Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 1162 (1958): Cane Molasses [FAD 2: Sugar Industry]

Gr5

IS : 1162 -1958( Reaffirmed 2004 )

Indian StandardSPECIFICATION FOR

CANE MOLASSES

Eighth Reprint JANUARY 2005( Incorporating Amendment No. I )

UOC 664.15

o Copyright 1966

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

July 1959

9

AMENDMENT NO. 2 JUNE 2011 TO

IS 1162 : 1958 SPECIFICATION FOR CANE MOLASSES [Page 6, clause 7.3(d)] — Substitute ‘Net quantity’ for ‘Net mass’. [Page 6, clause 7.3(d)] — Add the following after Sl No. (d):

‘e) Any other requirements as given under the Standards of Weights and Measures (Packaged Commodities) Rules, 1977 and the Prevention of Food Adulteration Act, 1955 and the Rules framed thereunder.’

(FAD 2)

Reprography Unit, BIS, New Delhi, India

Ministry of Food ~ Agriculture

( CDntinued Dn /Jagl 2 )

IS 11162.1958

Indian StandardSPECIFICATION FOR

CANE MOLASSES

Sugar Industry Sectional Committee, AFDC 8

Clttli""tJnSRRI T. PaA8AD

Memb"sAOBICTLTUBAL MARKETJNG Directorate of Marketing It Inspection ( Minish")- of

ADVI8EB TO THE GOVEBNMENT Food at Agriculture)01' INDIA

SHRI R. K. MALlE ( Alt"natt-)SaRI D. R. DANI Indian Sugar Mills Association, Calcutta

SHRI BRAHMA SWABUP ( Altematt)DIBECTOR "OR GUB AND KHAND- Khadi It Village Industries Commiuioh, Bombay

BARIDIRBCTOR. SUOARCANE RESEARCH Development (Agriculture) Department, Govern.. AND DEVBLOP,-ICNT mt-nt of BiharSURI A. L. GOENKA Indian Confectionery Manuracturen' Association.

CalcuttaSHftl J. S. MERTA ( AlImltlU )

S8RI GOLABCR,AND Hla,AOBAND Development Council (or Sugar Industry, New DelhiSHRI S. N. GUNDU RAO National Sugar Institute, KanpurSHill SUBE8B CSAJfDBA GUPTA SUI.r T~chnologiltJ·Association, KanpurSBRI GYAH eRA-MD.A Developmrnt Council for SUlar Industry, Nt'w DelhiSHIn HAl'S.AJ HARtRAIl Development Council for Supr Industry, New DelhiSHill J. S. HUJA. Development Council for Supr Industry. New DelhiSRIlI le. P. JAIN Ministry of Food at AgricultureSSBI MATADI. KRAITA. Bengal Sugar ~fercb_ntl·AlJOCiatioD, Calcutta

SRal BABULAL NSWAR ( Altmlt", )S8RI A. C. KHANNA Federation of Biscuit Manufacturen' of India, Dt'lhi

SaRI K. J. PAIINAIfI ( AllntUlt, )8.BI P. S. K"'.BKAN Central Revenues Control Laboratory (A-finiltry of

Finance)SRRI. N. K. CBOWDRt:BI ( AIlnntJl, ) .

DR P. K. K YMAL Ministry of Food &: AgricultureSaRI LAL SINGH Indian Central Sugarcane Committee, New DelhiSanl D. R. NAKANO Indian Sugar MiJJ. Association, CalcuttaSRIH GANGA SHANKER PANDEY Cawnpore Sugar Merchants' Association, KanpurSHar K. H. PAREKH Sugar Technologists' Association, KanpurSRRI K. U. PATEL All India Food Preservers' Association, Bombay

SHRI P. D. BHARGAVA ( AII~'''Qlt)

BUREAU OF INDIAN STANDARDSMANAK BRAVAN,' BAHADVR SHAH ZAFAR MARC

NEW DELHI 110002

15,1162·1958

( CDrrlu,wtlfrom /MI' J )M_.,SRRI J. hAIADSHBIl.P.SAXENASURf B. S. SETHDR Y. K. SUBRAUJIANYAIlDR W. M. VAJDY.4

SUBl N. VAlDYANA....BANDa LA.L C. VBRMAN (E,·offitiD)

S«r,ldrilsDR D. V. KARMA.EAR

Sum P. H. RAJIAlfATHAN

Government of BiharRohta. IDdustries Limited. DalmianagarGovernment of Uttar PradeshMini.try of HealthCouncil of Scientific & IndUitna) Research, New

DelhiDelhi Cloth It General Mills Co Ltd, DelhiDirector, lSI

Deputy Director ( Agri ) I lSIExtra Anistant Director ( Agri ), lSI

Molasses Subcommittee, AFDC 8 : 4

CO"HftIrSSBJ S. L. VBNKITEaWAltAN Developmmt Wing, Ministry of Comlnerc~ It

Industry

Af.",bnsSHBt D. G. CoWl!: The Indian Molasses Co Private Ltd. Calcutta

SH1\1 H. F. HO.Kllf8 ( All""., )SRBI S. N. GUKDt1 RAO' National Sugar Institute, Kanpur

SHltl J. P. SHOKLA ( AI,.",.,,)SKRt KEBAR SOIOR Government of Uttar Pradesh

SURI V. R. DAMLE ( .AllmuIU)581\1 B. L. KHANNA All India Distillers' Auociation, New DelhiSHRJ J. S. P.&BHU Indian Sugar MiJls Association, CalcuttaSBRI R. PRASAD Governm~ntof Bihar

SaRI M. P. RAY ( A".,.,,)SHBI M. A. RANOA.AMI All India Distillers' AlIOCiation, "New DelhiSRat J. M. SABA IDdian Supr Mills AuociatioD, CalcuttaSUPERlNTBNDSXT, Go.UNIII:~ Government or Bombay

CE!ft'BAL DJ8TlLLBBY. NAIIK

2

ISa 1112.1151

Indian StandardSPECIFICATION FOR

CANE MOLASSES

o. POREWORD

0.1 This Indian Standard was adopted by the Indian Standards Institu­tion on 23 December 1958, after the draft finalized by the Sugar IndustrySectional Committee bad been approved by the Agricultural and FoodProducts Division Council.

0.2 Cane molasses is an important by-product in the manufacture of canesugar. It is a dark coloured viscous syrupy liquid obtaintd in this coun.tryas a by-product both b)' the vacuum pan process and the Klta"dsar; processof manuracture of canc· sugar. The bulk of the supply of molas~s is,ho\\Oever, obtained in the vacuum pan process. The requirements pres­cribed in this standard are, therefore, rclat~d to the material producedfrom the vacuum paD p,·ocess.

U The composition of molasses depends on such factors as the qualityand variety of cane as well as the manurial process, climatic and soil con­ditions, the extent of milling and the mode of processing of the juice. Themethod of proc~ssingof the juice has, no doubt, a greater influence than.n other (actors. Because of the fact that, in India, molasse. is essentiailyobtained as a by-product during the manufacture of direct-consumptionwhile sugar by the vacuum pan process, the composition of molassesproduced in this country diffen from that obtained in other sugar·producing countries where it is obtained during the production of rawsurar.

1.4 Molasses is used in the fermentation industries for production of ethylalcohol, rum, yeast, acetone. butanol, certain organic acids, etc. It is alsoused for the manufacture of'HUKA Tobacco'. The largest utilization ofmolasaea in India at pre~nt is, however, in the alcohol industry. As such,this standard has been drawn up mainly keeping in view the requirementsof the alcohol industry. -

IS: 1162 .1951

0.5 The entire production of cane molasses is not being utilized, at present,in the country. Due to paucity of tank ~'agons, storage facilities at theport, and other economic factors, export of molasses is also not much.I,'or these reasons, molasses has often to be stor~d in sugar factories for anappr~ciable length of time. The storaKe conditions available at manyfactories are not as good as they should be. Under these conditions, thereis a gradual reduction of the percentage of its sugar content. After givingdue consideration 10 thc~ (actors as w~1l as to the existing rules laid downby the States of Uttar Pradesh, Bihar and Bombay, for controlling the saleof molasses, the Sectional Committee decided that there shall be threegrades of molasses with varying requirements as specified in Table I.

0.6 In view of th~ ease (Jf determination 'of total reducing matter whencompared to that of rernlentable sugars and because of the fact that about95 percent of the total sugars in molasses are fermentable, "the SectionalCommittee decided to prescribe r~qujrements for total reducing matte~

(Sft Table I ) as againsl f~rmentahle sugars.

0.7 Taking into consjd~ration the vi~ws of producers, consumers. testingauthorities and technologists, the Sectional Committee responsible for thepreparation of this standard felt that it should be related to the manu·facturing and trade practices foJlo\ved in the country in this fie.ld.Furthermore, due weightage had to be giv~n to the need for internationalco-ordination among standards prevailing in different countries of theworld in this field. These considerations led the Sectional Committee torefer to the following publications:

32.GP·211 (1954) SPECIFICATION FOR ~·IOLASSES. CanadianGovernment Specifications Board, National Research Council,Ottawa, Canada.

ID·~f-576 b( 1949) ~IOLASSESJ SUGAR-eANE. Bureau of FederalSupply, USA.

OFFICIAL METHODS OF ANAl.YSIS OP THB AasoclAnoN OF OFPICIALAGRICULT1J1lAL CHltMlSTI,8TH ED. Washington 1955.

0.8 This standard requires reference to the following Indian StandardSpecifications:

-IS :266·'1950 SULPHURIC ACID

.IS: 376-1952 SODIU)I HYDROXIDE, A~ALYTICAL REAGENT

0.8.1 Wherever a reference to any specification mentioned under 0.&appears in this standard, it shall be taken as a reference to the latestversion of the specification.

..

IS I 1162.1'51

0.9 For the purpose of deciding whether a particular requirement of thisstandard is complied \vith, the final value, observed or calculated,expressing the result of a test or analysis, shall be rounded off in accord­ance with -IS: 2·1949 Rules for Rounding Off Numerical Values. Thenumber of significant places retained in the rounded off value should bethe .same as that of the specified value in this standard.

0.10 This standard is intended chiefly to cover the technical provisionsrelating to cane molasses, and it does not include all the necessary provi­sions of a contract.

1. SCOPE

1.1 This standard prescribts the requirttmcntl and the methods of test forcane molasses obtained in the manufacture of direct--consumption whitesugar by the· vacuum pan process and meant primarily for use in thealcohol industry.

2. TERMINOLOGY

2.1 For the purpose of this standard, molasses shall mean the motherliquor left over, after the recovery of sugar in the vacuum pan process.

3. GRADES

S.I There shall be three grades of molasses, namely, Grade I, Grade 2and Grade 3.

4. SAMPLING

4.1 Representative samples of the material shall be drawn IrS prescribedin Appendix A.

5. REQ,UIREMENTS

5.1 Descriptio. - The materi,al shall be dark coloured ViSCOUl, syrupyJiq~id having a characteristic odour.

5.2 Tht; material shall comply with the requirements given in Table I.

6. Q,UAUTY OF REAGENTS

6.1 Unless specified otherwise, pure chemicals shall be employed in testsand distilled water shall be u~d where the ,use of water as it\ reagent isintended.

NOTa - 'PUle' chemicals· shall mean chemicaIt that do not contain inlpuritics whic'affect the rault. of aaalytis.

5

IS 11162 ;.1158

B

c

D

METBODOJITUT( RErTO

ApPENDIX)

(6)

80

40

17-5

(5)(4)

80

17-5

50

85

14·0

(3)

TABLE I RBQVIRDI£N'n FOR CANE MOLASSES

(CltUlS6 5.2)

RaqulBBIIDf'I' JIOa,-----~.&._----~Grade 1 Grade 2 Grade 3

(2)

Density. in deBtees Bria at27-5·0. Mill

Alb. I\IIphated, pcTCeDt bymass (calculated for100° Brix), kltl¥

Total reducing matter ..iDvert lUgar, percent bymass, Mi"

iii)

ii)

el)

i)

SL!'O.

7. PACKING AND MARKING

7.1 Balk Delivery - The material shall be delivered in bulk in tankers.

7.2 DeUver, I. Coatalaer. - The material shall be packed in clean,dry and leak-proof containers. Unless othtrwise agreed bet\veen thepurchaser and the vendorJ such containers shall be made of tin plate, orblack or galvanized iron sheets and may be of capacity between 175 and225 litres or 18 lit res.

7.3 MarIdaS - The (ollowing information shall be marked legibly andindelibly on each container:

a) Name of the material,b) Grade of the material,c) Name of the supplier, andd) Ne" mass

73.1 Each container may also be marked \yith th~ Standard Mark.

NOTE - The use of tho Standard Mark is governed by the provisions of thoBureau of Indian Standards Act, 1986 and tho Rules and Re,ulatjons made there­under. The Standard Mark on products covered by an Indian Standard conveystho assurance that they have been produced to comply with the requirements of thatstandard under a well defined system or inspection, tatinl and quality controlwhich is devised and supervised by DIS and operated by the producer. Standardmarked products are also continuously checked by DIS for confornlity to thatItandard as a further safoauard. Details of conditions under which a licence forthe use of the Standard Mark may be Iranted to manufacturers or producen maybe obtained from the Bureau of Indian Standards.

6

IS 11162-1958

APPENDIX A( Clause 4.1 )

SAMPLING ()F CANE MOLASSES

A-I. GENERAL REQ,UlREMENTS

A-I.O In drawing, preparing, storing and handling test samples, thefollowing precautions and directions shall be observed.

A-1.1 The sampling instrument shall be clean and dry when used.

..\-1.2 The samples, the material being sampled, the sampling instrumentand the containers for samples shall be protected from adventitiouscontamination.A-l.3 To draw a representative sample, the contents of each containerselected for sampling shall be mixed as thoroughly as possible by shakingor stirring or both, or by rolling so as to bring all portions into uniformdistribution.A-l.4 The samples shall be placed in suitable, clean, dry and air-tightmetal Of glass containers, on which the material has no action.

wu.oro

00 ••VI TID W,TN1.10 MOM ...ilOI

FlO. I SAJIPUNO CAM "OR T ANKrrANKER

7

IS 11162.1958

A-I.5 The sample containers shall be of such a size that they are almost,but not completely, filled by the sample.

A-I.6 Each sample container shall be sealed air-tight with a glass stopperafter filling, and marked with full details of the sample and the date ofsampling.

A.2. SAMPUNG INSTRUMENTS

A-2.1 Sa.pUDS ea. - consists of a weighted metal cylinder, withremovable top, to which a rod is attached (se, Fig. 1). The cylinder isfastened to a suitable rod. For taking a sample, it is lo\vered in the tankto the required depth, and the top is removed with the help of the rodand the can then filled.

A-2.I.l For other containers, the sampling device of the design shownin Fig. 2 may be used.

'IG. 2 SAJIItLIJfO DBVICE roa eoJrTAllUB.

A-3. SCALE or SAMPLING

A-3.1 Sappl)'" Is Taak/T••ker - Samples shall be drawn from eachtank/tanker as prescribed under A.~l.

A-3.2 Sappl)' Ja eo.talaen

A-3.2.1 All the containen in a single consignment shan constitute onelot.

A-3.2.2 GrDSS ~Ilmpl,-For the purpose of drawing samples for test, anumber of contalnen shall be selected at random Crom a lot. This num~rof containen in relation to the size of the lot, or the scale of sampling,

8

IS .1162 .1951

shall be subject to an agreement between the purchaser and the vendor.As a guide to such an agreement, a scale of the size of the sample issuggested in Table II.

TABLE U MINIMUM NUMBER OF CONTAINERS TO BE SELECTEDFOR SAMPLING FROM VARIOUS SIZES OF LOTS

LOT SIZE

2 to 8

9" 2728,. 6465 ., 125

126 n 216

SAJlPLB LoT SIZE SAXPUSua Swc

2 217 to 343 73 344 n 512 84 513 " 729 9.5 730 " I 000 106 1001 " 1 331 11

A-f. PROCEDURE

A-4.1 SaIDpiiDI from • TaDk/Taaker - Take equal portions of thematerial from different layers of the tank/tanker with the help of the samp­ling can (Sit A.2.1 ) to obtain a quantity not less than 2·5 liters and mixthorougly in a suitable container. which is dry and clean, to obtain a com­posite sample for the tank/tanker. Divide this composite sample in threeequal portions of nut less than 750 rol in dried bottles or other containers,seal air-tight and label with alJ the particulars of sampling givenunder A.I.6.

A-4.2 SampliDl r... CoDtaiaer8

A....2.1 Mixi., - Thoroughly mix the contents of all the containen inthe gross sample whether they are drums or cans of others, by shaking orstirring, or both, or by rolling so as to bring all portions into uniformdistribution.

..\-4.2.2 Drawing of Samples - Draw by inserting the sampling device(set A.2.I.l) through the bung hole or any other convenient opening,equal portions of the well-mixed material from each container in the grosssample so as to obtain a quantity not less than 2-5 litres. Divide thiscomposite sample into three equal portions of not less than 750 ml in driedbottles or othtr containers, seal cair-tight and label \\"ith all the particularsof sampling given under A-l.6_

A.4.3 Sample. for Purchaser aod Vendor - One. sample shall be sentto the purchaser and another to the vendor.

1S,1162.1'58

A-4.t Rei..... Sample - The third sample bearing the seals of thepurchaser and the vendor shall constitute the referee sample to be UJed incase of dispute between the purchaser and the vendor_ It shall be kept ata place agreed to between the purchaser and the vendor.

A-4.5 Time Limit lor Aaalysla-AU samples shan be tested within twomonths from the date of sampling.

A~6 CriterioD lor AcceptaDce - If, on testing, the sample is found toconform to the requirements specified in the standard, the consignmentshall be accepted.

AP1'ENDIX Bo[ Table I, lltm (i) ]

DETDMlNATION or DENSITY IN BIUX

8-1. APPARATUS

8-1.1 ..... Hydrometer-calibrated at 27-SoC and fitted with a ther­mometer.

8-1.2 lmIDenloD V...el-suitable for the hydrometer used.

8-2. PROCEDURE

11-2.1 Weigh 200 g of the material. Add 1400 g of cold water. Mixwell till a homogenous solution results. Determine the Brix using Brixhydrometer orsuitable range noting simultaneously the temperature of thesolution. Apply the temperature corrections to the readings by usingTable III. .

8-3. CALCtJIAnON

8-3.1 Multiply the corrected Brix reading (SI' 8-2.1) by 8. This givesthe density or the molasses in dqrees Brix at 27·5°C.

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0·88

0'88

0·88

&89

0-88

0-88

0'88

0-88

-39

0·9

00-

920'

920-

940'

950-

960·

9700

970-

970-

98()O

970

'97

0-97

0-97

.~

40

0·99

1·01

1-01

1'03

I-o

t1

'05

1-06

1·06

1'06

1-07

1'0

61

'05

1-05

1-05

451

'48

I'SO

I-50

1'52

1'53

1'5

3I-

531'

551·

52I-

52I'

S)

I'SO

1'5

01'

4850

2'0

32-

04-

2·M

2-05

2'06

2-05

2-04

-2'

032'

012·

001

'99

1'9

71

'96

)'9

255

2-62

2'63

2'6

!2-

642-

622'

602-

582-

552·

522-

502

'48

2-45

2-43

2-37

603'

26"2

83-

273·

253-

223'

18S-

133-

09'-0

43

'02

2-98

2-94

2-90

2'8

365

3·95

3'98

3'95

3'90

3'86

3'79

3-71

3·66

3-58

3'5

63-

503-

443

-38

3-30

704'

704-

7'4-

704-

604-

544

'44

4'3

24·

244'

144'

124'

033-

963-

S73-

7875

5'50

S'5

64-

485-

345

'26

5'1

24-

954-

864'

724-

704'

574

'SO

4-37

4-27

806'

356-

416'

S2

6'1

26-

02S·

845-

625-

5.5·

325-

305-

1f5·

044

'88

4'7

7

IS: IIG.I'5I!

10000 wWX==

APPENDIX C[ Table I, Item. (ii) ]

DETEIlMINATION or SULPHATED ASH

Cel. REAGENT

e-l.l Coaceatrated Salphurlc Add-sp gr 1·84 (conforming to analy­tical reagent grade of ·IS: 266-1950).

0.2. PROCEDUREC-2.1 Weigh accurately abOut 5 g of th«: material into a suitable taredplatinum dish or quartz crucible. Grad",ally add 2 ml of concentratedsulphuriC acid to the material in the dish. . Place the dish or crucible on ahot water oven. When the charred mass does not incr~ase in vol~me anylong~r, continue the heating ov~r ~ small flame, care being taken to avoidspurting, until the fumes of sulphur trioxide or sulphur dioxide are notevolved. Increase heat till a pinkish grey ash is obtained. ( Ifavailabte.a muffle furnace may be used at a temperature of 550° to 600°C.) Coolthe ash and moisten it with a few drops of concentrated sulphuric acid,heat strongly on a bot plate until fumes of sulphur trioxide cease to be.evolved and finally ash to constant mass.

C-3. CALCULAnON

c..3.1 Ash, sulphated, percentby mass {calculatedfor 1000 Brix )

whereIII =t ma.u in g of the ash,W - maa in g of the material taken for the test, andX -= density of molasses in degrees Briz ( SI' 8-3.1 ).

APPENDIX D[ Tablt I, Item (iii)]

DETERMINATION OF TOTAL REDUCING MArlER

1).1. REAGENTS

0.1.1 Stock Sol.d...'lavert SUlar- Weigh accurately· 9·500 0 g ofpure sucrose on a watch glas and transfer it to a one-litre volumetric flask

·Siace revilecl

13

1S.1162.I_

with 100 mJ water. Add 5 ml of concentrated hydrochloric acid(sp gr 1·19). Allow this to stand for 3 days at 20° to 25°C and thenmake up to volume with water. (This i. ltable (or several months. )0.1.2 Staacla.... Solati.. oll.vert hpr- Pipette'50 ml of the stocksolution of invert lugar (Sf' B-l.1) in a 250-ml volumetric flask. Neutra.lize carefully with sodium hydroxide of about -one percent ( wiD) and makeup to the volume.0-1.3 Medayl... BI•• 1_leato. 8olatt.a- DiIIolVe 1-0 lof methyleneblue in water and dilute to '00 mI.B-l.4 Felli"". Solad.. (Iodalet ModUlcad..) - Prepare by ~ixin8immediately before use. equal volumes of IOlution A, prepared .1 describ­ed under B-l....1. and solution B. prepared .. descri~d under B-1.4.2.

0.1....1 Solution ..4 - Dissolve 34~39 I of copper sulphate (CuSO••5H.0) in water t and 0-5 ml of concentrated sulphuric acid of sp II' 1-84(conforming to analytbl reasent ~ade oC-18:'66-1950), and dilute to500 ml in a volumetric &ask. Filter the solution through prepar~d

asbestos.0.1.4.2 Sol" B - DillOlve 173 g of Rochelle ..It [potassium sodium

tartrate ( KNaC.H.O't 4Ht O) 1and 50 g of lOClium hydroxide, analyticalreagent (conforming to IS: 376-1952) in water, dilute to 500 ml in avolumetric ftaak and allow the IOlution to stand for two days. Filter thissolution through prepared asbestos.

D-l.4.3 Sl(l"tlllrtli~tl'_ofF,"/i.,'s $01"';0"- Pour .tandard invert sugarsolution (III 1).1.2) into a 5O-ml burette (," Note 5, P 18). Pipette10 ml ofFehling'slOlution into a 30o-ml flask and run in from the burettealmost the whole of the standard invert sugar solution requ.ired to effectreduction of .n the copper. 10 that not more than one millilitre willbe required later to complete tbe titration. Heat the Sask containing themixture over a wire puze. Gently boil the contenb of the flask for2 minutes. At the end of 2 minutes of boiliDI, add, without intcrTUptingboilin,. 3 to 5 drops of methylene blue indicator IOlution. While thecontents of the flask continue to boil, begin to add Itandard invert lug.rsolution (one or two drops at a time) from the burette till the blue colourof the indicator just d.lappean. [The titration should be completedwithin one minute. 10 that the contents or tbe ftaak boil altopther for3 minutes without interruption ('11 Note 4, P 18 )~] Note the titre ( tbat ii,the total volUme in millilitrel of standard invert sugar solution used forthe reduction of aU the copper in 10 m1 of FehliDg'llOlution): Multiplythe titre (obtained ~ direct titration) by tbe Dumber of milligrams orinvert IUpr in one millilitre of the ttandard invert susar IOlution to obtainthe invert lugar factor. Compare this facto, with the invert l'!far factorliven in Table IV and de~ne correction, it any. to be applied to theinvert aapr kton derived Crom Table IV.

4JSince rcviIecI.

14

11.1162.1958

TABLE IV INVERT SUGAI\ FACTOR FOR 10 IDI OF FEHUNG'SSOLl.,.JON

( CltllUU 0-1.4_3 Glttl 1).3.1 )

Thil tabl~ shows. for the ItaDdard method or titration, the values corre.ponding tointep millilitrea or the lugar IOlutiODI, the values correspoDdiDI to inteqaediatefiprea heiDI obtaiDecl by iDterpolatioD_

Tlnl: JlIMlLLlLn'a.

I.-YDT Suo....FAaJIO.·

Mu.uOaAJl8 0 ..IJIYD'l' 500.&.I'D 100 MIr.LI.

Ll~... 01'501,172'10.

(I) (~)

15 50-516 50-617 50-718 SO·819 50-8

20 50-921 51-022 51-023 51·124 51·2

25 ~J·2

26 51-327 51·428 51-429 51-5

30 51-531 51-632 51-63S 51·734 51-7

35 51-836 51-837 51·938 51=939 52·0

40 52-041 52-142 52·143 52-244- 52-2

(3)

336316298282267

254-5242·9231-8222·2213·3

204-8197-4190·4183-1177-6

171-7166-'161-2156-6J52-2

. 130·1127-1124·2121-4118·7

.~{&1lilraml or invert IUlaf corresponding to 10 ml or FehJiDI'llOlution.

15

IS 111&2'.1951

E:cdmpl,:Concentration of invert sugar in

standard invert lugar solution tas mgJ100 ml - 200 mg

Titre obtained by direct titration .-: 26-2

Invert sugar factor for 26-2 ml - Titre in ml X number of mgofstandard invert sugar IOlution of invert sugar in I mI of

. Itandard

:II: 26'2 x 2-= 52-4

Invert Iupr factor Cor 26-2 mlfrom Table IV (calculated byinterpolation) - 51-32

Correction to be applied to thein~t' supr factolJ derivedfrom Table IV -= 52-4 - 51'32

-= + 1'08

0.1.5 N..tnl Lea. Acetate-Dissolve \00 I of ,lead acetate[Pb (CH,aOO )., 3H.0] in distilled water and dilute to one litre.

0-1.& SodJ... .......t ..Pot•••11llll Oxalate Sola__- Dissolve70 g of disodium hydrogen phosphate, dodecahydrate ( Na.HPO, t 12H.O)and 30 I of potassium oxalate (K.,C.O., H.O) in water and dilute to onelitre.

1).1.7 SodJ1I1D HJdrosW. SolatioD-approximately 6 N. prepared bydiaolving todium hydroxide analytical Ragent (conforming to~S: 376-1952).

B-l.1 Coaceatratecl aJtlroclaloric AcW-.p gr 1-029 at 200 /4°C.

B-2. PROCEDURE

D-2.1 ........... • 1 Sol.tloa- Weigh accurately about 12-5 g ofmolaael and tranlfer to • 250-ml volumetric flalk. Add 25 m) of the leadacetate IOlut~on. Make up to volume, mix alld filter. Reject iht! firstfew drops or the filtrate. To lOami of the clear filtrate in a 5~knl volu­metric ftask, add 10 ml of the sodium phosphate-potassium oxalatemixture. Make up to volume with water, shake and filter. Reject thefirst few drops of the filtrate and use the clear filtrate for preparation ofinvert solution (SI' D-2.1.1).

1).2.1.1 Pr'/Jllrlltio1l of I11vert Solution - To 50 ml of the filtrate'(SI' D-2.1), in a lOO-ml voluloetric flask, add 25 ml of water, and 10 ml~r c~ncen~~ted hydrochloric acid. Heat on a ,vater-bath to 700e and

16

lSI 1162.1958

regulate heat in such a way that the temperature is maintained at 70°C.Place the flask in a water-bath. insert a thermometer and heat with cons­tant agitation until the thermometer in the flask indicates 67°C. Fromthe moment the thermometer in the flask indicates 67°C, leave the flask inthe water·bath for exaclly 5 minutes, during which time the temperatureshould gradually rise to about 69·5°C. Plunge the flask at once intowater at 20°C. When the contenU have cooled to about 35°C, removethe thermometer from the flask. rinse it and add )0 ml of 6 N sodiumhydroxide IOlution for neutralization of acid, leave the- flask in the bath at2()OC for about 30 minutes and then make up exactly to volume withwater. Alix the solution well.

D-2.2 lacnlDeatai M.daoII 01 Titradoa- Pour the prepared solution( 1M 1).2.1.1) into a 5O-ml burette (SII Note 5 ). Pipette 10 ml of Fehling'ssolution into a 3()().ml conical flask and run in from the burette 15 ml ofthe prepared IOlution (su· 0-2.1 ). Without "furth~r dilution. heat thecontents of the flask over a wire gauze. and boil. (After the liquid hasbeen boiling for about 15 seconds it will be possible to judge if the copperis almost all reduced by the bright red colour im~rted to the boilingliquid by the suspended cuprous oxide.) When, it is judged that nearlyall the copper is r.educ~, .dd 3 to 5 drops of methylene blue indicatorsolution (set Note 1). Continue boiling the contents or the flask for one.to two minutes (rom the commtncement of ebulilion, and then add theprepared solution in small quantities (one millilitre or less at a time),allowing the liquid to boil for about 10 seconds between successiveadditions, till the blue colour of the indicator just disappears (St6 ~ote 4 ).In case there appears to be still much unreduced copper, after the mixtureof Fehling's solution with 15 m) of the prepared solution has been boilingfor a quarter of a minute, add the prepared solution from the burette inlarger increments (more than one millilitre at a time, according to judg~­

ment), and allow the mixture to boil for a quarter ora ~inule after eachaddition. Repeat the addition of the prepared solution at intervals of15 seconds until it is considered unsafe to add large increment of theprepared solution. At this stage continu~ the boiling for an additionalone to two minutes, add 3 to 4 drops of JIlethylcne blue indicator solution

.and complete the titration bOy adding the prepared solution in smallquantities (less than one· miUilitre at a time) (set also Note 2) .

......

Non I-It is .d,'isable not to'add the indicator uDtilabe nri,bbourbood of the endpoiat bas betn rracbed. because the indicator retains ils full colour until the end poin tis almost ftacbed and thuilivel no warning to the operator to go 110,,·1,.

N01T 2- \Vben the operator has had a fair amount or experience with the method,a sulicientJy accurate result may ofteo be obtain~ by a single estimation by theiDCraDenlal method or ti~tiOD, but Cor the utmost degree of accuracy of whichthe method is capable, a sr.cODd titration should be carried out by the standard methodor titratioG ( JH B-2.3 ). .

D-2.:J lta.cIaret Metlaocl or TitratloD- Pipette 10 ml of Fehling'ssolution into a 300-ml conical flask and run in from the burette almost the

17

,,"hole of the prepared solution required to effect reduction or- aU thecopper (determined under »-2.2) so that, if possible, not more than oneInillilitre shall be required later to complete the titration. Gently boil the.contents of the flask for 2 minutes. At the end of 2 minutes of boiling,add. without interrupting boiling, one millilitre of methylene blue indica­tor sol.ution. While the contents of the flask continue to boil. begin toadd the solution (one or two drops at a time). from the burette till theblue colour of the indicator just disappean (SII Note 3 ). The titrationshould be completed within one minute. 10 that the content. of the flaskboil altogether Cor 3 minutes without interruption (1M Note 4 ).

. .

NOH S - The iDdicator iI 10 Rnaitive that it is ~ible to Mtermine the end pointwithin oae drop oI'the prepared solution iii many cues. The complete d~colorizalion

or the methyJeae .blue it usually indicated by the whole reactioa liquid ill wbichtbe cuprous ~ide is continuously chumed up becominl brilbt red or oraDge in colour.In case or doubt, the Same may be removed Crom the wirc pUR Cor one or two secondsand the flak held .gainlt a sheet of white paper. (A bolder or paper, suitably fixedround ahe neck of the flask, is very convmient (or this purpose •• it can be Ielt roundthe neck of the flask ""ithout risk of over ba1ancing it.) The top~ or the liquidwould appear bluish if tbe indicator is not con.plctel, decoIorized. II is inadvisable toiMerrupt the boiling for more than a lew seconds .1 the indicator underlOCI backoxidation rather rapidly when air is allowed free accell into the flask. but there is nodanger or this u IODI u a continuous Itream of steam is iuuiDI Crom the mouth or theflask.

~OTI: .. -It .bowd be observed that with both incremental and .tandard methodsof titration, the flask contajoinl the reaction mixture ill left on the wire ,au. over ,hename throu,bout the titration except wben it may be removed lor • few secondsto ascertain if the end point i' reached.

NOTE 5-la addinllUlar IOhition to the reaction miatur.e, the burette may be heldin hand 0YtT the luk. The burette may be fitted with. mWl outlet tube bent __'keat right angles, 10 that the body or the burette caD be kept out or the Iteam while .eId·in. lu,ar IOlution. Burettes with rlua taps are unsuitable for this wor~ .. the tapl~me beated by the Iteam and are liable to jam.

D·3. CALCULADON

1).3.1 Refer to Table IV for the invert sugar factor corresponding to thetitre . (determined .1 given under 0-2.3) and apply the correctionpreviously determined.

MilligraDll of invert sugar present Invert SURar Factorin I ml of the prepared solution == Titre

1).3.2 Reduciul matter, percentmass

by 250 C== -W-

where

C == milligrams of the invert sugar in 1 ml of the preparedsolution (SI' D-3.1 ) J and

'.J' c= mall in g of the material taken for "the lest.

18

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