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Indian Standard – Packaged Natural Mineral Water (BIS IS: 13428), 2005

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IS 13428 : 2005

~~~~-~

( CJ\\lIYI ~8fUT )

Indian Standard

PACKAGED NATURAL MINERAL WATER­SPECIFICATION

(Second Revision)

First Reprint DECEMBER 2006

lCS 13.060.20

C BlS200S

BUREAU OF INDIAN STANDARDSMANAK BHAVAN. 9 BAHADUR SHAH ZAFAR MARG

NEWDELHI 110002

Price Group II

AMENDMENT NO. I DECEMBER 2005TO

IS 13428: 2005 PACKAGED NATURAL MINERALWATER - SPECIFICATION

(Second Revision)

( Page 2, clause 7.1, line 11 ) - Insert 'or polyethylene flexible pouchesconforming to IS 15609.' after the word 'water'

( Page 2. clause 7.1 ) -Insert the following at the end:

'Guidelinesfor handling of polyethylene flexible pouches is given in Annex E.'

( Page6, Annex A ) - .Insertthe following at the end:

IS No. Title

15609 : 2005 Polyethylene flexible pouches for the packingof natural mineral water and packaged drinkingwater - Specification'

( Page 21. Annex 20 ) - Insert the following new AnnexE after Annex2D and renumber the subsequent Annexes:

ANNEXE

(Clause 7.1)

Guidelines for Handling of Polyethylene Flexible Film Meant forPacking of Packaged Drinking Water in Pouches

E-l Polyethylene flexible film meant for packing of Packaged Drinking Waterin pouches should have suitable sturdy and dust proof outer packing to preventcontamination during transport, storage and handling. The supplier must beinstructed to apply such packing immediately after the film manufacture. Suchouter packaging must remainintact tin the final loadingof the film on the pouchfilling machine. Care should however be taken to clean such outer packagingand renderthe samedust-free beforethe same is carried into the fillingroom.

E-2 Printing of the film must be done in such a way that the printing materialdoes not interfere with the final product.

E-3 Such film must be stored in dry, cool and dust-free enviromnent away fromstrong smelling substances, chemicals, cleaning material etc. It will be ideal tohaveseparatestore roomsexclusive for packagingmaterial.

Amend No. 1 to IS 13428 : 2005

E-4 While handling the film the personnel should adhere to the followingbasichygiene precautions:

a) Finger nails of personnel should be trimmed close and well so that nounhygienic substancesare found below the nails.

b) Hands should be cleaned with disinfecting soap and dried, preferablygloved.

c) Personnel should wear head cover and mask while handling the film.

E-5 The pouch filling machine must have suitable means to sterilize the filmprior to forming the pouch. UV sterilization may be considered taking intoaccount the following aspects:

a) The length and intensity of the lamps must be suitable for sterilizingthe film on the active surface, that is, the surface that will be in contactwith the product and the speed of the machine. The equipmentsupplier's certificate to that effect must bemaintainedfor record.

b) The UV lamp supplier must certify as to the expected life in number ofhours. The filling machine should have a mechanism to monitor thenwnber of hours of usage, suitably interlocked with the rest of theequipment so that a reliable method to record the actual usage isavailable.

c) Partly used and unused film must be stored with all precautions inaccordance with E-3 above.

d) Guide-rods, etc, that maydirect the film in the formation of the flexiblepackaging and other contact parts must be suitably sanitized withHydrogen Peroxide before start of every filling operation and recordsof the'same maintained.

E-6 Fumigation of the filling room with suitable agent is recommended.

E-7 Size of the secondary packaging must take into account that at the retailpoint the flexible packaged drinking water is often refrigerated and so thesecondary packaging should be of appropriate size to facilitate refrigeration inthe secondary packaging itself This would shield the pouches fromcontaminations.

2

Amend No. 1 to IS 13428: 2005

E-8 The following storage instructions must be issued to retailer/whole sellerand all concerned in the supplychain:

a) PackagedDrinking Waterin flexible packagingmustbehandledwithcare.

b) It shouldbestoredaway from sunlightand in a cool place.

c) It shouldbe hygienically stored in a place away from chemicals,paints,pesticides and similarsubstances that canaffect the product.

d) It shouldalsobestoredawayfrom strong-smelling substances.

e) Chilling the product with commercially produced ice must bediscouraged as it would expose the consumer to product with possiblecontamination from ice produced with unsafewater.

f) To check for any leakage, etc, before opening.

g) Instruments used for opening/cutting sachets should be kept exclusivefor these pouches in a suitable place to avoid any contamination andshould not be used for cutting or openingany other non-food product.

h) Consumer mustbe advisedto use clean scissorsto open sachet.

j) Product shouldnot be consumed if any foreign material is found.

(FAD 14)

Printed at Simco Printing Press, Delhi

AMENDMENT NO. 2 NOVEMBER 2006TO

1S 13428 s 2005 pAc~GED NATURAL MINERAL

WATER — SPECIFICATION

. ( SecondRevision)

[P{zge 4, clause S.I(a)] — Substitute the following for the existing:

‘a) Name of the product (that is mtural mineral water);’

(FAD 14)

Reprography Unitj BIS, New Delhi, India

..

AMENDMENT NO. 3 JUNE 2010 TO

IS 13428 : 2005 PACKAGED NATURAL MINERAL WATER ― SPECIFICATION

( Second Revision )

[Page 3, Table 2, Sl No. (iv), col 5] — Substitute ‘3025 (Part 59)’ for ‘35

of IS 3025’.

[Page 3, Table 2, Sl No. (vii), col 5] — Substitute ‘3025 (Part 60)’ for ‘23 of IS 3025’.

[Page 3, Table 2, Sl No. (xvii), col 2] — Substitute ‘Alkalinity (as HCO3), mg/l’ for ‘Alkalinity (as HCO3), mg/l, Max’.

[Page 4, clause 8.1(h)] ― Substitute ‘Net quantity;’ for ‘Net volume;’.

(Page 5, Annex A) ― Delete IS No. ‘3025 : 1964 Methods of sampling and test (physical and chemical) for water used in industry’.

(Page 5, Annex A) ― Insert the following entries after ‘(Part 56) : 2003 Selenium (first revision)’: ‘(Part 59) : 2006 Manganese (first revision) (Part 60) : 2008 Fluoride (first revision).’ (FAD 14)

Reprography Unit, BIS, New Delhi, India

Drinks and Carbonated Beverages Sectional Committee, FAD 14

FOREWORD

This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards, after the draft finalizedby the Drinks and Carbonated Beverages Sectional Committee had been approved by the Food and AgricultureDivision Council.

This standard w~s published in 1992and subsequently revised in 1998 in view of the following:

a) To delete provisions of fortified mineral water which were covered in the earlier version;

b) To align with the revised Codex Standard for natural mineral water, except for the following which areeither not covered or partially covered in the Codex Standard:

1) Organoleptic and physical parameters have been retained. Minimum and maximum values havebeen indicated for total dissolved solids in order to ensure presence of minimum minerals contentin the water and at the same time limiting their content for the sake of palatability;

2) Requirements for zinc, silver, chloride, sulphate and alkalinity have been retained and therequirements ofmagnesium, calcium, sodium, and sulphide have been added as these were consideredrelevant characteristics from the point ofwater quality; and

3) In microbiological parameters, requirements for yeast and mould, salmonella and shigella, vibrio,cholera and V. parahaemolytlcus have been retained and that of staphylococcus aureus added inaddition to those specified in the Codex standard, to provide additional safeguard. The requirementof aerobic microbial count has been deleted as the same has not been prescribed in the CodexStandard.

c) To include hygienic practices in line with Codex (CAC/RCP 33-1985) 'Code of practice for collecting,processing and marketing of natural mineral waters'.

This revision has been undertaken to incorporate five amendments alongwith the technological developments,check list for hygienic requirements, and consumer requirements. It is expected that this standard would help inachieving the above objective.

In the preparation of this standard due consideration has been given to the provisions of the Prevention ofFoodAdulteration Act, 1954 and the Rules framed thereunder. The standard is, however, subject to the restrictionsimposed under this Act and Rules, wherever applicable.

In the preparation of this standard assistance has been derived from the EEC Directive, 80/778IEEC 'Councildirective relating to the quality of water intended for human consumption'.

A separate standard IS 14543 : 2004 'Packaged drinking water (other than packaged natural mineral water)' hasbeen established.

For the purpose of deciding whether a particular requirement of the standard is complied with, the final value,observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance withIS 2 : 1960 'Rules for rounding off numerical values (revised)'. The number ofsignificant places retained in the

.rounded off value should be the same as that of the specified value in this standard.

IS 13428 : 2005

Indian Standard

PACKAGED NATURAL MINERAL WATER­SPECIFICATION

( Second Revision)

1 SCOPE

This standard prescribes the requirements,methodsofsampling and test for natural mineral waters offeredfor sale in packaged fonn for human consumption.

NOTE-It does not apply to natural mineral water sold orusedforotherpurposes.

2 REFERENCES

The standards listed in Annex A contain provisions,which through reference in this text, constituteprovisions ofthis standard. At the time of publication,the editions indicated were valid. All standards aresubject to revision and parties to agreements based onthis standard are encouraged to investigate thepossibility of applying the most recent editions of thestandards indicated at Annex A.

3 DEFINITION

For the purpose of this standard the followingdefinitions shall apply.

3.1 Natural Mineral Water - Water clearlydistinguishable from ordinary drinking water because:

a) it is obtained directly from natural or drilledsources from underground water-bearingstrata for which all possible precautionsshouldbetakenwithintheprotected perimetersto avoidany pollutionof, or externalinfluenceon, the chemical and physical qualities;

b) it is characterized by its content of certainmineralsaltsand their relativeproportions andthe presence of trace elements or of otherconstituents;

c) of the constancy of its composition and thestability of its discharge and its temperature,due accountbeingtakenofthecyclesofminornatural fluctuations;

d) it iscollectedunderconditions whichguaranteethe original microbiological purity andchemicalcomposition of essential components;

e) it is packaged close to the point ofemergenceof the source with particular hygienicprecautions; and

f) it is not subjected to anytreatmentother thanthose permitted by this standard.

3.1.1 Naturally Carbonated Natural Mineral Water- Natural mineral water which, after possibletreatment in accordancewith 4.1 and re-incorporationof gas fromthesamesourceand after packagingtakinginto consideration usual technical tolerance, has thesame content of carbon dioxide spontaneously andvisibly given off under normal conditions oftemperature and pressure.

3.1.1 Non-carbonated Natural Mineral Water ­Natural mineral water which, by nature and afterpossible treatment in accordance with 4.1 and afterpackaging taking into consideration usual technicaltolerance, does not contain free carbon dioxide inexcess of the amount necessary to keep the hydrogencarbonate salts present in the water dissolved.

3.1.3 Decarbonated Natural Mineral Water ­Natural mineral water which, after possible treatmentin accordance with 4.1 and after packaging, has lesscarbon dioxide content than that at emergence anddoes not visibly and spontaneously give off carbondioxide under normal conditions of temperature andpressure.

3.1.4 Natural Mineral Water Fortified with CarbonDioxide from the Source - Natural mineral waterwhich,after possible treatment in accordance with 4.1and after packaging, has more carbon dioxide contentthan that at emergence.

3.1.5 Carbonated Natural Mineral Water - Naturalmineral water which, after possible treatment inaccordance with 4.1 and after packaging, has beenmade effervescent by the addition of carbon dioxidefrom another origin.

NOTE- Mineral watermeans natural mineral wateras definedin 3.1.

3.2 Packaged Natural Mineral Water - Naturalmineralwaterfilledintohermeticallysealedcontainersof various compositions, forms and capacities that is,suitable for direct consumption without furthertreatment.

4 TREATMENT AND HANDLING

4.1 Treatments permitted include separation fromunstable constituents, such as compounds containingiron, manganese, sulphur or arsenic, by decantation

IS 13428 : 2005

and/or simple filtration up to 0.5 microns, if necessary,accelerated by previous aeration.

4.2 The treatments provided in 3.1.1 to 3.1.5 and 4.1above may only be carried out on condition that themineral content of the water is not modified in itsessentialconstituents, whichgivethewateritsproperties.

4.3 The transport of natural mineral waters in bulkcontainers for packagingor for any other processbeforepackaging is prohibited,

5 HYGIENIC CONDITIONS

Natural mineral water shall be collected: processed,handled, packaged and marketed in accordance withthe hygienic practices given in Annex B. A check-listfor good hygienic practices and food safety system forpackaged natural mineral water processing units givenat the end of Annex B.

6 REQUIREMENTS

6.1 Microbiological Requirements

6.1.1 'Escherichia coli' (or Thermotolerant bacteria)shall be absent in any 250 ml sample when tested inaccordance with the method given in IS 5887 (Part 1)*or IS 15185.

6.1.2 Coliform, bacteria shall be absent in any 250 mlsample when tested in accordance with the methodgiven in IS 5401 (Part 1)* or IS 15185.

6.1.3 Faecal streptococci andStaphylococcus aureus,shall be absent in any 250 ml sample when tested inaccordance with the method given in IS 5887 (Part 2)*Streptococci (Enterococci) may also be tested by themethod specified in IS 15186.

6.1.4 Sulphite reducing anaerobes, shall be absent in50 ml sample when tested in accordance with themethod given in Annex C.

6.1.5 Pseudomonas aeruginosa, shall be absent in250 ml sample when tested in accordance with themethod given in Annex D.

6.1.6 Yeast and Mould, shall be absent in 250 mlsample when tested in accordance with the methodgiven in IS 5403.

6.1.7 Salmonella and·Shigella, shall be absent in any250 ml sample when tested in accordance with themethod given in IS 5887 (Part 3)* and IS 5887 (Part 7)respectively. Salmonella may also be tested by themethod specified in IS 15187.

6.1.8 Vibrio cholera and V. parahaemolyticus, shallbe absent in 250 ml sample when tested in accordancewith the method given in IS 5887 (Part S).

6.1.9 The membrane filtration technique outlined inIS 15188 may be used to pass the sample of water tobetestedthrough membrane before the microbiologicaltests specified from 6.1.1 to 6.1.8 are carried out.

NOTE - In case of dispute, the method indicated by'·'in 6.1.1 to 6.1.3 and 6.1.7 shall be the reference method.

6.2 Natural mineral water shall also comply with therequirements given in Table 1, Table 2, Table 3 andTable 4.

6.3 Residues of pesticides for pesticides as given inAnnex N shall be below the detectable limits. Theanalysisof pesticideshall be conductedby a recognizedlaboratory using internationally established testmethods as given in Annex N.

7 PACKING

7.1 Natural mineral water shall be packed in clean,hygienic, colourless, transparent and tamperproofbottles/containers, made of polyethylene (PE)conforming to IS 10146 or polyvinyl chloride (PVC)conforming to IS 10151 or polypropylene conformingto IS 10910 or polyalkylene terephthalate (PET andPBT) conforming to IS 12252 or polycarbonateconforming to IS 14971 or polystyrene conformingto IS 10142 or sterile glass bottles suitable forpreventing possible adulteration or contamination ofthe water. Plastic containers shall be conformingto IS 15410.

Table 1 Organoleptic and Physical Parameters

(Clause 6.2)

SINo. Characteristic Requirement Method orTest, Rtf to IS

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

i) Colour, true colour unit, Max 2 3025 (Part4)ii) Odour Agreeable 3025 (Part S)iii) Taste Agreeable 3025 (Part 8)

(Action tendency scale(a) or (b) or (c)]iv) Turbidity,NTU. Max 2 3025(Part 10)v) Total dissolvedsolids. m&ll 150 to 700 3025 (Part 16)vi) pH value 6.S to 8.5 302S(Part 11)

,

IS 13428 : 2005

Table 2 General Parameten ConeernlDI SubstaDca Undesirable In Escasive Amounts

(Clause 6.2)

SINo. Cb.r.cterildc Requlremeat Metlaod 01Test, ReI to

,.....Annexof this Standard......

Other Standards'(I) (2) (3) (4) (5)

i) Nitrite (u NO,), mgll, Max 50 3025 (part 34)iI) Nltrl. (M NOJ, mall, Max 0.02 3025 (Part34)iii) Sulphide (a "2S), man, MQ% 0.05 3025 (part 29)Iv) Manpnesc (II Mn), mall, Mta 2.0 35 of IS 3025v) Copper (u Cu), mill, MQJC 1.0 3025 (Part 42)

vi) llnc (asZn),mill, Max 5 3025 (part 49).vii) Fluoride (IS F), mgll, Max 1.0 13 of IS 3025viii) Barium (u Ba),mgll, Max 1.0 F· or IS 15302

ix) Antimony(u Sb), mill, Mta 0.005 G· or IS 15303x) Borate (u B), mgll, Mta 5 H

xi) Silver (as Ag), mg/l, Max 0.01 Jxii) Chloride (as CI), mg/l, Max 200 3025 (Part 32)

xiii) Sulphate (u S04)' mall, Max 200 3025 (part 24)xiv) Mqnesium (as Mg), mgll, Mta 50 3025 (part 46)xv) Calcium (as Cal, mgll, Max 100 3025 (part 40)

xvi) Sodium (as Na), mall, Max 150 3025 (part 45)xvii) Alkalinity (u HCO]),mg/l, Max 75 to 400 3025 (part 23)

xviii) Selenium (as Se), mg/l, Max 0.05 3025 (part 56)or IS 15303·

xix) Mineraloil, mgll. Max Absent 3025 (part 39)xx) Phenolic compounds(as C6H,OH) Absent 3025 (part 43)

xxi) Anionic surface active agents Not detectable K

NOTE- In case of dispute, the methodindicatedby '.' shall bethe referencemethod.

Table 3 P8"rameten Concerning Toxic Substances

(Clause 6.2)

SINo. Claar.cteri.de Requiremeat Method olTat, Rerto

----~ ~

Annexof this Standard Other Standards(1) (2) (3) (4) (5)

i) Arsenic (as As), mgll, Max 0.05 3025 (Part 37)ii) Cadmium (as Cd), mg/l, Max 0.003 3025 (Part 41)

iii) Cyanide (u CN). mall, Max Absent 3025 (Part 27)iv) Chromium (as Cr), mgll, Max 0.05v) Mercury(as HI), mill, Max 0.001 3025 (Part 48)

vi) Lead(asPb), mill, Max 0.01 3025 (Part 47)vii) Nickel (asNi), mall,Max 0.02 L

viii) Polychlorinatedbiphenyle(PCB) Not detectable MIx) Polynucleararomatic hydrocarbons Not detectable APHA6440 I

Table 4 Parameten Concerning Radio Active Residues

(Clause 6.2)

SINo. Cb.r.cterl.dc RequlremeDt Method01Tat, Rerto IS

(1) (2) (3) (4)

i) Alpha emiuen.BqII,Max 0.1 14194(Part 2)

ii) Betaemiuen.BqII, Max I 14194(Part 1)

NOTE - In case of non-eonformity of l'Idio lCtive residues, the source of water shall be abandoned and water shall be recalledimmediately.

3

IS 13428 : 2005

7.2 All packagingmaterialsofplasticoriginshallpassthe overall migration and colour migration limits aslaiddown inthe relevant IndianStandardsfor productsfor respective packaging materials when tested as permethod given in IS 9845.

8 MARKING

8.1 The following particulars shall bemarked legiblyand indelibly on the label of the bottle/container:

a) Name ofthe product(that is packagednaturalmineral water);

b) Supplementary designations, if any;c) Name and address of the processor;d) Brand name, if any;e) Batch or Code number;f) Date of processing/packing;g) Best for consumption up to ... (date/month!

year in capital letters); orBest for consumption within days or monthsfrom the date of processing/packing;

h) Net volume;j) Location and name of the source of natural

mineral water;k) Direction for storage; andm) Any other markings required under the

Standards of Weights and Measure(Packaged Commodities) Rules, 1977and thePrevention of Food Adulteration Act, 1954and the Rules framed thereunder.

8.2 Labelling ProhibitioDs

8.2.t No claims concerning medicinal (preventative,alleviativeor curative) effects shall be made in respectof the propertiesof the productcoveredbythe standard.

4

Claims of other beneficial effects related to the healthof the consumer shall not bemade.

8.2.2 The name of the locality, hamlet or specifiedplace may not form part of the brand name unlessit refers to packaged natural mineral water collected!processed at the place designated by that brandname.

8.2.3 The use of any statement or of any pictorialdevice which may create confusion in the mind ofthepublic or in any way mislead the public about thenature, origin, composition and properties of naturalmineral waters put on sale is prohibited.

8.3 DISCertification MarkiDg

8.3.1 The product may also be marked with theStandard Mark.

8.3.2The use of the Standard Mark is governed by theprovisions of Bureau of Indian Standards Act, 1986and the Rulesand Regulationsframedthereunder. Thedetails of the conditions under which the licence foruseof Standard' Markmaybegrantedto manufacturersor producers may be obtained from the Bureau ofIndian Standards.

9 SAMPLING

Representative samples of natural mineral water shallbedrawnandthecriteriafor confonnityto this standardshall beestablished,according to the method given inAnnex E.

10 QUALITY OF REAGENTS

Unless specified otherwise, pure chemicals anddistilledwater (see IS 1070)shallbeemployedin tests.

NOTE - 'Pure chemicals' shall mean chemicals that do notcontain impurities which affect the results of analysis.

IS 13428 : 2005

ANNEX A

(Clause 2)

LIST OF REFERRED INDIAN STANDARDS

[SNo.

1070 : 1992

3025 : 1964

3025

(Part 4) : 1983

(Part S) : 1983

(Part 8) : 1984

(Part 10): 1984

(Part 11) : 1983

(Part 16) : 1984

(Part 23) : 1986

(Part 24) : 1986

(Part 27) : 1986

(Part 29) : 1986

(Part 32) : 1988

(Part 34) : 1988

(Part 37) : 1988

(Part 39) : 1988

(Part 40) : 1991

(Part 41) : 1992

(Part 42) : 1992

(Part 43) : 1992

(Part 45) : 1993

(Part 46): 1994

(Part 47) : 1994

(Part 48) : 1994

(Part 49) : 1994

(Part 56) : 2003

4905 : 1968

5401

(Part 1) : 2002

5402: 2002

5403 : 1999

Title

Reagentgrade water (third revision)

Methods of sampling and test(physical and chemical) for waterused in industry.Methods of sampling and test(physicalandchemical)forwaterandwastewater:Colour (first revision)

Odour (first revision)

Taste rating (first revision)

Turbidity (first revision)

pH value (first revision)

Filterable residue (total dissolvedsolids) (first revision)

Alkalinity (first revision)

Sulphates (first revision)

Cyanide (first revision)

Sulphide (first revision)

Chloride (first revision)

Nitrogen (first revision)

Arsenic (first revision)

OiI and grease

CalciumCadmium (first revision)

Copper (first revision)

Phenols (first revision)

Sodiumand potassium (first revision)Magnesium (first revision)

Lead (first revision)

Mercury (first revision)

Zinc (first revision)

Selenium (first revision)

Methods for random sampling

Microbiology - General guidance

for enumeration of colifonns: Part IColonycounttechnique (f".strevision)

Microbiology - General guidancefor the enumeration of micro­organisms- Colonycounttechniqueat 30°C (first revision)

Method for yeast and mould countof foodstuffs and animal feeds (firstrevuion)

IS No.

5887

(Part I) : 1976

(Part 2) : 1976

(Part 3) : 1999

(Part 5) : 1976

(Part 7) : 1999

9845 : 1998

10142 : 1999

10146 : 1982

10lSI : 1982

10500 : 1991

10910 : 1984

12252 : 1987

14194

(Part 1) : 1994

Title

Methods for detection of bacteriaresponsible for food poisoning:

Isolation, identification andenumeration of Escherichia coli (firstrevision)

Isolation. identification andenumeration of Staphylococcusaureus andfaecal streptococci (firstrevision)

General guidance on methods fordetection of Salmonella (secondrevision)

Isolation, identification andenumeration of Vibrio cholerae andv. parahaemolyticus (first revision)

General guidance on methods forisolation and identification ofShigella

Determination of overall migrationof constituents of plastic materialsand articles intended to come incontactwithfoodstuffs - Methodofanalysis (second revision)

Polystyrene (crystalandhigh impact)for its safe use in contact withfoodstuffs, pharmaceuticals anddrinking water (first revision)

Polyethylene for its safe use incontact with food stuffs,pharmaceuticalsand drinking waterPolyvinyl chloride (PVC) and itscopolymersfor itssafe use in contactwithfoodstuffs, pharmaceuticals anddrinking waterDrinking water (first revision)

Polypropylene and its co-polymersfor its safe use in contact withfoodstuffs, pharmaceuticals anddrinking waterPolyalkylene terephthalates (PETandPBT)for their safeuse incontactwithfoodstuffs, pharmaceuticals anddrinking water

Radionuclides in environmentalsamples - Methods of estimation:Gross beta activity measurement

IS 13428 : 2005

IS No.

(Part 2) : 1994

14971 : 2001

15185 : 2002

15186: 2002

15187: 2002

Title

Gross alpha activity measurementPolycarbonate resins for its safeuse in contact with foodstuffs,pharmaceuticals and drinkingwaterWater quality - Detection andenumeration of Escherichia coli andcoliform bacteria - MembranefiltrationmethodWater quality - Detection andenumeration of intestinal enterococci- Membrane filtration methodWater quality - Detection ofsalmonella species

IS No.

15188: 2002

15302: 2002

15303 : 2002

15410: 2003

Title

Waterquality - General guideto theenumeration of micro-organisms byculture

Determination of aluminium andbarium in water by direct nitrousoxide-acetylene flame atomicabsorptionspectrometry

Detenninationof antimony, ironandselenium in water by electrothermalatomic absorption spectrometrymethodContainersfor packagingof naturalmineral waterandpackageddrinkingwater - Specification

ANNEX B

(Clause 5)

HYGIENIC PRACTICES

B-1 FIELD OF APPLICATION

The hygienic practices cover appropriate generaltechniques for collecting natural mineral water, itstreatment, bottling, packaging, storage, transport,distribution and sale for direct consumption, so as toguarantee a safe, healthy and wholesomeproduct.

B-2 PRESCRIPTIONS OF THE RESOURCESOF NATURAL MINERAL WATER

8-2.1 Protection of Alimentary Reservoirs andAquifen

8-2.1.1 Authorization

Any spring,wellor drilling intendedfor the collectionof natural mineral water should be approved by theLocal Health Authority or any other agency havingjurisdiction for the region.

8-2.1.2 Determination of the Genesis of NaturalMineral Water

As far as it is methodologically possible in each case,a precise analysis should becarried out on the originofnatural mineralwaters,the periodoftheir residencein thegroundbeforebeingcollectedandtheirchemical,physical and radiological qualities.

8-2.1.3 Perimeter ofProtection

Ifpossible areas wherein natural mineral water mightbe polluted or its chemical and physical qualitiesotherwise deteriorated should be determined by ahydrologist. Where indicated by hydrogeological

6

conditions and considering the risks of pollution andphysical,chemicaland biochemicalreactions, severalperimeterswith separatedimensionsmay beprovidedfor.

8-2.1.4 Protective Measures

All possible precautions should be taken within theprotected perimeters to avoid any pollution of, orexternal influence on, the chemical and physicalqualities of natural mineral water.

It is recommendedthat regulations beestablished forthe disposal of liquid, solid or gaseous waste, the useof substances that might deteriorate natural mineralwater as well as any possibility of accidentaldeterioration of natural mineral water by naturaloccurrences such as a change in the hydrogeologicalconditions. Particular consideration should be givento the following potential pollutants such as bacteria,viruses, fertilizers, hydrocarbons, detergents,pesticides, phenolic compounds, toxic metals,radioactive substances and other soluble organic orinorganic substances. Even where nature providesapparently sufficient protection against surface,pollution, potential hazards arising out of mining,hydraulic andengineering facilities etc,shouldbetakenintoconsideration.

8-2.2 HYllene Prescriptions for Collection ofNatural Mineral Water

8-2.2.1 Extraction

The withdrawal of natural mineral water shall be

performed in conformity with the hydrogeologicalconditions in such a manner as to prevent any waterotherthan the natural mineralwater from enteringor,should there be pumping facilities, prevent anyextraneouswater from entering. The natural mineralwaterthuscollectedor pumpedshouldbe protectedinsuch a way that it is not polluted(whethercaused bynaturaloccurrenceor actionsor neglector ill will).

8-2.1.1 Materials

The pipes, pumps or other possible devices cominginto contact with natural mineral water and used forits collection should be made of such material as toguarantee thatoriginalqualityof naturalmineral wateris not changed.

8-1.2.3 Protection ofthe Extraction Area

In the immediate surroundings of springs or wells,precautionary measures shouldbe taken to guaranteethat no pollutant whatsoever can enter the extractionarea.Theextraction areashould beinaccessible to non­authorizedpeople by providingadequate devices(forexample enclosure). Any use not aiming at thecollection of natural mineral watershould beforbiddenin this area.

8-2.2.4 Exploitation ofNatural Mineral Water

The condition of the extraction facilities, areas ofextraction and perimeter protection as well as thequalityof the natural mineral watershouldperiodicallybe checked. To control the stability of the chemicaland physical particulars of the natural mineral waterderived, besides the natural variations, automaticmeasurements of the typical characteristics of watershould be carried out and recorded (for example,electricalconductance, temperature, contentof carbondioxide) or frequent partial analysisshouldbe done.

8-2.3 Maintenance of Extraction Facilities

8-2.3.1 Technical Aspects

Methods andprocedures formaintaining theextractionfacilities should be hygienic and not be a potentialhazard to human health or a source of contaminationto naturalmineralwater.Fromthe hygiene standpoint,servicing of the extraction installations should meetthesame requirements asthoserequired forthebottlingor for treatment.

8-2.3.1 Equipment and Reservoirs

Equipment andreservoirs usedforextraction of naturalmineral water should be constructed and maintainedin order to minimizeall hazards to human healthandto avoid contamination.

8-2.3.3 Storage at the Point 01Extraction

Thequantity ofnatural mineralwaterstoredat thepoint

7

IS 13428 : 2005

of extraction shouldbeas lowas possible. Thestoringshould furthermore guarantee protection againstcontamination or deterioration.

8-2.4 Transport of Natural Mineral Water

8-2.4.1 Means ofTransport, Piping and Reservoirs

Anyvehicle, pipingor reservoir usedinthe processingof natural mineral water from its source to thebottlingfacilities, should comply with the necessaryrequirements and be, made-of inert material such asceramic and stainless steel which prevents anydeterioration, be it by water,handling, servicingor bydisinfection; it shouldalloweasy cleaning.

8-2.4.2 Maintenance 0/ Vehicles and Reservoirs

Any vehicle or reservoir should be properly cleanedand if necessary, disinfected and kept in good repairso as not to present any danger of contamination tonatural mineral water and of deterioration of theessential qualities of naturalmineral water.

B-3 ESTABLISHMENT FOR PROCESSINGNATURAL MINERAL WATERS - DESIGNAND FACILITIES

8-3.1 Location

Establishments should be located in areas which arefree from objectionable odours; smoke, dust or othercontaminants and are not subject to flooding.

8-3.2 Roadways and Areas Used by WheeledTrame

Such roadways and areas serving the establishmentwhich are within its boundaries or, in its immediatevicinityshouldhave a hard paved surfacesuitable forwheeled traffic. There should beadequate drainage andprovision should be made for protection of theextraction area in accordance with 8-2.2 whereappropriate. Adequate road signals may be providedto call the attention of road users to the existence ofnaturalmineralwater extraction area.

8-3.3 Buildings and Facilities

8-3.3.1 Type ofConstruction

Buildings andfacilities should beofsoundconstructionin accordance with the provisions of 8-2.2 andmaintained in good repair.

8-3.3.2 Disposition ofHolding Facilities

Rooms for recreation, for storingor packaging of rawmaterial and areas for cleaning of containers to bereused should be away from the bottling areas toprevent theendproduct from beingcontaminated. Rawmaterials and packaging materials which come into

IS 13428 : 2005

contact with natural mineral water should be storedapart from other material.

8-3.3.3 Adequateworkingspace shouldbeprovidedto allowfor satisfactory performance of all operations.

8-3.3.4 The design shouldbesuch as to permit easyand adequate cleaning and to facilitate propersupervision of hygieneof natural mineralwater.

8-3.3.5 Thebuildings and facilities shouldbedesignedto provide separation by partition, location or othereffectivemeansbetweenthose operationswhichmaycause cross contamination.

8-3.3.6 Buildings and facilities should be designedto facilitate hygienic operations by means ofa regulatedflow in the process from the anival of the naturalmineralwater at the premisesto the finishedproduct,and should provide for appropriate temperatureconditionsfor the process and the product.

8-3.3.7 Natural Mineral Water Handling, Storing andBottling Areas

8-3.3.7.1 Floors

Where appropriate, floors should be of water-proof,non-absorbent, washable, non-slip and non-toxicmaterials, withoutcrevices, andshouldbeeasyto cleanand disinfect. Where appropriate, floors should havesufficientslope for liquids to drain to trapped outlets.

8-3.3.7.2 Walls

Where appropriate, should be of water-proof, Don­absorbent, washable and non-toxic material andshouldbe light coloured. Up to a height appropriate for theoperation theyshouldbe smooth andwithoutcrevices,and should be easy to clean and disinfect. Whereappropriate, angles betweenwalls,betweenwallsandfloors, and between wallsandceilingsshouldbesealedand smoothento facilitate cleaning.

B-3.3.7.3 Ceilings

Ceilings should be so designed, constructed andfmished as to prevent the accumulation of dirt andminimize condensation, mouldgrowth andflaking, andshould beeasy to clean.

8-3.3.7.4 Windows

Windows andother openingsshouldbe soconstructedas to avoidaccumulationof dirt and thosewhichopenshouldbefittedwith screens. Screens shouldbeeasilymovable for cleaning and kept in good condition.Internal window sills, if present, should be sloped toprevent use as shelves.

B-3.3.7.5 Doors

Doorsshould havesmooth, non-absorbent surfaces and,whereappropriate, beself-closing andclosefJttina type.

8

8-3.3.7.6 Stairs, 11ft cages andmal/lory Itrllctllra

Platforms, ladden, chutes, should be so situated andconstructed as not to cause contamination. Chutesshouldbeconstructed withprovisionof inspection andc1eanina batches.

8-3.3.7.7 Piping

Piping for natural mineral water lines should beindependent of potableand non-potablewater.

8-3.3.,8 In natural mineral water handling area alloverheadstructures and fittingsshouldbe installed insuch a manner as to avoid contamination directly orindirectly of natural mineral water and raw materialsby condensation and drip, and should not hampercleaning operations. Theyshouldbe insulatedwhereappropriate and be so designed and finished as toprevent the accumulation of dirt and to minimizecondensation, mould development and flaking. Theyshouldbeeasy to clean.

8-3.3.9 Living quarters, toilets and areas whereanimalsarekeptshouldbe completelyseparatedfromandshouldnotopendirectly on to natural mineral waterhandlingareas.

8-3.3.10 Where appropriate, establishments shouldbeso designedthat accesscan be controlled.

8-3.3.11 The use of material which cannot beadequately cleaned and disinfected, such as wood,shouldbe avoidedunlessitsuse wouldnot be asourceof contamination.

8-3.3.12 Canalization, Drainage Lines

Canalization, drainageand used water linesas welluany possible waste storage area within the protectedperimeter should be built and maintained in such amanner as not to present any risk whatsoever ofpollutingaquifersand springs.

8-3.3.13 Fuel Storage Area

Any storage area or tank for the storing of fuels suchis coalor hydrocarbons shouldbedesigned, protected,controlledand maintained in such a manner as not topresent a risk of aquifen and springs being pollutedduringthe storageand manipulation ofthese fuels.

8-3.4 BYllenle Facilities

8-3.4.1 Waler Supply

8-3.4.LI Amplesupplyofpotablewaterunderadequatepressure and of suitable temperature should beavailable withadequatefacilitiesfor its storage,wherenecessary, and distribution with adequate protectionagainst contamination. The potable water shouldconform to the standard for drinking water (,eeIS 10Soo).

8-3.4.1.2 Natural mineralwater,potablewater, non­potablewaterforstearn production or forrefrigerationor any other use should be carried in separate lineswith no cross ccnnection between" them and withoutany chance of back siphonage. It would be desirablethatthese lines beidentified bydifferent colours. Steamused in directcontact with natural mineral water andalso natural mineral water contact surfaces shouldcontain no substances which may be hazardous tohealthor may cause contamination.

8-3.4.2 EfJluent and Waste Disposal

Establishments should have an efficient effluent andwaste disposal system which should at all times bemaintained in good orderand repair. All effluentlines(including sewer systems) should be large enough tocarry full loadsand shouldbeso constructed asto avoidcontamination of potable water supplies.

8-3.4.3 Changing Facilities and Toilets

Adequate, suitable and conveniently locatedchangingfacilities and toilets should be provided in allestablishments. Toilets should be so designed as toensure hygienic removal of waste matter. These areasshould be well lighted, ventilated and should not opendirectly on to natural mineral water handling areas.Hand washing facilities with warm or hot and coldwater, a suitable hand-cleaning preparation, and withsuitable hygienic means of drying hands, should beprovided adjacent to toilets and in such a position thatthe employee will have to use them when returning tothe processing area. Where hot and cold water areavailablemixingtaps shouldbeprovided. Wherepapertowels are used,a sufficient number ofdispensersandreceptacles should be provided near each washingfacility. Care should be taken that these receptaclesfor used paper towels areregularly emptied. Taps of anon-handoperatabletype are desirable.Noticesshouldbeposteddirecting personnel to wash their handsafterusing the toilet. ,

8-3.4.4 Hand Washing Facilities in Natural MineralWater Processing Areas

Adequate and conveniently located facilities for handwashing and drying should be provided wherever theprocessdemands.Whereappropriate, facilities forhanddisinfectionshould also be provided. Wannor hot andcold water should beavailable andtaps for mixing thetwo should be provided. There should be suitablehygienic means of drying hands. Where paper towelsare used, a sufficient number of dispensers andreceptacles should be provided adjacent to eachwashing facility. Taps ofa non-hand operatable typeare desirable. The facilities should be furnished withproperly trapped waste pipes leading to drains.

9

IS 13428 : 200S

8-3.4.5 Disinfection Facilities

Whereappropriate, adequatefacilitiesfor cleaninganddisinfection of working implements and equipmentshould be provided. These facilities should beconstructed of corrosion resistant materials, capableof being easily cleaned, and should be fitted withsuitable means of supplying hot and cold water insufficient quantities.

8-3.4.6 Lighting

Adequate natural or artificial lighting should beprovided throughout the establishment. Whereappropriate, the lighting should not alter colours andthe intensity should not be less than:

a) 540 lux (50 foot candles) at all inspectionpoints,

b) 220 lux (20 foot candles) in work rooms, andc) 110 lux (10 foot candles) in other areas.

Lightbulbsandfixtures suspended overnaturalmineralwater in any stage of production should be of a safertype and protectedto preventcontaminationof natura.Imineral water in case of breakage.

8-3.4.7 Ventilation

Adequate ventilation should be provided to preventexcessive heat, steam condensation and dust and toremovecontaminatedair. The direction of the air flowshould never be from a dirty area to a clean area.Ventilationopeningsshould be provided with a screenor other protecting enclosure of non-corrodiblematerial. Screens should be easily removable forcleaning.

8-3.4.8 Facilities for Storage of Waste and InedibleMaterial

Facilities should be provided for the storage of wasteand inedible material prior to removal from theestablishment. These facilities should be designed toprevent access to waste or inedible material by pestsand to avoid contamination of natural mineral water,potable water, equipment, buildings or roadways onthe premises.

8-3.5 Equipment and Utensils

8-3.5.1 Material

All equipment and utensils used in natural mineralwaterhandlingareasand whichmaycontactthe naturalmineral water should bemade ofmaterial which doesnot transmit toxic substances, odour or taste, is non­absorbent, is resistant to corrosion and is capable ofwithstanding repeated cleaning and disinfection.Surfaces should be smooth and free from pits andcrevices. The use of wood and other materials which

IS 13418 : 1005

cannot be adequately cleaned and disinfected shouldbeavoidedexceptwhentheirusewouldnotbea sourceof contamination. The use of different materials isexercized in such a way that contactcorrosionthat canoccur, should be avoided.

8-3.5.2 Hygienic Design, Construction andInstallation

All equipmentand utensils should be so designedandconstructedas to prevent hazardsand permiteasy andthorough cleaning and disinfection.

8-4 ESTABLISHMENT: HYGIENEREQUIREMENTS

8-4.1 Maintenance

The buildings, equipment, utensils and all otherphysical facilities of the establishment, includingdrains, should be maintained in good repair and in anorderly condition. As far as practicable,rooms shouldbe kept protected from steam, vapour and surpluswater.

8-4.2 Cleaning and Disinfection

8-4.2.1 Cleaning and disinfection should meet therequirements of this standard.

8-4.1.2 To prevent contaminationof natural mineralwater,all equipmentand utensilsshouldbecleaned asfrequently as necessary and disinfected, whenevercircumstances demand.

8-4.1.3 Adequate precautions should be taken topreventnaturalmineralwaterfrombeingcontaminatedduring cleaning or disinfection of rooms, equipmentor utensils,by waterand detergentsor by disinfectantsandtheirsolutions. Detergents anddisinfectants shouldbe suitable for the purpose intended and should beacceptable to the official agency having jurisdiction.Any, residuesof these agents on a surface which maycome in contact with natural mineral water should beremoved by thorough rinsing with water, before thearea or equipment is again used for handling naturalmineral water.

8-4.2.4 Eitherimmediately aftercessationof workforthe day or at such other times as may be appropriate,floors, includingdrains,auxiliarystructuresand wallsof natural mineral water handling areas should bethoroughly cleaned.

8-4.2.5 Changing facilitiesand toilets shouldbe keptclean at all times.

8-4.2.6 Roadwaysandyards in the immediate vicinityof and serving the premises should bekept clean.

8-4.3 HYIJene Control PrOlramme

A permanent cleaning and disinfection schedule should

10

be drawn up for each establishment to ensure that allareas areappropriatelycleaned and that critical areas,equipment and material are designated for specialattention. An individual, who should preferably be apermanent member of the staff of the establishmentandwhosedutiesshouldbe independent ofproduction,should be appointed' to be responsible for thecleanliness of the establishment. He should have athorough understanding of; the significance ofcontamination and the hazards involved. All cleaningpersonnel should be well-trained in cleaningtechniques.

8-4.4 Storage and Disposal of Waste

Waste material should be handled in such a manneras to avoid contamination ofnatural mineral water orpotable water.Care should be taken to prevent accessto waste by pests. Wasteshould be removed from thenatural mineral water handling and other workingareas as often as necessary and at least daily.Immediately after disposal of the waste, receptaclesused for storage and any equipment which has comeinto contact with the waste should be cleaned anddisinfected. The waste storage area should also becleaned and disinfected.

B-4.S Exclusion of Animals

Animalsthatare uncontrolled or that couldbe a hazardto health should be excluded from establishments.

8-4.6 Pest Control

8-4.6.1 There should be an effective and continuousprogramme forthe controlofpests. Establishments andsurrounding areas should be regularly examined forevidence of infestation.

8-4.6.2 Shouldpests gain entrance to theestablishment,eradication measures should be instituted. Controlmeasuresinvolvingtreatmentwith chemical, physicalor biological agents shouldo~ be undertaken by orunder direct supervision of personnel who have athorough understanding of the potential hazards tohealthresultingfromthe useoftheseagents, includingthose hazards which may arise from residues retainedinthenaturalmineral water,suchmeasures shouldonlybecarriedout inaccordance withthe recommendationsof the official agency havingjurisdiction.

8-4.6.3 Pesticides should only be used, if otherprecautionary measures cannot be used effectively.Beforepesticidesare applied, careshould be taken tosafeguard natural mineral water, equipment andutensils from contamination. After application,contaminated equipment and utensils should bethoroughlycleaned to removeresidues prior to beinaused again. '

11-4.1 Storaae 01Ruardo.. Sablta.eeI

8-4.~.1 Pesticides or other substances which maypresent. hazardto healthshouldbesuitably labelledwith • warning about their toxicity and use. Theyshouldbestored in loCked roomsor cabinets, usedonlyfor that purpose and dispened and handled only byauthorized IIKI properly trained personnel orbypersonsunder strict supervisionoftrained personnel, Extremecare shouldbetaken to avoidcontamination ofnaturalmineral water.

8-4.7.2 Except when necessary for hygienic orprocessing purposes, no substance which couldcontaminate natural mineral water should be used orstored in naturalmineral water handlingareas.

11-4.8 Peno••1Effects aDdClotblDI

Personal effects and clothing should not be depositedin natural mineral water handlingareas.

8-5 PERSONNEL HYGIENE AND HEALTHREQUIREMENTS

8-5.1 BYIleae Tntnlaa

Managers of establishments should arrange foradequate and continuingtrainingof all naturalmineralwater handlen in hygienichandlingofnatural mineralwater and in personalhygieneso that they undentandthe precautionsnecessaryto preventcontamination ofnatural mineral water.

8-5.% Medleal ExamlDatlon

Penons who come into contact with natural mineralwater in the courseof their workshouldhavea medicalexamination priorto employment, iftheofficialagencyhavingjurisdiction, actingon medical advice, considersthat this is necessary, whether because ofepidemioloaicalconsiderationsor the medicalhistoryof the prospective natural mineral water handler.Medicalexamination of naturalmineralwaterhandlersshouldbecarried out periodicallyandwhenclinicallyorepidemiologicallyindicated.

8-5.3 Com_uDteable Diseases

The manaaemlllt should take care to ensure that nopenon, whether known or suspected to be sufferingfrom, or to be a carrier of a disease likely to be 'transmitted or aft1icted with infected wounds, skininfections,sores or diarrhoea, is permittedto work illIllynaturalmineralwaterhand1ina area inanycapacityin which there is any likelihood of such a penondirectly or indirectly contaminating natural mineralwater with pathoaenic micro-oraanisms. Any penonso affected should immediately report to the,IDIIlalement.

11

IS 13428 : 2005

8-5.4 I.Jari.Anypersonwhohas a cutorwoundshouldnotcontinueto handle natural mineral waterornatural mineral watercontactsurfaces untilthe injuryiscompletely protectedwithwaterproofcovering which is finnly secured, andwhich is conspicuous in colour. Adequate first-aidfacilities shouldbeprovided for this purpose.

8-5.5 Wa.hlDI of Hands

Everyperson,whileon duty ina naturalmineralwaterhandling area, should wash hands frequently andthoroughlywith a suitable hand cleaning preparationunder running warm water. Hands should always bewashed before commencing work, immediately afterusing the toilet, after handlingcontaminatedmaterialand whenever else necessary. After handling anymaterial which might be capable of transmittingdisease, hands should be washed and disinfectedimmediately. Notices requiringhand-washing shouldbedisplayed. Thereshouldbe adequatesupervisiontoensurecompliance with this requirement.

8-5.6 Penon.1 Cleanliness

Every person engaged in a natural mineral waterhandling areashould maintain ahighdegreeof personalcleanliness whileonduty,andshould, at all timeswhilesoengaged, wearsuitable protective clothingincludinghead covering and footwear, all of which should becleanable, unlessdesigned to bedisposed of and shouldbe maintained in a cleanconditionconsistentwith thenature of the work in which the person is engaged.Apronsand similar itemsshouldDot be washedon thefloor. When natural mineral water is manipulated byhand, any jewellery that cannot be adequatelydisinfected should be removed from the hands.Personnel shouldnotwearany insecure jewellerywhenengaged in handlingof natural mineral water.

8-5.7 PenoDal Behaviour

Any behaviourwhichcould result incontamination ofnaturalmineral water, such as eating. use of tobacco,chewing(for examplegum, sticks, betel nuts, etc) orunhygienic practices such as spitting, should beprohibited in naturalmineralwater handling areas.

8-5.8 Vlliton

~utionsshouldbetakento preventas faras possiblevisiton from visiting natural mineral water handlingareas. If unavoidable, visitors should observethe provisions recommended in B-4.8t 8-5.3, 8-5.4and 8-5.7.

8-5.9 Supervision

Responsible for ensuringcomplianceby all personnel

IS 13428 : :ZOOS

with all requirements of B-5.1 to 8-5.8 and theresponsibility should be specifically allocated tocompetent supervisory personnel.

. B-6 ESTABLISHMENT: HYGIENICPROCESSING REQUIREMENTS

8-6.1 Raw Material Requirements

To guarantee a good and stable quality of naturalmineral water, certain criteria should be monitoredregularly, namely,

8-6.1.1 Spring discharge, temperature of the naturalmineral water.

8-6.1.2 Appearance of the natural mineral water.

8-6.1.3 Odour and taste of the natural mineralwater.

8-6.1.4 The conductance of natural mineral water orany other adequate parameter.

8-6.1.5 The microbiological flora.

8-6.2 Should there be a perceptible lack in meetingthe requirements, the necessary corrective measuresare immediatelyto be taken.

8-6.3 Treatment

The treatment may include decantation, filtration,airing and where necessary application of off take ofcarbon dioxide.

8-6.3.1 Processing should be supervised bytechnically competent personnel.

8-6.3.1 All steps in the productionprocess, includingpackaging, should beperformedwithout unnecessarydelay and under conditions which will preventthe possibility of contamination, deterioration ordevelopment of pathogenic and, spoilage micro­organisms.

8-6.3.3 Rough treatment of containers should beavoided to prevent the possibilityof contamination ofthe processed product.

8-6.3.4 Treatment are necessarycontrols and shouldbe such as to protect against contamination ordevelopment of a public health hazard. It also protectagainst deterioration within the limits of goodcommercial practice.

8-6.4 Packaging Material and Containen

8-6.4.1 All packaging material should be stored in aclean and hygienic manner. The material should beappropriate for the product to be packed and for theexpectedconditionsofstorageand shouldnot transmitto the product objectionable substances beyond thelimits specified. The packaging material should besound and should provide appropriateprotectionfrom

12

contamination. Only packaaina material required forimmediate use should be kept in the packingor fillingarea.

8-6.4.2 Productcontainersshouldnot have beenusedfor any purpose that may lead to contaminationof theproduct. In case of new containers, if there is apossibility that they have been contaminated shouldbecleaned and disinfected. When chemicals are usedfor these purposes, the container should be rinsed as ,prescribed under 8-4.2.3. Containers should be welldrained after rinsing. Used and, when necessary,unused containers should be inspected immediatelybefore filling.

8-6.5 Filling and Sealing of Containen

8-6.5.1 Packaging should be done under conditionsthat precludethe introductionofcontaminantsinto theproduct.

8-6.5.1 The methods, equipment and material usedfor sealing should guarantee a tight and impervioussealing and should not damage the containers, nordeteriorate the physical, chemical,microbiological andorganoleptic qualities of natural mineral water.

8-6.6 Packaging of Contalnen

The packaging of containers should protect the latterfromcontamination anddamageand allowappropriatehandling and storing.

8-6.7 Lot IdentiOcatlon

Eachcontainershallbepermanently markedwithcodeto identify the producing factory and the lot. A lot isquantity of natural mineral water produced underidentical conditions, all packagesof whichshouldbeara lot number that identifies the production during aparticulartime, interval,and usually from a particularprocessing line or other critical processing unit.

8-6.8 Processing and Production Records

Permanent, legible and dated records of pertinentprocessing and production details should be keptconcerningeach lot. These records should be retainedfor a period that exceeds the shelf life of the productor longer if required. Records should also bekept forthe initial distributionby lot.

8-6.9 Product Durability

Product durability shall be declared on the containeras per 8.1 (g). It shall be based on in house self lifestudy and proper checks and records be maintainedfor the confonnity of the declared product durability.

8-6.10 ~tor.le and Transport 01 the End-Product

The end-product should be stored and transported

under such conditions as will preclude contaminationwith and/or proliferation of micro-organisms, andprotect against deterioration ofthe product or damageto the container. During storage, periodic inspection

IS 13428 : 200s

of the end-product should take place to ensure thatonly natural mineral water which is fit for humanconsumption is despatched and that end-productspecificationsare complied with.

CHECKLIST FOR GOOD HYGIENE PRACTICES AND FOOD SAFETY SYSTEMS FORPACKAGED NATURAL MINERAL WATER PROCESSING UNITS

(Clause 5)

SINo.

Requirements Answers

Applied Not Applied

Remarks

A Building, Facilities and Locations

i) Is the facility location a area free from objectionableodour, smoke, dust or other contaminants and notsubject to flooding?

ii) Are the areas immediately surrounding thebuildings, roads, parking places, suitably paved,grassed and kept clean?

iii) Is adequate facility for drainage of surroundingswhich is designed to handle peak load?

iv) Is the facility used for processing water free fromdomestic animals?

v) Is the facility surroundings free from refuse, wastematerials, rubbish, over grown weeds and grasses?

vi) Are there adequate facilities for the disposal ofeffluents and wastes?

vii) Are the buildings and facilitiesof sound constructionand maintained in good repair?

viii) Are the buildings and facilities designed andmaintained to prevent entrance and harbouring ofpests and entry of contaminants?

ix) Are building and facilities designed to facilitatehygienic operations?

B Plant and Physical Facilities

i) Is adequate lighting provided at working station,hand washing area, and storage areas?

ii) Is the lighting intensityadequate:

a) 540 lux in all inspectionarea, and

b) 220 lux in work areas and walls

iii) Are light fixtures safety type and protected toprevent contamination in the event of breakage inthe processing and packing area?

13

IS 13418: 1005

Sf RequireIMnts AIUltWI Re",.uNo.

Applied Not Applied

iv) Is adequate ventilation provided in processina areastominimize 'odours, noxious fumesandcondensates?

v) Are the baniers/traps provided at dnins to preventthe entry of rodents from the dnins into the facility?

vi) Is effective screening provided against entry ofbirds, animals, insects, rodents,etc?

vii) Are doors, hatches and other openings to thebuilding are constructed to render opening pestproof'?

NOTE -instaliltlon of one or more of the foIlowlna whidleffcc:tively prevents pest cnuy willmeet tillsrcquirement

a) doon selfdosina type

b) haveair curtainsc) havestrip CW1ains

viii) Are floors, walls, ceilings, windows and doors sodesignedand constructedas to preventaccumulationofdust, dirt and render them washable?

ix) Is product in process and storage area adequatelyprotected from any leakage from external surfacesand other sourcesof contamination?

x) Are immediate surroundings of extraction orcollection protected from entry of unauthorizedpersons?

C Raw Water Processing

i) In case of extraction/collection for processing are thesources free fromcontaminations/impurities?

ii) Are water storage tanks, pipe lines utilized forhandling water constructed and so designed as tofacilitate cleaningand inspection?

iii) Are inspections of containers/carriers/pipe lines ofraw water supply performed for the material ofconstruction and cleanliness?

iv) Are possible chances of contamination fromincoming water assessed?

v) Are water storage tanks effectively cleaned toprevententry of pestsand potentialcontaminator?

vi) Are the storage tanks periodically cleaned andrecordsmaintained?

vii) Are the processed water contact surfaces regularlycleanedand sanitized?

viii) Is all equipmentutensilsso designedand constructedas to prevent hygiene hazards and prevent easycleaningand sanitation?

14

IS 13428 : 2005

Sl Requirements Answers RemarksNo. Applied Not Applied

D Post Processing HandUnl

i) Are cleaningoperations ofbottleslcontainers so doneas to precludecontamination of productand productcontactserviceswith residues?

ii) Has absence of residual cleaning chemicals beenensured?

iii) Is preventive maintenance in place for all processingmachinery and equipment?

iv) Are the primary packing material and containers offood grade conforming to relevant Indian Standards?

v) Are packingand sealing, whererequired, monitored?

vi) Are containers visually electronically inspected fortheir soundness?

vii) Are physical hazards prevented from entering intoprocessed water?

viii) Are glassware excluded from production area?

E Packaging Material and Finished Goods Storage

i) Are the primary packing material and containers offood grade conforming to relevant Indian Standards?

ii) Are packaging material inspected to ensure theirsuitability?

iii) Are the packing materials especially primarypacking material properly stored and properlyhandledto precludecontamination?

iv) Are packaging material purchased, stored andhandled in sanitarymanner?

F Finished Product Storage and Distribution

i) Is First-in-first out (FIFO) of stored productmaintained?

ii) Is storage properly sanitized and disinfectedperiodically?

iii) Are storesprotected from pest infestations?

iv) Are codingand trackingclear and in place?

v) Are the instruction clear and in place?

vi) Are hold/release procedure in place and productidentified?

vii) Are the recordsmaintained for batchnumber, dateofand volume of production?

viii) Are transportcontainers/vehicles maintained in cleancondition?

15

IS 13428 : 2005

SI Requirements AMWel'l R.maraNo. Applied Not Applied

G Customer Handling of Products

i) Are the storage instructions provided on containers?

ii) Is the shelf life periodlbest before mentioned oncontainers in accordance with PFA requirements?

iii) Are instructions provided for handling defective!damaged products?

H Sanitary Facilities and Control

i) Are toilet provided in sufficient numbers and arethey provided with:

a) doors of selfclosing type?b) opening directly into processing areas?c) hand washing signs provided in appropriate

language?d) proper lighting and ventilation?e) proper maintenance to keep in clean and tidy

manner?

ii) Are hand washing facilities provided adequately andconveniently to wash hands, foot, elbow or sensoroperated taps?

iii) Are germicidal soaps/soap solution and hand dryingfacility provided?

iv) Are notice/instructions prominently pasted in toiletdirecting employees to wash their hands on entryand re-entry in to the packaged natural mineral waterhandling areas?

v) Are the refuse receptacles self closing typemaintained in a manner to protect fromcontaminations?

J Penonnel Hygiene and Habits

i) Is any individual assigned to supervise overallsanitation of plant and personnel?

ii) Is there any person responsible for day-to-daymonitoring of health and hygiene?

iii) Have the employees in processing, packing andmaintenance been medically examined?

iv) Are the personnel with infectious diseases, skininfection and open lesion or any other source ofmicrobial contamination excluded from working inprocess/packing areas?

v) Are personnel hygiene practices regularly maintainedand monitored?

a) clean outer garments-protective clothing?b) personal cleanliness-fmger nails?

J6

IS 13418: 1005

Sl Rlquiremen18 A1I.fWI'.r Remarlc.rNo.

Applied Not Applied

c) head cover-hair restrints. caps, head bands,beardcover?

d) no tobacco in any fonn-smoking. chewing?e) no eatingat workstations?

vi) Are protective clothing stored on the premises andnot allowed to be used for outside wear?

vii) Are there clear legible notices defming limits of nosmoking areas such as 'NO SMOKING BEYONDTIllS POINT' displayed?

viii) Are personnel imparted regular training or hygienicfood handling, processing food and personalhygiene?

ix) Are unsecured jewellery and other objects such aswrist watches, cufflinks, ear rings, glass bangles,stickBINDIS removed at work?

ANNEX C

(Clause 6.1.4)

DETECfION ANDENUMERATION OF THE SPORES OF SULPHITE-REDUCINGANAEROBES (CLOSTRIDIA)

c-r PRINCIPLE

Thesporesofsulphite-reducing anaerobes (clostridia)are widespread in the environment. They are presentinhumanandanimalfaecalmatter, inwastewaterand,in soil. Unlike Escherichia coli and other coliformOrLllP;Sm, the sporessurvivein waterfor longperiodsas they are moreresistant than vegetative forms to theactionofchemical andphysical factors. Theymaythusgive an indication of remoteor intermittent pollution.They may even be resistant to chlorination at levelswhichare normally used for the treatmentof water.

C-1 APPARATUSANDGLASSWARE

C-1.1SCrew-cap bottles orvialsandstoppers of boronsilicateglassofcapacities 200. 100and 25 ml.

C-2-2 VolumetricPipettes- ofcapacities 10mlandI ml.

C-2-3 Water Batbs - thermostatically controlled.

C-2.4 Test Tubes - 150mm x 13mm.

C-2.S Iron Wire

C-2.6 Incubator - capable of being maintained at37~ 1°C.

C-3 ENRICHMENTCULTURE

Detection and enumeration of spores of sulphite­reducing anaerobes by inoculating volumes of thesample into liquid enrichment media. followed byincubation at 37 % loe for 44 % 4 h in anaerobicconditions.

C-4 CULTURE MEDIAAND REAGENTS

C-4.1 Basle Materials

In order to improve the reproducibility of the results,it is recommended that, for the preparation ofthe diluents and culture media, dehydrated basiccomponents or complete dehydrated media be used.Similarly. commen:ially prepared reagents may alsobe used. The manufacturer's instructions shall befollowed.

Thechemical products used for the preparation of theculturemediaand the reagents shallbeof recognizedanalytical quality.

. The waterused shall be distilledor deionized water,free from substances that might' inhibitthe growthofmicro-organisms underthe test conditions.

Measurement of pH shall bemadeusingapH-meter,

17

IS 13428 : 2005

C-4.2 Differential Reinforced Clostridial Medium(DRCM)

C-4.2.1 Single Strength Basal Medium

measurements being referred to a temperatureof 2SoC.

If thepreparedculturemediaare notused immediately,they shallunlessotherwisestated,bestored in the darkat approximately4°C, for no longer than 1 month.

C-4.2.2 Double Strength Basal Medium

Preparethe double strengthmediumas in C-4.1.1 butreduce the volumeof water by half.

Transfer 10ml and 50 ml aliquotsofthe mediumintoscrew-capped bottles of capacities25 ml and 100mlrespectively.

C-4.3 Sodium Sulphite (N~SOJ, 4 percent (mlIII)solution.

Dissolve4 g of anhydroussodium sulphite in 100mlof water. Sterilizeby filtration.

Store at between2 and SoC.

It isadvisableto preparea freshsolution every 14days.

Mixthepeptone,meatextract, sodiumacetate andyeastextract with 800 ml of water.

With the remaining200 ml of distilledwater, preparea starch solution by mixing the starch in a little coldwater to fonn a paste. Heat the rest of the water toboiling point and slowly add it to the paste withconstant stirring.

Then add this starch solution to the first mixture andheat to boiling point until it dissolves.

Finally,add the glucoseand L~ysteine-hydrochloride

and dissolve.

Adjust the pH between 7.1 and 7.2 with sodiumhydroxide.

Transfer 25 ml aliquots of the medium into screw­capped bottles of capacity 25 ml. Sterilize in theautoclaveat 121 ± 1°C for 1S min.

C-4.7 Inoculation and Incubation

Add SO ml of sample (lee C-4.6) to a 100 ml screw­cap bottle containing SO ml of the double strengthcompletemedium (see C-4.S.3).

Add 10 ml of sample (see C-4.~) to a series of five2S ml screw-cap bottles containing 10 ml of doublestrengthcompletemedium, (see C-4.5.3),

Add 1mlof sample(see C-4.6) to a seriesoffive25 mlscrew-cap bottles containing25 ml of single strengthcompletemedium(lee C-4.5.2).

Ifnecessarytadd I mlof. I to 10dilutionof thesample(see C-4.6) to a series of five 2Sml screw-cap bottlescontaining25 ml ofsingle strengthcompletemedium(see C-4.S.2).

In order to carry out a qualitative examination of100 ml of mineral water or packaged water withoutmakina anMPN count, usea 200 ml vial filled with amixture of100mlof doublestrenathcompletemedium(lee C-4.5.3) and 100ml ofsample (lee C-4.6).

If necessary, top up all the bottles with the singlestrenath complete medium (lee C-4.5.2) to brina thevolumeofiiquid levelwith the neckandto ensure that

C-4.4 IroD (III) Cltnte(C,H.,O, Fe),7 percent(mIm)solution.

Dissolve 7 g of iron(nl) citrate in 100 ml of water.Sterilizeby filtration.

Store at between2 and SoC.

It is advisable to prepafea fresh solutionevery 14 days.

C-4.! Complete Medium

C-4.S.1 On the day of analysis,mix equal volumesofthe solutionsof sodium sulphite (see C-4.3) and iron(III) citrate (see C-4.4).

C-4.!.2 Add 0.5 ml of the mixture (see C-4.S.I) toeach bottle of single strength medium (see C-4.1.1)which has been freshly heated and cooled.

C-4.S.3 Add 0.4 ml of the mixture (see C-4.S.1) toeach 10ml, and 2 ml to each SO mitof double strengthmedium (see C-4.2.2) similarlytreated.

C-4.6 SelectioD of Spores (Tecbnlque)

Before the test," thesample of water should beheatedin a water bath at 75 :i: SoC for 15min fromthe time itreaches that temperature. A similar bottle containingthe samevolumeof water as the test sampleshouldbeused periodically as a control in order to check theheatingtime required. The temperatureof the water inthe control bottle can be constantly recorded bythermometer.

10 g1091.S g1gSg1 gO.S g1000 ml

CompositionPeptone tryptic digest of meatMeat extractYeast extractStarchHydrated sodium acetateGlucoseL-Cysteine-hydrochlorideWater

18

IS 13418 : 2005

only a very small volume ofair remains, then seal thebottles hermetically, or incubate under anaerobicconditions.

Incubatethe inoculated bottlesat 37 ± I°Cfor44 ± 4 h.

Large volumes ofculture in hermetically sealed glassbottles may explode due to gas production. The

•

addition of iron wire, heated to redness and placedinto the medium before inoculation, may aidanaerobiosis.

Bottles in which blackeningis observed, as a result ofthe reduction of sulphite and the precipitation of iron(II) sulphide, shall beregarded as positive.

100g250ml15 g0.3 g

7S0 ml

0.5 CONFIRMATORY MEDIUM

Skim milk powderYeast extract broth (see5.1)AgarHexadecyltrimethylammonium

bromide (centrimide)Water

Single Strengh Concentrated

DL asparagine 2g 3.2 g

L Proline 1 g 1.6 g

Anhydrousdipotassium 1g 1.6ghydrogenphosphate

Magnesium sulphate 0.5 g 0.8 gheptahydrate

Anhydrous potassium 10 g 16gsulphate

Ethanol 25ml 40mlWater 1000 ml I 000 ml

0-4.1 Preparation

Dissolveall the constitutents in the water and proceedin either of the following ways:

Add the ethanol and distribute in sterile screw-cappedbottles. Tighten the caps on the bottles to the pointwherethe seal in the lid just begins to engage with thelip of the bottle, autoclave at 121 ± 1°C for 15 min.Tighten the caps on each bottle, immediately afterremovalfromthe autoclave,the preventlossof ethanolbyevlporation. Do not usepolypropylene capswithoutseals.

Alternatively, sterilizethe ethanolby filtration througha celluloseacetateor nitratemembraneof averageporesize0.22 JJ m and then add it asepticallyto the mediumafter autoclaving and cooling. Adjust the pH to7.2 ±0.2. Store in screw-capped bottles in the dark atroom temperature for up to a maximumof 3 months.

It is essential that the culture medium used besuitable for the type of water to be analysed and thepurpose of the analysis. Use the following mediumfor the determination of presumed Pseudomonasael1lginola:

Use reagents of analytical reagent quality in thepreparation of culture media and diluents, unlessotherwisespecified. Preparemediausing,reagentgradewater.

D-3 DILUENT, CULTURE MEDIA ANDREAGENTS

0-4 CULTURE MEDIA

0.2 PRINCIPLE

ANNEX D

(Clause 6.1.5)

DETECTION AND ENVMERATION OF PSEUDOMONAS AERUGINOSA

0.1 PSEUDOMONAS AERUGINOSA

Measured volumes of the water sample or a dilutionof the sample, are added to a selective medium incontainers and incubated under the conditions givenfor the medium. Examination of the containers eitherfor the presence of a water-soluble fluorescingpigment under ultraviolet irradiation or for growth isdone. Sub-cultures are made from each containershowing growth or fluorescene onto plates of milkagar medium. After incubation, the plates areexamined for typical colonies of Pseudomonasaeruginosa, sub-cultures are made from eachcontainer onto the surface of a solid agar plate andincubated. Pure cultures are obtained by further sub­culture onto plates of the same agar medium asrequired. Each pure culture is fmally tested for certainbio-chemical characteristics (see Annex 2D).

Micro-organisms capable of growth and producing awatersoluble,fluorescentpigment in mediacontainingasparagines and ethanol. They also producecharacteristic colonies when grown on agar mediumcontaining milk at 42°C. Some strains are non­pigmented.

19

IS 13428 : lOOS

Yeast extract broth:

Bacteriological yeast extractBacteriological peptoneSodium chlorideWater

3g10g5g1 000 ml

in either a darkened room or apparatus designed toexclude visible light.

NOTE- Incubation at 3aoc to3~ may be used if the watersamples are likely to contain large numbers of other bacteria.The possible adverse effect of this procedure on the numbersof organisms recovered should be considered.

0-9 ENUMERATION

0.8 CONFIRMATION

Table 5 Ps~lIdomonlU Aeruglnos« Reactions

(Clauses 0-8.1 and D-9)

I) Otherbacteriacan sometimeslive atypical rclCtiOns (4) and(S).ln such instancesthe proceduredescribed in D-9 shouldbe followed.

AtypicaiU

Reaction

rTypical

Reaction Mode

A

(I) (2) (3) #(4) (5) ,

i) Casein hydrolysis + + +ii) Growth at 42 ~ 0.5OC + + +iii) Fluorescence + +

(under UV irradiationonly)iv) Pyocyanine +

(blue-peen) pipnent+ - positivereKtion- - nqative reaction

81No.

All containers ofthe culture medium exhibitingeithergrowth or fluorescence,which yield colonies (after sub­culture on milk agar plates) that produce either reaction(3) or (4) (see Table 5) shall be regarded as positivefor the presence of Pseudomonas aeruginosa.

NOTE - Others identified as non-pigmented or atypicalPselldomolUU aeruglnola by the procedure in 0-10 may beincluded also.

0.8.1 Milk Agar

Sub-culture a loopful of culture medium from eachcontainer showing either fluorescence or growth ontoa milk agar plate (see D-5), incubate the milk agarplates at 42 ± O.SOC for 24 h. Examine the plates forgrowth, pigment production, and casein hydrolysis(clearing ofthe milk medium around the colonies) andrecord the reactions as shown in Table S.

D-6 APPARATUS AND GLASSWARE

a) All glassware shall be sterilized at 170 ± 5°Cfor 1h in a dry oven or at 121 ± 1°C for IS minin an autoclave before use.

b) Use sterile Petri-dishes with a diameter ofeither 90 mm or 100 mm.

c) Incubators, capable of being maintained, at37 ± 1°C and 42 ± 0.5°C.

d) Ultraviolet lamp emitting light ofwavelength360 ± 20 nm.

NOTE - Sterile square plastics Repli dishes may beusedas an alternative to glass bottles or tubes whenthevolume of sample or dilution of the sample underexamination is 1 ml or less.

Plastics Repli dishes aresquare dishes divided into 2Sidenticalcompartmentswhich canhold I ml ofmediumtogether with I ml of sample or sample dilution. Theuse of these dishes allow S replicates from each offive serial dilutions of the sample to be testedsimultaneously. The dishes can be obtainedpresterilized.

0-5.1 Preparation on Medium

Prepare the yeast extract broth by dissolving all theconstituents in the distilled water by steaming. Adjustthe pH between 7.2 and 7.4. Sterilize by autoclavingat 121 ± 1°C for 20 min.

Mix the sterile yeast extract broth, centrimide and agar,and steam this mixture until the agar has dissolved. Ina separate glass container, add the skim milk powderto the distilled water and mix, preferably with amagnetic stirrer, until the powder has completelydissolved. Autoclave both solutions separately at121 ± 1°Cfor 5 min. To prevent caramelization ofthemilk, take care to follow these instructions. Cool thesolutions to 50°C, aseptically add the milk solution tothe agar medium and mix well.

0.7 INOCULATION AND INCUBATION

Add I ml from each sample, or dilution ofthe sample,to 4 ml portions of the medium (see 0-4) in bottles ortubes. If larger portions of the sample (10 ml, SO ml)or Repli dishes are to be used, add the sample to anequal volume of the concentrated medium.

Incubate the containers at 37 * IOC for 48 h. Examinefor growth and fluorescence under an ultraviolet lamp

0.10 NON-PIGMENTED STRAINS

NOTE- As • further step, it is possibleto obtainconfirmationof non-pipnented strains. If required, a suitable method is totake aloopfbl ofculture medium and transfer it to • milk ...plate. The pate is incubated 'at. temperature of 37 ~ lee for24 h. A well-isolatedcolonyIsselected andOnalconftrmationII obtained by testinl for certain biochemical characteristici(••Annex2D).Commercially avaHable identiftCltIon kill maybeused.

20

IS 13428: 200S

ANNEX 2D

(Clauses D-2andD-IO)

FURTHER INFORMATION ABOUT PSEUDOMONAS AERUGINOSA

Pseudomonas aeruginosa is the type specie of thegenuS Pseudomonas.

It is agramnegative, non-sporingrod which isoxidaseand catalase positive. It is capable of growth at 42°Cbut not at 4°C; it usually produces a water solublefluorescentpigment(98 percentofstrains)and exhibitsoxidative metabolism as indicated by the Hugh and

Leifson test. It generally reduces nitrate beyond thestage of nitrite and produces ammonia from thebreakdown of acetamide.

Gelatin is liquefied, casein is hydrolysed, butstarch is not hydrolyzed. The pigment pyocyanine(blue-green) is produced by more than 90 percent ofstrains.

ANNEX E

(Clause 9)

SAMPLING PLAN FOR PACKAGE NATURAL MINERAL WATER

E-I GENERAL REQUIREMENTS OF SAMPLINGFOR CONTAINERS UP TO AND INCLUDING2 LITRES

E-I.I In drawing, preparing, storing and handlingsamples, the followingprecautionsand directionsshallbeobserved as far aspossible:

a) Sample shall be drawn in original sealedbottle/container and kept in protected placenot exposed to damp air, dust or soot; and

b) Each bottle/container in original shall besealed and marked with full details ofsampling.

E-I.2 Scale or Sampling

E-l.2.1 Lot

The quantity ofpackaged natural mineral water of thesame type belonging to the same batch ofmanufactureand packed in a day, shall constitute a lot.

£-1.2.2 Forascertainingtheconfonnity ofthe materialto the requirements ofthe specification, samples shallbe tested from each lot separately.

E-I.1.3 The number of bottles to be selected from alot shall depend on the size of the lot and shall beaccording to Table 6. Separate bottle(s) shall be drawnfor testing for the microbiological requirements.

Additional bottles may be drawn if required forcarrying out complete testing or when the samples arerequired to be sent in more than one laboratory.

E-L2.3.1 The bottles shall bechosen at random fromthe lot. Inordetto ensure the randomness of selection,procedure given in IS 4905 shall be followed.

21

Table 6 Scale of Sampling

(Clause E-l.2.3)

SINo. No. of Bottles in the Lot Number of Samples

(I) (2) (3)

i) Up to 5000 3ii) 500 1 to 10000 5iii) 10001 to IS 000 7iv) IS 001 and above 9

E-I.2.4 Initially the number of cartons equal to thenumber ofbottles to be taken from the lot (accordingto col 3 ofTable 6)t shall bechosen at random. Thesecartons thus selectedshall be opened and the bottles inthese cartons examined visually for the condition ofpacking, external appearance and the fill. The lot shallbe considered satisfactory for. inspection of othercharacteristics given in the specification, if all thebottles. in the cartons opened are found satisfactory forthese characteristics.

E-I.2.5 In case any defective bottle is foundaccordingto E-I.2.4,twice the number of cartons shall be openedand the bottles examined for these characteristics. Ifno defective bottle is found; the lot shall be consideredsatisfactoryfor inspectionof other characteristicgivenin the specification.

E-l.3 Preparation of Test Samples

E-I.3.1 From each of the cartons opened accordingto E-l.2.4, threebottlesshall be taken from itsdifferentlayers so as to obtain three times the required numberof bottles in the sample (seecol 3 of Table 6).

E-I.3.2 In case the number of cartons to be opened isaccording to E-I.1.4? the number of cartons equal to

IS 13428 : 2005

the number of bottles in the sample shall be taken atrandom from these cartons and then the requirednumber of bottles picked up according to E-l.3.1.

E-I.3.3 The sample bottles selected as in E-l.3.1or E-l.3.2 shall be divided at random into three equalsets and labelled with all the particulars of sampling.One of these sets of sample bottles shall be for thepurchaser, anotherfor vendorand the third for referee.

E-l.3.4 Referee Sample

Refereesample shall consist of a set ofsamplebottlesmarked for this purpose and shall bear the seals ofthe purchaser and the supplier. These shall be kept ata place agreed to between the purchaser and thesupplierso as to beused ina case ofa dispute betweenthe two.

E-l.4 Criteria for Conformity

The tot shall be declared as conforming to therequirements of the specification, ifallthe requirementsare complied with.

E-2 GENERALREQUIREMENTS OF SAMPLINGFOR ABOVE 2 LITRES CONTAINERS

E-2.1 In drawing, preparing, storing and handlingsamples,the following precautions anddirections shallbe observed as far as possible:

a) Sample shall be drawn in original sealedcontainer and kept in protected place notexposed to damp air, dust or soot; and

b) Eachcontainer in originalshallbesealedandmarked with full details of sampling.

£-2.2 Scale or Sampling

E-2.2.1 Lot

The quantityofpackagednatural mineralwater of thesametypebelongingto the samebatchof manufactureand packed in a day, shall constitutea lot.

E-2.2.2 Forascertaining the confonnityof the materialto the requirements ofthe specification, samplesshallbe tested from each lot separately.

E-2.2.3 The numberof containersto be selectedfroma lot shall depend on the size of the lot and shall bedrawn at random, according to Table 7. Separatecontainer(s) shall be drawn for testing for themicrobiological requirements. In order to ensure the

22

randomnessof selection, procedure given in IS 4905shall be followed.

Table 7 Scale 01SaDlpliBI

(Clause E-2.2.3)

SINo. No. 01CoataAnen i. tileLot N••ber olS.aapaa

(I) (2) (3)

i) 0-500 5iI) 501 to 1 200 8iii) 1201 to 3 200 13iv) 3 201 andabove 20

E-2.2.4 These containers shall first be examinedvisually for the condition of packing, externalappearance and the fill. The lot shall be consideredsatisfactory for inspection of othercharacteristics givenin the specification, if all the containers are foundsatisfactoryfor these characteristics.

E-2.2.S In case any defective container is foundaccording to E-2.2.4, twice the number of containersshall be examined for these characteristic(s). If nodefectivecontaineris found,the lotshallbeconsideredsatisfactory for inspection of othercharacteristics givenin the specification.

E-2.3 Preparation of Test Samples

E-2.3.1 Out of the containers selected accordingto E-2.2.3, any three containers shall be selected atrandom and stored separately.

E-2.3.2 Each of the sample containers selected asin E-2.3.1 shall be divided at random into three equalsets and labelledwith all the particulars of sampling.Oneof these sets of samplecontainersshall be for thepurchaser, anotherfor vendorand the third for referee.

E-2.3.3 Referee Sample

Referee sample shall consist of a set of samplecontainers marked for this purpose and shallbear thesealsof the purchaserand the supplier.These shall bekept at a place agreed to between the purchaser andthe supplierso as to be used in case of dispute betweenthe two.

E-2.4 Criteria for Conformity

The lot shall be declared as conforming to therequirements of thespecification, ifall therequirementsare compliedwith.

IS 13418 : lOGS

ANNEX F

[Table 2, Sl No. (viii)]

DETERMINATION OF BARIUM CONTENT

F-I GENERAL

It is not necessary to look for barium if sulphate ispresent in appreciable amount unless sample containlarge amount of bicarbonate or chloride which mayhold in solution small amounts of both sulphate andbarium (as Ba).

F-2 REAGENTS

F-2.1 Ammonium Dichromate Solution - Dissolve100 g ofsulphate free ammonium dichromate in waterand dilute to I 000 ml.

F-2.2 Ammonium Acetate Solution - Dissolve 300 gof ammonium acetate in water, neutralize withammonium hydroxide and dilute to 1 000 ml.

F-2.3 Dilute Ammonium Acetate Wash Solution­Dilute 20 ml of the ammonium acetate solution(see F-2.2) to 1 000 mi.

F-2.4 Potassium Iodide Solution - 10percent.

F-2.5 Standard Sodium Tbio5ulpbate Solution-0.1 N.

F-2.6 Hydrochloric Acid - I: 1 (vlv).

NOTE - Reaction of acetate solutions should be alkalinerather than acidic.

F-3 PROCEDURE

Acidify 1.5 litre portion of sample with hydrochloricacid and concentrate to about 200 ml (if precipitateforms, filter off and test for barium). Add about 0.5 gof ammonium chloride and precipitate iron andaluminium with ammonium hydroxide. Boil, filter andwash. To filtrate, add excess (10 ml) ammonium acetatesolution (see F-2.2) keeping total volume to about200 mi. Heat to boiling and add with stirring about5 ml ammonium dichromate solution. Allow to coolslowly and wash the precipitate free of chromate withdilute ammonium acetate wash solution by decantationand filtration. Dissolve the precipitate in about 10 mlhydrochloric acid (I: I, v/v) and hot water.

Wash the filter and dilute the solution to about 400 mland add about 50 ml freshly prepared 10 percentpotassium iodide solution. Mix carefully and titrateliberated iodine (12) after 3 or 4 min with 0.1 N sodiumthiosulphate.

1 ml 0.1 N sodium thiosulphate (N~S203)= 4.578 mgbarium (Ba).

ANNEX G

[Table 2, SfNo. (ix)]

DETERMINATION OF ANTIMONY BY SPECTROPHOTOMETRIC METHOD

G-I PRINCIPLE

Pentavalent antimony in aqueous hydrochloric acidsolution reacts with Rhodamine B to fonn colouredcomplex extractable with organic solvents. Intensityof extracted colour is measured spectrometrically atS6S om wavelength.

G-2 APPARATUS

G-1.1 A suitable spectrophotometer.

G-2.2 Erlenmeyer Flask

G-3 REAGENTS

G-3.1 Hydrocblorlc Acid Solution - 6 N.

G-3.2 Dilute Phospborlc Acid - 3 N.

Dilute 70 ml phosphoric acid (85 percent) to 1 litrewith distilled water.

23

G-3.3 Rbodamine B Solution - 0.02 percent (indistilled water).

G-3.4 Antimony Standard Solutions

a) Stock Solution - 100 J.Lg antimony/ml

Dissolve 0.100g pure Antimony in 2S mlsulphuric acid with gradual heating. Cool andthen cautiously dilute to I litre with distilledwater.

b) Working Solution - I J.1g/ml

Dilute 2.0 ml stock solution to 200 ml withdistilled water.

Cool reagents G-3.1, G-3.2, G-3.3 and approximately100ml benzene, andeight 125 mlseparators with teflonstopcocks in refrigerator before use. Maintaintemperature at SoC to 10°C during extraction andcolour development

IS 13428 : 200s

G-3.5 Sulphuric Acid

G-3.6 Perchloric Acid

G-3.7 Benzene

G-4 PROCEDURE

Caution: Safety practices should be followed forhandling perchloric acid and sulphuric acid. Contactof perchloric acid with oxidizable or combustiblematerialsor dehydratingor reducingagentsmayresultin fife or explosion. Use goggles, barrier shields andother devices as necessaryfor personal protection.

Transferaliquot to 125ml Erlenmeyerflask, add Smlof sulphuricacid, and evaporateto fumesofSOr Coolthe flask, add 10 drops of 70 percent perchloric acid(HCIO.) and again evaporate to white fumes. Coolthe digest in ice-bath for 30 min, and then slowly add5 ml pre-cooled 6 N hydrochloric acid with the helpof pipette. Let it stand in ice-bath for 1S min, thenadd 8 ml pre-cooled 3 N phosphoric acid. (Untilcolour is extracted into benzene, perform subsequent

operations as quickly as possible. Colour is stable inbenzene several hour). Immediately add S ml pre­cooled Rhodamine B solution, stopper, and shakevigorously. Transfer to pre-cooled 12S ml separator.Pipette 10 ml pre-cooled benzene into separator,shakevigorouslyfor 1min,and discardaqueous layer.Transfer benzene layer (red if antimony is present)into test tube and let water settle. Rinse 1 em cellwith extract, fill the cell, and read absorption at56S om against benzene blank taken through entire'determination.

G-S PREPARATION OF STANDARD CURVE

Pipette 0, 2, 4, 6, 8 and 10 ml antimony workingstandard solutions into 125 ml Erlenmeyer flask; addS ml sulphuric acid to each, and proceed as G-4. Plotabsorptionagainst J!& of antimony.

G-6 CALCULATION

Calculate the IJg (or mg) of antimony from the graphcorrespondingto the observed absorption value.

Reactionof azomethine-H, which is the condensationproductofH-acid (8-amino-naphth-l-ol-3. 6-disulfonicacid) and salicylaldehyde, with dissolved forms ofborate at a pH of about 6. Formation of a yellowcomplex that is measured spectrometrically at theabsorption maximum inthe rangeof410om to 420 om.

Store in a polyethylenebottle.

1 ml of this stock solution contains 1.0 mg of borate,expressed as B.

8-2.5 Boron, standard solution 1 corresponding to10.0mg of B per litre.

Dilute 10 ml of borate stock solution (,ee "-2.4) to1 000 ml with water.

I ml of this s~dard solution contains 10.0 J1& ofborate, expressed u B.

8-2.3 Reagent Solution

Mix equal volumes of reagents B-2.1 and 8-2.2.Prepare this solution on the day of use and store in apolyethylenebottle.

8-1.4 Borate, stock solution corresponding to 1.0 &of B per litre.

DissolveS.719 g ofboric acid <H,BO,) in 1000 ml ofwater.

ANNEX H

[Table 2, Sl No. (x)]

DETERMINATION OF BORATE

(p-l. 71 g/ml), 1.0g of citricacid (C6U.0AO) and 1.0g ofdisodiumethylenediamine-tetraaeetic aciddihydrate(CloHI.N2N~O.~O) by stirringand gentleheating.

8-2 REAGENTS

8-2.1 Azomethine-H, Solution

Dissolve 1.0 g of azomethine-H sodium salt [8-N­(2-hy,droxybenzy Iidene)-am ino-naphth-l-o1-3.6­disulfonic acid] (CI7HI2NNaO.S2) and 3.0 g of L ±ascorbic acid (C6H.0 6) in water and dilute to 100 mlin a volumetric flask.

The solution is stable for up to one week when storedin a polyethylene bottle at a temperature of between4°C and 6°C.

8-2.2 Buffer Solution (pH 5.9)

Mix 250 g of ammonium acetate (CH3COONH4) ,

250 ml of water, 80 ml of sulphuric acid (H'2804)(p-1.21 g/ml),S ml of phosphoric acid (H2P0 4)

H-l PRINCIPLE

24

H-2.6 Boron, standard solution 2 corresponding to1.0 mg of B per litre.

Dilute 10 ml of borate solution (see8-2.5) to 100 mlwith water.

1 mlofthis standard solution contains 1.0 ug ofborate,expressed as 8.

H-2.7 Calclumhydroslde ICa(OH)2)

8-3 APPARATUS

8-3.1 Ordinary laboratory apparatus made ofpolypropylene, polyethylene or polytetrafluoroethylene,where applicable.

8-3.2 Spectrometer, for use in the wavelength rangeof 410 om to 420 nm, with cells of an optical pathlength between 10 mm and SO mm.

8-4 PROCEDURE

8-4.1 Determination

Transfer 25.0 ml ofthe sample, or a smaller amount ofthe sample diluted to 25 ml with distilled water, into a100 ml polyethylene flask. Add 10ml ofazomethine-H(seeH-2.1). Mix and allow to stand in the dark for 2 hat 20 ± 1°C, then measure the absorbance at theabsorption maximum inthe range of410 nm to 420 nmagainst distilled water in a cell of optical path length10mm,using the spectrometer set up according to themanufacturer's instructions and after setting the zerowith distilled water in the cell. Alternatively use acell of SO mm optical path length for low boronconcentrations ofup to about 0.2 mg ofboron per litre.Check the wavelength of the absorption maximumwhenever a new batch of this reagent is used.

NOTE- The reactionIime maybeshortened by keeping thetreatedsampleat a temperature of300C. Inthiscasethesample,the blank and the calibration samples should be treatedaccordingly, because the intensity of colour is temperaturedependent.

8-4.2 Blank Test

Carry out a blank test by treating 25 ml of water asdescribed in 8-4.1. Ensure that the blank value is in therange of 0.1 absorption units to 0.17 absorption unitsper 10 mm; if the absorption is higher then check thereagents and the distilled water for their borate content.

NOTE- The following procedure maybe used to checkthequalityof reagentsand thedistilledwater.

Measure into three separate borate-free beakers(preferably polytetraf1uore~ylene) 2S ml, 100 ml and2S0 ml aliquots of the distilled water. Make eachslightly alkaline by the addition ofthe same small (forexample 200 mg) amount of calcium hydroxide(seeB-2. 7) t~ each. Evaporate the 100 ml and 250 ml

2S

IS 13428 : 2005

aliquots to a volume ofjust less than 25 rnl and adjusttheir volumes to precisely 25 ml by the addition of alittle extradistilled water, as necessary. Carry out theprocedure given in 8-4.1 on these aliquots.

Carry out a blank determination with each of thealiquots. Ifborate is present in the distilled water, theborate found increases in proportion to the volume ofthe aliquot taken. Erratic results indicate external boratecontamination. Relatively high but constant resultsindicate impure reagents.

8-4.3 Prevention of Contamination

As borate is widespread in the environment, significantcontamination may occur during trace determinations.

The following sources ofcontamination, and remedies,should be considered.

Laboratory glassware is usually made from borosilicateglass. Special borate-free thermally resistant glass isobtainable, but for routine purposes, old borosilicateglass, well rinsed in hydrochloric acid, may be usedfor acidic solutions, but should never be used forneutral or alkaline solutions, or for prolonged storageat any pH value. (Borosilicate glassware previouslyused with alkaline solutions shall not be used withoutvery thorough acid rinsing.) Polyethylene flasks andplastics pipettes are preferable.

Detergents and soaps used for glassware and labcoatsshould beborate free, and the use oftowels and tissues,for drying shall be avoided.

Toiletries, talcum powder and cosmetics used bytechnicians often contain borate and should beavoidedor removed, especially prior to undertaking accuratelow-level determinations.

Water and reagents may contain borate and blanksshould be carried out at least in duplicate and shouldagree.

"-4.4 Calibration

8-4.4.1 Zero mg/I to 0.20 mg/I ofBoron CalibrationGraph

To a series of six 25 ml one mark plastics flasks addrespectively 0 ml, 1 ml,2 ml, 3 ml, 4 ml and 5 ml ofboron standard solution .2 (see 8-1.6), dilute to themark with distilled water and mix. This givesconcentrations of 0 mg; 0.04 mg; 0.08 mg; 0.12 mg;0.16 mg and 0.20 mg of boron per litre respectively.Analyze each standard solution as described in H-4.1t

measuring the absorbance values in a SO mm opticalpath length cell compared against distilled water.Preparea calibration graph by plotting the absorbancevalues against the known concentrations in milligramsof boron per litre for each standard.

IS 13428 : 2005

H-4.4.2 Zero mg/I to 1.00 mg/I ofBoron CalibrationGraph

Repeatthe above calibration,using 0 ml, 5 ml, 10ml,15 ml, 20 ml and 25 ml of boron standard solution 2(see H-2.6) respectively to give concentrations ofomg; 0.2 mg; 0.4 mg; 0.6 mg; 0.8 mg and 1.0 mg ofboron per litre respectively. Analy~e each standardsolutionas described in 8-4.1, but this time measuringtheabsorbance valuesusinga 10mm opticalpathlengthcellcompared againstdistilledwater.Preparea separatecalibration graph.

H-4.4.3 Calculation ofFactor/

It isessential thata linearcalibration graphbe achievedinbothcases; ifnot then checkthe solutionsand repeatthe calibration. Calculate the reciprocal value for theslope, factorf, for each graph.

a-s CALCULATION

Calculate the borate content, in milligrams of boronper litre, from the formula

<As - Ao)f~ Ma

Jt;where

A I = absorbanceof the sample;Ao = absorbanceof the blank;VI = volume, in millilitres,of the sample;

. VI Max = maximum volume, in millilitres, of thesample; and

f = calibration factor, determined from theappropriatecalibrationcurve (reciprocalvalueof the slope, inmilligramsof boronper litre).

ANNEXJ

[Table 2, Sl No. (xi) and Table 3, SfNo. (iv)]

DETERMINATION OF SILVER AND CHROMIUM CONTENTS

J. J PRINCIPLE

Metals in solution are determined directly by atomicabsorption spectrophotometry. Suspended metals areseparated by membrane filtration or suspension isdissolved and analyzed.

J·2 APPARATUS

J·2. t Atomic Absorption Spectrophotometer

Spectrophotometercapable of operatingat conditionsare given in Table 8.

Table 8 Operating Parameten

(Clause J-2.1)

SI Metal Wavelength Flame Optimum RanleNo. mg/l(I) (2) (3) (4) (S)

i) Silver 328.1 Oxidizing 0.1 to 20air-acetylene

ii) Chromium 357.9 Reducing 1 to 200air-acetylene

J-3 REAGENTS

J-3.1 De-ionized Distilled Water

Distilled, ammonia free. Pass through ion exchangecolumn of mixed strongly acidic cation and stronglybasic anion exchange resins. Regenerate resinsaccording to manufacturer's instructions.

26

J-3.2 Nitric Acid

Dilute 500 ml redistilled nitric acid to I 000 ml withwater.

NOTE- Perform distillation in hood with protective ash inplace.

J·3.3 Hydrochloric Acid

Dilute 500 ml hydrochloric acid to 1 000 ml withwater and distill in all-Pyrex or equivalent glassapparatus.

J-3.4 Metal Solutions

J-3.4.1 Stock Solutions

Accurately weighamountof metalspecified in Table 9intoa beakerand add dissolvingmedium. Whenmetalis completely dissolved, transfer quantitatively into1 000 ml volumetric flask and dilute to volume withwater.

J-3.4.1 WorkingSolutions

Prepare daily. Dilute aliquots of stock solutions withwater to make more than or equal to 4 standardsolutionsofeachelementwithinthe rangeofdetectionas given in Table 9. Add 1.5 ml nitric acid per litre toall working standard solutions before diluting tovolume.Add 1mllanthanum chloride for every 10 mlmaking the working standard solution.

IS 13428 : 2005

Table 9 Preparation of Metal Staadard SolutioDS

(Clauses J-3.4.1 and J-3.4.2)

51 Metal Wel.llt Compo.ad DluoIvlDi MedlulDNo. (a) (I litre Total)

(1) (2) (3) (4) (5)

i) Silver 1.575 Silver nitrate Water+ 10ml(AgNO) redistilled nibic acid

ii) Chromium 1.923 Chromium Water+ 10mloxide (Cr103) redistilled nitricacid

J-3.S Lanthanum Stock Solution

Slowly add 250 ml hydrochloric acid to 58.65 gI~thanum oxide(L~03' purity99.9percentby mass),dissolve and dilute to 1000 ml.

J-3.6 Ammonium Pyrrolidine DitbiocarbamateSolution

Dissolve 1 g ammonium pyrrolidinedithiocarbamatein 100ml water. Prepare fresh daily.

J-4 PREPARATION OF SAMPLE

J-4.1 Dissolved Metals

As soon as practicable after collection, filter knownvolume of sample through 0.45 J.1m membrane. Usefirstly50-100ml to rinse the flaskand discard. Collectthe filtrate and preserve the solution by adding 3 mlnitric acid (I: I, vlv) per litre.

J-4.2 Suspended Metals

Transfer the residue and membrane from J-4.1 to a250 ml beaker and add 3 ml nitric acid. Cover withwatch-glassandheat gently to dissolvethe membrane.Increase heating and evaporate to dryness. Cool andadd3 mlnitricacidandheatuntildigestion iscomplete,generallyindicatedby lightcolouredresidue. Add2 mlhydrochloricacid (1:1,vlv) andheat gentlyto dissolve

the residue. Wash the watch-glass and beaker withwater and tilter. Wash the filter and discard. Dilutethe filtratewith waterto such a concentrationthat it iswithin the range of the instrument.

J-4.3 Total Metal

Transferanaliquotof wellmixedsampleto the beakerandadd3 ml nitricacid.Heatandevaporate to dryness(do not boil). Cool and add 3 ml nitric acid and heatuntildigestion iscomplete, generally indicated by lightcoloured residue. Add2 ml hydrochloric acid(I:I, vlv)andheatgentlyto dissolve theresidue. Wash thewatch­glass and beakerwith waterand filter. Washthe filterand discard. Dilute the filtrate with water to such aconcentration that it is within the range of theinstrument.

J-S DETERMINATION

Transfer an aliquot of the sample to a 250 ml beakerand dilute to 100 ml with water. Prepare blank andstandard solution in the same manner. Adjust the pHof the sample and standard solutions to 2.5 withhydrochloric acid using a pH-meter. Transferquantitatively to a 200 ml volumetric flask,add 2.5 mlof ammonium pyrrolidine dithiocarbamate solution andmix. Add 10 ml methyl isobutyl ketone and shakevigorously for I min. Let the layers be separated andthen add water until the ketone layer is in the neck ofthe flask. Centrifuge, ifnecessary. Aspiratethe ketonelayer and record readings of standards and samplesagainstblank.The fuel-to-air ratio shouldbeadjustedto as blue a flame as possible since organic solventsadd to fuel supply.Preparethe calibration curve fromthe average of each standard and read the sampleconcentration.

J-6 CALCULATION

Metalcontent,mg/l = Metal, in mg, in the aliquot/I.

ANNEX K

[Table 2, S/ No. (xxi)]

METHOD OF TEST FOR ANIONIC SURFACE ACTIVE AGENT

K-l PRINCIPLE

Fonnation of salts from methylene blue and anionicsurfactants in an alkalinemedium.Extraction of thesesalts with chloroform and acid treatment of thechlorofonn solution. Elimination of any interferencesby extraction of anionic surfactant-methylene bluecomplex from alkaline solutions and shaking withacidic methylene blue solution. Measurement of the

27

absorbance of the separated organic phase at themaximum absorption wavelength of 650 om. Thismethod is applicable to limit of detection of aboutO.OS mg/l for solutions of standard surfactants indistilledwater.

K-2 APPARATUS

K-1.1 pH-Meter, with suitable electrodes made ofglass.

IS 13428 : 2005

K-2.2 Spectrometer with Selectors forDiscontinuous Variation. capible ofmeasurement at650 nm, equipped with cells ofoptical pathlengths of10 mm and SO mm.

K-2.3 Gas-Stripplnl Apparatus - One litrecapacity (see Fig. 1).

K-) REAGENTS

K-).l Sodium Chloride

K-3.1 Ethyl Aeetate. freshly distilled.

C••tIoII- EthyllCCUlte Istl.....ableandtoxic.

K-3.J Chloroform

C••t10D - Chloroform Is• suspected carclnoaen. Ifnecessary.purify the chloroform by flItratlon throuah AIZO

J(neutral

...... W200). If it alves rise to hiah results in blankteat.

K-3.4 Ethanol. 95% (vlv).

K·3.S Metha.ol. freshly distilled.

ETHYLACETATE

,TESTSAMPLE

ItlQItl

SINTEREOGl.ASSFIllERGI

Alldimensions in m1l1imetres.

FlO. 1 GAS STIlIPPINO APPAaATUS

28

K-3.6 Sulphuric Acid Solution - 0.5 mill.

K-3.7 Ethanollc Sodium Hydroxide - 0.1 mol/I.

Dissolve 4 g of sodium hydroxide pellets in ethanoland dilute to 1 000 ml with the same ethanol.

K..3.8 Metbylene Blue, Neutral Solution

Dissolve0.350 g ofmethyleneblue in wateranddiluteto I 000 ml. Prepare the solution at least 24 h beforeuse.

NOTE- Theabsorbance of thechloroform phaseof theblanktest, measured against chloroform, shall not exceed 0.2 per10mm of optical pathlength at 6S0 nm. In the case of highabsorbances during the blank test, use other batches ofmethylene blue or purify the methylene blue solution byextractionas under:Placethemethylene bluesolutionina suitablylargeseparatingfunnel, For each 100 ml of methylene blue solution,add 200mlof butTer solutionand200 ml of chloroform. Shakefor 30sand allow to separate. Run off the chloroform layer ascompletely as possible and rinse the aqueous layer withoutshakinawith60 mlof chloroform foreach 100mlof methylenebluesolution. Repeattheextraction andrinseas before. Discardthechloroform extracts; collect for reuseafter treatment.

K-3.9 Methylene Blue, Acidic Solution

Dissolve0.350 g ofmethyleneblue in 500 ml of waterand add 6.50 ml of sulphuricacid(p-1.84 g/ml). Dilutewith water to 1 000 ml after mixing. Prepare thesolution at least 24 h before use.

The absorbance of the chloroform phase of the blanktest, measured against chloroform, shall not exceed0.02 per 10 mm of optical path length at 650 nm. Inthe case of higher blank absorbances, either wash themethylene blue solution twice with chloroform forpurification, as in K-3.8, or use other batches ofmethylene blue.

K-3.10 Burrer Solution,pH 10

Dissolve 24 g of sodium hydrogen carbonate(NaHC0 3) and 27 g of anhydrous sodium carbonate(N~C03) in water and dilute to I 000 ml.

K-J.ll Phenolpbthalein Indicator Solution

Dissolve 1.0 g of phenolphthalein in SO ml ofethanoland add, while stirring continuously, 50 ml of water.Filter offany precipitate that forms,

K-3.11 Dodecylbenzene Sulpbonic Acid MethylEster (Tetrapropylene Type), stockstandard solution.

Weigh to the nearest 0.1 mg, 400 mg to 450 mg ofdodecylbenzene sulphonic acid methyl ester, into around-bottomed flask, and add SO ml of ethanol­sodium hydroxide solution and some anti-bumpinggranules.Attach the refluxcondenserand boil for I h.Aftercooling,rinsethe condenserandtheground-glass

29

IS 13428: 2005

joint with about 30 ml of ethanol and add the rinsingsto thecontentsof the flask. Neutralize thesolutionwithsulphuric acidagainstphenolphthalein until itbecomescolourless. Transfer the solution to a I 000 mlvolumetric flask, dilute to the mark with water andmix. This standardsolution is stable for 6 months.

K-4 PROCEDURE

K-4.1 Separation of the Surfactant

Non-surfactant methyleneblue active substancescancause errors in the test of methylene blue index.Stripping is recommended for concentrating smallamount of surfactants from water samples. Separatesuspended matter by centrifugation, but note thatadsorbed surfactantson suspended matter will not bedetermined,

Place a measured quantity of the test sample, up to1 000 ml in the gas-stripping apparatus. Install thestripping apparatus in well ventilated hood to carryoff ethyl acetate vapour. Separation is improved byadditionof sodium chloride. If samplevolumeexceeds500 ml, add 100 g of sodiumchlorideand dissolve bypassingnitrogengas or air through it. I f a smaller testsample volume is used, dissolve 109 g of sodiumchloride in 400 ml of water and add this solution, tothe test sample.

Ifnecessary, add water to bring the sample surface upto the level of the upper stopcock. Add 100 ml ethylacetate.Fill the wash bottle in the gas line(nitrogen orair) two-thirdfull with ethyl acetate.Passa gas streamof20 Vb to so Vb through the gas-strippingapparatus.Adjustthegas flow in sucha waythatthephasesremainseparateand no turbulence is producedat the interface.The significant mixing of the phases and consequentsolutionof ethyl acetate in the water is avoided. Stopthe gas flow after 5 min.

If a loss of more than 20 percent (wv) of the organicphasehas occurreddue to solution in the water phase,discard the test sample.

Runoff the organicphasecompletelyintoa separatingfunnel. Return any water in the separating funnel tothe gas-strippingapparatus.

Filterthoethylacetate solution through a dry qualitativegas-filterpaper intoa 250mlflask. Adda further 100mlof ethylacetateto the gas-stripping apparatus and againpass nitrogen or air through it for S min. Separate theorganic layer as described above, using the sameseparating funnel, filter, and add it to the first portion.Rinse the filter paper and funnel with 25 ml of ethylacetate. Remove alltheethylacetate solution ona water­bath under a hood. To speed up the process, direct agentleair stream over the surface of the.solution.

IS 13428 : 2005

Dissolve the residue in about 5 ml of methanol and50 ml of water. Transfer the solution quantitativelytoa 100 ml volumetric flask and dilute to the mark withwater.

K-4.2 Blank Test

Carry out a blank test at 650 nm and subtract theinterpolated absorbance, Ao' from the absorbance Aiof the test sample. Under the given conditions, theabsorbance Ao of the blank test shall not exceed 0.02per 10 mm optical path length, otherwise equipmentand the reagents shall be checked carefully for anycontamination.

K-4.3 Test with the Sample

Transfer a measured volume of the test sample into aseparating funnel. This test portion should contain20 ~g to 200 Ilg of MBAS (methylene blue activesubstances). In the lower MBAS range, a test portionup to 100 ml may be used. If the volume of the testportionis lessthan 100 ml,dilute withwaterto 100 mJ.Add 5.0 ml of neutral methylene blue solution, 10 mlof butTer solutionand IS ml chloroform, Shakeevenlyand gently about twice a second for 1 min, preferablyin a horizontal plane. Allow the layers to separate as

completelyas possibleand swirl the funnel to dislodgedroplets from the sides of the funnel.

Allowto settle for 2 min, then run asmuch as possibleof thechloroform layerintoa secondseparatingfunnel,containing 110 ml of water and 5.0 ml of acidicmethylene blue solution. Shake uniformly but not toovigorously for 1 min as previously described. Filterthe chloroform layer through a cotton or glasswoolfilter wetted with chloroform into a 50 ml volumetricflask.

Repeattheextraction of the alkalineand acidicsolutionusinga 10 ml portionof chloroform for the extraction.Separatethe chloroform layer and filter it, through thesame filter, into the volumetric flask. Repeat theextraction using a further 10 ml portion ofchlorofonnand filter that into a SO ml volumetric flask. Dilute tothe mark with chloroform and mix.

For each test sample carry out the completeextractionfor a blank determination on 100 ml water.

Measurethe absorbancesfor the test sample as well asfor the blank test at 650 nm in cells of optical pathlength 10 mm to 50 mm against chloroform. Theabsorbanceof the test sample should not be more thanthat of the blank (see K-4.2).

ANNEX L

[Table 3, Sl No. (vii)]

DETERMINATION OF NICKEL BY FLAME ATOMIC ABSORPTIONSEPCTROMETRIC METHOD

L-I PRINCIPLE

Formation of a complex between the metals beingdetermined and ammonium l-pyrrolidinedithio­carbamate (APDC) and extraction at pH 2.5 withmetbyl-isobutylketone (MIBK).

Determination of the metals in this organic phase byflameatomic absorption spectrometry.

L-2 APPARATUS

L-2.1 Atomic absorption spectrometer fitted withhollow cathode lamps for appropriate metals orelectrodeless discharge lamps, and with a suitabledevice for allowing for the correction of the non­specific absorbance and with a nebulizer-burnerwithan acetylene-air flame.

L-3 REAGENTS

L-3.1 Concentrated Nitric Acid (p-I.4 alml)

L-3.2 Nitric Acid, 1.5 molll

30

Add 100 mlofnitric acid to 600 ml of water and diluteto I 000 ml.

L-3.3 Nickel Standard Solution Correspondingto 1 000 gil

Weigh 1.000 g of pure metal and dissolve it in cone,nitric acid, heating to effect complete dissolution.Allowto cool and transfer each solutionquantitativelyto a 1000ml volumetric flask, dilute to the mark withwater and mix.

For preparing standard solution, it is also permissibleto use metal salts of accurately known composition.

One ml of the standard solution contain 1.00 mg ofnickel.

L-3.4 Sodium Hydroxide - 2.S moVI.

Dissolve 100g of sodium hydroxideinwateranddiluteto 1 litre.

L-3.5 HydrOeblorie Aeld - 0.3 molll.

Mix 2S ml of concentrated hydrochloric acid(p-1.19g/ml) with water and dilute to 1 litre.

L-3.6 Methyl.isobutylketone (MIBK) (that is,4-methy 1-2-pentanone).

L-3.7 Ammonium I-PyrrolidlDedltblocarbamate(that I., Ammonium-Pyrrolidlnocarboditbioate)(APDC) Solution - 20 gil.

Dissolve 2.0 g ofAPDC in water. Make up the volumeto 100 ml with water and mix. Filter the solution if aprecipitate is present. Ifthe solution is coloured, purifyit by repeated extraction with MIBK until the solutionis colourless. Prepare this solution freshly for eachbatch of samples.

L-3.8 Bromophenol Blue Indicator Solution - t gof bromophenol blue per litre of 50 percent (v/v)ethanol solution.

L-4 PRE-TREATMENT OF SAMPLE

L-4.1 For majority of samples, mineralization usinghydrochloric acid or nitric acid will be satisfactory.

This alternative procedures of mineralization whichfollow are given as examples.

L-4.2 Add 5 ml of hydrochloric acid (p-I.19 g/ml)for each 100 ml of test portion. Heat in a steam-bathuntil the volume has been reduced to between IS mland 20 ml, making sure that the sample does not boil.

Cool and filter to remove insoluble materials that couldclog the nebulizer. Collect the filtrate in a 100 mlvolumetric flask. Wash the filter several times withwater.

L-4.3 Add 4 ml of 15 mol/l nitric acid to 100 ml ofthe sample and heat until the volume is reduced toSOmt.

Place the treated sample in a boiling flask. Add 12 mlofhydrochloric acid (p-l.19 g/ml), Connect the boilingflask to a condenser and reflux the solution for 2.5 h.

Cool and filter to remove insoluble materials that couldclog the nebulizer. Collect the filtrate in a 100 mlvolumetric flask.

Wash the condenser and filter several times with water,add this to the contents of the volumetric flask andmake up to the mark with water.

L-5 PROCEDURE

L-S.l Test Portion

Place in a 100 mIone-mark volumetric flask a testportion of the acidified sample containing S to 20 J.1gof nickel being determined. Make up to the mark withwater.

31

IS 13428 : 2005

L-5.2 Cbelation and Extraction

Place the test portion and 100 ml of each of thecalibration solutions into a series of250 ml separatingfunnels fitted with polytetrafluoroethylene (PTFE)taps.

Add to each funnel 2 to 3 drops of bromophenol blueindicator and sodium hydroxide until a blue colourpersists.

While stirring, add drop-wise hydrochloric acid untilthe blue colour just disappears. Then add 2 ml ofhydrochloric acid in excess. The pH value shall thenbe 2.3 to 2.5 (see Note I).

Add 5 ml of APDC, mix, then add 10.0 ml of MIBK.Shake vigorously for 2 min. The pH shall beapproximately 2.8.

Allow the mixture to settle for at least 1 h away fromlight or heat in the stoppered funnel. The settling timeshall be strictly the same for all the solutions. Collectthe organic layer taking care to avoid any trace of theaqueous phase (centrifuge if necessary, see Note 2).

NOTES

I ApH-meter may be used in place of indicator.

1 The settling period may be prolongedwithoutdisadvantageif it takes place in the dark at a temperatureof about SoC. Inthiscaseit maynotbenecessary to centrifuge theorganicphase.

L-5.3 Blank Test

Carryout a blank test in parallel with the determination,by the same procedure using the same quantities ofallthe reagents as in the sampling and chelation andextraction, but replacing the test portion by water.

L-5.4 Preparation of the Sets of CalibrationSolutions

Dilute with water immediately "before use, the nickelstandard solution in order to obtain diluted solutionscontaining 10 mg of nickel per litre.

In a SOO ml volumetric flask, place

a) 20 ml of nickel solution that contain 10 mg/lof nickel; and

b) O.S ml of nitric acid.

Make up to the mark with water. This is solution S.Prepare at least four calibration solutions by dilutingsolution S with water so as to cover the ranges ofconcentrations of nickel from 0 to 200 ug/l.

Acidify each calibration solution by adding the samenitric acid which has been added to preserve thesamples. The volume added shall be such that theconcentrations ofnitric acid are the same in the sampleand in the calibration solutions.

IS 1~28 : 2005

L-5.5 Calibration and Determl.atloD

Before carrying out the spectrometricmeasurements,setupthespectrometer accordingto themanufacturer'sinstructions by aspirating the organic extract of acalibration solution of nickel being determined andusingwave length232 om and oxidisingacetylene-airflame. Optimize the aspiration and flame conditions.Adjust the response of the instrument to zeroabsorbance with MIBK.

Aspirate the organic extracts of the calibrationsolutions. Plot a graph having the nickel content" inmicrograms per litre of the calibration solutions asabscissaeand the corresponding values of absorbanceas ordinates. It is advisable that the calibration graphbe checked, for example by measuringthe absorbanceof a calibration solution every S samples.

Aspirate the organic extract of the test portion.

Measure the absorbance and after each measurementaspirate MIBK in order to rinse the nebulizer system.

1.-5.6 Calculation

By reference to the calibration graph, detennine theconcentrationscorrespondingto the absorbanceofthetest portion and of the blank.

The concentration,expressed in micrograms per litre,of the sample is given by the formula:

100(Q. -Q..)xT

where

Q. = nickelconcentration, inmicrogramper litre,correspondingto the absorbance of the testportion;

Qb =nickelconeennadon, inmicrogramper litre,corresponding to the absorbance of theblank; and

V = volume,inmillilitre,ofthe acidifiedsampletaken for the analysis.

ANNEXM

[Table 3, Sl No. (viii)]

TEST FOR POLYCHLOROBIPHENYLES (PCB)

M-I PRINCIPLE

The procedure comprises separationof PCB from theorganochlorinepesticides residuesby meansofsilica­gel adsorption column and determination of itspresence by gas-liquid chromatography (GLe).

M-l APP~TUS

M-l.1 Glass Cbromatograpbic Column, 300 mmlong,8 nun 1D witha ground-glasssocketat the upperend and a stopcock at the lower end.

M-1.2 Ga. Cbromatolnpb

Equipped with electron capture detector and coupledwith printer-plotter-cum-integrator.

a) Column 1 - 1.8m long, 3 mm 1D; ApiezonL grease + 0.1S per cent Epikote Resin 1001on chromosorb G (acid-washed, DMCStreated, 60-80 mesh);

b) Column 2 - 1.8 m long, 3 mm 1 D; 1.3 percent siliconegum OE - SE-52+0.15 per centEpikote Resin 1 001, on the same supportmaterial;

Temperature: Column oven 200°CDetector 2000cInjection port 200°C

32

M-l.3 Electron Capture Detector

M-2.4 Kuderna-Danisb Type, Evaporator, withinterchangeable 10 ml graduated collection tubes.

M-l.S Snyder Columns, two-bubblemicro-columns,withgroundglassconesto fit the Kudema-Danish type,10 ml collection tubes.

M-2.6 Syrinle - S III capacity.

M-3 REAGENTS

M-3.1 Silica Gel, 60-100 mesh.

Heat the gel at 260°C for 4 h and, when it is cooled to6SoC, placeit in a desiccator. Whenithascooledfmallyto room temperature,weigh the required amount intoa glass-stoppered flaskand quicklyadd2.5 mldistilledwater to each 100g. Immediatelystopperthe flaskandshake it for 1.5 h on a shaker. The silica gel is readyfor use.

M-3.2 N-besane, redistilled from potassium hydroxidepellets. When concentrated IOo-fold, I S J-LI portionshould give no significantOLe peaks.

M-3.3 Sodium Hydroslde Solution - 5 N.

M-3.4 Dlethyl Etber, chromatographygrade.

M-3.'5 Cotton Wool, extracted with hexane anddiethyl ether.

M-3.~ Acetic Acid, glacial, redistilled.

M-3.7 Chromium Trioxide, re-crystallised.

M-4 SEPARATION OF PCB FROM THE MOREPOLAR PESTICIDE RESIDUES

Weigh s.o g of the prepared gel and rapidly transferit, by using small amounts of hexane, to thechromatographic column, in which a plug of cottonwool has been placed just above the stopcock. Thestopcock may be moistened with solvent but must notbe lubricated with grease. Allow the gel to settle in thecolumn and remove and trapped air bubbles by stirringwith a glass rod. Drain the surplus hexane from thecolumn until its meniscus just touches the surface ofthe gel. Introduce the cleaned-up sample extract as asolution in 1 ml of hexane, and allow the hexane todrain until the meniscus again just touches the surfaceof the gel. Wash the vessel that contained the extractwith two I-ml portions ofhexane, adding each washingseparately to the column' and allowing it to run justinto the gel. Place a receiver, preferably a Kudema­Danish evaporator, beneath the column and pass 42 mlof hexane through the column at a rate not exceeding0.7 mllmin. Collect the eluate, stopping the elutionwhen the meniscus reaches the top ofthe gel, and labelthis fraction I. It should contain all the PCB.Hexachlorobenzene, aldrin, O.p-DDT and pp' -DOE,if present, are also eluted in this fraction. Change thereceiver and pass 50 ml of a 10 percent solution ofdiethyl ether in hexane through the column. Collectthe eluate and label it fraction 2. This contains theremainder of the organochlorine pesticide residues,including usually a small amount ofpp'-DOE, and canbe used for the determination of these. Concentratefraction I to 5 ml in the Kudema-Danish evaporatorand examine it by GLe with electron capture detection,on at least two stationary phases ofdifferent polarities.Iffurther concentration is necessary, reduce the volumeof the solution with a gentle stream of dry airor nitrogen at room temperature. Compare thechromatograms from fraction 1 with zhose given bysolutions of commercial PCB preparations wheninjected on the same columns as well as the

33

IS'13428: 2005

correspondence between peak retention times whichgive indication of the presence of PCB in the sample.

M-5 OXIDATION OF pp'-DOE IN THE PCBFRACTION

M-S.1 Adjust the volume of fraction I to 2 ml,concentrating, if necessary, as described above. Add2 ml of acetic acid and, after replacing the micro­Snyder column, heat the tube cautiously in the steam­bath until all of the hexane has evaporated, as judgedby the reduction in volume. Introduce 100 mg ofchromium trioxide and place the tube in boiling waterfor 15-20 min. Cool the mixture and shake it vigorouslywith 2.0 ml of hexane (accurately measured) in thestoppered tube. Neutralize the acid with 6-7 ml of 5 Nsodium hydroxide, solution. Shake the tube again andthen set it aside until the two layers separate. Keep thetube well stoppered to prevent loss of hexane.

M-6 DETECTION OF PCB

Inject 5 J.11 of the upper hexane layer of the oxidizedmixture on to at least two GLC columns with differentliquid phases, one of which should be Apiezon L.Compare the retention times of the peaks so obtainedwith those given by the PCB reference material.Agreement between the retention times of the peaksso obtained now indicates the presence of PCBcompounds in the sample with a greater degree ofcertainty. Any pp'-DDE, which was present infraction 1, will have been converted into 4, 4'­dichlorobenzophenone. Under the GLC conditionsquoted, this compound has a retention time similar tothat of heptachlor epoxide and so gives a peak on thechromatogram before most of the PCB isomersencountered in practice. A comparison of the tracesbefore and after oxidation of fraction 1 will show howmuch pp' -DOE was originally present. Adjust thevolume of the hexane solution so that the individualheights ofthe PCB peaks are within the linear responserange of the electron capture detector. Under theprescribed GLC conditions for the Apiezon L. column,the last ofthe PCB isomers normally found in wildlifetissues emerges in about 120 min after injection.

IS 13428 : 2005

ANNEX N(Clause 6.3)

STANDARDS ON METHODSor REsmUE ANALYSIS

Sl Name ofPesticide Method01Test, &ftoNo. r ...... ,

USEPA AOACIISO(1) (2) (3) (4)

1. DDT(0, P &, p, p-isomers of DDT, DOE&, DOD) 508 AOAC990.062. y-HCH (Lindane) S08 AOAC990.063. a,p&5-HCH 508 AOAC990.064. Endosulfan(a, Pand Sulphate) 508 AOAC990.06s. Monocrotophos 8141A6. Ethion 16S7A7. Chlorpyrifos S2S.2, 8141A8. Phorate (Phorate and its oxygen analoguethat is, 8141A

phorate sulphoxideand phoratesulpbone)9. 2,4-D S15.110. Butachlor 525.2, 8141AII. Isoproturon 53212. Alachor 525.2, S0713. Atrazine 525.2, 8141A14. Methyl Parathion(Methyl Parathion and its oxygen 8141A ISO 10695

analogue that is, methyl-paraoxon)IS. Malathion(Malathionand its oxygen analoguethat 8141A

is, malaoxon)16. Aldrin and dieldrin 525.2 AOAC990.06

NOTE- Test methods R for Iuidance and reference for testina 11boratory. In case of two methods, USEPA method shill be thereference method.

34

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