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है”ह”ह

IS 15356 (2003): Acetaldehyde [PCD 9: Organic ChemicalsAlcohols and Allied Products and Dye Intermediates]

1S 15356:2003

Indian Standard

ACETALDEHYDE — SPECIFICATION

Ics 71.080.80

0 BIS 2003

BUREAU OF INDIAN STANDARDSMANAK EHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

June 2003 Price Group 4

Alcohols and Allied Products Sectional Committee, PCD 10

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Alcohols andAllied Products Sectional Committee had been approved by the Petroleum, Coal and Related Products DivisionCouncil.

Acetaldehyde is a normal intermediate product in the respiration of higher plants. It occurs in process in all ripefruits. Acetaldehyde is an intermediate product in the decomposition of sugars in the body and hence occurs intraces in blood. Acetaldehyde is also an important intermediate in the production of acetic acid, acetic anhydride,ethyl acetate, peracetic acid, pentaerythritol, chloral, glycol, alkylamines and pyridines.

Acetaldehyde has a general narcotic action, which prevents coughing. It causes irritation of the eye, mucusmembranes and accelerates heart action. Acetaldehyde also appears to paralyze respiratory muscles when breathedin high concentrate ion it causes headache and sore throat. Prolonged exposure causes a decrease of red and whiteblood cells and also sustained rise in blood pressure. The maximum allowable concentration of acetaldehyde in airis 200 ppm. However, in a normal industrial operation, there is no hazard in handling acetaldehyde providednormal precautions are taken.

The Committee responsible for the formulation of the standard felt the necessity of including a method fordetermination of formaldehyde content. The method is under development and till it is evolved, the requirementof’ formaldehyde content’ has not been included.

The composition of the Committee responsible for formulation of this standard is given in Annex D.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with1S 2:1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained in therounded off value should be the same as that of the specified value in this standard.

IS 15356:2003

Indian Standard

ACETALDEHYDE — SPECIFICATION

I SCOPE

This standard prescribes the requirements and themethods of sampling and test for acetaldehyde intendedfor industrial purposes.

2 REFERENCES

The following standards contain provisions, whichthrough reference in this text constitute provisions ofthe standard. At the time of publication, the editionsindicated were valid. All standards are subject torevision, and parties to agreements based on thisstandard are encouraged to investigate the possibilityof applying the most recent editions of the standardsindicated below:

[s No

361:1973

1070: 1992

1260 (Part 1) :1973

2362:1993

4905:1968

Title

Specification for normal butylalcohol, technical (secondrevision)

Reagent grade water (third revision)

Pictorial marking for handlingand labelling of goods : Part 1Dangerous goods (first revision)

Determination of water by KarlFischer method—Test method(second revision)

Methods for random sampling

3 REQUIREMENTS

3.1 Description

The material shall be clear liquid free from suspendedmatter and having a characteristic odour.

3.2 Colour

The material shall be colorless to light yellow.

3.3 The material shall also comply with therequirements given in Table 1 when tested accordingto the procedures given inCO14 of Table 1.

4 PACKING AND MARKING

4.1 Packing

4.1.1 The material shall be packed in suitable containersas agreed to between the purchaser and the supplierand subject to the provisions of Red TariffNo. 18 Rulesand Rates for Conveyance by Rail or Explosives andother Dangerous Goods, issued by the Indian Railways

Conference Association with any alternations oradditions made thereafter.

4.1.2 All containers in which the material is packedshall be dry and clean so that no impurities harmful tothe end use of the material are introduced.

4.2 Marking

4.2.1 Each container shall be marked with:

a) Name of the material,

b) Indication of the source of manufacture,

c) Net mass of the material,

d) Month and year of manufacture, and

e) Lot or batch number.

4.2.2 The material shall also be marked in accordancewith the marking and delivery instructions given bythe purchaser.

4.2.3 Each container shall also be marked with thecaution label ‘FLAMMABLE’ together with thecorresponding symbol for labelling [see IS 1260(Part l)].

4.2.4 BIS Certification Marking

The container may also be marked with the StandardMark.

4.2.4.1 The use of the Standard Mark is governed bythe provisions of the Bureau of Indian Standard Act,1986 and the RuIes and Regulations made thereunder.The details of conditions under which the Iicence forthe use of the Standard Mark may be granted tomanufacturers or producers may be obtained from theBureau of Indian Standards.

5 SAMPLING

Representative samples of the material shall be drawnas prescribed in Annex C.

6 TEST METHODS

6.1 Test shall be conducted according to the methodsprescribed inCO14 of Table 1.

6.2 Quality of Reagents

Unless specified otherwise, pure chemicals and distilledwater (see IS 1070) shall be employed in the test.

NOTE—’Pure chemicals’ shall mean chemicals that do notcontain impurities which affect the results of analysis,

1

IS 15356:2003

Table 1 Requirements of Acetaldehyde

(Ckmses 3.3 and 6. 1)

SI No. Characteristic Requirement Method of Test, Ref toc \

Annex IS No.

(i) (2) (3) (4) (5)

i) Total aldehydes as acetaldehyde, 98.5 Annex A —

percent by mass, Min

ii) Total acidity as acetic acid, 0.1 — A-6 of 1S 361

percent by mass, Max

iii) Water content, percent by mass, Max 0.5 . 1S 2362

iv) Paraldehyde content, percent by mass, Mux 0.7 Annex B —

ANNEX A

[Table 1, S1No. (i)]

DETERMINATION OF TOTAL ALDEHYDES AS ACETALDEHYDE

A-1 OU;’LINE OF THE METHOD

A known amount of sample is treated withilydroxylarnine hydrochloride solution and thehydrochloric acid liberated in the oximating reaction istitrated with standard sodium hydroxide solution. Fromthe titre values, the acetaldehyde content is calculated.

A-2 APPARATUS

A-2.1 Conical Flask—250-ml capacity fitted with aB24 stopper.

A-3 REAGENTS

A-3.1 Standard Sodium Hydroxide Solution— 1 N.

A-3.2 Hydroxylamine Hydrochloride Solution —1 N, neutral to bromophenol blue.

A-3.3 Bromophenol Blue Aqueous Solution -–0.02percent.

A-4 PROCEDURE

To 50 ml of hydroxylamine hydrochloride solution ina stoppered conical flask and 4 to 5 drops ofbromopheno] blue solution (weigh to the nearest0.002 g). Transfer about 1 g sample in the flask and

mix thoroughly. Open the flask to let air in, stopper itagain and weigh. Titrate the liberated acid with standardsodium hydroxide solution until blue green colourappears. Allow the flask with the contents to stand for15 min and if the colour changes, titrate again withsodium hydroxide. Note the volume of NaOH used(V ml). Carry out a blank titration using all reagentsexcept the sample. Note the volume of NaOH used(v ml).

A-5 CALCULATION

Calculate the total percentage of acetaldehyde (JJ bythe following formula:

x

where

J/.

v=

N=

M=

_ (V- V) X4.4XN—

M

volume, in ml, of 1 N standard sodiumhydroxide solution used;

volume, in ml, of 1 N standard sodiumhydroxide solution used for blank titration;

normality of standard sodium hydroxidesolution; and

mass, in g, of the sample taken.

IS 15356:2003

ANNEX B

[Table 1, S1No. (iv)]

DETERMINATION OF PARALDEHYDE CONTENT

B-1 OUTLINE OF THE METHOD

A 4 percent water solution of acetaldehyde is injectedinto the heated injection port of the gas chromatography.The vapours are lead into the chromatographic columnwherein the vaporized constituents of the sample areseparated out by virtue of their differing physicothem ical interaction with the stationary phase. For theseparation to be efficient, it is necessary that the columnis maintained at the temperature suggested throughoutthe time required for the resolution of the constituents.As the sample enters the detector, it gives a signalcorresponding to the amount of particular constituentleaving the column. From the specific area undervarious peaks corresponding to specific constituents,the quantities of different constituents are determined.

B-2 APPARATUS

B-2. 1 Gas Chromatography —Any gas chromato-graphy fitted with flame ionization detector and capableof meeting the required operating conditions may beused.

B-3 REAGENTS

B-3. 1 Pure Acetaldehyde (Not Containing AnyParaldehyde) — 99 percent purity.

B-3.2 Paraldehyde— 99 percent purity.

B-4 PROCEDURE

B-4. 1 The sample and calibration blends to be injectedas given in B-4.3.

B-4.2 Typical Column and Operating Conditions

a) Column: 3.18 mm, 1 m stainless steel columnpacked with 10 percent carbowax 20 M TPA onchromosorb G, AW - DMCS 80-100mesh.

b) Column temperature : 70 “c

c) Injection and detector : 230 ‘Ctemperature

d) Carrier gas Nitrogen

e) Carrier flow rate 10 ml/min

t) Detector Flame ionization

g) Chart speed 10 mm/min

h) Sample size 1.0pl

B-4.3 Calibration

a) Chill the acetaldehyde to 5°C prepare 4calibration blends of acetaldehyde containingparaldehyde as follows:

Around (1) 0.2 percent (2) 0.4 percent (3)0.6 percent (4) 0.7 percent immediately dilute1.5 ml of each of these calibration blends to25 ml with distii;ed water.

b) Sample preparation— Chill the sample to5 “C, dilute 1.5 ml of the sample to 25 mlwith distilled water.

Inject 1.0 pl of the diluted samples of calibrationblends and sample into the gas chromatography.

B-5 CALCULATIONS

B-5.1 a)

b)

c)

Inject 1.0 PI of the diluted calibration blendNo. 2.

Generate a normalization method on anintegrator.

Calibrate the tile by entering the percentageof acetaldehyde and paraldehyde of theundiluted calibration blend No. 2.

B-5.2 Inject the remaining diluted calibration blendsand obtain the percentage of paraldehyde.

NOTE — The deviations from the actual and experimental values

of paraldehyde shoold not be more than + 0.05 percent.

B-5.3 a) Inject the diluted sample solution.

b) Determine the percentage of paraldehyde inthe sample.

NOTE — Typical rctentioh times (RT), relative retention times(RRT) and response factors (RF) ofacetaldehyde and prrraldehydeis shown in Fig. 1.

3

ImV

14.04

6.23

-1.59

0.00 4.91 9.83—

MIN.

FIG. 1 TYPICAL CHROMATOGRAM

4

IS 15356:2003

ANNEX C

(Ckmse 5)

SAMPLING OF ACETALDEHYDE

C-1 GENERAL REQUIREMENTS OFSAMPLING

C-1. 1 In drawing, preparing, storing and handling testsamples the following precautions and directions shallbe observed.

C-1.2 Samples shall be taken in a protected area withgood ventilation.

C-1.3 Precautions shall be taken to protect the samples,the material being sampled, the sampling instrumentand the containers for samples from adventitiouscontamination.

C-1.4 To draw a representative sample, the contentsof each container selected for sampling shall be mixedas thoroughly as possible by shaking, stirring, rollingor by any other suitable means.

C-1.5 The samples shall be placed in suitable, clean,dry and air-tight, atnber-coloured glass or metalcontainers on which the material has no action.

C-1.6 The sample containers shall be of such a sizethat they are almost completely tilled by the sample.

C-1.7 Each sample container shall be sealed air-tightwith a suitable stopper after filling and marked withthe manufacturer’s name or trade-mark, the month andyear of manufacture.of the material, the batch number(if available) and other details of sampling, such as thedate of sampling, sampler’s name, etc.

C-1.8 The sample of acetaldehyde should be handledonly in a fume hood which is free from open flames,electric heaters and other sources of ignitions. Allsamples shall be cooled in ice baths before thecontainers are opened. Acetaldehyde is weighed insealed glass atnpou]e. The actual procedure for fillingand sealing the ampoule varies. One convenient methodis to pack commercial available ampoules in powderedsolid carbon dioxide, introduce the specimen by meansof chilled hypodermic syringe and seal the ampoulewith a glass torch.

C-2 SAMPLING INSTRUMENT

C-2.1 It is made of thick glass or metal on which thematerial has no action and is 20 to 40 mm in diameterand 400 to 800 mm in length (see Fig. 2).

The upper and lower ends are conical and reach 5 to10 mm diameter at the narrow ends. Handling isfacilitated by two rings at the upper end. For drawingsample, the apparatus is first closed at the top with the

5TO100

All dimensions in millimetres

FIG. 2 SAMPLING TUBE

thumb or a stopper and lowered till a desired depth isreached. It is then opened for a short period to admitthe material at the desired depth and finally closed andwithdrawn.

C-2.1.1 For small containers, the size of the samplingtube may be altered suitably.

C-3 SCALE OF SAMPLING

C-3.1 Lot

In any consignment, all the containers of the same sizeand drawn from the same batch of manufacture shallconstitute a lot. If a consignment is known to consistof different batches of manufacture or different sizesof containers, the containers belonging to same batchand size shall be grouped together and each such groupshall constitute a separate lot.

C-3.2 For ascertaining the conformity of the materialin a lot to the requirements of the specification, testsshall be carried out for each lot separately. For thispurpose the number of containers to be selected from alot shall depend on the size of the lot and shall be inaccordance with the CO12 and 3 of Table 2.

C-3.3 These containers shall be selected at randomfrom the lot. For this purpose, reference may be madeto 1S 4905. However, if this standard is not available,

5

IS 15356:2003

Table 2 Scale of Sampling

(Ckmw C-3.2)

s) No.

(1)

i)

ii)

iii)

iv)

v)

vi)

vii)

Lot Size

N

(2)

Up to 2

3 to 15

16 to 25

26 to 100

10 I to 150

151 to 500

~()] and above

No. of Containersto be Selected

n

(3)

All

2

3

5

8

13

20

the following procedure may be followed:

Arrange all the containers in the lot in a systematicmanner and starting from any container, countthem as 1, 2 .....up to r, where r is the integral partof the N/n (N being the lot size and n the numberof containers to be selected). Every rth containerthus counted shall be withdrawn till the requisitenumber of containers is obtained.

C-4 PREPARATION OF TEST SAMPLES

C-4. 1 From each of the containers selected accordingto C-3.3, a small representative portion of the materialsufficient for carrying out tests as indicated in 3shzill be drawn with the help of the sampling tube(.YCWC-2.1). These shall constitute the individualsamples.

C-4.2 Out of these portions, equal quantity of materialshall be taken and mixed thoroughly to form acomposite sample, not less than 1 500 ml. Thecomposite test sample shall be divided into three equalparts, one for the purchaser, another for the supplierand the third to be used as a referee sample.

C-4.3 The composite samples shall be transferred tocontainers of 600-ml capacity and shall be sealed andmarked with full identification particulars givenin C-1.7.

C-4.4 The referee test samples shall also bear the sealof both the purchaser and the supplier. It shall be keptat a place agreed to between the purchaser and thesupplier, to be used in the case of any dispute betweenthe two.

C-5 NUMBER OF TESTS

C-5.1 Test for ‘total aldehydes as acetaldehyde’ (asper Table 1) shall be performed on the individualsample.

C-5.2 Tests for the determination of all the remainingcharacteristics, specified in 3, shall be performed onthe composite sample.

C-6 CRITERIA FOR CONFORMITY

The lot shall be declared as conforming to therequirements of the specification, if the test results foreach of the characteristic satisfy the relevantrequirement as given in 3. Otherwise, the lot shall berejected.

ANNEX D

(Foreword)COMMITTEE COMPOSITION

Alcohols and Allied Products Sectional Committee, PCD 10

Organization

Central Forensic Science Laboratory, New Delhi

Directorate of Forensic Science Laboratories, Mumbai

Somaiya Organic (India) Ltd, Barabanki

All India Distillers Association, New Delhi

Directorate of Quality Assurance (Ministry of Defence), Kanpur

Central Revenues Control Laboratory, New Delhi

National Test House, Kolkata

National Sugar Institute (Ministry of Food & Civil Supplies),

Kanpur

‘The Indian Drugs and Pharmaceuticals Ltd, Muzaffarpur

National Organic Chemical Industries Limited, Mumbai

JMohan Meakin Ltd, Ghaziabad

Indian Organic Chemicals Ltd, Distt Raigad, Khopoli

hlinistry of Chemicals & Fertilizers, Department of Industrial

Chemicals, New DelhiI Iindustan Polymers Ltd, Mumbai

I icrdillia Chemicals Ltd, Navi Mumbai

State Forensic Science Laboratories, Lucknow

Satya Winery & Distillery Pvt Ltd, Hyderabad

Organization of Pharmaceutical Producers of India, Delhi

Vam Organic Chemicals Ltd, Gajraula, U.P.

IMumla Sugars, Meerut

131Sllircctorate General

Representative(s)

DR S. R. S~NGH(Chairman)SHRJ K. S. CHABRA(Alternate 1)

SHRJN, K, PRASAD(Alternate 11)

DIRECTORDR M. V. GARAV(Alternate)

DR S. K. SOMAIYASHRIR. B. SRJVASTAVA(Alternate)

SHRJ0. P. BHATIASHRIK. P. SINGH(Alfernate)

SHRJS, S. RAO

SHY S. C. SRJVASTAVA(Alternate)

CHIEFCHEMISTDEPUTYCHIEFCHEMJST(Alternate)

DRY, C. NIJHAWAN

SHRJPK. CHAKRABORTY(,4/ternate)

LJRP. K. AGRAWALDR MAHENDRAPRASAD(Alternate)

SHRIR. V. GARGSHRIR. K. BANDOPADHYAYA(Alfernafe)

DR B. V, BAPATSHRIK. P. S. CHAUHAN(Alfermzte)

Dtt E. K. JAYANARAYA~ANSHRIJITENDERMOHAN(Alterrrate)

SHRIA, A. MAIUMDARDR K. J. DIVAKAR(Alternu/e)

SHIU A. K. DASS

SHRIS. K. MANAJANS}iRIA. K. MUKHERJEE(Alfernafe)

DR V, V. PAVLESHRJR. G, PATKIE(/f//errrate)

Smu 0. P. TANEJASHRIARWNDLINGALA

DR B. K. JHA(Alterrrate)

SHRIV. V. BODKEDR M. K. BIYANI(Alternate)

DR J. C, CHAWLA

DR A. AGARWAL(Alternate)

DR M, C, BARDIYASHRIS. CHANDANA.(Alternate)

SHRIANJANKAR, Director & Head (PCD)[Representing Director General (Ex’-oflcio)]

Member Secretary

SHRIH. S. SIDHUJoint Director (PCD), BIS

7

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Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewedperiodically; a standard along with amendments is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshou Id ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Dot: No. PCD 10 (821).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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