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IS 323 (2009): Rectified spirit for industrial use [PCD 9:Organic Chemicals Alcohols and Allied Products and DyeIntermediates]

IS 323 : 2009

Indian Standard

RECTIFIED SPIRIT FOR INDUSTRIAL USE­SPECIFICATION

( Second Revision)

ICS 71.100 .80

© SIS 2009

BUREAU OF INDIAN STANDARDSMANAK BHAVAN. 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Mar ch 2009 Price Group 6

Organic Chemicals, Alcohols and Allied Products and Dye Intermediate Sectional Committee, PCD 9

FOREWORD

This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards, after the draftfinalized by the Organic Chemicals, Alcohols and Allied Products and Dye Intermediate SectionalCommittee had been approved by the Petroleum, Coal and Related Products Division Council.

This standard was first published in 1952. At that time, the minimum ethanol content of rectified spirit hadbeen left to the option of the purchaser and the vendor subject to a minimum of 91.27 percent by volume[60° Overproof (OP)].

The first revision of this standard was carried out in 1959 to upgrade ethanol content and also to modifyacidity, residue on evaporation, besides, potassium ferro-cyanide method was prescribed as an alternatemethod for the determination of copper. This standard covered two grades, Grade 1 suitable for use as areagent for pharmaceutical/medicinal purposes and for the production of alcoholic beverages and Grade 2was intended for other industrial purposes. Besides, additional requirement to Grade 1 were laid down tocater to the needs of the acetone industry. The computation of strength of aqueous solutions containingethanol was made from specific gravity figures at 15.6°C (60°F) and the strength was expressed in terms ofpercent by volume or of proof spirit in line with prevailing practices in the country.

In this standard, grade relevant for pharmaceutical, medicinal and production of alcoholic beverages hasbeen deleted. A separate standard for potable applications is under formulation. The rectified spirit intendedfor industrial purpose only is being retained in this revision. The Committee responsible for the formulationof this standard, however, felt that it would be advisable to retain the proof spirit method of expressingstrength of alcoholic solutions and its co-relation with specific gravity and percentage of alcohol by volumeas well as weight at 20°C as routine method for ease of testing. In this revision, GC method has also beenincluded for determination of ethanol, methyl alcohol, n-propanol and iso-amyl alcohol. Instrumentalmethods have been included for determination of specific gravity as an alternative to specific gravity bottlemethod in this standard.

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

18323:2009

Indian Standard

RECTIFIED SPIRIT FOR INDUSTRIAL USE ­SPECIFICATION

( Second Revision)

1 SCOPE

2 REFERENCES

This standard prescribes the requirements and themethods of sampling and test for rectified spirit. Thematerial is intended for industrial applications only.

The following standards contain provisions, whichthrough reference in this text constitute provisionsof the standards. At the time of publication, theeditions indicated were valid. All standards aresubject to revision and parties to agreements basedon this standard are encouraged to investigate thepossibility of applying the latest edition of thestandards indicated below:

5 PACKING AND MARKING

4 REQUIREMENTS

4.1 Description

The material shall be a clear, colourless, homogenousliquid free from suspended matter and consistessentially of ethyl alcohol admixed with water.

4.2 The material shall also comply with therequirements prescribed in Table I.

3.3 Proof Spirit - A measure of the absolute alcoholcontent of a mixture of ethanol and water, whichshall, at a temperature of I 0.6°C (or 51°F), weighexactly 12l13th part of an equal volume of distilledwater at the same temperature. It has a density of0.915 5 at 20°C and contains 49.28 percent byweight of alcohol or 57.10 percent of alcohol byvolume at 20°C .

3.4 Overproot Spirit (OP) - Mixture of ethanoland water containing a greater percentage of ethanolthan is contained in proof spirit, especiallycontaining more than 50 percent alcohol by volume.If an overproof strength is added to 100, the sumrepresents the volumes of spirit at proof strengthwhich 100 volumes of spirit of that particularoverproof strength would yield when diluted withwater. For example, 100 volume of 60° OP spiritwould yield 160 volumes of proof spirit.

TItle

Sulphuric acid (third revision)Reagent grade water (thirdrevision)Tables for alcoholometry byhydrometer method (first revision)Determination of water by KarlFischer method - Test method(second revision)Glossary of terms relating toalcohol (ethyl) industry and tradeAnhydrous ethanol for use inautomotive fuel - Specification

IS No.

266 : 19931070: 1992

2302 : 1989

2362 : 1993

6749: 1972

15464 : 2004

3 TERMINOLOGY

For the purpose of this standard, the followingdefinitions shall apply. Besides, IS 6749 may also bereferred for other definitions.

3.1 Ethyl Alcohol- Ethyl alcohol (CAS No. 64-17-5)also referred to as ethanol, alcohol or grain alcoholis a flammable colourless liquid with a characteristicodour having a molecular formula as C2H,OH.

3.2 Rectified Spirit - Spirit purified by distillationto achieve strength of not less than 95 percent byvolume of ethyl alcohol is a mixture of ethyl alcoholand water.

5.1 Packing

5.1.1 The material shall be packed in such containersas agreed to between the purchaser and the vendorunder provisions of law in force from time-to-time.

5.1.2 All containers, in which the material is packed,shall be dry, clean. and leak-free.

5.1.3 Necessary safeguards against the risk arisingfrom the storage and handling of-large volume offlammable liquids shall be provided. and all dueprecautions shall be taken at all times to preventaccident by fire or explosion.

IS 323: 2009

Table 1 Requirements for Rectified Spirit for Industrial Use(Clause 4.2)

SI No. Characteristics Requirement Method of Test, Ref to- -IS No. Annex

(I) (2) (3) (4) (S)

i) Specific gravity at 20·C, Max 0.8126 IS IS464 A

ii) Ethanol conlent:

a) Percent by volume al 20·C, Min 9S .0 IS 2302 8

b) Degree overproof, Min 66

iii) Miscibilily wilb water Miscible C

iv) Alkalinity Nil D

v) Total acidity (as CHJCOOH ), mgll, Max 100 D

vi) Residue on evaporation percent by mass, Max 0 .01 E

vii) Aldehyde content (as CHJCHO), mgll, Max 100 F

viii) Ester conlent (as CHJCOOC1H,), mgll, Max 200 G

ix) Melbyl alcohol, mgll, Max 100 H

x) II-Propanol, mgll, Mtu 1000 8

xi) Iso-amyl alcohol mgll, Max 300 8

5.1.4 Except when they are opened for the purposeof cleaning and rendering them free from alcoholvapour, all empty tanks or other containers shall bekept securely closed unless they have beenthoroughly cleansed and freed from alcohol vapour.

5.2 Marking

All containers in which the material is stored ortransported shall be marked as prescribed by law inforce from time-to-time, The labels shall be legibleand indelible with the following information:

a) Name of the material;

b) Manufacturer's name;

c) Net gross and tare weight;

d) Recognized trade-mark, if any;

e) Date of packing;

f) Highly flammable; and

g) Hazardous chemical and injurious to health.

5.2.1 BIS Certification Marling

The container may also be marked with the StandardMark.

2

5.2.1.1 The use of the Standard Mark is governed bythe provisions of Bureau of Indian Standards Act,1986 and the Rules and Regulations madethereunder. The details of conditions under whichthe licence for the use of the Standard Mark may begranted to manufacturers or producers may beobtained from the Bureau of Indian Standards.

6 SAMPLING

Representative samples of the material shall bedrawn as prescribed in Annex J.

7 TEST METHODS

7.1 Tests shall be conducted as prescribed in col 4and S of Table 1.

7.2 Quality of Reagents

Unless specified otherwise, pure chemicals anddistilled water (see IS 1070) shall be employed intests.

NOTE - 'Pure chemicals' shall mean chemicals thatdo not coetain impurities, which affec;t the results ofanalysis.

IS 323 : 2009

ANNEX A[Table 1, Sl No. (i)]

DETERMINATION OF SPECIFIC GRAVITY

A-I DEFINITION

For the purpose of this standard, the specific gravityof a material shall mean the ratio of the weight of agiven volume of the material at a specifiedtemperature to the weight of an equal volume ofdistilled water at the same temperature.

A-2 METHOD I - SPECIFIC GRAVITYBOTTLE METHOD

A-2.1 The specific gravity may be determined bymeans of a pyknometer or a specific gravity bottle,or a special hydrometer. Specific gravity bottlemethod is referee method.

A-2.1.1 Apparatus

For determination of specific gravity, two alternatespecific gravity bottles shown in Fig.lA and Fig.lBare prescribed. In case of a dispute, the vacuumjacketed specific gravity bottles shown in Fig. IAshall be used.

A-2.1.2 Procedure

Clean the specific gravity bottle, its stopper and dryit in an oven. Cool the bottle, its stopper under adesiccator to 20° C and record the initial weight (B)

Fill the specific gravity bottle with the material toover-flowing ensuring no entrapment of air bubbles.Insert the stopper, immerse the bottle in the waterbath maintained at 20 ± 0.2°C and hold for 30 min.Remove the specific gravity bottle from the bath andclean and dry it thoroughly and weigh (A). Repeatthe experiment with distilled water (C)

A-2.1.3 Calculation

Specific gravity, at 20°C = ~=~where

A = weight of the specific gravity bottle withthe material at 20°C, in g;

B = weight of empty specific gravity bottle,in g; and

C = weight of the specific gravity bottle withwater at 20°C, in g.

A-3 METHOD 2 - OSCILLATING SAMPLETUBE METHOD

Determine the specific gravity of rectified spmtusing Method 2 (see A-3 of IS 15464 or any otherinstrumental method such as PAAR Density Meter,etc, provided the method has been validated).

FIG. IA VACUUM JACJCE1B) SPECIFIC GRAVllY Borns FlO. IB REoNAUU'S SPECIAC GRAVllY Borns

3

IS 323 : 2009

ANNEX B

[Table 1, Sl No. (ii), (x) and (xi)]

DETERMINATION OF ETHANOL CONTENT

concentration of all components are determined inmass percent area by normalization of the peak areas.

140°C2:10.1 to 0.5 Joll

B-3.3.3.1 Column temperature programme

Column Capillary column coated with 6percent cyanopropylphenyl, 94percent dimethylpoly-siloxane

30 m0.53 mm3J.lffi40°C5 min30°C/min230°C2 min

8-3.3 Apparatus

8-3.3.1 Gas Chromatograph, capable of operating atthe conditions listed below. A heated flashvaporizing injector designed to provide a linearsample spilt injection (for example, 2:1) is requiredfor proper sample introduction. Carrier gas controlsshall be of adequate precision to providereproducible column flows and split ratios in orderto maintain analytical integrity. Pressure controldevices and gauges shall be designed to attain thelinear velocity required in the column used. Ahydrogen flame ionization detector with associatedgas controls and electronics, designed for optimumresponse with open tabular columns, is required.

8-3.3.2 Sample Introduction - Manual or automaticliquid syringe sample injection to the splittinginjector is employed. Devices capable of 0.1 to 0.5 Jollinjections are suitable. It should be noted thatinadequate splitter design, poor injection technique,and overloading the column can result in poorresolution. Avoid overloading, particularly of theethanol peak and eliminate this condition duringanalysis.

8-3.3.3 Column - This test method utilizes a fusedsilica open tubular column with non-polar methylsilicone bonded (cross-linked) phase internalcoating. Any column with equivalent or betterchromatographic efficiency and selectivity to thosedescribed in B-3.3.3.1 can be used .

Column lengthInternal diameterFilm thicknessInitial temperature:Initial hold timeProgramme rateFinal temperatureFinal hold time

InjectorTemperatureSplit ratioSample size

8-1 GENERAL

8-3.2 Summary of Test Method

8-3.2.1 A representative aliquot of the ethanolsample is introduced into a gas chromatographequipped with a methyl silicone bonded phase fusedsilica capillary column. Suitable carrier gas transportsthe vapourized aliquot through the column where thecomponents are separated by the chromatographicprocess. Components are sensed by a flameionization detector as they elute from the column.The detector signal is processed by an electronicdata acquisition system. The ethanol, methanol andother components are identified by comparing theirretention, times to the ones identified by analyzingstandards under identical conditions. The

8-3 METHOD 2 - GAS CHROMATOGRAPHICMETHOD

Determine the ethanol content of anhydrous ethanolusing method given in IS 2302.

8-2 METHOD 1 - ALCOHOLOMETRICMETHOD USING HYDROMETER

Two methods have been prescribed for determinationof ethanol content in rectified spirit. Both themethods can be used for determination of ethanolcontent on routine basis. However, in the event ofany dispute, Method 2 should be treated as a refereemethod.

This test method covers the determination of theethanol content and other components such asaldehyde, ester (as ethyl acetate), methyl alcohol,n-propanol and iso-amyl alcohol of denaturedrectified spirit by gas chromatography.

8-3.1.1 The chromatographic analysis given here isfor information and guidance only:

8-3.1.2 Water cannot be determined by this testmethod and shall be measured by a procedure asgiven in IS 2362 and the result used to correct thechromatographic values.

8-3.1.3 This test method is inappropriate forimpurities that boil at temperatures higher than225°C or for impurities that cause poor or noresponse in a flame ionization detector, such as water.

8-3.1 General

4

IS 323: 2009

8-3.4 Approximate Retention Time

DetectorType

Temperature

Carr ier gas

Flame ionization

240°CNitrogen (3 rnl/min)

8 -3.5 Procedure

Retention TImesmin

15.50

17.78

20.88NOTE - Retention time may change slightly as peractual GC cond itions .

Sf No. Name of theComponent

ix) n-Bu tanol

x) Acetal

xi) Iso-amyl alcohol

Separately inject 0.5 J.11each of standard and sampleand record the chromatogram. Calculate theacetaldehyde. methanol. ethyl acetate. n-propanoland iso-amyl alcohol in the sample by areanormal isation method . Reference may be made toIS 15464 for detailed analysis. A typ ical gaschromotogram using flO showing retention time isgiven in Fig. 2.

3.96

4.205.65

9.12

10.53

12.75

13.46

14.83

Retention TImesmin

Name of theComponent

Acetaldehyde

Methyl alcohol

Ethyl alcohol

n-Propanol

Ethyl acetate

iso-Butanol

Benzene

Crotonaldehyde

i)

ii)

iii)

iv)

v)

vi)

vii)

viii)

Sf No.

591

~-'>0

-'XX s -'wOa~ 0

Cf :I:mV ~ < w 0w-, 0 ... w o

0> a:~ ~

...J

<~Cl. -' -c0 W

~:x: -'

~W W >-

:E z 0 :Ii!..J W -'

~398 >- J N

~~X III Z-' ~\Aj 0 W <

!!?lD ...~~ W

Uu~ <

IIIZ

2 00

000 1474 MIN. 2949

FIG. 2 TYPICAL CHROMATOGRAM R)R REcnFmo SPIRIT

ANNEX C

[Table 1, Sl No. (iii)]

TEST FOR MISCIBILITY WITH WATER

C·I PROCEDURE

C·I.I Mix 10 ml of the material with 190 ml ofwater in a suitable glass vine and allow to stand atambient temperature for minimum 10 min.

Compare the clarity of the mixture with that of anequal volume of water.

C-I.I.IThe material shall be taken to comply with thespecified requirement. if there is no noticeabledifference in clarity between the mixture and water.

5

IS 323 : 2009

ANNEX D

[Table 1, Sl No.(iv) and (v)]

TEST FOR ALKALINITY AND DETERMINATION OF ACIDITY

0-2.2 Determine the specific gravity of the materialat room temperature using a specific gravity bottleor a pyknometer or a suitable hydrometer.

0-3 CALCULATION AND REPORT

0-3.1 Report whether the material is alkaline oracidic.

0-3.2 Calculate the acidity. if any, in terms of aceticacid and express as percentage by weight of thematerial taken for the test:

Acidity (as CH)COOH), mgllitre = 600 VN

where

V = volume of standard sodium hydroxidesolution required for the titration, in ml ;and

N = normality of standard sodium hydroxidesolution.

0-1.1 Standard Sodium Hydroxide Solution ­O.IN.

0-1.2 Phenolphthalein Indicator - Dissolve 0.5gof phenolphthalein in 100 ml of rectified spirit andcarefully add standard sodium hydroxide solutiontill the colour is rendered faintly pink.

0-1 REAGENTS

0-2 PROCEDURE

0-2.1 Place 100 ml of water and a few pieces ofclean porous pot in a 500 ml conical flask ofresistance glass, and boil gently for 5 min toeliminate carbon dioxide. Cool slightly and add100 ml of the material. Boil gently for a furtherperiod of 5 min. At the end of this period, close theneck of the flask with a stopper carrying a soda-limeguard tube, and allow to cool. When cool, examinefor alkalinity; if not alkaline, titrate with standardsodium hydroxide solution using a micro-burette.

ANNEX E

[Table 1, Sl No. (vi)]

DETERMINATION OF RESIDUE ON EVAPORATION

E-l PROCEDURE

Evaporate, on a water bath, 100 ml or more of thematerial to dryness in a weighed, clean, dryplatinum, silica or resistance glass dish . Dry theresidue for 30 min in an oven at a temperature of100 ± 2°C. Cool in a desiccator and weigh.

E-2 CALCULATION

Residue on evaporation,percent by mass = B-A x 100

VS

where

B = weight of dish after evaporation, dryingand cooling, in g;

A = weight of empty dish, in g;

V = volume of the material taken for the test,in 00: and

S = specific gravity of the materialdetermined at room temperature (see0-2) .

ANNEX F

[Table 1, Sl No. (vii))

DEl'ERMINATION 0"ALDEHYDE CONTENT

F·I METHODS

F-1.1 For Low Aldehyde Content

A suitable colour reaction is available when thealdehyde content (as CH)CHO) is expected not toexceed 60 mg per litre of the material. This is basedon the resinification that takes place and the yellow

colour that results on treatment of acetaldehyde withsodium hydroxide. The procedure described underF-4.1 provides as satisfactory qualitative limit test,but in case of dispute, the quantitative proceduredescribed under F-4,2 shall be adopted in thequalitative procedure, acetals are also included asaldehydes.

6

F·L2 For Higher Aldehyde Content

For materials containing 0.05 to 0.5 percent ofaldehydes . only the quantitative procedure describedunder F-4.2 shall be adopted.

F-2 APPARATUS

F-2.1 Stoppered Flasks - Two. each of 250 mlcapacity and identical in shape, size and colour.

F·3 REAGENTS

F-3.1 Sodium Hydroxide Solution - Dissolve 20 gof sodium hydroxide in water and dilute to 100 mlwith water.

F-3.2 Stock Solution of HydroxylamineHydrochloride - Dissolve 20 g of hydroxylaminehydrochloride in 100 ml of water.

F·3.3 Metaphenylenediamine Hydrochloride

F·3.4 Aldehyde Free Alcohol- Re-distill rectifiedspirit over solid caustic soda or caustic potash. add2 to 3 g of metaphenylenediamine hydrochloride perlitre of rectified spirit, digest at ordinary temperaturefor several days or under a reflux condenser on astream bath for several hours and distil slowly.reject ing the first 100 ml and the last 200 mI of thedistillate.

F-3.5 Standard Sodium Hydroxide Solution-O.1N.

F-3.6 Bromophenol Blue Solution - Dissolve 0.1 gof bromophenol blue in 1.5 ml of standard sodiumhydroxide solution and dilute with water to 250 ml.

F-3.7 Hydroxylamine Reagent (Neutral AlcoholSolution of Hydroxylamine) - Dilute 10 ml of thestock solution of hydroxylamine hydrochloride with100 ml of aldehyde-free alcohol, add 2 ml of

IS323:2009

bromophenol blue solution, and then add standardhydroxide solution till the characteristic dichloricyellowish green colour is obtained.

F-4 PROCEDURE

F-4.1 Qualitative Test

F-4.1.1 Mix 10 ml of the material with 5 ml ofsodium hydroxide solution and set aside for 5 min.

F-4.1.2 The limit prescribed for aldehyde content(0.006 g per 100 ml) shall be taken as not haveexceeded, if no yellowish colour is produced in 5 min.

F-4.2 Quantitative Test

F-4.2.l Take 50 ml of the material in a flask, add25 ml of hydroxylamine reagent and 25 mI ofdistilled water. Allow to stand for 15 min. Meanwhileprepare a blank in a similar flask by using 25 ml ofhydroxylamine reagent and 75 mI of distilled water.Titrate this solution with standard sodium hydroxidesolution until the characteristic dichromic yellowishgreen colour appears. Titrate the sample solutionwith standard sodium hydroxide solution until thecolour matches with that of the blank solution.

F-4.2.2 Calculation

Aldehyde content (as CH3CHO), = 880 (V - v) Nmgllitre

whereV = volume of standard sodium hydroxide

solution required for the titration, in ml;v = volume of standard sodium hydroxide

solution required, if any, in the blank, inml; and

N = normality of standard sodium hydroxidesolution.

ANNEX G[Table I, Sl No. (viii)]

DETERMINATION OF ESTER CONTENT (AS ETIlYL ACETATE)

G-l REAGENTS

G-l.1 Standard PotaSsium Hydroxide Solutions ­Two, 0.1 Nand 0.5 N.

G-l.2 Standard Sulphuric Acid (see IS 266) - 0.1 N.

G·l.3 Phenolphthalein Indicator - Dissolve 0.5 gof phenolphthalein in 100 mI of rectified spirit andcarefully add standard potassium hydroxide solution(0.1 N) till the colour is rendered faintly pink.

G-2 PROCEDURE

G-2.1 Transfer exactly 100 ml of the material into aheat resistant flask of about 200-ml capacity, add a

7

few drops of phenolphthalein indicator andneutralize, in the cold (temperature below 10°C). thefree acid, if present, with standard potassiumhydroxide solution (0.1 N). Add 2 ml of standardpotassium hydroxide solution (0.5 N) attach the flaskto a reflux condenser provided with a soda-limeguard tube and reflux the contents on a water bathfor at least one hour. Cool the contents (temperaturebelow 10°C), pour into another flask, wash theoriginal flask with 100 ml of freshly distilled water,add the washings to the original liquor and thentitrate with standard sulphuric acid adding a fewdrops of phenolphthalein indicator.

IS 323 : 2009

G-2.2 Carry out a blank, using 100 ml of water inplace of the neutralized material.

G-) CALCULATION

Calculate the percentage of esters (as ethyl acetate)as follows:Esters as ethyl acetate(CH

1COOC1H1) g 1100 litre = 880 (V2 - VI) N

where

VI =

Vz =

N =

volume of standard sulphuric acidrequired in the blank, in ml;volume of standard sulphuric acidrequired with the material, in ml; andNormality of standard sulphuric acid.

ANNEX H

[Table I, stNo. (ix)]

DETERNUNATIONOFMETHYLALCOHOL

H-O Two methods, namely, spectrophotometric H-l.2.5 Methanol Standard Solutions - Dilutemethod and gas chromatography methods are appropriate volume of methanol stock solutionemployed . The spectrophotometric method is (see H-2.4) to 100 ml volumetric flask withsufficiently sensitive for routine type of analysis. The 40 percent (v/v) ethanol (methanol free) to get finalgas chromatography method is more sensitive and concentration 20, 40, 60, 80, 100 ppm of methanol.shall serve as a reference method.

H-1.3 Procedure

Calculate methanol content in g/IOO litre of absoluteethanol as follows:

where

A2 = absorbance for sample standard solution;C = concentration of methanol standard

solution, in g/ml;D =dilution factor for sample solution;AI = absorbance for methanol standard

solution; andS = ethanol content in sample, in percent

(vlv).

Take 50 ml of sample in a distillation flask anddistil, collecting about 40 ml of distillate. DiluteI ml of distillate to 5 ml with distilled water andshake well. Take l ml of this solut ion, 1 ml ofdistilled water (for blank) and I ml of methanolstandard solution in to 50 ml stoppered test tubes andkeep them in an ice cold water bath. Add to each testtube 2 ml of potassium permanganate reagent andkeep aside for 30 min. Decolorize the solution byadding a little sodium bisulphite and add 1 ml ofchromotropic acid solution. Mix well and 15 ml ofsulphuric acid slowly with swirling and place in hotwater bath maintained at 80"C for 20 min. Observethe colour development from violet to red. Cool thereaction mixture to 20°C and measure the absorbanceat 575 nm using 1 em path length cell.

H-1.4 Calculation

H-l SPECTROPHOTOMETRIC METHOD

H-1.1 ApparaM

H-1.1.1 Spectrophotometer, of any make withwavelength range from 350 to 700 nm and amaximum band width of 5 nm.

H-l.2 Reagents

H-1.2.1 Sodium Bisulphite, AR grade.

H-l.2.2 Potassium Permanganate Solution­Dissolve 3.0 gm of potassium permanganate and15 ml of phosphoric acid in 100 ml distilled water.The solution shall be prepared monthly.

H-l.2.3 Sodium salt of chromotropic acid solution(SodiumI, 8-dihydoxy naphthalene - 3. 6 -disulphonate),5 percentAqueous solution (mIv)

a) Prepare fresh solution every week of eitheracid or salt and filter, if not clear.

b) If necessary, prepare purified chromotropicacid by dissolving 109 of chromotropic acidor its sodium salt in 25 ml water (add 2 mlsulphuric acid to aqueous solution of salt toconvert it to free acid). Add 50 ml of methylalcohol heat just to boiling and filter. Add100 ml iso-propyl alcohol to precipitate freeacid-chromotropic acid. Add more iso-propylalcohol to complete precipitation of acid.

H-l.2.4 Methanol Stock Solution - Dilute 1 g ofmethanol [99.9 percent (v/v)] to 100 ml with40 percent (v/v) ethanol (methanol free). Dilute to mlof this solution to 100 ml with 40 percent ethanol(methanol free).

8

Methanol content =A2 x CxDx 1000 x lOOx100

A1xS

IS 323 : 2009

H-2 GAS CHROMATOGRAPWC METHOD H-2.1.2.1 Identification

H-2.1.2.2 Calibration and standardization

The response of any given detector varies from onechemical to another. Therefore, calibration is must.Calibration allows the computation of responsefactor which express the relative response of differentcomponents to the detector.

Calibration standard is prepared containing theimpurities present in anhydrous alcohol. Duringstandard preparation the exact amounts of all thecomponents is noted. Inject 0.2 ~l of calibrationstandard in the chromatographic column inaccordance with the specified conditions.

Calculate response factor to four decimal places forall components relative to anhydrous alcohol usingfollowing equation:

WxAMRI.= A 'xWM

•where

RJ. = response factor for component .r relativeto acetone,

W. = weight of component x, in the calibrationstandard,

A. = area of component x, in the calibrationrun,

WM = weight of acetone in the calibrationstandard, and

AM = area of acetone in the calibrationstandard run which is selected asreference component.

The component which is unknown in the sample isassigned the relative response factor 1.000 O. It isadvisable that the determination of response factorsbe made on the basis of duplicate analysis.

Response factor should be re-checked after anyperceptible change in column or instrumentsperformance.

H-3 PROCEDURE

Inject 0.2 ~I of sample into the chromatographiccolumn, using the same conditions as for componentsidentification and standardization. Record andintegrate the chromatogram using appropriateattenuation setting that provide optimum peakheights. Measure the area of all the peaks.

andCalibration

Chromosorb 101

801100

3m

3mm

Stainless steel (tubing must benon-reactive with substrate,sample and carrier gas)

Hydrogen for TCD and Heliumor Argon or Nitrogen for FID(Purity - 99.99 mole percent,Min)

10 ml

0.2 ml

For computation of resultsintegration

This test method is related to determination of Determine the retention time of each component bymethyl alcohol content by gas chromatography. injecting small amount either separately or in known

mixture.H-2.1 Apparatus

Gas Chromatograph Any gas liquidchromatograph equipped with FlO or TCD detectorcan be used with following accessories and operatingconditions:

Column

Mesh size

Column length

I.D.

Column tubing :material

Carrier gas

Syringe

Sample size

Electronic

H-2.1.1 Instrument Condition

Detector TCD or FlO

Oven temperature I WOC

Injector, temperature 280°C

Detector, temperature 200°C

Carrier gas flow rate . 30 ml/min

NOTE - The above gas chromatographic conditionsare suggestive. However. any GC with different columnmay be used provided standardization/calibration aredone after selling up chromatographic conditions forthe required resolution.

H-2.1.2 Identification.Standardization

Install the column in the chromatograph. Set theconditions given above, of column temperature andcarrier gas flow that gives the necessary resolutionof the components in the sample being analyzed. Setthe conditions as such which gives a minimum 10percent recorder deflection for a 0.1 percentconcentration at the most sensitive setting ofinstrument. Allow sufficient time for the instrumentto reach equilibrium as indicated by stable base line.Adjust carrier gas flow rate to a constant value.

9

IS 323 : 2009

8-4 CALCULATION

Calculate the concentrations of sample componentsusing the following equation:

f.xRC

I, percent = ~ Xf.· x 100

I •

whereC

I= component .r, mass percent,

R. = peak response of component x.f

l= relative response factor of componen z;

and(R

I) x If,) = sum of the individual component peak

responses (R.) multiplied by theirrelative response factors if.).

ANNEX J(Clause 6)

SAMPLING OF RECnF'IED SPIRIT

J-l GENERAL REQUIREMENTS

J-l.0 In drawing, preparing. storing and handlingtest samples. the following precautions anddirections shall be observed.

J-l.l Samples shall not be taken in an exposedplace.

J-1.2 The sampling instrument shall be clean and drywhen used.

J-l.3 The samples. the material being sampled. thesampling instrument and the containers for samplesshall be protected from adventitious contaminations.

J-l.4 To draw a representative sample. the contentsof each container selected for sampling shall bemixed as thoroughly as possible by shaking orstirring or both by suitable means. or by rolling soas to bring all ponions into uniform distribution.

J-l.5 The samples shall be placed in suitable. clean.dry and air-tight metal or glass containers, on whichthe material has no action.

J·l.6 The sample containers shall be of such a sizethat they are almost but not completely, filled by thesample.

J·l.7 Eacb sample containers shall be sealed air­tight with a glass stopper after filling, and markedwith full details of sampling, the date of sampling,and the year of manufacture of the material.

J-l.8 Samples shall be stored in such a manner thatthe temperature of the material does not vary undulyfrom the normal temperature.

J-l.9 Samples shall be protected from light as far aspossible.

J-2 SAMPLING INSTRUMENTS

J-2.0 The following forms of sampling instrumentsmay be used:

a) Sampling bottle or can for taking samplesfrom various depths in large tanks, and

b) Sampling tube for sampling homogeneousmaterials.

J-2.1 Sampling bottle or can consists of a weighedbottle or metal container with removable stopper ortop, to which is attached a light chain. The bottle orcan is fastened to a suitable pole. For taking asample. it is lowered in the tank to the requireddepth. and the stopper or top is removed by meansof the chain for filling the container.

J-2.2 Sampling tube for homogeneous liquids ismade of metal or thick glass, of 20 to 40 mmdiameter and 400 to 800 rom length. The upper andlower ends are conical and reach 5 to 10 mmdiameter at the narrow ends. Handling is facilitatedby two rings at the upper end. For taking a sample,the apparatus is first closed at the top with the thumbor a stopper and lowered until the desired depth isreached. It is then opened for a short time to admitthe material and finally closed and withdrawn.

J·2~1 For small containers, the size of the samplingtube may be altered suitably.

J-3 SCALE OF SAMPLING

J-3.1 From a Tank

Take two sets of samples, one from the top andanother from the bottom, and test them separately.

J·3.2 Material from a Single RUD

Select one container at random and sample asdescribed under J-4.2.

J·3~1 If the single sample fails to comply with therequirements of the standard, procedure for samplingof material from mixed batches, described underJ·3.3, may be followed for re-test, if so agreed.

10

J-3.3 Material from Mixed Batches

J-3.3.1 Lot

All the containers in single consignment of materialdrawn from a single batch of manufacture shallconstitute the lot. If a consignment is declared toconsist of different batches of manufacture, thebatches shall be marked separately and the groupsof containers in each batch shall constitute separatelots.

J-3.3.2 Gross Sample

A number of containers shall be selected at randomfrom a lot for the purpose of drawing samples for test.This number of containers shall constitute the grosssample. Size of the gross sample in relation to thesize of the lot, or the scale of sampling, shall besubject to agreement between the purchaser and thevendor.

J-3.3.3 Suggested Scales of Sampling

In the absence of an agreement as to the scale ofsampling and a guide to such an agreement, twoscales are suggested, namely the normal scale and thelow scale, as given in Table 2. The normal scale isto be used wherever possible and the low scalewherever the cost of the tests (including cost ofmaterial) is likely to be relatively high.

Table 2 Minimum Number of Containers to beSelected for Sampling from Various SiZes of Lots

SI No. Size or Lot Size of Gross Sample-(I) (2) (3) (4)

i) Under 2S 10 Sii) 2S 10 49 IS S

iii) SO 10 99 20 10iv) 100 to 199 30 ISv) 200 10 299 40 20

vi) 300 to 499 SS 30vii) SOO to 799 7S 40

viii) 800 to 1299 us SSix) 1300 to 3199 ISO 7S

x) 3200 to 8000 22S liS

NOTE - The two scales of sampling suggested arebased on statislical consideration. By using one of thesescales, the risk of accept ing a defective lot or rejeclinga good lot, as judged by the inspection of the numberof containers in the gross sample. remains the same.irrespective of lhe lot size. These risks, however. aredifferent for the two scales of sampling. All samplingplans requiring a given percentage of the lot to bechosen as a sample are considered basically unsoundfor they invariably lead to relatively higher risks incase of smaller lots. These risks progressively decreaseas the size of the lot increases. Furthennore, in thecase of very big lou, the percentage sampling plansbecome uneconomical because of the unnecessarilylarge size of sample.

II

IS 323 : 2009

J-4 PROCEDURE

J-4.1 Sampling from a Tank

With the help of a sampling bottle or can. draw asufficient number of samples from the top and thebottom. Keep, the top samples separate from thebottom samples, but mix each of these thoroughlyand draw from each three test samples. each not lessthan 750 ml in volume.

J-4.2 Sampling from Containers

J-4.2.1 The procedure varies according to the size ofthe containers , namely whether the material issupplied in large containers of 180 litre and more,or in smaller containers .

J-4.2.2 Mixing Contents of Containers

Before drawing the test sample, thoroughly mix thecontents of all containers in a gross sample, whetherthey are drums, bottles, cans or others, by shaking orstirring or both by suitable means, or by rolling soas to bring all portions into uniform distribution.

J-4.2.3 Drawing ofSamples

Draw by inserting the sampling instrument throughthe bung hole or any other convenient opening,small portions of the material from different parts ofeach container in the gross sample.

J-4.2.4 Reduced Samples

Separatelymix the samples drawn from each containerobtain a composite sample for the container whichshall be not less than 3 litre. Divide this compositesample in to the required number of reduced samplesof not less than 750 ml in dried bottles or othercontainers. seal air-tight and label with all theparticulars of sampling given under J-l.7.

J-4.2.5 Test Samples

The set of samples consisting of one each of thereduced samples, representatives of each of thecontainers in the gross sample, shall constitute thetest sample.

J-4.2.6 Referee Samples

One of the test samples, bearing the seals of thepurchaser and the vendor, shall constitute the refereesample, to be used in case of dispute between thepurchaser and the vendor. It shall be kept at a placeagreed between the purchaser and the vendor.

J-S TESTS FOR ACCEPTANCE

J-S.l Examination and Tests

The purchaser may examine and test each of thereduced samples constituting a test sample separately

jUdging the quality of the lot for the purpose ofacceptance on the basis of the result obtained shallbe as given below, unless otherwise previouslyagreed between the purchaser and the vendor:

TestRes~U Atean Range

IS 313: 2009

for compliance with the requirements of thisstandard, or be may prepare, for the purpose of suchexamination and at any stage of the progress of theexamination, a composite sample representative ofthe whole lot, by mixing all the reduced samplesconstituting the test sample.

J-5.2 Criteria for Judgment

When the individual reduced samples in a testsample are separately examined and the results varyfrom one reduced sample to another, the criterion for

12

1,2, , n R

Criterion forAcceptance

( X - O.6R) shall benot less than 94.85percent by volumeat 20°C or 66° OP.

Bureau or Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act . 1986 to promotel:armonious development of the activities of standard izat ion. marking and quality certification of goodsand attending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced in any formwithout the prior permission in writing of BIS . Th is does not preclude the free use, in the course ofimplementing the standard. of necessary details, such as symbols and sizes, type or grade designations.Enquiries relating to copyright be addressed to the Director (Publications). BIS.

Review of Indian Standards

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 rev iew indicates that no changes areneeded: if the review indicates that changes are needed. it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issueof 'BIS Catalogue' and 'Standards : Monthly Additions'.

This Indian Standard has been developed from Doc: No. PCD 9 (2156).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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