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BỘ Y TẾ |
CỘNG HÒA XÃ HỘI CHỦ NGHĨA VIỆT NAM |
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Số: 44/2010/TT-BYT |
Hà Nội, ngày 22 tháng 12 năm 2010 |
BAN HÀNH CÁC QUY CHUẨN KỸ THUẬT QUỐC GIA VỀ PHỤ GIA THỰC PHẨM
BỘ TRƯỞNG BỘ Y TẾ
Căn cứ Luật Tiêu chuẩn và
Quy chuẩn kỹ thuật ngày 29 tháng 6 năm 2006 và Nghị định số 127/2007/NĐ-CP ngày 01 tháng 8 năm 2007 của
Chính phủ quy định chi tiết thi hành một số điều của Luật Tiêu chuẩn và Quy chuẩn kỹ thuật;
Căn cứ Pháp lệnh Vệ sinh an toàn thực phẩm
ngày 07 tháng 8 năm 2003 và Nghị định số 163/2004/NĐ-CP
ngày 07 tháng 9 năm 2004 của Chính phủ quy định chi tiết thi hành một số điều của
Pháp lệnh Vệ sinh an toàn thực phẩm;
Căn cứ Nghị định số 188/2007/NĐ-CP ngày 27
tháng 12 năm 2007 của Chính phủ quy định chức năng, nhiệm vụ, quyền hạn và cơ cấu
tổ chức của Bộ Y tế;
Theo đề nghị của Cục trưởng Cục An toàn vệ sinh thực phẩm, Vụ trưởng Vụ Khoa học
và Đào tạo, Vụ trưởng Vụ Pháp chế,
QUY ĐỊNH:
Điều 1. Ban hành kèm theo Thông tư này các Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm, bao gồm
1. QCVN 4-12:2010/BYT - Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm - Chất bảo quản;
2. QCVN 4-13:2010/BYT - Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm - Chất ổn định;
3. QCVN 4-14:2010/BYT - Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm - Chất tạo phức kim loại;
4. QCVN 4-15:2010/BYT - Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm - Chất xử lý bột;
5. QCVN 4-16:2010/BYT - Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm - Chất chất độn;
6. QCVN 4-17:2010/BYT - Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm - Chất khí đẩy.
Điều 2. Thông tư này có hiệu lực từ ngày 01 tháng 7 năm 2011.
Điều 3. Cục trưởng Cục An toàn vệ sinh thực phẩm, Thủ trưởng các đơn vị thuộc Bộ Y tế, các đơn vị trực thuộc Bộ Y tế; Giám đốc Sở Y tế các tỉnh, thành phố trực thuộc trung ương và các tổ chức, cá nhân có liên quan chịu trách nhiệm thi hành Thông tư này. /.
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Nơi nhận: |
KT. BỘ TRƯỞNG |
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FILE ĐƯỢC ĐÍNH KÈM THEO VĂN BẢN
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MINISTRY OF HEALTH |
THE SOCIALIST REPUBLIC OF VIETNAM |
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No. 44/2010/TT-BYT |
Hanoi, December 22, 2010 |
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
...
...
...
Solubility
Freely soluble in water, soluble in ethanol.
Test for potassium
Passes test.
Test for benzoate
Passes test.
5.2. Purity
...
...
...
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”).
...
...
...
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.
...
...
...
- 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.
...
...
...
- 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.
...
...
...
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
...
...
...
INS 213
ADI = 0 - 5 mg/kg bw
2. Definition
Chemical names
Calcium benzoate
C.A.S. number
2090-05-3
Chemical formula
...
...
...
Monohydrate: C14H10CaO4.H2O
Trihydrate: C14H10CaO4.3H2O
Structural formula
Anhydrous
Formula weight
Anhydrous: 282.31
Monohydrate: 300.32
Trihydrate: 336.36
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
- 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.
...
...
...
- 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
...
...
...
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
...
...
...
Chemical names
Ethyl p-hydroxybenzoate, ethyl ester of p-hydroxybenzoic acid
C.A.S. number
120-47-8
Chemical formula
C9H10O3
Structural formula
...
...
...
166.18
3. Description
Almost odourless, small, colourless crystals or a white, crystalline powder.
4. Functional uses
Preservative
5. Specifications
5.1. Identification
Solubility
...
...
...
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%.
...
...
...
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.
...
...
...
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).
...
...
...
- 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.”
...
...
...
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
...
...
...
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
...
...
...
Structural formula
Formula weight
152.15
3. Description
Almost odourless, small, colourless crystals or a white, crystalline powder.
4. Functional uses
Preservative
5. Specifications
...
...
...
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
...
...
...
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.
...
...
...
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
...
...
...
- 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
...
...
...
- 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
...
...
...
INS 220
ADI = 0 - 0.7 mg/kg bw
2. Definition
C.A.S. number
7446-09-5
Structural formula
SO2
Formula weight
...
...
...
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
...
...
...
Test for sulfurous substances
Passes test.
Oxidizing activity
Passes test.
5.2. Purity
Water
Not more than 0.05%.
Non-volatile residue
...
...
...
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
...
...
...
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
...
...
...
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.
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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).
...
...
...
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%.
...
...
...
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
...
...
...
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)
...
...
...
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.
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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.
...
...
...
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.”
...
...
...
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
...
...
...
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
...
...
...
Chemical names
Sodium disulfite, disodium pentaoxodisulfate, disodium pyrosulfite
C.A.S. number
7681-57-4
Chemical formula
Na2S2O5
Formula weight
190.11
3. Description
...
...
...
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.
...
...
...
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%.
...
...
...
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
...
...
...
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
...
...
...
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)
...
...
...
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.
...
...
...
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
...
...
...
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
...
...
...
5.1. Identification
Solubility
Soluble in water; insoluble in ethanol.
Test for potassium
Passes test.
Test for sulfite
Passes test.
5.2. Purity
...
...
...
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
...
...
...
5.3. K2S2O5 content
Not less than 90.0%.
6. Tests
6.1. Identification
Test for potassium
Passes test.
Test for sulfite
Passes test.
...
...
...
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
...
...
...
- 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
...
...
...
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
...
...
...
2. Definition
Chemical names
Potassium sulfite
C.A.S. number
10117-38-1
Chemical formula
K2SO3
Formula weight
...
...
...
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.
...
...
...
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.
...
...
...
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
...
...
...
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.
...
...
...
- 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.
...
...
...
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
...
...
...
Dhb=dehydrobutyrine
Formula weight
Ca. 3354
3. Description
White to light brown micronized powder
4. Functional uses
Antimicrobial preservative
5. Specifications
5.1. Identification
...
...
...
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
...
...
...
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):
...
...
...
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
...
...
...
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
...
...
...
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.
...
...
...
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:
...
...
...
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
...
...
...
Propionic acid
C.A.S. number
79-09-4
Chemical formula
C3H6O2
Structural formula
Formula weight
74.08
...
...
...
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
...
...
...
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
...
...
...
C.A.S. number
137-40-6
Chemical formula
C3H5NaO2
Structural formula
Formula weight
96.06
3. Description
...
...
...
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.
...
...
...
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).
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
Passes test.
Test for sodium
Passes test.
Thiosulfate
Passes test.
5.2. Purity
Loss on drying
32-37% (40-45o , 16 h, under vacuum).
...
...
...
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
...
...
...
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
...
...
...
- 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
...
...
...
- 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
...
...
...
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%.
...
...
...
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
...
...
...
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
...
...
...
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.
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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.
...
...
...
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.
...
...
...
ANNEX 6
SPECIFICATIONS AND TESTS FOR PENTASODIUM TRIPHOSPHATE
1. Synonyms
Penta sodium tripolyphosphate, sodium triphosphate,
sodium tripolyphosphae, triphosphate;
INS 451i
2. Definition
Chemical names
...
...
...
C.A.S. number
7758-29-4
Chemical formula
Na5O10P3.x H2O (x = 0 or 6)
Structural formula
Formula weight
Anhydrous: 367.86
...
...
...
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
...
...
...
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).
...
...
...
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)
...
...
...
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
...
...
...
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.
...
...
...
- 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:
...
...
...
+ 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:
...
...
...
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
...
...
...
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;
...
...
...
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
...
...
...
448.42
3. Description
Hygroscopic white granules or powder
4. Functional uses
Sequestrant, texturizer
5. Specifications
5.1. Identification
Solubility
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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:
...
...
...
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
...
...
...
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
...
...
...
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.
...
...
...
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
...
...
...
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.
...
...
...
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
...
...
...
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.
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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
...
...
...
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).
...
...
...
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.
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Thông tư 44/2010/TT-BYT về Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm do Bộ trưởng Bộ Y tế ban hành
| Số hiệu: | 44/2010/TT-BYT |
|---|---|
| Loại văn bản: | Thông tư |
| Nơi ban hành: | Bộ Y tế |
| Người ký: | Trịnh Quân Huấn |
| Ngày ban hành: | 22/12/2010 |
| Ngày hiệu lực: | Đã biết |
| Tình trạng: | Đã biết |
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Thông tư 44/2010/TT-BYT về Quy chuẩn kỹ thuật quốc gia về phụ gia thực phẩm do Bộ trưởng Bộ Y tế ban hành
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