each time. Wash the combined
extracts, with vigorous shaking, with 25-ml portions of 10% ethanol until the
wash water is neutral to phenolphthalein, and discard the washings. Transfer
the ether extract to a tared beaker and rinse the separator with 10-ml of
ether, adding the rinsings to the beaker. Evaporate the ether at a steam bath
just to dryness, and dry the residue to constant weight, preferably at 75º to
80º under vacuum of not more than 200 mm of Hg, or at 100º for 30 min. Cool
in a desiccator and weigh to obtain weight of unsaponifiable matter.
Dissolve the residue
in 50 ml of warm neutral ethanol and titrate with 0.02N sodium hydroxide
using phenolphthalein as indicator. Each ml of 0.02N sodium hydroxide is
equivalent to 5.659 mg of fatty acids, calculated as oleic acid.
Subtract the
calculated weight of fatty acids from the weight of the residue to obtain the
corrected weight of unsaponifiable matter in the sample.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
ANNEX 3
SPECIFICATIONS
AND TESTS FOR SODIUM ALGINATE
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INS 401
ADI “Not limited”
2. Definition
Sodium salt of alginic
acid
C.A.S. number
9005-38-3
Chemical formula
(C6H7NaO6)n
Structural formula
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The number and
sequence of the Mannuronate and Glucuronate residues shown above vary in the
naturally occurring alginate. The water molecules associated with the
alginate molecule are not shown in the above structural formula.
Formula weight
Structural unit:
198.11 (theoretical), 222 (actual average)
Macromolecule: 10,000
- 600,000 (typical average)
3. Description
White to yellowish
brown filamentous, grainy, granular or powdered forms.
4. Functional uses
Bulking agent,
stabilizer, thickener, gelling agent, emulsifier
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5.1. Identification
Solubility
Dissolves slowly in
water, forming a viscous solution. Insoluble in ethanol and ether.
Precipitate formation
with calcium chloride
Passes test.
Precipitate formation
with ammonium sulphate
Passes test.
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Test for alginate
Passes test.
Test for sodium
Passes test.
5.2. Purity
Loss on drying
Not more than 15% (105o,
4 h).
Water-insoluble matter
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Arsenic
Not more than 3.0
mg/kg.
Lead
Not more than 5 mg/kg.
5.3. Microbiological criteria
Total plate count
Not more than 5,000
colonies per gram.
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Not more than 500
colonies per gram
Coliforms
Negative by test
Salmonella
Negative by test
5.3. (C6H7NaO6)n
content
Yields, on the dried
basis, not less than 18.0% and not more than 21.0% of carbon dioxide (CO2),
equivalent to not less than 90.8% and not more than 106.0% of sodium alginate
(C6H7NaO6)n.
6. Tests
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Precipitate formation
with calcium chloride
To a 0.5% solution of
the sample in sodium hydroxide TS add one-fifth of its volume of a 2.5%
solution of calcium chloride. A voluminous, gelatinous precipitate is formed.
This test distinguishes sodium alginate from gum arabic, sodium carboxymethyl
cellulose, carrageenan, gelatin, gum ghatti, karaya gum, carob bean gum,
methyl cellulose and tragacanth gum.
Precipitate formation
with ammonium sulphate
To a 0.5% solution of
the sample in sodium hydroxide TS add one-half of its volume of a saturated
solution of ammonium sulfate. No precipitate is formed. This test
distinguishes sodium alginate from agar, sodium carboxymethyl cellulose,
carrageenan, de-esterified pectin, gelatin, carob bean gum, methyl cellulose
and starch.
Test for alginate
Tested according to
JECFA monograph 1 - Vol.4.
Test for sodium
Tested according to
JECFA monograph 1 - Vol.4.
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Water-insoluble matter
Disperse 2 g of the
sample, weighed to the nearest 0.1 mg, in 800 ml of water in a 2,000-ml
flask. Neutralize to pH 7 with sodium hydroxide TS and then add 3 ml in
excess. Add 40 ml of hydrogen peroxide solution containing 30% by weight
H2O2, cover the flask and boil for 1 h with frequent stirring. Filter while
hot through a tared Gooch crucible provided with a glass fibre filter (2.4
cm, No 934 AH, Reeve Angel & Co, Clifton, N.Y.,USA, or equivalent). If
slow filtration is caused by high viscosity of the sample solution, boil
until the viscosity is reduced enough to permit filtration. Wash the crucible
thoroughly with hot water, dry the crucible and its contents at 105o for 1 h,
cool and weigh. Calculate as percentage of the dry weight.
Arsenic
Tested according to
JECFA monograph 1 - Vol.4, Method II.
Lead
- Tested according to
JECFA monograph 1 - Vol.4.
- Determine using an
atomic absorption technique appropriate to the specified level. The selection
of sample size and method of sample preparation may be based on the
principles of the method described in JECFA monograph 1 - Vol.4,
“Instrumental Methods.”
6.3. Microbiological
criteria
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Total plate count
Initially prepare a
10-1 dilution by adding a 50 g sample to 450 ml of Butterfield’s phosphate
buffered dilution water and homogenizing in a high speed blender.
6.2. Method of essay
Proceed as directed
under Carbon Dioxide Determination by Decarboxylation in JECFA monograph 1 -
Vol. 4.
Each ml of 0.25 N
sodium hydroxide consumed is equivalent to 5.5 mg of carbon dioxide (CO2) or
27.75 mg of sodium alginate (equivalent weight 222).
FOOD ADDITIVE - PROPELLANT
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QCVN 4- :2010/BYT is
developed by the Drafting Board for National technical regulation on food
additives and food processing aids, submitted by the Vietnam Food
Administration for approval and promulgated together with the Circular No.
44/2010/TT-BYT dated December 22, 2010 of the Minister of Health.
NATIONAL TECHNICAL REGULATION ON FOOD ADDITIVE - PROPELLANT
I. GENERAL
1. Scope
This National technical
regulation (hereinafter referred to as “the Regulation”) provides for
specifications and regulatory requirements for quality, hygiene and safety of
propellants used as food additives.
2. Regulated entities
This Regulation applies
to:
2.1. Importers,
exporters, producers, traders and users of preservatives used as propellants
used as food additives (hereinafter referred to as “entities”).
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3. Interpretation of
terms and acronyms:
3.1. “propellant” refers
to a gaseous food additive that is added to food.
3.2. JECFA monograph 1 -
Vol. 4 (JECFA monographs 1 - Combined compendium of food additive
specifications; Joint FAO/WHO expert committee on food additives; Volume 4 -
Analytical methods, test procedures and laboratory solutions used by and
referenced in the food additive specifications; FAO, 2006) is developed by
JECFA and was published by FAO in 2006.
3.3. “C.A.S number”
(Chemical Abstracts Service) refers to registry numbers of chemical substances
identified by the American Chemical Society.
3.4. “TS” stands for
test solution.
3.5. “ADI” stands for
acceptable daily intake.
3.6. “INS” stands for
international numbering system.
II. SPECIFICATIONS,
TESTS AND SAMPLING
1. Specifications and
tests for propellants are specified in the annexes to this Regulation as
follows:
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Annex 1:
Specifications and
tests for nitrogen
1.2.
Annex 2:
Specifications and
tests for nitrogen oxyde
2. Specifications
specified in this Regulation are tested under JECFA monograph 1 - Vol. 4,
except for some specific tests described in the annexes. The tests provided in
this Regulation are optional. Other equivalent tests may be used.
3. Sampling adheres to
the guidelines in the Circular No. 16/2009/TT-BKHCN dated June 02, 2009 by the
Ministry of Science and Technology and relevant regulations of law.
III. REGULATORY
REQUIREMENTS
1. Declaration of
conformity
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1.2. Methods and
procedures for declaration of conformity shall comply with the Regulation on
certification and declaration of conformity with regulations and standards
under the Decision No. 24/2007/QĐ-BKHCN dated September 28, 2007 of the
Minister of Science and Technology and regulations of laws.
2. Inspection of
propellants
The quality, hygiene and
safety of propellants must be inspected in accordance with the regulations of
law.
IV. RESPONSIBILITIES OF
ENTITIES
1. Entities must declare
conformity according to the specifications mentioned in this Regulation,
register their declarations of conformity at the Vietnam Food Administration
and ensure the quality, hygiene and safety as declared.
2. Entities are only
entitled to import, export, produce, sell and use propellants as declared after
their completion of registration of declarations of conformity and their
compliance with regulations of law on quality, hygiene, safety and labeling.
V. IMPLEMENTATION
1. The Vietnam Food
Administration shall preside over and cooperate with competent authorities
concerned to provide guidance on and organize the implementation of this
Regulation.
2. The Vietnam Food
Administration shall, according to its managerial duties, suggest amendments to
this Regulation to the Ministry of Health.
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ANNEX 1
YÊU CẦU KỸ THUẬT VÀ PHƯƠNG PHÁP THỬ ĐỐI VỚI KHÍ
NITROGEN
1. Synonyms
Nitrogen
INS 941
ADI “Not limited”
2. Definition
This monograph defines
nitrogen with a maximum oxygen content of 1%, which is suitable only for some
food applications. There are food applications that require a higher purity
(i.e., lower oxygen content).
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Nitrogen
C.A.S. number
7727-37-9
Chemical formula
N2
Formula weight
28.0
3. Description
Colourless, odourless
gas or liquid.
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Freezing agent,
propellant, packaging gas
5. Specifications
5.1. Identification
Flame test
A flame is
extinguished in an atmosphere of the sample.
5.2. Purity
Oxygen
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Carbon monoxide
Not more than 10 µl/l
(see description under Tests).
5.3. Content
Not less than 99.0%
v/v.
6. Tests
6.1. Purity
Oxygen
Use an oxygen analyser
with a detector scale ranging from 0 µl/l to 100 µl/l and equipped with an
electrochemical cell. The gas to be examined is passed through a detection
cell containing an aqueous solution, generally potassium hydroxide. Oxygen in
the sample gas produces variation in the electrical signal recorded at the
outlet of the cell that is proportional to the oxygen content.
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Carbon monoxide
Pass 1050 ± 50 ml of
the gas sample through a carbon monoxide detector tube at the rate specified
for the tube. The indicator change corresponds to not more than 10 µl/l.
6.2. Method of essay
Determine by Gas
chromatography using the following conditions:
Column:
material: stainless
steel
length: 2 m
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packing material:
appropriate molecular sieve capable of absorbing molecules with diameters up
to 0.5 nm.
Carrier gas:
- gas: helium (not
less than 99.995 % (v/v) of He)
- flow: 40 ml/min
Detector: thermal
conductivity detector
Injector: loop
injector
Column temperature:
50°
Detector temperature:
130°
Reference gas (a):
ambient air
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Procedure:
Inject reference gas
(a). Adjust the injected volumes and operating conditions so that the height
of the peak due to nitrogen in the chromatogram is at least 35 % of full
scale of the recorder. The assay is not valid unless the chromatograms
obtained show a clear separation of oxygen and nitrogen.
Inject the gas to be
examined and the reference gas (b). In the chromatogram obtained with the gas
to be examined, the area of the principal peak is at least 99.0 % of the area
of the principal peak in the chromatogram obtained with reference gas (b).
ANNEX 2
SPECIFICATIONS
AND TESTS FOR NITROGEN OXYDE
1. Synonyms
Nitrogen oxyde,
dinitrogen monoxyde,
INS 942
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2. Definition
Chemical names
Dinitrogen monoxyd
C.A.S. number
10024-97-2
Chemical formula
N2O
Formula weight
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3. Description
Colourless, odourless
gas.
4. Functional uses
Propellant,
antioxidant, packaging gas, foaming agent
5. Specifications
5.1. Identification
Solubility
1 volume dissolves in
1.5 volumes of water (20o, 760 mm Hg)
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A glowing splinter of
wood in contact with nitrous oxide bursts into flame (distinction from
nitrogen).
Pyrogallol test
Passes test
(distinction from oxygen).
5.2. Purity
Carbon monoxide
Not more than 10 µl/l.
Nitric oxide and
nitrogen dioxide
Not more than 5 µl/l.
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Not more than 5 µl/l.
Arsine and phosphine
Passes test.
5.3. Content
Not less than 97%
(v/v).
6. Tests
6.1. Identification
Pyrogallol test
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6.2. Purity
NOTE: For the
following tests keep the cylinder of gas from which the sample is taken at
room temperature for not less than 6 h before carrying out the tests. In all
the tests the cylinder is kept in the vertical position with the outlet valve
uppermost when delivering the gas. Pass the gas at a steady rate of 4 l/h
unless otherwise stated and carry out the tests or calculate the results with
reference to the gas at 20o and 760 mm Hg.
Carbon monoxide
Principle:
Carry out the test on
the first portion of gas issuing from the cylinder. Use 5.0 l of the nitrous
oxide in the test and 5.0 l of carbon monoxide-free air as the control. The
difference between the volumes of 0.002 N sodium thiosulfate used in the two
titrations is not greater than 0.5 ml.
Apparatus:
The apparatus consists
of the following parts connected in series:
- U-tube containing
anhydrous silica gel impregnated with chromium trioxide.
- Scrubber bottle
(dreschel type) containing 100 ml of a 40% w/v solution of potassium
hydroxide.
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- U-tube containing
phosphorous pentoxide dispersed on previously granulated, fused pumice.
- Tube containing
recrystallized iodic anhydride (I2O5) in granules, previously dried at 200o and kept at a temperature of
120o. The iodic anhydride is packed in the tube in 1 cm columns
separated by 1 cm columns of glass wool to give an effective length of 5 cm.
- Flask containing 2.0
ml of potassium iodide TS and 3 drops of starch solution TS.
Procedure
Flush the apparatus
with 5.0 l of carbon dioxide-free air and, if necessary, discharge the blue
colour in the iodide solution by adding the smallest necessary quantity of
freshly prepared 0.002 N sodium thiosulfate. Continue flushing until not more
than 0.045 ml of 0.002 N sodium thiosulfate is required after passing 5.0 l
of carbon dioxide-free air.
Pass the gas from the
cylinder through the apparatus, using the volume and the rate of flow
prescribed in the monograph. Flush the last traces of liberated iodine into
the reaction flask by passing through the apparatus 1.0 l of carbon
monoxide-free air. Titrate the liberated iodine with 0.002 N sodium
thiosulfate.
Carry out a blank
assay under the same conditions, using the carbon monoxide-free gas
prescribed in the monograph. The difference between the volumes of 0.002 N
sodium thiosulfate used in the two titrations is not greater than the limit prescribed in the monographs.
Nitric oxide and
nitrogen dioxide
Principle:
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Sulfanilic
acid/naphthylenediamine TS:
Solution I: Dissolve 2
g of sulfanilic acid TS in a mixture of 10 ml of glacial acetic acid and 180
ml of water.
Solution II: Dissolve
0.2 g of naphthylenediamine dihydrochloride in 10 ml of a 50% v/v glacial
acetic acid solution heating gently and dilute to 200 ml with water.
Mix 9 volumes of
Solution I with 1 volume of Solution II
Procedure
Introduce 20.0 ml of
sulfanilic acid/naphthylenediamine TS into the sampling tube by dipping the
end into a dish containing the mixture and carefully opening the tap. Shake
the tube and allow to stand for 10 min with occasional shaking. Prepare the
reference solution by adding 0.25 ml of 0.00308% w/v sodium nitrite solution
to 20.0 ml of the sulfanilic acid/naphthylenediamine TS. Measure the
absorbance of a 1 cm layer of the resulting solutions at 550 nm and correct
the result to 1.0 l of the gas at 20o and 760 mm Hg.
The extinction of 1.0
l of the test substance is not greater than that of the reference solution.
Halogens and hydrogen
sulfide
NOTE: For the
following test pass the gas into a closed, flat-bottomed glass cylinder
fitted with (a) a delivery tube having an orifice of 1 mm internal diameter
and reaching to 2 mm from the bottom of the cylinder and (b) an outlet tube.
The delivery tube is immersed in the reagent to a depth of 12 to 14 cm.
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Arsine and phosphine
Silver DDC/Quinoline
TS: Dissolve 50 mg of finely powdered silver nitrate in 100 ml of quinoline
and add 0.2 g of silver diethyldithiocarbamate. The reagent should be freshly
prepared.
Procedure: Pass 10.0 l
at a rate of 1.0 l/min through a glass tube packed with lead acetate TS on
cotton wool and a gas distribution head of the domed, sintered type, of
porosity 100, into a tube of about 2.5 cm internal diameter, containing 5 ml
of Silver DDC/Quinoline TS, the domed head being almost in contact with the
bottom of the tube. The colour of the Silver DDC/Quinoline TS is not changed.
6.3. Method of essay
Use a gas burette (see
Figure below) of 100 ml capacity having as its upper end a two-way tap
connected to two capillaries, one of which (tube A) is used to introduce the
gas into the apparatus, the other (tube B) connected to the condenser (C) and
the manometer (M). The lower part of the gas burette has a one-way tap
connected to a mercury reservoir by a rubber tube. The gas burette is
graduated form 0 to 5 ml in tenths of a ml in the upper part and from 99.5 to
100.5 ml in tenths of a ml in the lower part. The capillary tube (B) is
connected to a vertical capillary arm to form a four-way junction. The
descending arm of the junction is connected to a condenser (C) of about 60 ml
capacity. The right arm of the junction is connected to a mercury manometer
(M). A tap (D) on the upper vertical arm of the junction opens to the air.
Close the three taps
and immerse the condenser in liquid nitrogen, keeping the level slightly
above the upper part of the condenser. By manipulating the two-way tap and
the mobile reservoir create a partial vacuum in the apparatus, choosing an
arbitrary pressure Po between 50 and 60 mm Hg, accurately measured. This
pressure must remain constant for 10 min to demonstrate that the apparatus is
gas-tight.
Open the two-way tap
to tube (A) and completely fill the burette and tube (A) with mercury. Close
the two-way tap. Connect a rubber tube to the exit valve of the nitrous oxide
cylinder through a suitable pressure relieving device and pass a current of
nitrous oxide through the rubber tube for 1 min. Whilst the gas is still
flowing, connect the rubber tube to the end of tube (A) and immediately open
the two-way tap to tube (A). Allow 100 ml of nitrous oxide to enter the
burette by lowering the mercury reservoir. Close the two-way taps.
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Place the mercury
reservoir in its bottom position, open the tap of the burette to make
connection with the condenser. Move the mercury reservoir until the manometer
reading is the same as the initial pressure Po. Close the tap of the burette
and by means of the mercury reservoir bring the pressure of the gas in the
burette to atmospheric pressure. The number of ml of gas represents the
non-condensible volume in 100 ml of nitrous oxide. The volume of
non-condensible gas must not exceed 3 ml. After each series of 10
determinations allow atmospheric air to enter by opening the tap (D), remove
the liquid nitrogen from the condenser and allow the condenser to warm to
room temperature.