[PDF] EAS 216-5: Ethanol for industrial use ⎯ Methods of test



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EAS 216-5: Ethanol for industrial use ⎯ Methods of test

1 Scope and field of application This part of IS0 1388 specifies a visual calorimetric method for the determination of the aldehydes content of ethanol for industrial use The method is applicable to products having aldehyde con- tents, expressed as acetaldehyde, in the range 0,000 25 to 0,001 25 (m/m)



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EAS 216-5 (2001) (English): Ethanol for

industrial use Methods of test Part 5:

Determination of aldehydes content

Visual calorimetric method

EAS 216-5:2001

ICS 71.080.60

© EAC 2001 First Edition 2001

EAST AFRICAN STANDARD

Ethanol for industrial use Methods of test Part 5: Determination of aldehydes content Visual calorimetric method

EAST AFRICAN COMMUNITY

EAS 216-5:2001

ii © EAC 2001 - All rights reserved

Foreword

Development of the East African Standards has been necessitated by the need for harmonizing requirements governing quality of products and services in East Africa. It is envisaged that through harmonized standardization, trade barriers which are encountered when goods and services are exchanged within the Community will be removed.

In order to achieve this objective, the Partner States in the Community through their National Bureaux

of Standards, have established an East African Standards Committee. The Committee is composed of representatives of the National Standards Bodies in Partner States, together with the representatives from the private sectors and consumer organizations. Draft East

African Standards are circulated to stakeholders through the National Standards Bodies in the Partner

States. The comments received are discussed and incorporated before finalization of standards, in accordance with the procedures of the Community. East African Standards are subject to review, to keep pace with technological advances. Users of the East African Standards are therefore expected to ensure that they always have the latest versions of the standards they are implementing. © East African Community 2001 - All rights reserved

East African Community

P O Box 1096

Arusha

Tanzania

Tel: 255 27 2504253/8

Fax: 255-27-2504481/2504255

E-Mail: eac@eachq.org

Web: www.each.org

* 2001 EAC - All rights of exploitation in any form and by any means reserved worldwide for EAC Partner States' NSBs.

International Standard 138815

INTERNATIONAL ORGANIZATION FOR STANDARDIZATlON.MEIKJlYHAPOL(HAR OPTAHl43A~MR fl0 CTAH,QAPTM3ALWlMWIRGANlSATlON INTERNATIONALE DE 6JORMALISATtON

Ethanol for industrial use - Methods of

test - Part 5 : Determination of aldehydes content - Visual calorimetric method Ethanol ;i usage industriel - M&hodes d'essai - Partie 5 : Dosage des afdkhydes - M6 thode colorim6 trique visuelle First edition - 1981-12-01

UDC 661.722 : 543.432 : 547.281 Ref. No. IS0

1388/5-1981 (E) Descriptors : industrial products, ethanols, tests, determination of content, aldhehydes, calorimetric analysis.

Price based on 3 pages

Preisgr. C

Foreword

IS0 (the International Organization for Standardization) is a worldwide federation of national standards institutes (IS0 member bodies). The work of developing Inter- national Standards is carried out through IS0 technical committees. Every member body interested in a subject for which a technical committee has been set up has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the IS0 Council. International Standard IS0 1388/5 was developed by Technical Committee ISO/TC 47, Chemistry, and was circulated to the member bodies in February 1980. It has been approved by the member bodies of the following countries :

Australia Germany, F. R.

Austria

Hungary

Belgium India

Brazil

Italy

Bulgaria Korea, Rep. of

China

Netherlands

Czechoslovakia

Philippines

France

Poland Romania

South Africa, Rep. of

Switzerland

Thailand

United Kingdom

USSR No member body expressed disapproval of the document. This International Standard has also been approved by the International Union of Pure and Applied Chemistry (IUPAC). International Standards IS0 1388/l to IS0 1388/12 cancel and replace IS0 Recom- mendation R 1388-1970, of which they constitute a technical revision. International Organization for Standardization, 1981

Printed in Switzerland

INTERNATIONAL STANDARD IS0 1388/5-1981 (E)

Ethanol for industrial use - Methods of test -

Part 5 : Determination of aldehydes content - Visual calorimetric method

1 Scope and field of application

This part of IS0 1388 specifies a visual calorimetric method for the determination of the aldehydes content of ethanol for industrial use. The method is applicable to products having aldehyde con- tents, expressed as acetaldehyde, in the range 0,000 25 to

0,001 25 % (m/m).

This document should be read in conjunction with IS0 4388/l (see the annex).

2 Principle

Reaction of the aldehydes present in a test portion with Schiff reagent. Visual comparison of the colour obtained with the col- ours of standard calorimetric solutions containing known quan- tities of acetaldehyde.

3 Reagents

During the analysis, use only reagents of recognized analytical grade, and distilled water or water of equivalent purity.

3.1 Ethanol, 95 % (V/VI, aldehydes-free, purified as

follows. Boil 1 500 ml of absolute ethanol, under reflux, for 2 h, with

15 g of m-phenylenediamine. Distil the mixture, rejecting the

first and last 50 ml fractions of the distillate. Adjust the concen- tration to 95 % (V/v) by adding an appropriate volume of water and mix. Use the procedure specified in clause 5 to verify that the purified ethanol is free from aldehydes.

3.2 Schiff reagent.

WARNING

- Basic fuchsin is carcinogenic. Avoid skin contact with basic fuchsin and its solutions and inhala- tion of its dust.

3.21 Preparation

Place 1 500 ml of water in a 3 000 ml conical flask, add

4,500 + 0,005 g of p-rosaniline hydrochloride (basic fuchsin), -

and swirl to dissolve. Add 9,60 + 0,05 g of disodium disulphite [sodium metabisulphite (Na&O& mix and allow to stand for

5 to 10 min. Add 40 ml of approximately 295 g/l sulphuric acid

solution, mix thoroughly, stopper the flask and allow to stand for about 12 h. Decolorize the solution if necessary, by treat- ment with activated carbon.

3.2.2 Determination and adjustment of free sulphur

dioxide content Transfer 10 ml of the colourless reagent (3.2.1) to a 250 ml con- ical flask. Add 20 ml of water and 5 ml of freshly prepared starch solution, and titrate the solution with standard volumetric iodine solution, c(l/2 12) = 0,l mol/l, until the characteristic dark blue colour is just obtained. NOTE - 1 ml of iodine solution, c(l/2 12) = 0,l mol/l, corresponds to

0,003 2 g of so2.

If the free sulphur dioxide content does not fall within the op- timum range (0,iS to 0,31 g per 100 ml of reagent), adjust it as appropriate, increasing the level by adding a calculated quantity of disodium disulphite or decreasing it by bubbling air through the reagent solution.

3.3 Acetaldehyde, standard solution corresponding to 1 g

of acetaldehyde per litre. Weigh, to the nearest 0,000 1 g, 0,693 0 g of acetaldehyde am- monia [CH&H(NH,)OHl and dissolve it in the ethanol (3.1). Transfer the solution quantitatively to a 500 ml one-mark volumetric flask, dilute to the mark with ethanol of the same quality and mix.

1 ml of this standard solution contains 0,001 g of acetaldehyde.

NOTE - If acetaldehyde ammonia of analytical grade is not available, purify the commercial product as follows. Dissolve about 5 g of acetaldehyde ammonia in a small quantity of ab- solute ethanol and precipitate it by adding twice the volume of dry diethyl ether &H50C2H5). Using a Buchner funnel, filter the precipitate and, after washing it with more of the diethyl ether, transfer it immediately to a vacuum desiccator containing sulphuric acid, Q ap- proximately I,84 g/ml, 98 % (m/m) solution, as desiccant, and allow to dry for 3 to 4 h. Repeat the purification if necessary, until the product is colourless. WARNING - Diethyl ether is highly flammable and its vapour is harmful. Avoid breathing vapour.

3.4 Acetaldehyde, standard solution corresponding to

0,l g of acetaldehyde per Iitre.

IS0 1388/5-1981 (E)

Transfer 25,0 ml of the standard acetaldehyde solution (3.3) to a 250 ml one-mark volumetric flask, dilute to the mark with the ethanol (3.1) and mix.

1 ml of this standard solution contains 0,000 1 g of

acetaldehyde.

4 Apparatus

Ordinary laboratory apparatus, and

4.1 Calorimetric tubes, fitted with ground glass stoppers,

of capacity about 20 ml, and graduated at 10 and 14 ml.

4.2 Graduated pipettes, of capacity 5 ml, graduated in

0,02 ml divisions.

5 Procedure

Using the graduated pipettes (4.21, measure, into a series of six of the calorimetric tubes (4.11, 3,0 ml of each of these diluted standard acetaldehyde solutions. Treat the contents of each tube, including those of the tube containing the test portion (5.1), as follows. Dilute to 10 ml with water and add sufficient of the Schiff reagent (3.2) to bring the volume to 14 ml. Stopper the tubes, mix the solutions (preferably simultaneously) and allow to stand in a rack for 25 min.

5.3 Determination *

Compare the colour of the test solution with the colours of the standard calorimetric solutions, in dispersed daylight. NOTE - If the colour of the test solution is deeper than that of the most concentrated standard calorimetric solution, repeat the test using more of the laboratory sample suitably diluted with the ethanol (3.11, and take this into account in the calculation of results.

5.1 Test portion 6 Expression of results

Using one of the graduated pipettes (4.21, measure 3,0 ml of the laboratory sample into one of the calorimetric tubes (4.1).

5.2 Preparation of the test solution and standard

calorimetric solutions Into a series of six 100 ml one-mark volumetric flasks, place the volumes of 'the standard acetaldehyde solution (3.4) indicated in the following table, dilute to the mark with the ethanol (3.1) and mix.

Standard acetaldehyde Corresponding mass

solution (3.4) of acetaldehyde ml 9 zo

0,ooo 2

3,o

0,ooo 3

5,o

0,ooo 5

7,o

0,ooo 7

w

0,ooo 9

10,o

0,0010

The aldehydes content, expressed as acetaldehyde KH$HO) as a percentage by mass, is given by the formula m Q where m is the mass, in grams (see the table), of acetaldehyde used to prepare the diluted standard solution giving a colour matching most closely that developed in the test solution. Q is the density, in grams per millilitre, of the sample at

20 OC (see IS0 1388/l, clause 4).

lSO1388/5-1981(E) Annex IS0 Publications relating to ethanol for industrial use

IS0 1388/l - General.

IS0 1388/2 - Detection of alkalinity or determination of acidity to phenolphthalein.

IS0 1388/3 - Estimation of content of carbonyl compounds present in small amounts - Photometric method.

IS0 138814 - Estimation of content of carbonyl compounds present in moderate amounts - Titrimetric method.

IS0 1388/5 - Determination of aldehydes content - Visual calorimetric method.

IS0 138816 - Test for miscibility with water.

IS0 138817 - Determination of methanol content [methanol contents between 0,Ol and 0,20 % (V/ WI - Photometric method. IS0 1388/8 - Determination of methanol content [methanol contents between 0,lO and 150 % (

V/ U] - Visual calorimetric

method. IS0 138819 - Determination of esters content - Titrimetric method after saponification. IS0 1388/10 - Estimation of hydrocarbons content - Distillation method.

IS0 1388111 - Test for detection of futfural.

IS0 1388112 - Determination of permanganate time.

3

EAS 216-5:2001

© EAC 2001 - All rights reserved

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