SPECIFICATIONS FOR THE IDENTITY

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INOE., .;J

SPECIFICATIONS FOR THE IDENTITY

AND PURITY OF SOME EXTRACTION SOLVENTS AND CERTAIN OTHER SUBSTANCES

•

Food and Acriculture Orcanization of the United Nations World Health Orcanization

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FAO Nutrition Meetings Report Series No. 48B;

WHO/Food

Add./70.40

SPECIFICATIONS FOR THE IDENTI'l'Y AND PURI'l'Y OF SOME EXTRACTION SOLVEH'l'S AND

CERTAIN O'l'HER SUBSTANCES

Issued jointl.7 b7 PAO and WHO

The contents of this document are the result of the deliberations of the J~int FAO/WH.O Expert Conmittee on Food Additives which met in Geneva, 24 June - 2 July

197o1/

World Health Organization

Food and Agriculture Organization of the United Nations Rome, 1971

J/

Evaluation of Food Additives:

Fourteenth Report of the Joint FAO/WHO Expert Committee on Food Additives. FAO Nutrition Meetings Report Series No.

48;

Wld. Hlth.Org. Tech. Rep. Ser.,

1970,

No. 462

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TABLE OF CONTENTS

~

Introduction 1

A. Miscellaneous Food Additives and Contaminants 3

Brominated Vegetable Oils

5

Cupric Sulfate

7

Curcumin 9

Cyclamates, Calcium, Sodiu~ and Cyclohex;yl-

sulfamic Acid 12

Ethyl Maltol

15

Gelatin - edible

17

Mineral Oil - libod Grade 20

Monosodium L-Glutamate 23

Oleoresin Paprika

25

Sodium Caseinate 27

Stannous Chloride 30

Turmeric

B. Filtration Aids and Related Substances Activated Vegetable Carbon (Food Grade) Tannina(Food Grade)

c.

Extraction Solvents Acetone

1₁2-Dichlorethane Dichloromethane Ethanol

Methanol Hexane

32

37 39

41

45

47 49

51

53

56

58

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IV

Heptane Propan-2-ol.

1,1,2-Trichloroethylene Annex

Methods of Analysis for Solvents

1. Determination of Residue on Evaporation 2. Determination of Distillation Range

2.1 Method A 2.2 Method B

3. Determination of Acidity and Alkalinity 3.1 Acetone, Ethanol, Propan-2-ol, and

Methanol

~

62 64 67 69 69 69 69 69

75

77

77 3.2 1,2-Dichlorethane and Dichloromethane 78

3.3 Trichloroethylene 79

4. Determination of Aldehydes and Ketones 4.1 Ethanol, Propan-2-ol

4.2 Methanol

5. Determination of Aromatic Hydrocarbons in Hexane and Heptane

6. Determination of Ultraviolet Absorbance in Hexane and Heptane

82 82 83

88

7.

Determination of Sulfur in Hexane and Heptane 104 8. Determination of Lead in Hexa..~e and Heptane 120

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INTRODUCTION

The specifications and identity tests contained in this publication were prepared at the Fourteenth Session of the Joint

.

FAO/WHO Expert Committee on Food Additives (Geneva, 24 June to 2 July 1970) for the substances for which, in the consideration of the Committee, adequate information a.nd data were available.

The Monographs should therefore be consulted together with the Report of the above mentioned meetingl/. In particular, attention is drawn to the following paragraphs, namely, the principles goveni.ing the establishment of chemical specifica,- tions (Section 2), special considerations relating to solvents (Section 4) and the comments on substances on the agenda

(Section

5).

Here are explained the reasons for the absence of specifications for certain substances which were on the agenda and th.e tentative nature of others or their presence as

identification tests rather than as full specifications. The test solutions and some general method.a of eJCamination mentioned in the specifications are those appearing in earlier

publications listed in the General References.

For detailed monographs on to%icological evaluation of these substances, a reference is invited to the publication

"To%ioological Evaluation of Some Extraction Solvents and Certain Other Substances", FAO Nutrition Meetings Report Series 48A, WHO/Food Add. 70.39.

Evaluation of Food Additives.

Fourteenth Report of the Joint FAO/WHO Expert Committee on Food Additives. FAO Nutrition Meetings Report Series No.

48,

World Health Organization Technical Report, Series HO. 462

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2

Any information and comments relating to the specificatiorE or methods of examination of these substances should be addressed to: Food Control, Standards and Additives Section,

Nutrition Division, FAO, Rome, Italy.

Comments and additional information, if any, relating to biological data should be addressed to: Food Additives Unit, World Health Organization, Avenue Appia, Geneva, Switzerland.

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A. MISCELLANEOUS FOOD ADDITIVES AND CONTAMINANTS

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SYNONYMS CHEMICAL NAMES

BROMINATED VEGETABLE

ons

(Identification only) Brominated oils

CHEMICAL DF.sCRIPTION A bromine addition product of vegetable

DF.sCRI~ION

IDENTIFICATION TESTS A. Solubility

oil or oils.

A pale yellow to dark brown, viscous oily liquid having a bland or fruity odour and a bland taste.

Water: insoluble Ethanol: insoluble Chlorofonn: soluble Ether: soluble Hexane: soluble

B. To 0.2 g of the sample, add 1 g of a.neydrous sodium carbo- nate, and heat gently to carbonize. Cool, add 5·m1 of water, stir and filter. Acidify slightly the filtrate with dilute nitric acid, heat in a water bath for 5 minutes, and cool. The solution responds to the tests mentioned below:

(i) Addition of silver nitrate T.S. yields a light yellow precipitate which is insoluble in dilute nitric acid or ammonia T.s. Separate the precipitate. Add strong ammon:ia.

T.S. to the precipitate and shake. The separated liquid When acidified with dilute nitric acid, yields white turbidity.

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6

(ii) Addition of chlorine T.S. yields a yellow to reddish brown colour. When a. portion of the resultant solution is shaken with chlorofonn or carbon disulfide, the lower layer produces yellow to reddish brown colour. Another portion of the resultant solution yields a white precipitate with phenol.

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SYNONYMS CHEMICAL NAME

CUPRIC SULFA'l'E

Copper sulfate, blue stone Cupric sulfate

CHEMICAL ^FORMtJIA CuS0

4 •

5H₂

o

MOLECULAR WEIGHT 249.68 DEFINITION

DESCRIPrIOH

USES

Cupric sulfate contains not less than 98.5 per cent and not more than 104.5% of CuS0

4• 5H2

o.

It conforms ·to the following specifications.

Deep blue, triclinic crystals, or blue, crystalline granules or powder. Has a nauseous, metallic taste, and effloresces slowly in dry air.

Colour fixation, selective antimicrobial in some particular cheese ripening.

IDERTIFICATIOH TESTS A. Solubility Water:

Boiling water:

Alcohol:

freely soluble very soluble slightly soluble B. The solution is acid to litmus.

c.

A solution of Cupric Sulfate { 1 in 10) responds to the tes1B tor copper and for sulfate.

PURI'l'Y T!3TS

Acidity and clarity of solutioe: Dissolve 1 gin 20 ml of wattr a clear blue solution is produced. Add 0.1 ml of methyl orange solution: the soluticn

turns brownish green.

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8

Insoluble matter: Not more than 50

mg/kg

Arseni~: Not more than 8

mg/kg

Hea~ metals: Not more than 20 mg/kg ASSAY

Weigh accurately about 1 g of Cupric Sulfate, dissolve it in 50 ml of water, add

4

ml of acetic acid and 3 g of potassium iodide, and titrate the liberated iodine with 0.1

!

Sodium thiosulfate, using starch T.S. as the indicator. Perform a blank determination, and make a:ny necessary correction. Each ml of 0.1

!

Sodium thiosulfate is equivalent to 24.97 mg of CuS0

4 •

5H

20.

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CURCUMIN*

SYNONYMS AND VARIETIES C.I. Natural Yellow 3; Lebensmittel-

CLASS

CODE NUMBERS

CHEMICAL NAME

EMPIRICAL FORMULA STRUCTURAL FORMULA

MOLECUIAR WEIGHT DEFINITION

DISCRIPl'ION

Gelb Nr. 6

Curcuma; Curcumine Di-cinnamoyl methane

c.I.

(1956) No. 75300 ( 1924) No. 1238 Schultz (1931) No. 1374

1,7-bis (4-hyd.ro:r;y-3-metho:x;yphenyl)- 1,6-heptadiene-3.5-dione

368.39

The content of curcumin is usually stated in the conunercial product used for colouring food.

Curcumin is an orange-yellow, crystalline powder, insoluble in water and

• Th.is specification for curcumin replaces the one given in

"Specifications for Identity and Purity of Food Additives (Food Colors): Fourth Report" subsequently published as

"Specifications for Identity and Purity of Food Additives.

Vol. II. Food Colors, FAO, Rome, 1963^{11 •}

9

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10

USES

IDENTIFICATION TESTS

ether, soluble in ethanol and glacial acetic acid.

Colour

A. Curcwnin solution in alcohol is characterized by pure yellow colour and light green fluorescence; if this ethanolic extract is added to concentrate eulfuric acid, a deep crimson colour is produced.

B. Melting point: 183°

c.

Boric acid test: Treat an aqueous or dilute ethanolic solution of ^ourcwninwith hydrochloric acid until a slightly orange colour begins to appear. Divide mixture into 2 parts and add some boric acid powder or crystals to one portion. Marked reddening will be quickly apparent, best seen by comparison with portion to which the boric acid has not been added. The test ffl8u' also be made by dipping pieces of filter paper in ethanolic solution of colouring matter, drying at 100°, a.nd then moistening with a weak solution of boric acid to which a few drops of hydrochloric acid have been added. On drying, a cherry-red colour will develop.

PURITY TESTS

Arsenic {as As): Not more than 2 mg/kg Lead (as Pb): Not more than 2.5 mg/kg

ASSAY

A. Place on a water bath at 90° a 100 ml grad~ated flask containing 60 ml of glaci~l acetic acid and 0.100 g of curcumin. Keep it on the bath for 1 hour. Then add 2 g <:f

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boric acid and 2 g of oxalic acid and keep the flask on the bath for 10 minutes more. Cool at room temperature and fill it to the mark with glacial acetic acid. Shake very well. Pipette 5 ml of the mixture to a 50 ml measuring flask and fill it to the mark with glacial acetic acid.

Then measure the extinction of the red coloured solution and that of the glacial acetic acid in a 1 cm cell at 540 nm.

B. Calibration curve: Dissolve 0.100 g of pure curcumin, by heating, with glacial acetic acid in a 1000 ml measuring flask. Pipette

5,

10, 15 ml, etc. of this solution into 100 ml meaBllring flasks together with boric acid and oxalic acid as under A. Prepare the calibration curve.

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12

CYCLAMATES₁CAWIUM₁ SODitJM;AND CYCLOHEXYIBULFAXIC ACID (Amendments to the Specifications*)

- Under "Purity Tests":

Cyclohex;yla.mine: reduce 100 mg/kg to 25 mg/kg

Di-cyclohex;yla.mine: not more than 2 mg/kg After ¹¹Assa.y'1 , add the following:

EXAMINATION

Determination of cyclohexylamine

Methyl orange-boric acid solution. Dissolve 200 mg of methyl orange and 3.5 grams of boric acid in 100 ml of water, heating on a steam bath to effect solution. Allow to stand for at least 24 hours, and filter before use.

Standard solution. Transfer 100.0 mg of cyclohex;yla.mine into a 100-ml volumetric flask, dissolve in 50 ml of water and 0.5 ml of hydrochloric acid, dilute to volume with water, and mix. Transfer 5.0 ml of the solution into a second 100-ml volumetric flask, dilute to volume with water, and mix.

Transfer 5.0 ml of this solution into a third 100-ml volumetr:ic flask, dilute to volume with water, and mix. Each ml of this solution contains 2.5 mcg of cyclohex;ylamine.

Test preparation. Transfer 10.0 grams of the sample into a 100-ml volumetric flask, dissolve in water, dilute to volume with water, and mix.

*

Specifications and Criteria for Identity and Purity of Some Flavouring Substances a.nd Non-Nutritive Sweetening Agents.

FAQ Nutrition Meetings Report Series No. 44B; WHO/Food Add./

69.31, Rome 1969. JECFA/45/11/1967, JECFA/50/11/1967 and JECFA,747/11/1967.

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Procedure. Transfer 10.0 ml each of the Standard prepara-

~ and of the Teat preparation into separate 5o-m1 glass- stoppered centrifuge tubes, and transfer 10.0 ml of water to a third tube to serve as a blank. To each tube add 3.0 ml of disodium ethylenediaminetetraacetate solution {prepared·by dissolving 10 grams of disodium ethylenediaminetetraacetate and 3.4 grams of sodium hydroxide in 100 ml of water) and 15.0 ml of a 20 : mixture of chloroform and n-butanol, shake the tubes for 2 minutes, and centrifuge. Remove and discard the aqueous l&iYer in each tube, and then transfer 10.0 ml of the chloroform solution from each tube into separate centrifuge tubes. 'l'o ea.eh tube add 2.0 ml of Methyl orange-boric acid solution, shake the tubes for 2 minutes, and centrifuge. Remove and discard the aqueous l&iYer in each tube, then add to each tube 1 gram of anhydrous sodium sulfate, shake well, and allow to settle. Transfer 5.0 ml of each clear chloroform solution into separate test tubes, add 0.5 ml of a 50: 1 mixture of methanol and sulfuric acid, and mix. Concomitantly determine the absorbance of the solutions in 1-cm cells at 520 nm with a suitable spectrophotometer, using the blank to set the inatru- ment. The absorbance of the solution from the Test prepa.ratim does not exceed that from the Standard preparation.

For Cyclohexylsulfamic acid

Proceed as above using the following as the Teat prepa.ra-

!!2!=

Transfer 10.0 grams of the sample into a 100-ml volumetric flaalc containing 20 ml of water, mix, and add 60 ml of sodium hydroxide 'l'.S. Add dilute hydrochloric acid 'l'.S. or sodium eydroxide 'l'.S., if neceaaary, to make the solution

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alkaline to 1i tmu.s.

Determination of di-cyclohexylamine

Dissolve 50 g of cyclamate in 300 ml of water, add 3 ml of sodium hydroxide T.s., and extract with 50 ml and 30 ml of chloroform. Combine the extracts, add 2 g of anhydrous potassium carbonate and filter. Wash the container and the residue on the filter paper several times with

5

ml chloroform-. combine the washings to the filtrate and concentrate to 1 ml under 30°c. To this solution add 1 ml of nitrobensene standard solution (100 mg in 500 ml chloroform) as an internal standard and examine for di-cyclohe:z;ylamine by gas chromatography using a flame ionization detector under the conditions described below. Calculate the di-cyclohe:z;ylamine content from a standard curve.

- Di-cyclohe:z;ylamine (c

12H

23) N for the standard curve:

Ref. index ~5 1.480-1.488 Relative density d~~- 0.905-0.915 Boiling point 254-256°

1.-5 m stainless steel column 3-4 mm of inside diameter packed with 6o-80 mesh diatomaceous earth (gas chromatographic grade) in a solution of methanolic potassium hydroxide: the final potassium hydroxide concentration should be about 3 per cent of the diatamaceous support. Evaporate off the methyl alcohol, add a chloroform solution of polyethyleneglycol 6000, and evaporate the chloroform. The content of polyethyleneglycol 6000 should be about 10 per cent of the diatemaceous support.

- Colunm temperature: 130-140°.

Carrier gas: Nitrogen or helium. Flow rate should be 14 that to outflow nitrobenzene after about 7 minutes.

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CHEMICAL NAMES EMPIRICAL FORMULA STRUCTURAL FORMULA

MOIECULAR WEIGHT DEFINITION

DESCRIPJ.'ION

USES

IDENTIFICATION TESTS A. Solubility

B. Melting range:

PURITY 'l'ESTS

ETHYL MALTOL

3-Hyd.ro::x;y-2-ethyl-4-pyrone

140.14

Ethyl maltol contains not less than 98 percent of

c

7^H8

o

3 and conforms to the following specifications.

A white, cr,ystailine powder having a characteristic odour and a sweet, fruit- like flavour in dilute solution.

Flavouring agent, flavour enhancer.

Water: sparingly soluble Alcohol: soluble

Chloroform: freely soluble

Not more than 0.5 percent by weight (Karl Fischer Method)

Su.lfated asht Not more than 0.2 percent by weight Arsenic: Not more than 3 mg/kg

Heavy metals (as Pb): Not more than 20 mg/kg

~ : Not more than 10 mg/kg

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16

ASSAY

Prepare a solution of ethyl maltol in 0.1

!!

hydrochloric acid containing 10 )Lg/ml, and determine the extinction at 276 nm.

Calculation:

E1

1

%

of sample

- cm ^~

- - - x 100 • 70 ethyl maltol E1

1% of a pure - cm

EXAMINATION

standard reference specimen

Determination of water: Karl Fischer Method - See "Specifica,- tions for Identity and Purity of Food Additives" Vol. I.

Antimicrobial preservatives and antioxidants. FAO, Rome 1962.

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EDIBLE GELATIN

SYNONYMS Edible gelatin

CHEMICAL NAMES Gelatin

CHEMICAL DESCRIPl'ION A protein produced by partial hydrolysis of collagen in skin, tendons, ligaments, bones, etc. of animals.

DESCRIPl'ION Sheets, flakes, or shreds, or coarse to fine powder, fainty yellow or amber in colour, the shade varying in depth according to the particle size and with a slight characteristic bouillon-like odour and taste. Stable in air when dry, but is subdeot to microbial decom- position when moist or in solution.

ADDITIONAL CRITERIA. The article of commerce~ further specify special requirements for criteria such as gel strength and limits of iron, calcium, lactose or other chemical.

or microbiological* requirements.

USES Stabilizing agent, gelling agent, emul- sifying agent and crystallization inhi- bitor in food.

ID!S!IFICJ..TION TESTS

A. Solubility Insoluble in cold water, but swells and soft- ens when immersed, gradually

• e.g. concerning selected pathogenic organisms including Salmonella, Stapn.ylococcus aureus, Clostridium spp. and

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18

absorbing from 5 to 10 times its own weight of water; soluble in hot water, forming a jelly on cooling.

Acetic acid: soluble Ethanol: insoluble Chloroform: insoluble Ether: insoluble

B. To a solution {1 in 100) add trinitrophenol T.S. or a solution of potassium dichromate {1 in 15) previously mixed with about one-fourth its volume of dilute hydrochloric acid: a yellow precipitate is formed.

c.

^To a solution {1 in 5000) add tannic acid T.S.: Solution becomes turbid.

D. When heated with soda lime, ammonia is evolved.

E. To a solution {1 in 100) add mercuric nitrate solution; a white precipitate is formed which develops a brick red colour on warming.

PURITY TESTS Loss on drying:

Ash:

Odour and water insoluble substances:

Not more than 18 per cent by weight (100-105°, 6 h)

Not more than 2 per cent

A hot solution (1 in 40) is free from any disagreeable odour and taste; whei viewed in a layer 2 cm thick, shows not more than a slight opalescence.

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Microbiological*

requirements:

Sulfur dioxide:

Arsenic:

Heavy metals:

1. Standard plate count

<

104/g

2. Enterobacteriaceae or bacteria of the coli-aerogenes group <::.10/g

3. La.ncefield group D streptococci <.102 / g Not more than 40

mg/kg

Not more tha.n mg/kg Not more tha.n 5

mg/kg

Not more tha.n 50 mg/kg

* Tentative only. More infonnation required.

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20

FOOD GRADE MINERAL OIL SYNONYMS

CHEMICAL DESCRIPTION

DEFINITION

DESCRIPI'ION

USES

Liquid petrolatwn

A mixture of refined liquid .hydrocarbon obtained from petroleum

This specification excludes certain other types of white mineral oil to which anti-oxidants 11183' be added for technological purposes.

Addit;onal criteriaa

'l'he article of oonnerce ma.v be further specified as to its specific gravity, viscosity, depending upon its technological use.

Food grade mineral oil is a colourless transparent and oily liquid and nearly free from fluorescence. It is odourlem

and tasteless.

Release a.gent, sealing reagent.

A. It burns with bright flame and with paraffin-like characteristic offensive smell.

B. When heated with sulfur, it produces .hydrogen sulfide-like smell.

PURITY TESTS

Free acid and free alkali: Passes test

Add a.bout 10 ml of hot water and a drop of phenolphthalain ,n.s. to 10 ml of' the sample a.>J.d

shake vigoroasly. The sobtion

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Petroleum:

Readily carbonizable substances:

PolYnuclear aromatic .tqdrocarbons:

does not turn red. Furthermore, add about 0.2 ml of 0.02

!!

sodium hydroxide solution to the mixture, and shake it. The mixture turns red.

When heated on a wateI'-bath, it does not produce petroleum-like smell.

Passes test

Place 5 ml of the sample into a cleaned and dried glass stoppered test tube, add

5

ml of

94.5i

to

94.~

sulfuric acid. Shake up and down vigorously for 5 seconds at intervals of 2 minutes each while heating for 10 minutes on a water-bath. White mineral oil does not change colour and the colour of the sulfuric acid laiyer is not darker than that of a standard colour produced by mixing in a similar tube 3 ml of ferric chlori12

c.s.,

1.5 ml of cobaltous chloride

c.s.

and 0.5 ml of cupric sulfate c.s., this mixture being overlaid with 5 ml of mineral oil.

The abaorbance does not exceed 0.10 at wave lengths between 260 nm and 350 Diile

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Sulfur compounds:

Arsenic:

22

Passes test

Prepare a saturated solution of lead monoxide in a solution of sodium hydroxide (1 in 5)1 and mix 2 drops of the clear solution with

4

ml of the sample and 2 ml of absolute alcohol. The mixture, after being heated at 70° for 10 minutes and then cooled, is not darker than a blank consisting of

4

ml of the sample and 2 ml of absolute alcohol.

Not more than 1

mg/kg

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SYNONYMS CHEMICAL NAMES EMPIRICAL FORMULA.

STRUCTURAL FORXULA.

DEPIJIITION

DllSCRIPl'IOJI

MONOSODIUM IALUTAMA'l'E*

Sodium glutamate, MSG

Monosodium L-gluta.mate monohydrate

c

5

liao

₄^'NNa.H₂⁰

HOOC

9H

^CH_2cH2^{COOHa - H}₂^o

I .

NH2

Monosodium L-glutamate contains not leas than 9~ of

c

58e,O lDla.H2

o

and conforms to the following specification.

White, pracUcally odourless crystals or crystalline powder, with a characteristic taste.

Flavour enhancer IDEllTIFICA'l'ION 'l'ES'l'S

A.

B.

Solubility Water: freely soluble Ethanol: sparingly soluble Ether: practically insoluble

Positive teat f'or amino acid: to 1 ml of' a 1 in 30 aoluticn add 1 al of ~ 'l'.S. and 100 mg of sodium acetate,

and. heat in a boiling water bath for 10 minutes. An intense violet-blue colour is formed..

c.

^Foai^{t i}ve teats f'or aodiwa.

*

Replaces tentative specifications given earlier in ¹¹Specifi- oationa for the.Identity and Purity of some Food Colours, Blllu.laif'iera, Stabilisers, Anti-caking Agents and Certain

Otiher Su.bataaoe.-. FAO Butrition Meetings Report. Series

•o.

46B;

WID/Poo4 AM./70.37, Rome 1970.

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24

PURITY TESTS Loss on drying:

.ll!!=

Not more than 0.5% (97-99°, 5 h)

pH of a 1 in 20 solution is between 6.7 and 7.2

Specific rotation~~o + 24.8 to+ 25.30 (10 gin 100 ml of

Chloride:

Arsenic:

~ :

HeavY metals:

7%

hydrochloric acid, 200 mm tube) Not more than

o. 21,

Not more than 2

mg/kg

Not more than 5 mg/kg Not more than 10 mg/kg

ASSAY

Dissolve about 250 mg accurately weighed, in 100 ml of glacial acetic acid. A few drops of water may be added prior to the addition of the acetic acid to effect faster dissolution of the sample. Titrate with 0.1 N perohloric acid in glacial acetic acid, detennining the end-point potentio-metrically.

Each ml of 0.1 N perohloric acid is equivalent to 9.356 mg of

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OLEORESIN PAPRIKA

SYNO:tlYMS Paprika oleoresin, paprilc&-extract CHEMICAL NAME

CHEMICAL DESORIP!'ION The product obtained by solvent extract- iont&ethylene chloride, ethylene dichlo-

DESCRIPl'ION

USBS

IDDHPICA'fION .l. Solubility

ride, trichloroethylene, acetone, propan-2~1, metlcy-1 alcohol, he%.&ne₁ ethyl alcohol} of the pods of Capsicum an.nuum L. , with the subsequent removal of the solvent. Contains capsaicin (c₁₈H

2-,Ho

3} carotenoid pigment with the following structural formula:

capco(CH2)4CH • CH CH (C~)2

0

^OH ⁰⁰^~

A deep red somewhat _,,,..

vi,soid.

liquid with characteristic odour and peppery (hot) taste. Article of commerce ID8u' also be specified for its colour value.

Colouring and flavouring a.gent.

Waters almost insoluble

Ethanol: partly soluble with oily separation

Glycerine: insoluble

Mineral oil: very slightly soluble

25

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26

Ethyl acetate: soluble Halogenated

hydrocarbons: soluble

B. '!'he solution in n-hexa.ne shows maximum absorptions at the wave lengths of about 470 run.

c.

To one drop, add 2-3 drops of chloroform and one drop of sulfuric acid. Deep blue colour is produced.

PURITY TESTS

Methylene chloride:

l

Ethylene dichloride:

Trichloroetn.ylene:

Acetone:

Propan-2-ol:

Methyl alcohol:

Henne:

Arsenic:

Heav:y metals:

Not more than 30 mg/kg singly or in combination

Not more than 30 mg/kg Not more than 50 mg/kg Not more than 50 mg/kg Not more than 25 mg/kg Not more than 3 mg/kg Not more than 5 mg/kg Not more than 20 mg/kg

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SYNONYMS CHEMICAL NAME DEFINITION

DESCRIPl'ION

USES

SODIUM CASEINATE Casein-sodium

Sodium caseinate

Sodium caseinate is an addition compound of sodium and casein. It, after drying'for 3 hours at 100° ₁ contains not less than 12.~

of nitrogen, and conforms to the following specifications.

Add.i tional cri terias

Article of commerce ma.y also be further specified for maximum limits of fat and lacto·

se content, or other chemical or microbiological* requirement.

White or pale yellow granules or powder, practically odourless.

Emulsifier and stabilizer.

A. Solubility Water: disperses slowly with some turbidi\

Soluble in boiling water.

Ethanol: insoluble

B.

on

ignition, sodium caseinate emits a characteristic and disagreeable odour, and leaves a residue which is alkaline to litmu.s.

c.

Dissolve 0.1 g in 10 ml of sodium hydroxide T.S. ₁ add 1 drq, of cupric sulfate

T.s.,

^andshake. A blue precipitate is formed, and a violet colour is produced.

*

e.g. concerning selected pathogenic organisms including Salmonella, Staphylococcus aureus, Clostridium spp. and mould spores.

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D. Dissolve 0.1 g in 10 ml of sodium hydroxide T.s., and acidify slightly with acetic acid. A white woolly precipitate is formed.

E. To 0.1 g add 5 ml of water, shake, add 10 drops of mercuric nitrate T.s. and 1 drop of sodium nitrite T.s., and heat in a water bath for 3 minutes. A reddish brown to reddish violet colour/is produced on the surface of swelled sodium caseinate.

PURITY TESTS

Solubility in water:

Loss on drying:

Sulfated ash:

Bacteriological requirements*:

Passes test

To 0.1 g previously dried over sulfuric acid in a vacuum desiccator for

4

hours and powdered finely, a.dd 30 ml of water, shake and allow to stand for 10 minutes.

Add 2 ml of 0.1 N sodium hydroxide, warm at 40°, and dissolve by shaking.

Cool, add water to 100 ml. The solutiai is colourless, and shows no more turbidity than slightly turbid.

6.0,..7.5

of a solution

(1

in

50)

Not more than 15'%> after drying for 3 hours at 100°.

Not more than 6'fo on dry basis 1. Standard plate count

2. Enterobacteriaceae or bacteria of the coli-aerogenes group

28

*

Tentative only. More information required.

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Arsenic:

Heavy metals:

3. La.ncd'iald group D steptococci Not more than 2 mg/kg

Not more than 20 mg/kg ASSAY

Nitrogen content. Weigh about 0.15 g of sodium caseinate accurately, previously dried 3 hours a .. 100° , and proceed as directed under the assay of nitrogen (Kjeldahl method). Each ml of

o.

1 H sulfuric acid is equivalent to 1.401 mg of nitrogen

29

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SYNONYMS CHEMICAL NAME CHEMICAL FORMULA.

MOLECULAR WEIGHT DEFINITION

DESCRI?rION

USES

STANNOUS CHI.ORIDE Tin dichloride

Stannous chloride dihydrate

Stannous chloride contains not less than 98 per cent and not more than 102 per cent of SnCL

2 • 2H

2

o.

It conforms to the following specifications.

Colourless or white crystals. Is odourless or having slight odour of hydrochloric acid.

Reducer or antioxidant in some bottled or lacquered canned vegetables.

A. Solubility Water: soluble in less than its own weight of water, but it forms an insoluble basic salt with much water.

Dilute hydro-

chloric acid: very soluble Ethanol:

Glaoia.l acetic acid:

soluble soluble

B. To a solution of Stannous chloride in dilute hydrochloric acid T.s. add mercuric chloride T.s. White or greyish white precipitate forms.

c.

^Toa solution of Stannous chloride in dilute hydrochloric acid T.s. add a solution of arsenious acid. Black precipi- 30 tate forms.

(36)

PURITY TESTS Hydrochloric acid

insolubles:

Sulfate:

Arsenic:

Other heavy metals:

Passes test

Heat 5 g of Stannous chloride to 40°

in a mixture of 5 ml of water and 5 ml of hydrochloric acid. The salt should dissolve completely, and the solution should be clear.

Passes test (limit about 30 mg/kg) Not more than 2 mg/kg

Not more than 60 mg/kg ASSAY

Transfer about 2 g of sample, accurately weighed, to a 250 ml volumetric flask, dissolve in 15 ml of hydrochloric acic dilute to volume with water, and mix well. Transfer 50 ml of this solution to a 500 ml Erlenmeyer flask, and add 5 g of potassium sodium tartrate, and then a cold saturated solution of sodium bicarbonate until the solution is alkaline to litmus paper. Titrate at once with iodine solution using starch indicator solution. Each ml of 0.1

M

iodine solution consumed is equivalent to 0.01128 g of SnC12 • 2H20.

31

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32

SYNONYMS

DEFINITION

DESCRIPrION

USES

TURMERIC*

Powdered turmeric; curcuma; curcumine; sa.fran des Indes; Indian saffron

The ground rhizome of Curcuma. IDnga. L. contairs usually

1-5%

of curcumin, orange-yellow pigmeri;

having the following structural formula:

Yellow-brown to dark yellow-brown powder with characteristic flavour and taste. It contains yellow gelatinized starch masses; vascular bundles; and broken pieces of oil cells.

Does not contain stone cells, collenchymatous cells, and raphids or rosette aggregates of calcium oxalate. It should be free from dirt, mould growth and insect infestation, and free from musty odour.

Food colour

*

This specification for turmeric replaces the one given in

"Specifications for Identity and Puri t.v of Food A.ddi ti ves food Colours): Fourth Report", subsequently published as

"Specifications for Identity and Purity of Food Additives, Vol. II, Food Colours,,FAO, Rome 1963.

(38)

A. Solubility Water: insoluble Ethanol: insoluble

B. Add 1 drop of boric acid solution ( 1 in 50). A dark red- brown colour develops.

loaa on ciqing:

Total ash:

Acid :insoluble ash:

Artificial colouring matter:

Chromate test:

Not more than 10 per cent Not more than 7 per cent Not more than 1.5 per cent Passes teat

To 1.0 g of pulverized turmeric add 20 ml of 60 v/v 1, ethanol, boil for 30 minutes under a reflux condenser, then cool, and filter. Place 3 ml of the filtrate in a small beaker of 30 mm each in internal diameter and height, hang a piece of filter paper, 20 mm by 300 mm, over the beaker so that one end of the filter paper reaches the bottom of the vessel; allow the paper to soak the liquid for 1 hour, and pull up the paper; no yellow or red colour retains in the upper portion of the paper.

Irradiate this paper with filtered ultraviolet ra.ys in a dark room: ^any fluorescence is not observable.

Passes. test

(39)

34

Lead ( as Pb) : EXAMINATION

4 to 5 ml of dil. sulfuric acid in a test-tube and 1 ml of diphenyl carbazide solution

(O.~

v/w in 95i alcohol) added.

The presence of chromate is indicated by the production of violet colour.

Not more than 2.5 mg/kg

Estimation of Curcwnin content Apparatus

1. 100 ml flat-bottomed extraction flask with TS 24/40 ground joint.

2. West type condenser with water cooled drip-tip and TS 24/40 ground joint 300-400 mm in length.

3. 250 ml and 10 ml volumetric flasks with TS stoppers.

4. Spectrophotometer capable of accurately measuring absorbance at 425 nm.

Reagents

1. Ethano 1 95~

2. Standard curcwnin solution: 25 mg of purified curcwnin is weighed into a 100 ml volumetric flask, dissolved and diluted to mark with alcohol. 1 ml of the solution is transferred to a 100 ml volumetric flask and diluted to mark with alcohol. This standard solution contains 0.0025 g/litre.

Procedure. 0.1 g of turmeric powder is weighed in the extraction flask. 30 ml of the alcohol is added and refluxed for 2

i

hrs. The extract is cooled and filtered quantitatively into a 100 ml volumetric flask. The extracted residue is transferred to the filter. The residue is thoroughly washed

(40)

and diluted to mark with alcohol. 20 ml of the filtered extrad;

is pipetted into a 250 ml volumetric flask and diluted to volume with the alcohol. The absorbance of the extract and the standard solution is measured at 425 nm in 1 cm cells against an alcohol blank.

Calculations

~ Curcumin in turmeric • Absorbance of extract at Cell length cmJ x a x Where (a) ^M Absorbance of Std solution nm

cell length cm x cone.

35

(41)

(42)

B. FILTRATION AIDS AND REIATED SUBSTANCES

(43)

(44)

SYNONYMS

DESCRIPl'ION

USES

ACTIVATED VEGETABLE CARBON (Food Grade)

Activated charcoal, pure vegetable carbon, activated vegetable carbon.

Activated vegetable carbon is prepared by car- bonising under controlled conditions of vegetable matter, such as lignite, peat, wood and coconut shell. It may then be further treated by physical or chemical processes to increase its adsorptive power. It is a black, odourless, tasteless solid of particle size varying from coarse granular to fine powder, conforming to the following specifications. In addition, the article of commerce may specify adsorption power, and iron, Ca or Zn content.

Decolourizing and deodorizing agent, purifying and clarifying agent applied to both aqueous and non-aqueous media.

A. Solubility water insoluble

B. Mix well with water and filter; the filtrate has no colour and no odour.

c.

Ignite in a crucible without a lid; it is rod-heated and produces ash gradually.

D. Suspend 2.5 g of the sample in 50 ml of water; add 2 ml of 4N hydrochloric acid to acidify the suspension and boil gently for 5 minutes. After cooling; add 2 ml of iodine TS,

(45)

40

Mix well and filter. The colour of the filtrate is not darker than that produced by the sA.me procedure without using activated vegetable carbon.

PURITY TESTS Loss on dging:

Sulfated ash:

Acid-soluble substances:

Uncarbonized constituents:

Higher aromatic hydrocarbon:

Arsenic:

Not more than 15 per cent ( 120°, 4 h) Not more than 10 per cent

Not more than

3.5

per cent Passes test

Boil 250 mg with 10 ml of sodium hydroxide T.S. for 5 seconds, and filter: the filtrate is colourless.

Passes test

Extract 1 g of sample with 10 g of pure cyclohexane for 2 hours. The extract should show no colour and no more fluorescence than a solution of 0.1 mg of quinine sulfate in

litre of 0.1 N sulfuric acid in ultraviolet light. Also, the extract should leave no residue on evaporation.

Not more than 2 mg/kg in dilute nitric acid extract

Not more than 10 mg/kg

(46)

TANNINS

(Food Grade) (Tentative) SYNONYMS

CHEMICAL DESCRIPTION

Tannic acid; gallotannic acid

This specification relates only to hydrolysable tannins which yield gallotannins (based on derivatives of gallic acid) on hydrolysis. Many other kinds of tannins also occur in nature, including condensed (non-hydrolysable) tannins and those which on hydrolysis yield ellagitannins (based on derivatives of hexahydro.x;y o-dibenzoic acid); the hydrolysable tannins can also be dis- tinguished from the condensed tannins in that the latter yield catechol (o-dihydro:zybenzene) on dry distillation while the former pyrogallol (1, 21

3-trihydro.x;ybenzene). Hydrolysable gallotannins may be obtained from nut- galls, the excrescences which form on young twigs of various Quercus spp.

e.g. Q. infectoria; these include Chinese and Aleppo tannins. They may also be obtained from various Sumac species, e.g. Rhus Corieria, R. galabra1

R. typhia; these include Sicilian and American Sumacs. All of these consist essentially of polydigalloyl esters of

(47)

42

DESCRIPl'ION

USES

glucose. A further source of hydrolysa,.

ble gallota.nnins are seed pods of Tara (Caesalpinia Spinosa): these tannins consist essentially of the polydigalloy.1.

esters of quinic acid.

An amorphous powder, as glistening scalEB or spongy masses, varying in colour fran yellov:i.ah white to light brown. Odour-

less or with a faint, characteristic odour a.nd an astringent taste.

Clarifying agent.

A. Solubility Water: very soluble Alcohol: very soluble Absolute alcohol: slightly soluble Acetone: very soluble

Benzene: practically insoluble Chloroform: practically insoluble Ether: practically insoluble B. To a 1 in 10 solution add a small quantity of ferric chlo-

ride T.S. A bluish black colour or precipitate forms. This colour disappears by adding a strong acid.

c.

A solution is acid to methyl red T.S.

PURITY TESTS

loss on ·drying: Not more than 12 per cent when dried at 105 for 2 hours. 0

Gum or dextrin: Dissolve 1 gin 5 ml of hot water, cool, filter, and to the filtrate add 10 ml

(48)

Resinous substances:

Sulfated ash:

Arsenic:

~ :

Heavy metals:

of alcohol. No turbidity is produced within 15 minutes.

Dissolve 1 gin 5 ml of hot water, cool1

filter, and dilute the filtrate to 15 m:

No turbidity is produced.

Not more than 1 per cent Not more than 3 mg/kg Not more than 10 mg/kg Not more than 30 mg/kg

(49)

(50)

C. EXTRAC'l'ION SOLVEN'l'S

(51)

(52)

SYNONYMS CHEMICAL NAME EMPIRICAL FORMULA STRUCTURA.L FORMULA MOLECULAR WEIGHT DEFINITION

DESCRI~ION

USES

ACETONE

Dimethyl ketone; propanone Acetone

c

3H6

o

CH3.co.cH

3 58.08

The specification is based upon a product containing not less than 99.5% m/m acetom.

Clear colourless volatile, highly flammable liquid with a characteristic odour, free from sediment and suspended matter.

Extraction of natural fats and oils, including essential oils; other uses are as a precipitation agent for the purifi- cation of starches, sugars and their derivatives.

A. Solubility Water: miscible in all proportions Ethanol: miscible in all proportions B. Relative density at 20°/20°: 0.790 to 0.793

c.

Refractive index n²~: 1.358 to 1.360 PURITY TESTS

Residue on evaporation: Not more than 0.001% m/m Distillation range: 55.5 to 57.0 ⁰ ⁰

Acidity: Not more than 0.002% rn/m, calculated as acetic acid.

Phenol: Not more than 0.001%

47

(53)

Substances reducing permanganate:

EXAMINA'l'ION

30 ml does not discolour 0.1 ml of

3'/o

m/v freshly prepared aqueous potaa- sium permanganate solution when aha,-

ken and allowed to stand at' 20° for 15 minutes.

Asaa.y: Weigh accurately about 1 g of acetone in a flask: containing 20 ml of water, and add water to 1,000 ml.

Place 1~ ml of the solution in a glass stoppered flask:, add 25 ml of 1 N sodium hydroxide, and allow to stand for 5 minutes. Add 25 ml of

o.

lN iodine, stopper, allow to stand in a cold and dark place for 10 minu- tea, and add 30 ml of 1 N sulfuric acid. Titrate the excess iodine with

o.

lN sodium thiosulfate, using starch T.S. as the indicator. Perform a blank test in the same manner as the sa.mpl_e to make any necessary correction.

1 ml of

o.

l N iodine= 0.9675 mg of

c

3H 6

o

Residue on evaporation: See Annex - 1

Distillation range: See Annex - 2.1 Method A

Acidity: See Annex - 3.1

Phenol determination:

Procedure: Place 3 ml of acetone in a crucible and evaporate to dryness at 60, add 3 drops of a solution of 0.1 g sodium 0

nitrite dissolved in 5 ml of sulfuric acid and allow to stand for 2-3 minutes; carefully add 3 ml of 2N sodium hydroxide.

No colour is produced.

Determination of residues in food: Food Additives Analytical 48 Manual.

u.s.

Food and Drug Administration, ,.Washington, D.C.

(54)

SYNONYMS CHEMICAL NAME EMPIRICAL FORMULA STfilIC'l'URAL FORMUIA MOLECULAR WEIGHT DESC.tlIPTION

USES

IDENTIFICATION TESTS A. Solubility:

1,2-DICHLOl:ETHANE Dichloretha.ne

1,2-dichlorethane c2H

4^c1² CH2Cl.CHfl 98.96

Clear, colourless mobile liquid with a sweet chloroform-like odour; free from sediment and suspended matter.

Extraction of essential oils from spices, hops: decaffeination of coffee.

immiscible with water B. Relative density 20°/20°: 1.251 to 1.256

1.444 to 1.446

C _• Rf _e ractive in ex n . "d 20 n=

PffiUTY TESTS

Resi".l.•.1c on P.vaooration:

Distillation range:

Aciditv:

Free chlorine:

EXAMINATION

Residue on evaporation:

Distillation range:

Acidity:

Not more than 0.00~~ m/m

Not less than 98.5% v/v distils between 82.5° to 04.5°

Not more than 0.003% m/m as HCl

Passes test

See Annex - 2.2 Method B See Annex_- 3.2

49

(55)

50

Free chlorine:

Reagents: o-tolidine reagent. Dissolve 1 g o-tolidine in 100 ml hydrochloric acid (sp.gr. - 1.18) and dilute to 1000 ml with water.

Procedure: To 25 ml of the sample in a glass stoppered measuring cylinder add 0.5 ml of the o-tolidine reagent and shake the cylinder for 30 seconds. No yellow colour is produced.

Determination of residues in food:

(a) L.A. Roberts, J. Assoc. Offic. Anal. Chem. 19681

.2.1,

825-828

(b) S.E. Heuser and K.A. Scudamore, J. Sci. Food Agric.1 1969, 20, 566-572

(c) For decaffeinated coffee only: H. Hadorn₁ Mitt. aus dem Gebiet der Lebensmittelunters. u. Hygiene, .,22(1):

1-16 (1965)

(56)

SYNONYMS CHEMICAL NAME EMPIRICAL AND

STRUCTURAL FORMULA MOLECULAR WEIGHT DESCRIPI'ION

USES

ID!}{TIFICATION TESTS A. Solubility:

DICHLOROMETHANE

Methylene chloride Dichloromethane

Clear colourless volatile liquid with a sweet chloroform-like odour: free from sediment and suspended matter.

Extraction of fats and oils, including extraction of spice oils; decaffeination of coffee.·

immiscible with water B. Relative density 20°/20°: 1.323 to 1.326

1.423 to 1.425 C. Refractive index n²~:

PURITY TESTS

Residue on evaP9ration:

Distillation range:

Acidity:

Alkalinity:

Pree chlorine:

EXAMINATION

Distillation range:

Acidity:

Allcalinity:

Pree chlorine:

Not more than 0.002% m/m 39° to 41°

Not more than 0.002'.'1, m/m as HCl Not more than 0.01% m/v as NaOH Confonns with the test

See Annex - 1

See Annex - 2.1 Method A See Annex - 3.2

See Annex - 3.2 See 1₁2-diohlorethane

51

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52

Determination of residues in foods:

References

A gas chromatographic method for residues in spice oleoresins is described under "methylene chloride", and a similar method under "isopropyl alcohol", in the Food Additives Analyti- cal Manual ( 1): A collaborative study of a similar method is described by Roberts (2) and the general method of Heuser and Scudamore (3) should also be applicable.

(1) Food Additives Analytical Manual,

u.s.

Food & Drug Administration, Washington,

n.c.

(2) L.A. Roberts, J. Assoc. Offic. Anal. Chem., 1968,

i!,

825-828

(3) S.G. Heuser and K.A. Scudamore, J. Sci. Food Agric., 1969, _g,Q, 566-572

(58)

SYIIOHYMS CHDIICAL HANE EMPIRICAL FORMULA.

STRUCTURAL FOHMULl

MOLECUL&R WEIGHT DEFINITION

DESCRIPrION

USES

ETHANOL Ethyl alcohol Ethanol c₂H6o C~CH20H

46.07

This specification is based on a product containing about 95% v/v (i.e. with about 5% v/v water)

c

₂H6

o.

other grades wi. th a different water content ma.y be used depending on the technological requirement. The specification for these should be similar to that below, apart from characteristics dependent on the water content. Where for revenue purposes a denaturent is used, it should be compati- ble with food use.

Clear colourless mobile liquid with a mild, spiritous odour, free from sediment and suspended water.

Occasional food extraction uses; as a precipitating solvent in pectin processirg and also in preparation of starch conversion products for food use. Carrier solvent for food adjuncts (flavours, colours, etc.)

53

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54

A. Solubility: miscible in water in all proportions

B. Relative density 20°/20°:

25°/25°:

0.812-0.814 0.809-0.811 1.3635 to 1.3645 C. Refractive index n2

~:

PURITY TESTS

!!.!!&:

Acidity:

Allcalini ty:

Aldehydes and ketones:

EXAMINATION

Acidity:

Allcalini ty:

Alde~ydes and ketones:

Shall conform with identification tests Band C

Not more than 0.003% m/m

Not more than 0.005% m/m as aoetic acid

Shall conform with the test

Not more than 0.02% m/m calculated as acetone

See Annex - 1 See Annex - 3.1 See Annex - 3.1

$ee Annex - 4. 1

(60)

There is a large literature on the analysis of mixtures containing alcohol, much of it related to the needs of revenue control.

The phthalic ester method of Black et al. (1) for 0.2 to

10%

alcohol in soy-bean flakes described under propan-2~1 should be adequate tor ethanol.

Reference

(1) L.T. Black, L.D. Kirk and

a.c.

Jihstakas, J. Amer. Oil.

Chem. Soc., 19611

1§,

483-485

55

(61)

56

SYNONYMS CHEMICAL NAME EMPIRICAL FORMULA S'l'RUCTURAL FOIOOJIA MOLECULAR WEIGHT DEFINITION

DESCRIPTION

USES

Mm'HANOL Methyl alcohol Methanol

This specification is based upon a. product containing a.bout

99%

v/v methanol.

Clear, colourless mobile flunma.ble liquid with a mild spirituous odour; free from sediment a.nd suspended matter.

Extraction of spice oils, hops.

miscible with water in all proportions

B. Relative density a.t 20°/20°:

at 25°/25°:

c.

Refractive ind~x at n2

~:

0.791 to 0.795 0.786 to 0.790 1.328 - 1.330 PURITY TESTS

Assay:

Acidity:

Alkalinity:

Alde;ydes a.nd ketones:

Shall conform with identification tests B a.nd C

Not more tha.n 0.003% m/m

Not more tha.n 0.003% m/m a.s formic acid

Conforms with the test

Not more tha.n 0.003% m/m, calculated as acetone

(62)

Distillation range:

EXAMINATION

Acidity:

Al.kalini ty:

Aldehydes and ketones:

Distillation range:

References

~ot less than 95% distils between

See Annex - 1 See Annex - 3.1 See Annex - 3.1 See Annex -

4.

2

See Annex - 2.2 Method B

A gas chromatographic method for residues in spice oleoresins is described under "isopropyl alcohol"

in the Food Additives Analytical Manual (1) and should be considered adequate; a similar method is also described under "methylene chloride''•

The phthalic ester method of Black et al. (2) for 0.2 to

10%

alcohol in soybean flakes descriced under propan-2-ol is applicable to methanol.

(1) Food Additives Analytical Manual,

u.s.

Food & Drug Administration, Washington, D.C.

(2) L.'l'. Black, L.D. Kirk and G.C. Mustalcas, J. Amer. Oil.

Chem,

Soc.,

1961,

38, 483-485

57

(63)

58

CHEMICAL NAME EMPIRICAL FORMULA.

STRUCTURAL FORMULA MOLECULAR WEIGHT DEFINITION

DESCRIPI'ION

HEXANE (Tentative)

Mixed paraffin hydrocarbons Approximating to

c

6H 14 C~(cH2)n CH

3 ^andisomers About 86

The term "hexane" here refers to the hexane petroleum hydrocarbon fraction:

this may, or may not, contain a high proportion of n-hexa.ne. Typically, how- ever, hexane contains mainly n-hexane, 2-methylpentane, 3-methylpentane or mixtures of these with smaller amounts of n-pentane, isopenta.ne, cyclohexa.ne n-heptane, dimet~ylbutanes and methylcy- clopentane.

Where, as is understood to be occasional- l;v the case, there is need for a lighter petroleu~ hydrocarbon fraction for food extraction use, this should comply with the general requirement of this specification apart from minor variations in identification tests and in distillation range. For a higher petroleum fraction for food extraction use, see hentane.

A clear colourless mobile hjt_rhly flamma.- ble liquid with a characteristic petroleum-like odour. Free from sediment and

(64)

suspended matter.

USES Extraction of edible oils, cocoa butter;

extraction of essential oils from spices and hops; defatting of fish meal.

IDENTIFICATION TESTs!I

A. Solubility: immiscible with water

B. Relative density at 20°/20°: 0.665 to 0.687 1 • 381 to 1 • 384

c.

Refractive index:

PURITY TESTS

Residue on evaporation: Not exceeding 0.0005% m/v Reaction of residue: Neutral to methyl orange

Distillation range: 95% v/v distils between 64° to 70°

Aromatic h.ydrocarbon~ Not more than

o.2%

v/v

Ultraviolet absorbanceJl (for polynuclear aromatic hydrocar- bans)

The following absorbance limits per cm optical pathlength shall not be exceeded:

Wavelength (nm)

280-289 0.15

290-299 0.13

300-359 0.08

360-400 0.02

Sulphur: Not more than 5 mg/kg

~ : Not more than 1 mg/kg

j/

Pure n-hexane has relative density of about o.660 at 20°/20°

and refractive index n2~ of about 1.375

y

More information required.

59

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60

EXAMINATION

Distillation range:

Aromatic hydrocarbons:

Utraviolet absorbance:

Sulphur:

~ :

See Annex - 1

See Annex - 202 Method B See Annex - 5

See Annex - 6 See Annex - 7 See Annex - 8

An immediate difficulty arises from the fact that solvent hexanes are a mixture of various aliphatic hydrocarbons. Thus the method of Black et al. (1) in which hexane residues are extracted from soya meal with pure iso-octane and the extract exa,- mined gas chromatographically could be used for the estimation of n-hexa,- ne residues as such. A more recent account is given by Watts and Holswade (2) in which a sample of the edible oil is injected directly onto the column. An alternative approach, used by Lewis et al. (3) is based on the measurement of the ( 1) L.T. Black and

G.c.

Mustakas, .T. Am. Oil Chem. Soc •. , 1965,

~ ' 62-64

(2) J .A. Watts and W. Hols-.·,a.de, ;[..! Assoc. Offic. fcnal. Chem.!., 1967,

22,

71?-7?6

O)

^Y

.s.

Lewis and

s.

Neelak,1-nta.n, sT. Am. O i ~ ~ ! . ' 1964,

.1.1,

211-212

(66)

vapour pressure of extracted meal and Lab1'113'\re.et al. (4) described a gas chromatographic techniqu.e for he:rane residues in spice oleoresins based on the examination of head.space gases. . A gas chromatographic method for residues in spice oleoresins is described under "isopropyl alcohol"

in the Food Additives Ana~ical Manual (5): a similar method is also described under "met~lene chloride".

(4) B. Labl'll3'\re,

c.

Olsthoorn - de Leeuw and F. Smeerage, Perfumery & Ess. Oil Record, 1968, ..22_, 206-211 (5) Food Additives Analytical Manual,

u.s.

Food & Drug

Administration, Washington,

D.c.

(67)

62

CHEMICAL NAME EMPIRICAL FORMUIA

STRUC'l'URA.L FORMULA

DESCRIPTION

USES

HEPTANE ('l'entative)

Mixed paraffin hydrocarbons Approximating to c

7H16 CH3^(cH2^{)n cH}3 and isomers About 100

'!'he term "heptane" here refers to the heptane petroleum hydrocarbon fraction:

this m~, or lll8iY not, contain a high proportion of n-heptane. Typically it is a mixture containing branched heptanes such as methylhexanes and dimethylpentar- nes.

Clear colourless mobile highly flammable liquid with.a characteristic petroleum- like odour, immiscible with water. Free from sediment and suspended matter.

Extraction of edible oils.

A. Relative density at 20°/20°: 0.700-0.720

PURI'l'Y TESTS

Distillation range:

Aromatic h..ydrocarboneY:

Ultraviolet absorba.nceJ./:

Hot exceeding 0.0005% m/v 95% v/v distils between 94° -99°

Not more than 0.5% v/v

'!'he following absorba.nce limits

Ji

More information required.

(68)

per cm optical pathlength shall not

Sulphur.:

~·

ED.MIRATIOH

be exceeded: . Wavelength (nm),

280-289 290-299 300-359 360-400

Not more than 5 mg/kg Not more than 1 mg/kg

Residues on evaporation: See Annex • 1

Distillation range: See Annex - 2.2 Method B Aromatic hydrocarbons: See Annex -

5

Ultraviolet absorbance:

Sulphurs

~·

Determination ot residues in tooda

S.ee Annex - 6

See Annex - 1

See Annex - 8

See Hexane

0.15 0.13 0.08 0.02

(69)

64

SYNONYMS CHEMICAL NAME EMPIRICAL FORMULA.

STRUCTURAL FORMULA.

DESCRIPI'ION

USES

PROPAN-2-0L (Isoprcpyl Alcohol)

Iso-propyl alcohol; propanol-2 Propan-2-ol

c3H 8o CH3.cHOH.cH

3 60.10

The specification is based upon a product containing not less than

99.5% v/v

propan- 2-ol. other grades with different water content m~ be used depending uuon technological requirements. The specification for these should be similar to that below apart from characteristics dependent on water content.

Clear colourless liquid with a spiritous odour, free from sediment and su.spended matter.

Extraction solvent e.g. in protein concentrate manufacture; carrier solvent for food adjuncts (flavours, colours etc.)

miscible with water in all proportions

B. Relative density at 20°/20°:

c.

Refractive index n2

~:

0.785 to 0.788 1.376 to 1.378

(70)

PURITY TESTS

Distillation range:

Acidity:

Aldeh.ydes and ketones:

EXAMINATION

Distillation range:

Acidity:

Aldeh.ydes and ketones:

Shall conform.with identification tests Band C

Not more than 0.002%

m/m

81.0 to 83.0°

Not more than

0.005% m/m

calculated as acetic acid

Not more than 0.1'%

m/m

calculated as acetone

See Anne% - 1

See Annu - 2.1 Method A See Anne% - 3.1

See Annu - 4• 1

In considering methods for the deteo- tion and estimation of residual tra..- ces of propan-2-ol, regard should be had for the need for these in rela..- tion to the significance, to%icological or otherwise, of ^8:t1yresidues likely to be encountered. Propan-2- ol is itself a minor constituent of various alcohol_ic beverages. Black et al. (1) have estimated residues 'in defatted soybean by conversion to

(1) L.T. Black, L.D. Kirk and

a.c.

Mu.stakas, J. Am. Oil Chem.·