for bis use only doc no.: sm/is14543 & is13428/03 … · 3 0. foreword 0.1 bis has published...

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FOR BIS USE ONLY Doc No.: SM/IS14543 & IS13428/03

MANUAL

FOR

PACKAGED WATER

(Third Issue)

Date of Issue: March 2013

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CONTENTS

Item Chapter Page No

0 Foreword 3

1 Introduction 4

2 Scope 5

3 Product Description 5-8

4 Grant of Licence 8-14

5 Operation of Certification 14-19

6 Guidelines for Assessment of Hygienic Conditions with Explanatory Notes

19-35

7 Useful Tips for Inspecting Personnel & Guidelines for Reused Containers

35-37

ANNEXES

1 Check List For Scrutiny of Application 38-39

2 Report of Preliminary Inspection 40-45

3 Verification Report By BIS IO 46-47

3A Factory Testing Report 48

3B Samples for Independent Testing 49

4 Check List For Good Hygiene (Applications) 50-54

5 Typical Manufacturing Process, Process Flow Chart,CIP Process 55-58

6 Check List for Red Form Processing 59-61

7 Report of Periodic Inspection 62-65

7A Assessment of Compliance to IS 13428/IS 14543 66-67

7B Details of Testing from OSL 68

8 Hygiene Check List (Licences) 69-70

9 List of Test Facilities

A Organoleptic and Physical Requirements 71-73

B Chemical Requirements 74-98

C -Toxic Substances 99-105

D -Microbiological Requirements 106-113

E -Bottle / Container Requirements 114

F -PE Flexible Pouch Requirements 115-116

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0. FOREWORD 0.1 BIS has published two Indian Standards on packaged water for drinking purpose, namely, IS 13428 for Packaged Natural Mineral Water (PNMW) and IS 14543 for Packaged Drinking Water (Other Than Packaged Natural Mineral Water) (PDW). Both the products were brought under mandatory BIS certification effective from 29 March 2001 through two gazette notifications issued by Ministry of Health and Family Welfare, namely GSR No. 759 for Packaged Natural Mineral Water (PNMW) and GSR No. 760 for Packaged Drinking Water (PDW) as amendments to Prevention of Food Adulteration Rules. Presently, these products under mandatory BIS certification are covered under FSSAI regulation.

0.2 In the early stages of certification of PDW, different situations were handled differently by ROs/BOs. This had necessitated issuance of several guidelines for creating uniformity in certification of PDW throughout the country. Further, a need was felt to compile all these guidelines into a manual. Thus, the Manual for PDW was brought out in the year 2005. 0.3 Revision of the Manual has been taken up to suitably incorporate the changes that had taken place since 2005 in the certification of PDW and also in the general policies of product certification. A specific sub-section for guidelines related to PNMW such as for constancy of source water and criteria for decision seasonal variations etc introduced. 0.4 Packaged Drinking Water (Other Than Packaged Natural Mineral Water) (PDW) Packaged Natural Mineral Water (PNMW) are basically packaged water for drinking purpose. Therefore, title of this MANUAL is “MANUAL FOR PACKAGED WATER”. 0.5 Salient changes in this version of the Manual are as follows:

updation of the manual with respect to various amendments to IS 14543 and IS 13428 and guidelines issued from time to time; incorporation of guidelines under simplified procedure for GOL and inclusion; updation of the list of test equipment as per revised test methods wherever applicable; inclusion of the list of test equipment for Bottles/Containers and PE Flexible Pouch for Packaged Water; and exclusion of the provision of verification by Chartered Engineer under the simplified

scheme for grant of licence.

This Manual is intended only for internal use by BIS officers and inspection personnel working on behalf of BIS. However, others can draw benefit from the Manual to improve their activities related to certification of PDW and PNMW. Suggestions for any improvement in this Manual may be sent to CMD – 2.

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1 INTRODUCTION 1.1. The Standard IS 14543 provides sufficient freedom to the manufacturer to adopt any process for converting raw water into packaged water for drinking purposes. Therefore, the required manufacturing machinery for the purpose is neither specified in the respective Indian Standard nor in this Manual. Illustrative examples have been given of typical manufacturing process with process flow diagram, cleaning and disinfection (CIP) of plant and machinery, pipelines as well as of containers in Annex 5. 1.2. However, there are restrictions with regard to processing of PNMW as specified in IS 13428, such as the source water shall not be subjected to process steps, such as reverse osmosis, demineralization or disinfection before packaging.

1.3. IS 13428 and 14543 prescribe a large number of requirements to be tested as per the methods of tests given in the various cross-referred standards. Further, many requirements have options for selection of test method to be followed. This has made the task of the inspecting official difficult and time consuming for complete assessment of adequacy of the test facilities. This Manual provides a ready reference for the inspecting official to check facilities for each of the requirements against the method given under the relevant Indian Standard and the method chosen by the firm (Annex 9).

1.4. All efforts have been made to incorporate details as per the latest versions of the standards. However, as the standards are dynamic and subject to amendments and revisions, users are encouraged to check the latest versions of the respective methods of test subsequent to issuance of this issue of the Manual, before using the information contained herein.

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2. SCOPE 2.1 This Manual of Packaged Water provides guidelines for various aspects related to certification of Packaged Natural Mineral Water and Packaged Drinking Water (Other Than Packaged Natural Mineral Water) according to IS 13428 and IS 14543 respectively along with the respective STIs. The provisions of these Indian Standards, STIs, as also the various guidelines issued from time to time for certification of packaged water have been kept in view while preparing this Manual. 2.2 Explanatory notes have been incorporated wherever necessary to take care of subjective interpretations. 2.3 Specific proformas have been included for submission of reports of preliminary, periodic and verification inspections so as to facilitate uniform reporting by all concerned, covering all essential parameters required to be reported as per the relevant ISS, STI. Other proformas for checking plant, process and personnel hygiene; processing of application; preparation of red form for grant of licence; test equipment details etc have also been included. 2.4 In case of any deviation, the requirements of the Indian Standards and the corresponding STIs shall prevail. 3. PRODUCT DESCRIPTION 3.1 Packaged Drinking Water 3.1.1 Packaged drinking water means water derived from surface water or underground water or sea water which may be subjected to specified treatments, namely, decantation, filtration, combination of filtrations, aeration, filtration with membrane filter, depth filter, cartridge filter, activated carbon filtration, demineralization, remineralization, reverse osmosis and packed after disinfecting the water to a level that shall not lead to any harmful contamination in the drinking water by means of chemical agents or physical methods to reduce the number of microorganisms to a level beyond scientifically accepted level for food safety or its suitability: Provided that sea water, before being subjected to the above treatments, shall be subjected to desalination and related processes. It shall be filled in sealed containers of various compositions, forms and capacities that is suitable for direct consumption without further treatment. 3.1.2 The water used for production of drinking water is water derived from any source of surface water or underground water or sea water received on regular basis. Supplies of such water through pipelines, tankers would be acceptable provided the source remains the same.

Note 1: It is the responsibility of the manufacturer to ensure that the source of raw water remains the same. An undertaking in this regard shall be obtained from the manufacturer. Note 2: Raw water supplies received through tankers, river, lake, pond etc. is acceptable, provided treatment of such water is done as mentioned in 3.1.1.

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3.1.3 As indicated above, in the manufacturing of the packaged drinking water, remineralization may also be done. This process involves addition of ingredients. In case remineralization is carried out by any manufacturer, ingredients used for the purpose shall be of food grade/pharmaceutical grade quality.

Note: With respect to the conformity of ingredients used for remineralization to food grade/pharmaceutical grade, original manufacturer’s declaration through labels or certificate/test certificate from a BIS approved laboratory as per relevant Indian Standard or IP/NFP/USP/BP requirements, in this respect will be accepted.

3.1.4 Processed water may be disinfected by means of chemical agents and/or physical methods to control the micro-organisms to a level that does not compromise food safety or suitability for consumption. Various means adopted for disinfection include ozonation, ultraviolet treatment, silver ionization, etc. and/or combination thereof. 3.2 Packaged Natural Mineral Water 3.2.1 Packaged natural mineral water shall be water obtained directly from natural or drilled sources from underground water-bearing strata. 3.2.2 Packaged natural mineral water is collected under conditions which guarantee the original microbiological purity and chemical composition of essential components and subjected to permitted treatments which include separation from unstable constituents, such as compounds containing iron, manganese, sulphur or arsenic, by decantation and/or simple filtration, if necessary, accelerated by previous aeration. No disinfection process is permitted.

Note: Only simple filtrations through filters of pore size not finer than 0.5 microns which do not change the composition of the source water are permitted. Processes like reverse osmosis, activated carbon bed filtration etc. are not permitted.

3.2.3 Packaged natural mineral water shall be packaged close to the point of emergence of the source with particular hygienic precautions. 3.2.4 The transport of natural mineral water in bulk container is prohibited. 3.2.5 Natural mineral water shall have the constancy of its composition and the stability of its discharge and temperature, due account being taken of the cycles of minor natural fluctuations. Evidences for constancy of water composition at source on account of cycles of minor natural fluctuations during different seasons in a year shall comprise of the following: a) Test report (from any BIS approved OSL) of all the major seasons covering major physico-

chemical parameters;

b) Record of temperature at discharge point/ point of emergence (by manufacturer); c) The reports of all the seasons shall be reasonably comparable and conforming to IS 13428; and

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d) Report from the Hydrogeologist covering genesis of natural mineral water; period of its

residence in the ground; chemical, physical and radiological qualities; and the risk of pollution. 3.3 Packaging 3.3.1 The packaged water shall be packed in clean, hygienic, colourless, transparent, tamperproof and sealed containers of various types/sizes/ made from plastic materials as permitted in either IS 13428 or IS 14543. Containers with features like Cool Jugs, Jugs with built-in taps, Jars with threaded (reusable) caps without seal etc. shall not be permitted. Single-use disposable/collapsible jars are also not permitted 3.3.2 There are many terminologies presently adopted by the industry and consumer for describing the different packaging containers of packaged water. For the purpose of uniformity in describing the various types of containers, descriptions as given in Table 1 have been derived. In case of change in material (i.e., PET/PC) it shall be treated as separate type (ex. PET Jar,PC Jar).

Table 1: Description of Containers for Packaged Water

CONTAINER DESCRIPTION

Jars Reusable plastic containers with capacity above 5 litres

Plastic Bottles One time use plastic containers with capacity upto and including 5 litres.

Cup/Tumbler One time use plastic container in cup shape or tumbler (glass shape) with a peelable seal

Glass Bottle Reusable containers made of glass material.

Pouches Flexible Pouches made from plastic films.

3.3.3 The standards prescribe use of colourless and transparent containers. Therefore tinted containers are not permitted.

Note: Use of HDPE containers had been discontinued after 31 July 2003, as communicated by CMD-II vide note dated 01 08 2003 and 01 10 2003.

3.3.4 Cup/tumbler/pouch shall be filled with drinking water/natural mineral water followed by heat sealing of cup/tumbler with peelable seal through automatic process. Manual filling and sealing shall not be allowed so as to maintain hygiene and sanitation. Manual loading of packaging material (cup/tumbler) may be accepted. 3.4 Assessment of Hygienic Conditions

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Guidelines for assessment of hygienic conditions with explanatory notes have been given at Item 6 for the inspecting personnel. 4. GRANT OF LICENCE 4.1 General 4.1.1. This section gives the guidelines on actions related to receiving of an application and its processing for grant of licence (GOL). The pre-requisites for GOL shall be as per the requirements published in BIS website, (www.bis.org.in) either for normal procedure or for simplified procedure. 4.1.2 Application for grant of licence for packaged water shall be accompanied by the list of documents given in BIS Web site (www.bis.org.in). An application under simplified procedure shall be accompanied with original test reports of PDW/PNMW as per relevant specifications and on entire range of containers, their materials, caps and closures for which GOL has been requested. 4.2 Recording of Application An application with its enclosures shall be scrutinized as per the check-list given in Annex 1. Recording shall be done when all pre-requisites have been addressed in the application with supporting documents. 4.3 Inspection 4.3.1 The format for Preliminary Inspection Report specific to PDW/PNMW shall be as given at Annex 2, in case of application received under normal procedure. 4.3.2 The verification by BIS Inspecting Officer shall be reported in the format specific to PDW/PNMW and as given at Annex 3, in case of application received under simplified procedure. 4.3.3 Aspects to be inspected During preliminary inspection/verification visit, for assessing capabilities of the applicant organization, with respect to manufacturing and testing facilities; competence of Quality Assurance Personnel and hygienic conditions, following shall be verified: a) Correctness of documents and declarations submitted with the application and self evaluation

report (in case of application under simplified procedure); b) Availability of all manufacturing facilities including filling and/or packaging machinery; c) Process capability, starting with collection of raw water to packaged water including

intermediate checks; d) Filling and packing capabilities for all capacities and types of containers used in packaging

of water;

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e) Availability of required testing facilities, as per the relevant ISS. List of test equipment and chemicals required for testing of packaged water is given at Annex 9.

f) For testing certain requirements, as specified in the STI, the applicant may avail the

provision of STI for getting some tests done from outside BIS recognized laboratories (OSL), if in-house facilities are not available. The applicant shall furnish an undertaking that they shall get samples tested as per the frequency of STI at any BIS recognized laboratory (test requirements which are to be conducted once in a month or beyond shall only be permitted to be tested at OSL);

g) Competence of Quality Assurance Personnel. There shall be at least two (2) Quality

Assurance Personnel, one of whom shall be a Chemist, the other a Microbiologist. For further details, 4.7 shall be referred;

h) Compliance to Hygienic Practices as per Annex B of IS 13428:2005 or Annex B of IS

14543:2004 ( Item 6 of this Manual); i) Availability of adequate storage facility for raw water, finished product and packaging

materials, keeping in view the installed capacity of the firm for packaging in 24 hours and storage capacity of finished product for 48 hours;

j) The correctness of plant layout with respect to following:

i) Source of raw water and raw water storage facility ii) pipeline, storage tanks etc;

iii) Plant for the manufacture of PDW and/or PNMW, as the case may be (with various

process stages);

iv) Filling/packing/loading/ unloading areas;

v) Storages for packaging material and finished product ;

vi) Entry/exit with indications of double door/door closures/air curtains, wherever provided;

vii) Laboratory;

viii) Actual boundary/perimeter of the establishment;

ix) change room, toilet(s), whether the premises also used for residential/other purposes,

with identified locations.

Note: A typical manufacturing process; process flow chart; CIP process for plant and machinery and pipelines; and cleaning process for reusable jars are given at Annex 5.

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4.3.4 Hygiene Practices Hygienic practices in the plant shall be verified as per Annex B of IS 13428:2005 or Annex B of IS 14543:2004 ( Item 6 of this Manual and Annex 4). Explanatory notes provided at the end for guidance only.

4.4 Sample for Independent Testing 4.4.1 Packaged Water (Packaged Drinking Water and/or Packaged Natural Mineral Water)

One sample of packaged water shall be drawn and sent for complete testing for all requirements of the relevant Indian Standard. 4.4.1.1 In case the applicant is adopting more than one type of processes/sources of raw water, separate samples shall be drawn for each process/source. 4.4.1.2 In the event of more than one bore well /open well located in the same premises, they shall be considered as a single source for the purpose of drawing of sample of PACKAGED DRINKING WATER as well as for exercising quality control, provided there is only one processing line. 4.4.1.3 Samples shall be drawn in sealed containers only, which shall not be leaking. During sampling, the container of packaged water sample shall never be opened for any purpose as the water will get contaminated. 4.4.2 Packaging Material 4.4.2.1 When an application is received under normal procedure for GOL, during preliminary inspection, along with one sample of packaged water, samples of all containers,( of each type, each size and each material) and their material (for example, film with pouch) shall be drawn for complete testing as per IS 15410 and/or IS 15609 as applicable and for which application has been made to include in the licence 4.4.2.2 When an application has been received under simplified scheme, during verification inspection by BIS officer before GOL, one sample (any one size, type and material) for one type of container shall be drawn for complete testing as per IS 15410 and/or IS 15609 respectively.. 4.4.3 Sample Size 4.4.3.1 Packaged Water a) For all parameters other than radio active residues - A sample containing approximately 18 litres of packaged water (PDW/PNMW) is adequate, if packed in 2 litres or smaller containers but in case the samples are available in large size packages, minimum two such packages are

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required as microbiological laboratory needs separate sample for ensuring aseptic handling. For example:

Capacity of bottle/Jar in litres

Numbers to be drawn

1 18 2 9 5 4 10 2 20 2 24 2

Pouches: 2 bags of 100 pouches each + Film. A sample of 4 bags shall be drawn in case each bag contains 50/60 pouches.

b) For Parameters concerning Radio-active Residue

In addition to the above, sample shall also be drawn for testing parameters concerning radio active residues. A sample of 10 litres is adequate.

Note: If a fresh application has been submitted after closure of earlier application or expiry/cancellation of earlier licence and the closure of application/licence was for reasons other than failure in radioactive residues, fresh sample of water need not be drawn for testing of radioactive residues, if evidence is available that the source of raw water remained the same as that in earlier application/licence, provided that radioactive residue TR of the sample drawn by BIS during verification visit passes and is not older than two years. The earlier test reports of sample drawn by BIS (not older than two years) shall be accepted within a period of two years.

4.4.3.2 Sample of packaging material (containers) PET Bottles upto 2 litres – 18 Empty (with caps) + 12 filled

5 litres – 12 Empty (with caps) + 9 filled 10 litres & above – 6 Empty (with caps) + 3 filled

Pouches: 4 bags of 50/100 pouches each + one meter film used for making the pouches. Cup/Glass along with peelable seal: 25 Empty + 25 filled + lids (25)

Note 1: The pouches shall be made in the presence of BIS officer, during inspection, and may be printed with only details like batch number, date of manufacturing, best before date, capacity, using ink to be used by the manufacturer for marking on the pouches. This will facilitate testing of pouches for ink adhesion test and product resistance test. This is being allowed as manufacturer can not get the pouch film rolls printed with all other details such as Standard Mark etc. before the GOL.

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Note 2: As there is presently no Indian Standard for glass bottle/tumbler, such containers need not be tested. However, if any manufacturer intends to use such container, it shall be included in the licence.

4.4.4 Samples shall not be drawn for independent testing for the following:

a) Product Durability Assessment (shelf life study), and b) Raw Water Requirements

4.5 Test Request and Selection of Laboratory 4.5.1 Masking of sample Effort shall be made, as far as possible, to send samples without the manufacturer’s identification and/or markings. Any label and/or manufacturer's identification from the bottles/Jars shall be removed or defaced. 4.5.2 Test request Test request shall clearly indicate the following:

a) Date of processing/packing; b) Best Before Date; c) Quantity (in litre or milliliter), d) Type, material and capacity of container e) Declared wall thickness of container(s)/width of film of pouch

4.5.3 Selection of laboratory for independent testing: Samples shall be tested either at a BIS laboratory or BIS recognized laboratory .List of recognized laboratories is given on BIS website. Selection of laboratory for independent testing shall be as per provisions of OMPC. 4.6 Verification of Calibration of Test Equipment 4.6.1 Records of calibration of test equipment need to be maintained by the applicant. Although the test equipment will depend upon the selection of test method by the applicant from the options available in the respective Indian Standard, calibration of following test equipment is considered necessary at least once a year. The calibration certificates shall be from NABL accredited laboratory or from laboratory having traceability to national level.

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a) Analytical balance (electronic)/weight box (including fractional weights), b) Temperature indicators of all incubators, c) Pressure gauge of Autoclave, and d) Temperature indicator of Autoclave (optional)

4.6.2 Other instruments, such as spectrophotometer, turbidity meter, pH meter are to be standardized as per the standard operating procedures supplied with respective instrument. 4.7 Quality Assurance Personnel 4.7.1 There shall be minimum two Quality Assurance Personnel, one for carrying out chemical testing and the other for microbiological testing. 4.7.2 The personnel for chemical testing shall be minimum science graduate with chemistry as one of the subjects. Microbiologist shall be a science graduate with preferably Botany or Microbiology as a subject or a graduate in Food Technology/science or Dairy Technology/science or Agriculture. Both shall have necessary competence to carry out testing of the respective tests (chemical or microbiological). 4.7.3 The IO shall witness all possible tests that can be conducted during the inspection. For those tests which are not possible to be carried out during inspection, assessment of competence may be made through interview of the testing personnel, demonstration of initiation of tests, equipment, interpretation of results etc., which shall be suitably recorded in IR. 4.8 STI Acceptance of existing scheme of testing and inspection (STI) shall be obtained from the applicant during the inspection visit, if the same has not been received earlier. 4.9 Marking Fee Acceptance of existing rate of marking fee shall be obtained from the applicant during the inspection visit, if the same has not been received earlier. 4.10 Processing for Grant of Licence The Red Form shall be put up as per the check-list given in Annex 6 with all attached documents serially page-numbered. In case of GOL under normal procedure, if the product water is conforming and failure(s) of Container samples are reported, grant of licence shall be processed for the product water as per IS 14543/IS 13428, as the case may be along with the remaining container(s) which have been reported as passing. Note 1 under 2.9.1 of OMPC is not applicable in such cases.

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4.11 Scope of Licence Licence shall be granted with scope specifying the type(s) and material(s) of container(s) permitted to be used for packing the product. Licence shall not be granted with “open scope”. A container shall be included in the licence subject to availability of proof of conformity to the relevant Indian Standard for each of such container(s). The grant of licence letter and the Licence Document shall clearly indicate the following:

a) Packaged Natural Mineral Water/ Packaged Drinking Water with corresponding Indian Standard;

b) Type of each container (Jar, Bottle, Cup/Tumbler, Pouch); c) Material of construction of each container (PC/PET/PP/PS/PE/Glass);and d) Size/Capacity of the container.

(see Clause 3.3.2 for Guidelines for above classification)

5 OPERATION OF LICENCE 5.1 General This section provides guidelines for operation of licence based on IS 13428 or IS 14543 and the corresponding Scheme of Testing and Inspection. The operational guidelines as given under Operating Manual for Product Certification shall be followed for those situations that are not specifically covered in this Manual. 5.2 Periodic (Surveillance) Inspection At least two surveillance inspections are required to be done in an operative year of a licence, as per the requirements of the BIS (Certification) Regulations, 1988. The inspections shall be planned in a manner to evenly spread over during the period of a licence’s validity. A surveillance inspection shall not be done after validity of a licence is over and decision is pending for its renewal. The report of surveillance Inspection of a packaged water licensee shall be submitted as per the format given at Annex 7 along with Hygiene Checklist as given at Annex 8. 5.2.1 Scheme of testing & inspection(STI) The STIs for IS 13428 and 14543 as in force shall be applicable. The implementation of STI shall be verified during surveillance inspection. 5.2.2 Marking fee The details of rate of marking fee are available on BIS intranet/website.

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5.2.3 List of laboratories for independent testing The list of BIS laboratories and laboratories recognized by BIS, where sample of packaged water and/or its container can be sent for independent testing, are available on BIS intranet/website. The inspecting officer/agent shall collect latest status in respect of any laboratory before proceeding for inspection. 5.2.4 Sample from factory and market Sample of packaged water shall be drawn during surveillance inspection from the available stock or from production with Standard Mark observed during such inspection (FS). Two FS shall be drawn and independently tested during an operative period of a licence (drawing one sample during one inspection). Four market samples (MS) of packaged water shall also be drawn during an operative year of the licence. Samples of containers and packaging materials are also required to be drawn for testing by rotation pertaining to various containers as permitted in the licence as it is essential to monitor the quality of container(s) being used for filling with packaged water. The details of samples that should be drawn in one operative year of a licence are given in Table 2 and Table 3:

Table 2 - Sampling from Factory during surveillance inspection

Particulars of sample

No. of sample(s)

Details of tests to be conducted

FS 2 During the operative period, at least one FS/MS shall be tested for all requirements including pesticide residues. Note: One FS shall be tested every two (2) years for parameters concerning radio-active residues. If FS could not be drawn for testing for Radioactive residues due to any reason then, MS shall be tested for the same

Container 1 From the first periodic inspection /surveillance visit (verification visit by BIS in case of GOL under simplified procedure) onwards, one sample of any one type of container ( one size and material) shall be tested once a year for all requirements of relevant Indian Standard. Sampling of container shall be done in a manner so as to cover all type, sizes &

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material on rotational basis during the operation of the licence. Sample of container shall be drawn at the same time when a FS is being drawn.

Table 3 - Sampling from Market

Particulars of sample

No. of sample(s)

Details of tests to be conducted

MS 4 All 4 MS shall be tested for all requirements of the Indian Standard, except for pesticides residues and parameters concerning radio-active residues. Also refer Table 2 above for FS

5.3 Hygienic Conditions Plant, process and personnel hygiene shall be assessed during every surveillance inspection as per Hygienic Practices at Annex B of IS 14543:2004 or Annex B of IS 13428:2005 (Item 6 of this Manual). The filled up Checklist (Annex 8 of this Manual) also shall be attached with Surveillance Inspection Report. 5.4 Operational Issues 5.4.1 Change of source of raw water or change in process 5.4.1.1 Packaged natural mineral water In case of change of source of raw water by the licensee, documentary evidence shall be collected as stated under 3.2.5 of this Manual and examined vis-à-vis the requirements of IS 13428 for constancy of source water quality. An inspection shall be carried out to verify that the restrictions specified in the standard with respect to processing and disinfection are complied; to verify plant machinery and to check hygienic conditions. A sample of packaged natural mineral water produced by using changed source shall then be drawn for independent testing for its conformity to all requirements of the standard including parameters concerning radio-active residues. CM/PF 305 shall be submitted by the licensee and countersigned by the inspecting official after due verification of declarations made therein. Permission for use of Standard Mark shall be given on receipt of test reports indicating conformity of the sample. 5.4.1.2 Packaged Drinking Water In case of change of source of raw water by the licensee, an inspection shall be carried out to verify the changes made in processing of raw water, if any; to verify plant machinery and to check hygienic conditions. CM/PF 305 shall be prepared by the licensee and countersigned by the inspecting official after due verification of details. A sample of packaged drinking water produced

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by using changed source shall then be drawn for independent testing for its conformity to all requirements of the standard including parameters concerning radio-active residues. Permission for use of Standard Mark shall be given on receipt of test reports indicating conformity of the sample. Clause 4.4.1.2 of this manual may also be referred. 5.4.1.3 Concurrent use of raw water from two different sources In case of concurrent use of raw water of two different types of sources (for example water being extracted through own bore-well and also obtained from municipal source), the production from each source shall be assigned a different batch number and separately tested as per STI for conformity of the product water, provided production lines are separate. Accordingly, records of production and testing of packaged drinking water produced using both the sources shall be kept by the licensee. However, when there is more than one source of raw water but processing plant is one, testing of packaged drinking water shall be done after duly verifying the additional source(s) being introduced and appropriate record in CM/PF 305, if necessary shall be made. Such testing shall include parameters concerning radio-active residues. 5.4.2 Change in the process In case of any addition, alteration and/or change in the production process without any change in raw water source (for example, remineralization has been added after reverse osmosis in production of packaged drinking water or decantation has been introduced as a process step in production of packaged natural mineral water), necessary verification of plant and machinery shall be done with duly filling up of CM/PF 305. A sample is required to be drawn for independent testing for its conformity to the relevant Indian Standard, except for parameters concerning radio-active residues, before permitting the same to be marked. Testing of product water so produced by using different processes shall be carried out as per STI and records be kept separately by the licensee.

Note 1: Testing for parameters concerning radio-active residues need not be done under above circumstances provided the source of raw water remains the same. Note 2: Any change in process may require fresh approval of label. Therefore licensee shall be advised to prepare fresh label incorporating all marking details and obtain approval.

5.4.3 Shelf-life The shelf-life of packaged natural mineral water/packaged drinking water shall be minimum 30 days. If the manufacturer intends to declare a longer shelf-life than minimum 30 days, study shall be conducted on each type of packing at least once a year or whenever there is a change in the source of raw water/manufacturing/packing process, whichever is earlier. The shelf-life period shall be declared on the labels suitably as “Best for consumption within -----days or -----months from the date of packing” based on the shelf life studies (but not less than 30 days). Subsequently, for any change in the shelf life declared on the labels, the manufacturer shall inform BIS in advance along with shelf- life study reports and submit fresh label for approval. Tests to be carried out for shelf life studies are requirements given

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in Table 1 of IS 14543/IS13428 along with routine microbiological tests as per IS 14543/IS13428. 5.4.4 Change in the scope of licence 5.4.4.1 Extension of scope There are many instances when licensees request for permitting use of additional types of packaging materials/filling capacities, although basically the packaged water may remain the same (i.e., other than those related to remineralization). These may be considered based on the following: Under Normal Procedure a) Packing/filling/cleaning and disinfection (in case of reusable containers) arrangements

related to proposed inclusion such as required infrastructure, filling facilities, flow process and intermediate checks etc., are verified and recorded on CM/PF305;

b) Associated hygienic conditions are verified, if applicable; c) Raw water shall not be tested; d) Sample for shelf-life test shall not be drawn. Only declaration in this regard shall be

obtained; and e) Sampling of container for independent testing should be done as follows: Irrespective of whether, the test certificate of containers with respect to conformity to IS 15410 or 15609, as applicable, is available or not, sample of each type/ size/material shall be drawn for complete testing. Endorsement to the licence shall be issued for including the particular type of container in the licence after sample of such container is found conforming to the standard. Under Simplified Procedure For inclusion under the simplified procedure, in case the licensee submits the complete test report of containers from OSL along with modified process flow chart if any, additional infrastructure facilities if required, intermediate checks etc., inclusion as per the simplified procedure shall be permitted without any further testing. The variety so included may be drawn for independent testing during subsequent visits on rotational basis, so as to cover the entire range and the changes intimated shall be verified during the subsequent visit. The licensee shall submit an undertaking that in case of failure of sample in independent testing, he shall abide by the instructions of BIS for stop marking/withdrawal of permission to use the particular type of container/cancellation of licence, as the case may be. 5.5 Stop Marking - Resumption of Marking

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The procedure given in OMPC shall be followed. 5.6 Handling Complaints on Packaged Water 5.6.1 As the packaged water is meant for mass consumption and also related directly to the health and safety of the consumer, it is quite likely that complaints may arise for the same. The product is not expensive. Therefore, as per the OMPC a replacement can straight away be arranged to the complainant. However, the following aspects need to be addressed suitably. 5.6.2 Redressal to the complainant may be arranged either from the existing stock (if declared to be conforming) or from the fresh production after resumption of marking is permitted to the licensee (in case Firm is under stop marking for any reason or has been placed under stop marking due to complaint or any other reason). 5.6.3 If it is not possible to establish the complaint by visual examination, it would be necessary to send material under complaint for independent testing. However, if the container has already been opened and the packaged water is not available in originally packed condition, it shall not be sent for testing. Only unopened sealed container (packing with intact cap/closure/seal) shall be sent for tests. Attempts may be made to procure material pertaining to the same lot/batch/manufacturing date from the market, if available and sent for independent testing to establish the complaint. However, such sample purchased from the market shall not have the status of complaint sample but would only be treated as a market sample and would be handled in the manner in which any other market sample is handled. 5.6.4 The above procedure is to be followed in addition to the procedure of handling of complaints as given in the OMPC.

6 GUIDELINES FOR ASSESSMENT OF HYGIENIC CONDITIONS IN PACKAGED

DRINKING WATER UNIT WITH EXPLANATORY NOTE (BASED ON IS 14543:2004) REQUIREMENT OF INDIAN STANDARD

EXPLANATORY NOTES FOR GUIDANCE

B-1 FIELD OF APPLICATION The hygienic practices cover the appropriate general techniques for collecting drinking water, its treatment, bottling, packaging, storage, transport, distribution and sale for direct consumption, so as to guarantee a safe healthy and whole some product.

B-2 HYGIENE PRESCRIPTIONS FOR COLLECTION OF DRINKING WATER B-2.1 Extraction or Collection In the case of extraction or collection of water intended for packaging from ground water sources, it should be ensured that it is safe from pollution, whether caused by

It may be ensured that the ground water source is reasonably away from any polluting source like drain/ sewer/ septic tank. Ground water source (whether owned/ shared) shall be under the direct control and supervision

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natural occurrence or actions or neglect or ill-will.

of the manufacturer. Clear declaration from the manufacturer for ensuring that the ground water source is safe from pollution either by natural occurrence or because of action/ neglect/ ill-will shall be taken.

B-2.2 If water to be processed for packing is obtained from any other potable source it should be protected from being contaminated.

B-2.3 The firms using waters from drinking water systems intended for packaging should ensure that it meets the requirements of the standard.

B-2.4 Materials The pipes, pumps or other possible devices coming into contact with water and used for its collection should be made of such material that they do not change the quality of water.

The material should preferably be of stainless steel. However, GI or plastic material may also be used. In case of plastic materials, it should be supported with certificate for its food-grade quality. Rubber pipe shall not be permitted.

B-3 PROTECTIVE MEASURES B-3.1 All possible precautions should be taken within the protected perimeter to avoid any pollution of, or external influence on, the quality of the ground or surface water. Preventive measures should be taken for disposal of liquid, solid or gaseous waste that could pollute the ground or surface water. Drinking water resources should not be in the path of potential source of underground contamination.

The surrounding of the source water outlet should be completely covered with pucca construction to avoid contamination due to ingress of external causes. If it is at ground level then it should be covered with a boundary wall upto an adequate height.

B-3.2 Protection of the Area of Origin The immediate surroundings of the extraction or collection area should be protected by limiting access to authorized persons only. Wellheads and spring outflows should be protected by a suitable structure to prevent entry by unauthorized individuals, pests and other sources of extraneous matter.

Outlets of bore well/ well heads should be covered and locked. Units should prevent entries of individuals, pests and other sources of extraneous matter to the immediate surroundings of source of water.

B-4 TRANSPORT OF DRINKING WATER B-4.1 Means of Transport, Piping and Reservoirs Any vehicle, piping or reservoir used in the processing of water from its source to the bottling facilities, should be made of inert material such as ceramic and stainless steel

Water from the source to processing unit may be transported through pipes. Piping used should preferably be of SS. However, food grade plastics or GI may also be permitted. Rubber pipe should not be permitted. Reservoir should preferably be of SS. In case

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which prevent any deterioration, be it by water, handling, servicing or by disinfection; it should allow easy cleaning.

of plastic reservoir, inside layer should be of food grade plastic (certificate may be collected). Cemented (underground/ overground) reservoir should be properly tiled from inside.

B-4.2 Maintenance of Vehicles and Reservoirs Any vehicle or reservoir should be properly cleaned and, if necessary, disinfected and kept in good repair so as not to present any danger of contamination to drinking water and of deterioration of its quality.

The design of reservoir should be such as to enable easy cleaning or disinfection and it should be properly maintained throughout the operation of licence.

B-5 ESTABLISHMENT FOR PROCESSING OF DRINKING WATER – DESIGN AND FACILITIES B-5.1 Location Establishments should be located in areas which are free from objectionable odours, smoke, dust or other contaminants and are not subject to flooding.

The unit should not be in low lying area to avoid collection of dust, contaminant, rain and flood water. Factories in open area/ field should have its proper boundaries with controlled access.

B-5.2 Roadways and Areas Used by Wheeled Traffic Such roadways and areas serving the establishment which are within its boundaries or in its immediate vicinity should have a hard paved surface suitable for wheeled traffic. There should be adequate drainage and provision should be made for protection of the extraction area.

Areas in front of main entry to the unit and immediate surroundings should be paved (pucca) or properly grassed to prevent dust contamination due to vehicular traffic.

B-5.3 Buildings and Facilities B-5.3.1 Type of construction Buildings and facilities should be of sound construction and maintained in good repair.

Buildings should be sound pucca construction, preferably plastered and properly painted/ white washed. Internal partitions made of plastic may be accepted.

B-5.3.2 Disposition of Holding Facilities Rooms for recreation, for storing or packaging of water and areas for cleaning of containers to be reused should be apart from the bottling areas to prevent the end products from being contaminated. Raw materials and packaging materials and any other materials which come into contact with drinking water should be stored apart from other material.

The manufacturing area should not be permitted for general residence or recreation purposes. In case of any duty quarters for workers/ residential area, the same should be reasonably away from the plant and clearly demarcated and maintained. Area for cleaning of reusable containers, packaging material and storage of finished water should be separate from processing/ filling area. All types of packaging materials should be stored in a separate room/ area.

B-5.3.3 Adequate working space should be provided to allow for satisfactory

Sufficient space should be available for easy movement in different operations of

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performance of all operations. manufacturing. B-5.3.4 The design should be such as to permit easy and adequate cleaning and to facilitate proper supervision of hygiene for drinking water.

B-5.3.5 The buildings and facilities should be designed to provide separation by partition, location or other effective means between those operations which may cause cross-contamination.

There should not be any other activity except production and packing of water. In case similar products like cold drink/ beverages/ soda are also manufactured in the same premises, these activities should be clearly and entirely separated from water manufacturing and packing facilities. However, for such food items manufacturing, use of processed water through a separate pipe line and separate plant and machinery may be permitted. There should be proper separation between different processing activities like blowing of bottles/ storage of containers: cleaning of reusable containers: raw water storage tank: filtration (ROs/Micron) disinfection and filling. Exhaust of laboratory should not open in processing/ filling area.

B-5.3.6 Buildings and facilities should be designed to facilitate hygienic operations by means of a regulated flow in the process from the arrival of the drinking water at the premises to the finished product, and should provide for appropriate conditions for the process and the product.

As far as possible the flow of air should be from filling room to the outer area and not the other way round.

B-5.3.7 Drinking Water Handling, Storing and Bottling Areas B-5.3.7.1 Floors Where appropriate, should be of water-proof, non-absorbent, washable, non-slip and non-toxic materials, without crevices, and should be easy to clean and disinfect. Where appropriate, floors should have sufficient slope for liquids to drain to trapped outlet.

The flooring should be smooth, without any cracks/ broken surfaces. Joints shall be properly filled and smooth. The slope of the flooring in processing and filling area should be such as to avoid any stagnation of water. The inside drains, if kept open, should be properly tiled for easy and effective cleaning. Drains should always be in clean condition and provided with traps to prevent the entries of rats/ pests.

B-5.3.7.2 Walls Where appropriate, should be of water proof, non-absorbent, washable and non-toxic materials and should be light coloured. Up to a height appropriate for the operation they should be smooth and without crevices,

In case of cemented walls, tiles upto height of about 5 to 8 feet from floor level should be provided. Wall made of smooth plastic material may be accepted.

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and should be easy to clean and disinfect. Where appropriate, angles between walls, between walls and floors and between walls and ceilings should be sealed and smoothen to facilitate cleaning. B-5.3.7.3 Ceilings Should be so designed, constructed and finished as to prevent the accumulation of dirt and minimize, condensation, mould growth and flaking, and should be easy to clean.

Ceiling should preferably be pucca cemented and smooth. However, factories with tin/ aluminum/ asbestos shed should have proper smooth false ceiling made of non absorbent material (like plastic). Wood or similar material should not be used as it may attract fungal/ mould growth.

B-5.3.7.4 Windows Windows and other openings should be so constructed as to avoid accumulation of dirt and those which open should be fitted with screens. Screens should be easily movable and cleaning and kept in good repair. Internal window sills should be sloped to prevent use as shelves.

Open windows should not be permitted. Windows shall be provided with net screens which are easily cleanable and moveable. Fittings shall be so intact as to prevent entry of mosquitoes/ flies.

B-5.3.7.5 Doors Should have smooth, non-absorbent surfaces and, where appropriate, be self-closing and close fitting type.

Each door should have door closure. Air curtains should preferably be provided at different entries including all inlets and outlets of filling room. The surface of doors should be of non absorbent material.

B-5.3.7.6 Stairs, lift cages and auxiliary structures Platforms, ladders, chutes, should be so situated and constructed as not to cause contamination to drinking water. Chutes should be constructed with provision of inspection and cleaning hatches.

All stairs, lifts, chutes and ladders should be of sound construction and properly painted.

B-5.3.7.7 Piping Piping for drinking water lines should be independent of non-potable water.

Different colour coding should be provided so as to easily distinguish between different pipe lines. The pipe line meant for potable water should preferably be green in colour. The entire pipe line for production water including joints after RO shall be made of stainless steel. The joints should preferably be of dairy fitting type.

B-5.3.8 In drinking water handling areas all overhead structures and fittings should be installed in such a manner as to avoid contamination directly or indirectly of drinking water and raw materials by condensation and drip and should not

In case false ceiling is provided, care should be taken to periodically clean the same and it should be ensured that ceiling is perfect (without any breakage/ seepage) at all times.

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hamper cleaning operations. They should be insulated where appropriate and be so designed and finished as to prevent the accumulation of dirt and to minimize condensation, mould growth and flaking. They should be easy to clean. B-5.3.9 Living quarters, toilets and areas where animals are kept should be completely separated and should not open directly on to drinking water handling areas.

B-5.3.10 Where appropriate, establishments should be so designed that access can be controlled.

Entry to different water processing area should be controlled in such a way that only the authorized persons have the access.

B-5.3.11 The use of material which cannot be adequately cleaned and disinfected, such as, wood, should be avoided unless its use would not be a source of contamination.

Wood in any form should not be used in processing and filling area.

B-5.3.12 Canalization, Drainage Lines Canalization and drainage and used water lines should be built and maintained in such a manner as not to present any risk whatsoever of polluting the underground water source. .

The drainage line of plant should have proper slope and should be made of material which facilitate easy cleaning. There should not be any stagnation of water/ effluent. The main drainage line of the plant should be of sound structure, fully covered and should open outside the plant only, away from underground water source.

B-5.3.13 Fuel Storage Area Any storage area for the storing of fuels, such as, coal or hydrocarbons should be designed, protected, controlled and maintained in such a manner as not to present a risk of pollution during the storage and manipulation of these fuels.

B-5.4 Hygienic Facilities B-5.4.1 Water Supply B-5.4.1.1 Ample supply of potable water under adequate pressure and of suitable temperature should be available with adequate facilities for its storage, where necessary, and distribution with adequate protection against contamination. The potable water should conform to IS 10500.

Conformity of raw water is for guidance only. It should be ensured that the source of raw water (potable) remains uniform. The use of raw water from different sources shall not be done unless permitted (see Section 5 of the manual). However in case of change of source, provisions of STI shall be followed. In order to monitor the uniform supply of raw water, testing of the same should be carried out as per the frequency prescribed in STI and records be maintained.

B-5.4.1.2 Potable water, non-potable water See Explanatory notes against Cl. B-5.3.7.7

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for steam production or for refrigeration or for any other use should be carried in separate lines with no cross connection between them and without any chance of back siphonage. It would be desirable that these lines be identified by different colours. B-5.4.2 Effluent and Waste Disposal Establishments should have an efficient effluent and waste disposal system which should at all times be maintained in good order and repair. All effluent lines (including sewer system) should be large enough to carry the full loads and should be so constructed as to avoid contamination of potable water supplies.

Pipe line carrying the effluent and waste should preferably be of red in colour.

B-5.4.3 Changing Facilities and Toilets Adequate, suitable and conveniently located changing facilities and toilets should be provided in all establishments. Toilets should be so designed as to ensure hygienic removal of waste matter. These areas should be well lighted, ventilated and should not open directly on to drinking water handling areas. Hand washing facilities with warm or hot and cold water, a suitable hand-cleaning preparation, and with suitable hygienic means of drying hands, should be provided adjacent to toilets and in such a position that the employee will have to use them when returning to the processing area. Where hot and cold water are available mixing taps should be provided. Where paper towels are used, a sufficient number of dispensers and receptacles should be provided near each washing facility. Care should be taken that these receptacles for used paper towels are regularly emptied. Taps of a non-hand operatable type are desirable. Notices should be posted directing personnel to wash their hands after using the toilets.

Entrance to the production unit should be through change room. Change room should have hand washing facilities (with hot and cold water) wash basin, foot cleaning and drying facilities. Protective clothing, footwear and head gear should be changed inside the change room only. The protective clothings should be taken out as and when workers go out of the production hall, so as to prevent any contamination of the same. Toilets should be provided for workers and should always be kept clean. These should be properly separated from water handling areas. Toilets should be made of pucca structured preferably tiled with proper doors and water facilities. Hand and foot washing facilities should be provided adjacent to toilets. Notices giving instructions for hand and foot washing after using toilets (in local languages) should be pasted at proper places.

B-5.4.4 Hand Washing Facilities in Processing Area Adequate and conveniently located facilities for hand washing and drying should be

See explanatory notes against Cl. No. B-5.4.3

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provided wherever the process demands. Where appropriate facilities for hand disinfection should also be provided. Warm or hot and cold water should be available and taps for mixing the two should be provided. There should be suitable hygienic means of drying hands. Where paper towels are used, a sufficient number of dispensers and receptacles should be provided adjacent to each washing facility. Taps of a non-hand operatable type are desirable. The facilities should be furnished with properly trapped waste pipes leading to drains. B-5.4.5 Disinfection Facilities Where appropriate, adequate facilities for cleaning and disinfection of equipment should be provided. These facilities should be constructed of corrosion resistant materials, capable of being easily cleaned, and should be fitted with suitable means of supplying hot and cold water in sufficient quantities.

Disinfection of pipe lines and process equipments should preferably be done before commencement of production.

B-5.4.6 Lighting Adequate lighting should be provided throughout the establishment. Where appropriate, the lighting should not alter colours and the intensity should not be less than: 540 lux (50 foot candles) at all inspection points, 220 lux (20 foot candles) in work rooms, and 110 lux (10 foot candles) in other areas. Suspended light bulbs and fixtures in any stage of production should be of a safer type and protected to prevent contamination of drinking water in case of breakage.

Intensity of light is given only for guidance. However the IO should judge the adequacy of light intensity required for carrying out various activities. Suspended light bulbs and fixtures should be protected by providing suitable covers.

B-5.4.7 Ventilation Adequate ventilation should be provided to prevent excessive heat, steam condensation and dust and to remove contaminated air. The direction of the air flow should never be from a dirty area to a clean area. Ventilation openings should be provided with a screen or other protecting enclosure

Exhaust openings should be covered with wiremesh or with suitable flaps. Air curtains should be fitted in such a way that air should not flow towards water filling room/ area.

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of non-corrodible material. Screens should be easily removable for cleaning. B-5.4.8 Facilities for Storage of Waste and Inedible Material Facilities should be provided for the storage of waste and inedible material prior to removal from the establishment. These facilities should be designed to prevent access to waste or inedible material by pests and to avoid contamination of drinking water; equipment, buildings or roadways on the premises.

Facilities for storage of waste and inedible material should be outside the processing plant and finished product storage area.

B-5.5 Equipments and Utensils B-5.5.1 Materials All equipment and utensils used in drinking water handling areas and which may contact the drinking water should be made of material which does not transmit toxic substances, odour or taste, is non-absorbent, is resistant to corrosion and is capable of withstanding repeated cleaning and disinfection. Surfaces should be smooth and free from pits and crevices. The use of wood and other materials which cannot be adequately cleaned and disinfected should be avoided except when their use would not be a source of contamination.

B-5.5.2. Hygienic Design, Construction and Installation B-5.5.2.1 All equipment and utensils should be so designed and constructed as to prevent hazards and permit easy and thorough cleaning and disinfection.

B-6 ESTABLISHMENT B-6.1 Maintenance The buildings, equipments, utensils and all other physical facilities of the establishment, including drains, should be maintained in good repair and in an orderly condition.

B-6.2 Cleaning and Disinfection B-6.2.1 To prevent contamination of drinking water, all equipment and utensils should be cleaned as frequently as necessary and disinfected whenever circumstances demand.

All equipments and utensils should be cleaned and preferably disinfected, every day before commencement of production.

B-6.2.2 Adequate precautions should be See explanatory note as given in B-5.4.5

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taken to prevent drinking water from being contaminated during cleaning or disinfection of rooms, equipment or utensils, by wash water and detergents or by disinfectants and their solutions. Detergents and disinfectants should be suitable for the purpose intended. Any residues of these agents on a surface which with may come in contact with drinking water should be removed by thorough rinsing with water, before the area or equipment is again used for handling drinking water. B-6.2.3 Either immediately after cessation of work for the day or at such other times as may be appropriate, floors, including drains, auxiliary structures and walls of water handling areas should be thoroughly cleaned.

B-6.2.4 Changing facilities and toilets should be kept clean at all times

Changing facilities like aprons, headgears, mask etc. should be available in sufficient numbers to meet daily and contingency requirement.

B-6.2.5 Roadways and yards in the immediate vicinity of and serving the premises should be kept clean.

The area surrounding the unit may be grassed to prevent entry of dirt and dust in the plant. Construction of wall of adequate height (approximate 8 feet) is required when the immediate surrounding is not in the control of the unit.

B-6.3 Hygiene Control Programme A permanent cleaning and disinfection should be drawn up for establishment to ensure that all areas are appropriately cleaned and that critical areas, equipment and material are designated for special attention. An individual, who should preferably be a permanent member of the staff of the establishment and whose duties should be independent of production, should be appointed to be responsible for the cleanliness of the establishment. He should have a thorough understanding of the significance of contamination and the hazards involved. All cleaning personnel should be well-trained in cleaning techniques.

The hygiene control programme should cover all aspects. An elaborate hygiene control plan should be drawn for monitoring the hygienic conditions of the plant and personnel. The plan should invariably include the following: Hygiene requirement Frequency Name of the person directly responsible for supervision The above plan should be monitored by a designated person who has thorough understanding of significance of contaminants and hazards. The hygiene control schedule should be properly displayed at different points like

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processing/ filling/ storage. B-6.4 Storage and Disposal of Waste Waste material should be handled in such a manner as to avoid contamination of drinking water. Care should be taken to prevent access to waste by pests. Waste should be removed from the water handling and other working areas as often as necessary and at least daily. Immediately after disposal of the waste, receptacles used for storage and any equipment which has come into contact with the waste should be cleaned and disinfected. The waste storage area should also be cleaned and disinfected.

See explanatory notes as given in Cl. B-5.4.2

B-6.5 Exclusion of Animals Animals that are uncontrolled or that could be a hazard to health should be excluded from establishments.

No animal should be allowed inside the plant area. If any stray intrusion of pest like lizard, flies are found, immediate action shall be taken to remove them and further necessary preventive measures shall be taken.

B-6.6 Pest Control B-6.6.1 There should be an effective and continuous programme for the control of pests. Establishments and surrounding area should be regularly examined for evidence of infestation.

Pest control measures should preferably be got done through professional agencies with clear indication of validity period, through a certificate for the same. Fly catchers should be provided in processing/ filling area.

B-6.6.2 If pests gain entrance to the establishment, eradication measures should be instituted. Control measures involving treatment with chemical, physical or biological agents should only be undertaken by or under direct supervision of personnel who have a thorough understanding of the potential hazards to health resulting from the use of these agents, including those hazards which may arise from residues retained in the drinking water.

Pesticides designated safe for use in food industry should only be used under direct supervision of trained personnel.

B-6.6.3 Pesticides should only be used if other precautionary measures cannot be used effectively. Before pesticides are applied, care should be taken to safeguard drinking water, equipment and utensils from contamination. After application, contaminated equipment and utensils should be thoroughly cleaned to remove residues prior to be used again.

See explanatory note as given in Cl. B—6.6.2

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B-6.7 Storage of Hazardous Substances B-6.7.1 Pesticides or other substances which may present a hazard to health should be suitably labeled with a warning about their toxicity and use. They should be stored in locked rooms or cabinets, and dispersed and handled only by authorized and properly trained personnel or by persons under strict supervision of trained personnel. Extreme care should be taken to avoid contamination.

B-6.7.2 Except when necessary for hygienic or processing purposes, no substance which could contaminate drinking water should be used or stored in drinking water handling areas.

B-6.8 Personal Effects and Clothing Personal effects and clothing should not be deposited in drinking water handling areas.

Protective clothing should not be permitted to be taken out beyond change room. Separate cabinets for storage of personal belongings should preferably be provided.

B-7 Personnel; Hygiene and Health Requirements. B-7.1 Hygiene Training Managers of establishments should arrange for adequate and continuing training of all water handlers in hygienic handling of water and in personal hygiene so that they understand the precautions necessary to prevent contamination of drinking water.

B-7.2 Medical Examination Persons who come into contact with drinking water in the course of their work should have a medical examination prior to employment, if the official agency having jurisdiction acting on medical advice, considers that this is necessary, whether because of epidemiological considerations or the medical history of the prospective water handler. Medical examination of water handlers should be periodically carried out and when clinically or epidemiologically indicated.

Medical examination of all workers, testing personnel and supervisors should be got done at least once in a year or as and when required. In case any new worker joins, his fitness with respect to freedom from communicable diseases should be first medically examined before permitting work in water processing area.

B-7.3 Communicable Diseases The management should take care to ensure that no person, whether known or suspected to be suffering from, or to be a carrier of a

Medical examination report should clearly indicate that the workers are free from any communicable diseases.

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disease likely to be transmitted or afflicted with infected wounds, skin infections, sores or diarrhea, is permitted to work in any drinking water handling area in any capacity in which there is any likelihood of such a person directly or indirectly contaminating drinking water with pathogenic micro-organisms. Any person so affected should immediately report to the management. B-7.4 Injuries Any person who has a cut or wound should not continue to handle drinking water or contact surfaces until the injury is completely protected with a waterproof covering which is firmly secured and which is conspicuous in colour. Adequate first-aid facilities should be provided for this purpose.

Availability of first aid box should be ensured.

B-7.5 Washing of Hands Every person, while on duty in a drinking water handling area, should wash the hands frequently and thoroughly with a suitable hand cleaning preparation under running warm water. Hands should always be washed before commencing work, immediately after using the toilet, after handling contaminated material and whenever necessary. After handling any material which might be capable of transmitting disease, hands should be washed and disinfected immediately. Notices requiring hand-washing should be displayed. There should be adequate supervision to ensure compliance with this requirement.

Foot operated or photo sensitive taps may preferably be used.

B-7.6 Personal Cleanliness Every person engaged in a drinking water handling area should maintain a high degree of personal cleanliness while on duty and should, at all times while so engaged, wear suitable protective clothing including head covering and footwear, all of which should be cleanable, unless designed to be disposed off and should be maintained in a clean condition consistent with the nature of the work in which the person is engaged.

Wearing of protective clothing should be ensured when the plant is in operation.

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Aprons and similar items should not be washed on the floor. When drinking water is manipulated by hand, any jewellery that cannot be adequately disinfected should be removed from the hands. Personnel should not wear any insecure jewellery when engaged in handling drinking water. B-7.7 Personal Behaviour Any behavior which could result in contamination of drinking water, such as eating, use of tobacco, chewing (for example, gum, sticks, betel nuts, etc.) or unhygienic practices, such as, spitting, should be prohibited in drinking water handling areas.

Proper notices in this regard should be displayed in local languages at appropriate places.

B-7.8 Visitors Precautions should be taken to prevent visitors as far as possible from visiting the drinking water handling areas. If unavoidable, the visitors should observe the provisions of B-6.8 and B-7.3

General visitors should be prohibited for entering into processing area.

B-7.9 Supervision Responsible for ensuring compliance by all personnel with the requirements of B-6.1 to B-6.8 and the responsibility should be specifically allocated to competent supervisory personnel.

Hygiene supervisor should be other than the one responsible for production. However, the overall supervision for requirements of B-6.1 to B-6.8 may be done by a senior person irrespective of actual work area.

B-8 ESTABLISHMENT: HYGIENIC PROCESSING REQUIREMENTS B-8.1 Raw material Requirements To guarantee a good and stable quality of drinking water, the quality criteria should be monitored regularly.

See explanatory note given in Cl. B-5.4.1.1

B-8.2 Should there be a perceptible lacking in meeting the requirements, necessary corrective measures are immediately to be taken.

B-8.3 Treatment The treatment may include decantation, filtration, combination filtration (for example, membrane filters, depth filters, cartridge filters, activated carbon), demineralization, reverse osmosis, aeration, and disinfection.

IO should specifically report the type of processes adopted by the firm for production and disinfection.. Any subsequent change in the process should be positively informed to BIS for action (see Section 5 of Manual)

B-8.3.1 Processing should be supervised by technically competent personnel.

B-8.3.2 All steps in the production process, The water processed in a day should be filled/

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including packaging, should be performed without unnecessary delay and under conditions which will prevent the possibility of contamination, deterioration, or the growth of pathogenic and spoilage micro-organisms.

packed on the same day. The left out processed water should be either drained or reprocessed (on the subsequent day).

B-8.3.3 Rough treatment of containers should be avoided to prevent the possibility of contamination of the processed product.

Reusable containers where transparency or shape is impaired because of repeated use, should be rejected.

B-8.3.4 Treatment are necessary controls and should be such as to protect against contamination or development of a public health hazard and against deterioration within the limits of good commercial practice.

B-8.4 Packaging Material and Containers B-8.4.1 All packaging materials should be stored in a clean and hygienic manner. The material should be appropriate for the product to be packed and for the expected conditions of storage and should not transmit to the product objectionable substances beyond the limits specified. The packaging material should be sound and should provide appropriate protection from contamination. Only packaging material required for immediate use should be kept in the packing or filling area.

Separate stores should be available for packaging material, finished products and other items. Containers/ bottles received or blown by the firm should preferably be stored in a closed mouth polybag/ caps to avoid any contamination.

B-8.4.2 Product containers should not have been used for any purpose that may lead to contamination of the product. In case of new containers if there is a possibility that they have been contaminated, they should be cleaned and disinfected. When chemicals are used for these purposes, the container should be rinsed. Containers should be well drained after rinsing. Used and, when necessary; unused containers should be inspected immediately before filling.

The reusable containers and caps should be cleaned, disinfected, washed and jet rinsed (with processed water) before filling. Various options are available for disinfection like use of chlorinated water (using hypochlorite), food grade detergents like Ranocide etc. However, use of disinfectants (one or a combination) should be left to the discretion of the manufacturer. Due care should be taken that no residue of disinfectant is left in the pipeline/ container.

B-8.5 Filling and Sealing of Containers B-8.5.1 Packaging should be done under conditions that preclude the introduction of contaminants in the product.

Filling room should be regularly disinfected. For this purpose, various options may be assessed such as use of UV light, filling under sterile positive pressure etc. However, selection of disinfectant should be left at the discretion of

34

manufacturer. Air conditioner may also be provided in the filling room, if required in view of ventilation/ environmental conditions of the area.

B-8.5.2 The methods, equipment and material used for sealing should guarantee a tight and impervious sealing and should not damage the containers nor deteriorate the physical, chemical, microbiological and organoleptic qualities of drinking water.

To ensure tight and impervious sealing, the shrinkable sleeve may be used on caps and the container may be held upside down to check for any leakage. The above method is suggestive. However, any other suitable method may be used. The container should be visually inspected for any suspended particle etc. against an illuminated screen.

B-8.6 Packaging of Containers The packaging of containers should protect the latter from contamination and damage and allow appropriate handling and storing.

The reusable containers may preferably be wrapped in a plastic (polyethylene) film/ bag to avoid any damage/ transparency to the container. Every time new polyethylene cover should be used.

B-8.7 Lot Identification Each container shall be permanently marked with code to identify the producing factory and the lot. A lot is quantity of drinking water produced under identical conditions, all packages of which should bear a lot number that identifies the production during a particular time, interval and usually from a particular ‘processing line’ or other processing unit.

The date of manufacturing should be clearly indicated on the container itself, in one straight line instead of any other combination which may not be consumer friendly. Writing of batch No. in place of manufacturing date should not be practiced unless it is declared that batch number and manufacturing date are the same.

B-8.8 Processing and Production Records Permanent, legible and dated records of pertinent processing and production details should be kept concerning each lot. These records should be retained for a period that exceeds the shelf life of the product or longer if required. Records should also be kept of the initial distribution by lot.

Batch wise records of production and dispatch for each type of container should be maintained separately.

B-8.9 Product Durability Product durability shall be declared on the container as per 7.1 (g). It shall be based on in-house shelf life study and proper checks and records be maintained for the conformity of the declared product durability.

Product durability should not be less than one month. Each type of container should be subjected for durability assessment and based on the study conducted by the manufacturer, the shelf life should be declared. Records of the same should be maintained and may be verified by IO. Decision about the type of study should be left

35

with the manufacturer. Durability study should be reassessed by the licensee at least once in a year for each type of container.

B-8.10 Storage and Transport of the End-Product The end-product should be stored and transported under such conditions as will preclude contamination with and/or proliferation of micro-organisms and protect against deterioration of the product or damage to the container. During storage, periodic inspection of the end-product should take place to ensure that only drinking water which is fit for human consumption is dispatched and that the end-product specifications are complied with.

The finished product should not be stored under direct sun light. Manufacturer should invariably exercise to inspect the end product available in distribution chain to ensure its compliance to the specification. This may be done either directly or through proper arrangements with their dealer/ distributor. Manufacturer should provide proper training to the distributor/ marketer for its proper storage and distribution. Manufacturer is liable for the product quality till it reaches the consumer.

7. USEFUL TIPS FOR INSPECTING PERSONNEL 7.1 To verify the actual factory layout. The layout should clearly indicate the different locations preferably including the following: a) Bore well or entry point for the source of raw water, pipeline etc. b) Raw water storage facility c) Plant for the manufacture of the product (with various stages) d) Filling/packing areas, change room, toilet(s), loading/unloading points e) Entry/exit with indications of double door/door closures/Air curtains wherever provided

f) Stores for packaging material and finished product g) Laboratory h) Actual boundary/perimeter of the establishment i) If the premises are also used for residential quarters/other purposes, then specific mention of the

same be made with identified locations. 7.2 As product is under mandatory certification, it is unlikely to be in “production” during PI. It is therefore essential to get some production & filling/packing done during the visit and then make comments on the firm’s capability for the same.

36

7.3 It should be clearly reported in the PIR as to whether the filling/packaging adopted are manually operated or automatic. It may be noted that the plastic cups, tumbler, pouch are required to be filled only through automatic machine. 7.4 Sample be got tested in factory for some requirements possible to be tested, with purpose of verifying manufacturing capability (process controls), competence of the QC personnel and working conditions of test equipment. 7.5 For sample drawn for independent testing, requirement of Description, Odour & Taste should be tested and reported in PIR, as these are subjective tests. 7.6 Shelf-Life (“Best Before”) Period should be clearly indicated on the test request. 7.7 STI requires holding material till such time the test results for Each Control Unit are known. However in case of microbiological parameters each batch of Packaged drinking water is required to be held for 48 hours so as to ensure that it conforms to all the microbiological parameters applicable for each control unit except for the tests of aerobic microbial count at 210 C and yeast and mould, which shall be reviewed for conformity on availability of their test reports after 72 hours and 5 days respectively.Therefore it is important to assess the firm’s installed production capacity as well as capability to “store” the product. Accordingly both the production capacity and storage facility need to be reported. 7.8 Hygienic conditions need to be assessed as per every clause of Annex B of ISS. Declarations made by the firm with respect to medical examination, Pest Control, Hygiene Schedule, Supervisor designated for Hygiene maintenance, Overall Supervision, Criteria devised for assessing product durability etc. be verified and reported.All aspects related to reusable containers, availability of arrangements for washing, cleaning (outer surface), disinfection and rinsing be also verified and reported. 7.9 Sample size for Testing of Packaged Drinking Water for Independent Testing 7.9.1 For all requirements except radio-active residues Approximate 18 litre quantity is adequate if the samples are supplied in 2 litre or smaller containers but in case the samples are available in large size packages, minimum two packages are required as microbiological lab needs separate sample for ensuring aseptic handling. For example:

Capacity of bottle/Jar in litres

Numbers to be drawn

1 18 2 9 5 4 10 2 20 2 24 2

37

7.9.2 For Radio-active residues Approximate 10 litre quantity: one carton of bottles (containing 12 bottles/ cups) or one jar (of 10 litres and above) is adequate. 7.10 Guidelines for Reused Containers Licensees are required to ensure use of only such jars whose transparency continues to meet the minimum requirements of 85% as per IS 15410 even after its repeated use. BO may draw sample of reusable container for ascertaining continued suitability over a period of time by getting the same tested for transparency requirement. Every market sample of processed water filled in reusable jar shall be got tested for transparency requirement also as per IS 15410. Jars which get deshaped and mutilated during the course of use shall not be permitted. Licensees may be advised in this regard strictly. Further action may be taken as per OMPC. .

38

ANNEX 1 (Clause Ref. 4.2)

CHECK LIST FOR SCRUTINY OF APPLICATION

PACKAGED DRINKING WATER (IS 14543) & PACKAGED NATURAL MINERAL WATER (IS 13428)

A. CHECKPOINTS Complies (Yes/No) 1 Application is submitted with the required Fees 2 Complete Office address & Manufacturing address are given 3 Manufacturing address in various documents is same 4 Composition of Top Management is indicated and tallying with other

documents submitted with application (such as at 1, 6 etc.)

5 Copy of Partnership Deeds, List of Director etc., as applicable 6 Copy of Registration of the firm (if applicable) 7 Documentary evidence submitted for status as Small Scale etc 8 Type, Material and Capacity is clearly indicated 9 Brand Name Declaration a) CM/PF 307 is submitted b) Copies of agreements with Brand owners are submitted (wherever

applicable)

10 Plant Machinery declaration is submitted on CM/PF 305 11 Test Equipment a) Declaration submitted on CM/PF 306 (covering equipment, glassware,

chemicals and media)

b) Least Count, Range and quantity of equipment are as per ISS c) Calibration reports of required equipment are submitted d) Consent letter from approved OSL is submitted for testing of

requirements for which in-house facilities are not available

12 Personnel for Chemical & Microbiological Test a) Whether copies of appointment letters submitted b) Whether qualification of personnel are in order c) Whether copies of qualification certificates submitted 13 Raw Water-Permissible source of raw water is used 14 Details regarding procurement/manufacturing facilities for packing

materials are submitted

15 Details of Manufacturing Process with Treatment for Disinfection and Process Flow Chart are submitted

16 Factory Layout Plan indicating locations of important facilities (source water, processing stages, disinfection, packing, storing, testing etc) is submitted

17 Location and Route Map to factory is submitted 18 Production Figures for previous/current periods (as applicable) 19 Installed Capacity is clearly indicated 20 Acceptance of STI is submitted/ indicated

39

21 Acceptance to pay Marking Fees is submitted/indicated 22 Hygienic Conditions – whether copies of reports submitted for a) compliance to Annex B b) medical examination of concerned staff c) Pest Control Treatment (if got done from outside source 23 Declaration submitted for Shelf-Life of product packed in all

containers

24 Details of previous application/licence provided, as applicable 25 Whether request made for blocking of Licence No. If so, whether Indemnity

Bond submitted

B CHECKPOINTS SPECIFIC TO NORMAL PROCEDURE Complies(Yes/No) 1 Whether date for preliminary inspection is proposed 2 Whether details of samples being offered for inspection (water and

packaging materials) are indicated

C CHECKPOINTS SPECIFIC TO SIMPLIFIED PROCEDURE Complies(Yes/No 1 Whether Self-Evaluation Report submitted 2 Original Test Report for Water & Containers a) Whether the reports submitted are from approved Labs b) Whether the reports are not older than 30 days 3 Whether undertaking for compliance to Labeling Prohibition

submitted

4 Whether undertaking submitted for stoppage of marking in case of failure of verification sample in independent testing

Any other details/comments Recommendations of Dealing Officer

Sign. Dealing Officer

Name Date

Decision of Group Leader

40

CM/PF 201 Sept 1995

ANNEX 2

(Clause Ref. 4.3.1)

BUREAU OF INDIAN STANDARDS REPORT OF PRELIMINARY INSPECTION

Application No. CM/A- IR No.. . . . . . . . .. IS Date of writing IR . . . . . . . Product Type/ Size/Grade/Variety 1. GENERAL INFORMATION

a) Applicant’s Name b) Address: i) Factory ii) Office: c) Date of inspection d) Situation of factory e) Telephone/Fax i) Factory ii) Office

2. Management Staff 3. Person(s) contacted 4. BIS Licences, if any, held by the applicant ________________________________________________________________________ REMARKS OF THE REVIEWING OFFICER (ON IRS, TRS , GENERAL ETC) _____________________________________________________________________________

41

(2)

CM/PF 201 Sept 1995

5. RAWMATERIALS a) Raw Materials Used: Sl. No. Raw Material Name of With or Test How Supplier Without Certificate Received BIS Certi- of the Batches/ fication Supplier Lots Mark Nature of Package ____________________________________________________________________________ b) Arrangement for testing as received c) Details of sampling d) Methods of disposal of sub-standard raw materials e) Record of tests with proforma of records 6. MANUFACTURE a) Type/ Size/Grade/Variety being manufactured at the time of inspection b) Description of the process from raw material to finished product stage ready for dispatch (Also enclose Layout plan of the factory)

42

(3)

CM/PF 201

Sept 1995 c) Intermediate points where control is exercised d) Details of records maintained and control used e) Method(s) of disposal of sub-standard products f) Units of production g) Production per day or per shift h) Details of manufacturing machinery (See proforma PF 305 Annexed) i) Technical comments on the manufacturing capabilities and inprocess controls 7. PACKING AND MARKING a) Nature of packing b) Quantity per package c) Marking on article d) Method of marking (printing, stenciling, embossing etc) e) Form of label(s), if any f) Batch or Code numbering for identification g) In what manner marking differs from the provisions in the Indian Standard Specification

43

(4)

CM/PF 201

Sept 1995 8. LABORATORY AND INSPECTION

a) Details of Staff: Sl. No. Name of Qualification Experience Person ____________________________________________________________________________ b) Competency of testing personnel c) Equipment and other facilities for complete specification testing. Test equipment/chemicals not available d) Accuracy of instruments and arrangements for calibration e) Records maintained in laboratory for routine tests: Sl. No. Requirement/Characteristic Value ____________________________________________________________________________ f) Stage of processing where laboratory reports are made available g) Sampling and testing of end products

44

(5)

CM/PF 201

Sept 1995 9. SAMPLE

a) Source of drawl: stock/production b) Size of lot from which sampled c) Type/ Size/Grade/Variety of the sample d) Details of the counter sample left with the firm e) Manner of packing, labeling, coding and sealing f) How sealed ? Give impression of the seal used g) Laboratory to which dispatched h) Test results on a sample tested in the factory: Requirements Value Value Remarks Tested Obtained Recorded By Firm i) Any further information regarding sample drawn j) Information regarding sample of other type/grade/variety applied for k) Comment in the testing capabilities

45

(6)

CM/PF 201

Sept 1995

10. OTHER INFORMATIONS a) Main buyers and selling price b) Storage facilities c) Hygienic conditions (in case of food products, give complete note as per relevant hygienic code) d) Discussion with the firm on: e) STI and marking fee rate i) The manner of putting the Standard Mark ii) Manner of manufacture and dispatches without Standard Mark in case of stoppage of marking 11. INSPECTION/TESTING CHARGES Collected/Not Collected 12. CONCLUSIONS, RECOMMENDATIONS AND POINTS FOR ACTION Signature: No. of Encl.: Inspected by: (Name) Designation: Station: Date:

46

ANNEX 3 (Clause Ref. 4.3.2)

VERIFICATION REPORT BY BIS INSPECTING OFFICER

(The Inspecting Officer(s) shall give technical comments on manufacturing capability, in process controls, competency of testing personnel and testing capability. Any discrepancy observed during verification at factory shall be conveyed formally through D/V Report) 1. Application No. : 2. Applicant : 3. Address : 4. Date of Visit : 5. IS No. : 6. Product : 7. Person(s) Contacted: 8. VERIFICATIONS S.No.

Aspect Verification Observation *

a Manufacturing Facilities

Applicant’s declaration on PF 305 be verified for completeness and correctness and countersigned

Complete or Incomplete

b Manufacturing process including filling and packing

Applicant’s declaration regarding process, filling and packing be verified for correctness and countersigned

Conforming or Non conforming

c Testing Facilities

Applicant’s declaration on PF 306 be verified for completeness and correctness and countersigned

Complete or Incomplete

d Requirements for which Testing facilities are not available

Copy of consent letter from OSL including each requirement and frequency specified in STI, be obtained and enclosed with this report

Available and complete or not available/incomplete

e Factory Testing Sample be got tested in factory and test report be submitted in format Annex-3A

Sample Pass or Fail

d Competence of Q.C. personnel

Competence be assessed for Microbiological and Chemical testing through factory testing, interview etc.

Q.C competent or Not competent

47

f Hygienic Conditions

Assessment be made as per Annex B of the Indian standard and reported using Annex 4 of this manual duly countersigned by IO and applicant’s Hygiene Incharge .

Satisfactory or Needs improvement

* In case the observations are not satisfactory for any of the aspects and for which actions are required to be taken by the applicant, details be given in D/V Report. 9. SAMPLES FOR INDEPENDENT TESTING a) Details of samples drawn for independent testing be given in the Annex-3 B. Whether left with the applicant for dispatch to Lab or brought to office? 10. ACCEPTANCES & DECLARATIONS BY THE APPLICANT

Whether already submitted

Whether obtained now

S.No. Subject

Yes No Yes * N.A. a Acceptance of STI b Acceptance of Marking Fee c Brand Name Declaration with Copies

of Agreement, if applicable

d Undertaking for stoppage of marking if verification sample fails in independent testing

* Documents which are obtained during verification visit be Annexed with the report, duly marked. 11. ANY OTHER POINT/COMMENT (Give details of verification of other actions taken by applicant on advise rendered by BIS based on scrutiny of application or otherwise asked for, if any) 12. RECOMMENDATIONS 13. POINTS FOR ACTIONS (Give details of all actions required to be taken by the applicant as per deficiencies indicated on the D/V Report)

Signature Name Designation Date

Group Leader

48

ANNEX 3A

FACTORY TESTING REPORT P D water/ P NM Water Manufacturing Date Batch No. (if applicable) Type of Container from which sample drawn Quantity in stock pertaining to above Batch/Mfg. Date S.No.

IS clause Ref.

Requirement Specified Value Observed Value

Result : Pass for the requirements tested or Fail in the requirement(s) …… (strike out whichever is not applicable) Signature Name Designation Chemist Microbiologist Representing (BIS) Firm:

49

ANNEX 3B

SAMPLES FOR INDEPENDENT TESTING

1. Sampling of P D Water or PNM Water a) Source of drawl (Stock/production) b) Size of lot (quantity) from which sample is drawn with details of type/material/Capacity c) Batch No. (if applicable) and Mfg. Date of Water d) Declared shelf-life e) Quantity drawn (indicate no. of packing & capacity) f) Code assigned to the sample (Give separate codes for samples sent to different Labs., such as for chemical & radiological) g) Manner of packing, labeling and sealing h) Tests to be carried out and name of the Lab. where sample is to be tested (Chemical, Physical, Microbiological, Radiological) 2. Sampling of Packaging Material for Water a) Type, Material and Capacity of container(s) b) IS No. and Standard c) Size(s) of lot(s) from which sample(s) drawn d) Quantity drawn (indicate no. of packing & capacity) e) Declared parameters (Width of PE Film, Wall Thickness of plastic container) e) Code assigned to the sample f) Manner of packing, labeling and sealing g) Tests to be carried out and name of the Lab. where sample is to be tested 3. Details of counter samples left with the firm:

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ANNEX 4

(Clause 4.3.4 and 4.3.6) CHECKLIST FOR GOOD HYGIENE PRACTICES AND FOOD SAFETY SYSTEMS FOR PACKAGED NATURAL MINERAL WATER PROCESSING UNITS AS PER CLAUSE 5 OF IS 13428:2005 OR CHECKLIST FOR GOOD HYGIENE PRACTICES AND FOOD SAFETY SYSTEMS FOR PACKAGED DRINKING WATER PROCESSING UNITS AS PER CLAUSE 4, ANNEX C OF IS 14543:2004 (TO BE VERIFIED BY IO DURING PRELIMINARY/VERIFICATION VISIT)

Answers Sl. No.

Requirements Satisf-actory

Unsatisfactory

Remarks (briefly describe how required is met or not )

A Building, Facilities and Locations i) Is the facility located in an area free from

objectionable odour, smoke, dust or other contaminants and not subject to flooding?

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

iii) Is adequate facility for drainage of surroundings available and designed to handle peak load?

iv) 1s the facility used for processing water free from domestic animals?

v) Are the facility surroundings free from refuse, waste materials, rubbish, over grown weeds and grasses?

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

vii) Are the buildings and facilities of sound construction and maintained in good repair?

viii) Are the buildings and facilities designed and maintained to prevent entrance and harboring of pests and entry of contaminants?

ix) Are building and facilities designed to facilitate hygienic operations?

B. Plant and Physical Facilities i) Is adequate lighting provided at working

station, hand washing area, and storage areas?

ii) Is the lighting intensity adequate:1) 540 lux in all inspection area, and 2) 220 lux in work areas and walls

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iii) Are light fixtures safety types and protected to prevent contamination in the event of breakage in the processing and packing area?

iv) 1s adequate ventilation provided in processing areas to minimize odours, noxious fumes and condensates?

v) Are barrier traps provided at drains to prevent the entry of rodents from the drains into the facility?

vi) Is effective screening provided against entry of birds, animals, insects, rodents, etc

vii) Are doors, hatches and other openings to the building constructed in such a way to render opening pest proof? NOTE — Installation of one or more of the following, which effectively prevents pest entry, will meet this requirement: a) Doors self closing type, b) Have air curtains, and c) Have strip curtains.

viii) Are floors, walls, ceilings, windows and doors so designed and constructed as to prevent accumulation of dust, dirt and render them washable?

ix) Is product in process and storage area adequately protected from any leakage from external surfaces and other sources of contamination?

x) Are immediate surroundings of extraction or collection protected from entry of unauthorized persons?

C Raw Water Processing i) In case of extraction /collection for processing

are the sources free from contaminations/ impurities?

ii) Are water storage tanks, pipe lines utilized for handling water constructed and so designed as to facilitate cleaning and inspection?

iii) Are inspections of containers/ carriers/ pipelines of raw water supply performed for the material of construction and cleanliness?

iv) Are possible chances of contamination from incoming water assessed?

v) Are water storage tanks effectively cleaned to prevent entry of pests and potential

52

contaminator? vi) Are the storage tanks periodically cleaned and

records maintained?

vii) Are the processed water contact surfaces regularly cleaned and sanitized?

viii) Are all equipment and utensils so designed and constructed as to prevent hygiene hazards and allow easy cleaning and sanitation?

D Post-Processing Handling i) Are cleaning operations of bottles/containers

so done as to preclude contamination of product and product contact services with residues?

ii) Has absence of residual cleaning chemicals been ensured?

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

iii) Are the primary packing material and containers of food grade conforming to relevant Indian Standards?

iv) Are packing and sealing, where required, monitored?

v) Are containers visually/electronically inspected for their soundness?

vi) Are physical hazards prevented from entering into processed water?

vii) Are glassware excluded from production area?

E Packaging Material and Finished Goods Storage

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

ii) Are packaging material inspected to ensure their suitability?

iii) Are the packing materials especially primary packing material properly stored and properly handled to preclude contamination?

iv) Are packaging material purchased, stored and handled in sanitary manner?

F Finished Product Storage and Distribution i) Is first-in-first out (FIFO) of stored product

maintained?

ii) 1s storage properly sanitized and disinfected periodically?

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iii) Are stores protected from pest infestations?

iv) Are coding and tracking clear and in place? v) Are the instructions clear and in place? vi) Are hold release procedure in place and

product identified?

vii) Are the records maintained for batch number, date and volume of production?

viii) Are transport containers/vehicles maintained in clean condition?

G Customer Handling of Products i) Are the storage instructions provided on

containers?

ii) Is the shelf life period (best before) mentioned on containers 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

are they provided with: 1) Doors of self closing type? 2) Opening directly into processing areas? 3) Hand washing signs provided in appropriate language? 4) Proper lighting and ventilation? 5)Proper maintenance to keep in clean and tidy manner?

ii) Are hand washing facilities provided adequately and conveniently to wash hands, foot, elbow with sensor operated taps?

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

iv) Are notice/instructions prominently pasted in toilet directing employees to wash their hands on entry and re-entry into the food handling areas?

v) Are the refuse receptacles, self closing type, maintained in a manner to protect from

J Personnel Hygiene and Habits i) Is any individual assigned to supervise overall

sanitation of plant and personnel?

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

54

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

iv) Are the personnel with infectious diseases, skin infection and open lesion or any other source of microbial contamination excluded from working in process/packing areas?

v) Are personnel hygiene practices regularly maintained and monitored? 1) Clean outer garments — protective clothing? 2) Personal cleanliness — finger nails? 3) Head cover— hair restraints, caps, head bands, beard cover 4) No tobacco in any form— smoking, chewing 5) No eating at work stations

vi) Are protective clothing stored on the premises and not allowed to be used for outside wear

vii) Are there clear legible notices defining limits of no smoking areas such as “NO SMOKING BEYOND THIS POINT” displayed?

viii) Are personnel imparted regular training or hygienic food handling, processing food and personal hygiene?

ix) Are unsecured jewellery and other objects, such as, wrist watches, cufflinks, ear rings, glass bangles, stick BINDIS removed at work?

CONCLUSION: OVERALL ASSESSMENT OF HYGIENIC CONDITIONS - SATISFACTORY / NOT SATISFACTORY

NAME OF UNIT Signature ………………….…. CM/A.............. Name ..……………

Designation ………………….. Date…………………….

55

ANNEX 5

(Clauses 1.1, 4.3.3)

A TYPICAL MANUFACTURING PROCESS Following treatment steps are involved in the manufacturing process for packaged drinking water: Raw Water →Raw Water Storage Tank→ Raw Water Feed Pump→ dosing system 1 & 2→ Pressure Sand Filter→ Activated Carbon Filter → Micron Cartridge Filter High Pressure Pump→ Reverse Osmosis→ Ozone generator and re circulation → Finished Water Storage → U.V System → Filling and Packing → Visual Examination →Storage for testing → Forwarding. 1) DOSING SYSTEM 1 & 2 - The water is drawn from Bore Well or any source and collected in

storage tank. It then goes to dosing system through raw water feed pump with use of antiscalant for softening the water.

2) PRESSURE SAND FILTER - From softener, the water is transferred to pressure sand filter for removing the impurities.

3) ACTIVATED CARBON FILTER - The water is then passed through activated carbon filter to

remove organic impurities. 4) MICRON CARTRIDGE FILTER (MCF) - Water is then passed through a micron filter or a

series of such filters (0.1 – 0.5 u) for removal of fine particles. 5) DEMINERALISATION BY REVERSE OSMOSIS SYSTEM (R.O.) - Water from MCF goes

to R.O. System through High Pressure Pump. R.O. removes 90-95% of dissolved solids. The finished water is passed into Storage Tank through SS/ inert pipe line.

6) OZONE GENERATOR WITH RE-CIRCUALTION - Finished water from R.O. system is

stored in S.S storage tank. The tank is provided with a Man Hole so that the tank can be cleaned. This tank is used as ozone circulation tank. The ozone is passed to this tank for disinfection.

7) U.V. SYSTEM - Water from S.S. tank is passed through MCF to U.V. disinfection system,

where the bacteria are inactivated. 8) FILLING AND PACKING - Water is then filled in cleaned and rinsed containers. 9) VISUAL EXAMINATION - Containers are visually inspected for any leakage and suspended

matter against illuminated screen. 10) TESTING - The raw water is tested once in three months. Finished water is tested as per

scheme of testing prescribed by BIS.

56

A TYPICAL PROCESS FLOW CHART

RAW WATER EXTRACTION THROUGH BORE WELL ↓

RAW WATER STORAGE TESTING

CHLORINE DOSING ↓

FILTRATION THROUGH SAND BED ↓

FILTRATION THROUGH ACTIVATED CARBON BED ↓

MICRON CARTRIDGES FILTRATION ↓

FEEDING BY HIGH PRESSURE PUMP ↓ ANTISCALANT DOSING

REVERSE OSMOSIS ↓

RO OUTPUT OZONE INJECTION WITH ↓ RE-CIRCULATION

U.V. SYSTEM ↓

FINAL PRODUCT STORAGE

FILLING AND PACKING ↓

PRODUCT TESTING ↓

DESPATCH

57

A TYPICAL CIP PROCESS

Sanitization and Sterilization is done daily before resuming production

SANITIZATION

1. Take sufficient quantity of soft water in CIP tank. 2. Add required quantity Sodium Hypochlorite solution in CIP tank containing soft water. 3. Now start CIP pump. 4. Let the chlorine solution go into tank through CIP line. 5. Solution will go from top through CIP volume which distributes solution in entire tank. 6. Check the available chlorine. 7. Chlorine (free) should be 10-15 PPM. 8. If percentage of chlorine is less then add more Sodium Hypochlorite solution till required strength

of chlorine is achieved in water. 9. Start feed pump and pass solution through sand filter, (bypassing carbon filter since it removes

chlorine), all micron filters, Ozone contact column etc. and filling machine. 10. Hold this solution at least for 30 minutes which can be extended to overnight. 11. Drain out the solution from the whole system. 12. Take fresh water and remove the chlorine of storage tank. 13. After removing chlorine traces from storage tank, fill with fresh bore well water. 14. Remove the chlorine traces from each points upto filling machine by flushing with fresh water. 15. Check for residual chlorine. 16. Do final washing with product water.

STERLIZATION

1. Produce soft water by softener 2. Generate steam by boiler using soft water. 3. Supply steam in storage tanks, bore well line and pipe lines upto filling machine. 4. Continue the steam supply in tanks till attains required temperature. 5. Continue the steam supply to filling machine till steam comes out from all rinsing and filling

nozzle of machines. 6. Stop steam supply and disconnect the hose pipe. 7. Rinse the whole system with product water.

58

TYPICAL CLEANING AND WASHING SYSTEM OF RE-USABLE JARS The process of cleaning and washing of re-usable jars is as follows:-

1. Check the jars for crack, contamination and foul odors. Reject jars not fit for re-use.

2. Wash the outside of jars thoroughly with detergent solution and normal water.

3. After outer cleaning, wash jars internally with food grade detergents (like iodine based) and then thoroughly wash till free of last traces of detergent.

4. Send clean jars to filling station.

5. Rinse jars internally with product water, before final filling at filling station.

59

ANNEX 6

(Clause 4.10)

CHECK LIST FOR RED FORM OF PACKAGED DRINKING WATER (IS 14543) and NATURAL MINERAL WATER (IS 13428)

ITEM CHECK POINT DOCUMENT

No. (Tick) REMARKS

Address Same address given in Application Form, PIR, RF and Other Documents

1 1 (a) etc.

Verify in application. Plot Purchase/ Rent agreement or lease agreement etc.

Authorized Person Authority Letter (In case application and other documents are signed by person other than Proprietor/Partner/ Director of the applicant)

2

Status of Unit Manufacturing status is clearly stated as large/small scale in order to give concession in marking fee.

3 SSI Certificate/Chartered Accountant/ Certificate from any other agency.

STI Acceptance of STI is for the latest version

4 Should not be signed on blank proforma

Marking fee Acceptance of applicable Marking Fee with complete details

5 Should not be signed on blank proforma

Brand Name(s) Proforma CM/PF 307 Agreement with Brand Owner, if applicable

6 6 (a) 6 (b) etc.

Enclose copies as applicable, for each brand

Test Reports Reports for Water cover all the requirements for

Physical/ Chemical Tests Microbiological Test Pesticides Residues Radio Active Residues

Packaging material report for the relevant type, material and capacity

7 7 (a) 7(b) 7 (c) etc.

Reports of all samples to be attached, i.e., including those of failures, if any. Pass/Fail to be clearly mentioned on each test report by Dealing officer for samples drawn by BIS for test reports verified by him/her Code numbers and details of samples in TR and IR tally. Test reports under Simplified should not be older than 30 days

Approval of Testing

Approval of Competent Authority for change of lab, if applicable

8(a)

Factory Testing in lieu of I/T

Permission of Competent Authority

8 (b)

Factory test report should be as per CL proforma,

Manufacturing Facilities

Plant machinery declaration including details for source and storage of raw water

9 CM/PF 305 should be countersigned by IO on all pages.

Testing Testing facilities including 10 CM/PF 306 should be countersigned by IO on

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Facilities details of test method adopted by the firm, wherever options available

all pages.

Consent Letter for testing in Outside Lab

Firm’s request for permitting testing at OSL, Consent from OSL for testing on behalf of applicant, Permission by the CA

11 (a) 11 (b) 11 ( c)

Permission should to be granted only for requirements having frequencies of test as monthly & above

Calibration of Instruments

As a minimum, following instruments shall be got calibrated: Analytical Balance All Incubators

12 (a) 12 (b) etc.

Copies of calibration certificates to clearly indicate the validity status and traceability

Quality Control Personnel

Appointment letters of testing personnel Qualification certificates of testing personnel

13 (a) Testing personnel should be employed as full-time. Verification of competence should be clearly recorded by IO.

Preliminary Inspection Report (for Old Procedure)

Preliminary Inspection Report Raw Material receipt details Manufacturing Process – indicating complete process, treatment for disinfection (for each type of packing, if different) Process Flow Diagram Layout Plan of Factory – clearly indicating locations of raw water source & storage, process equipment, plant machinery, Packing & Storage Area, Change Room, Toilet etc. Report of testing of raw water Firm’s own testing of processed water indicating conformity to ISS Reports of plastic containers submitted by firm, as applicable Any other document such as : Test Results of samples tested in factory (if not reported in PIR) Sample Labels, if available

14(a) 14(b) 14( c) 14(d) 14(e) 14(f) 14(g) 14(h) 14 (i) 14 (j)

Report to clearly indicate availability of infrastructure for manufacturing & testing of product as declared by the applicant. Declarations made by the applicant on the prescribed proforma should be verified and countersigned by the IO. Discrepancies, if observed during the Preliminary Inspection, should have been conveyed through D/V report and also attached with the preliminary inspection report

61

Contact Report Visits other than Preliminary Inspection

15(a) 15 (b) etc.

Verification Visit under Simplified Procedure

Report of verification Factory testing Report

16 (a) 16 (b)

Annex III or Annex IV to be used by IO. All the declarations made by the applicants shall be verified and countersigned.

Hygienic Conditions

Complete assessment as per Annex B Medical Examination of employees Pest Control treatment (as applicable)

17(a) 17(b) 17( c)

Assessment report should be countersigned by IO.

Declarations by the firm

Undertaking to intimate BIS regarding shifting of Plant Machinery/Test Equipment Ownership of Plant Machinery/Test Equipment (if not covered under Doc. No. 9 & 10) Affidavit on Stamp paper for material offered for inspection (for sample drawn from stock) Indemnity Bond (for Blocking of CM/L-No.) Undertaking regarding cancellation of licence in case verification sample fails

18 19 20 21 22

Any Other Documents

Other documents, as relevant to the Application

23 onwards

Red Form Should be complete in all respect

Clear recommendations for scope w.r.t Type, Material & Capacity of containers

Recommendations of Dealing Officer & Date GL Head

62

CM/PF /PDW

AUG 2009 ANNEX 7

(Clause 5.2) BUREAU OF INDIAN STANDARDS REPORT OF PERIODIC INSPECTION

(. .. . . . . . . . . . . . inspection since the grant of licence/Renewal)

CM/L - IR No.. . . . Valid upto: Date of writing IR . . . . . . . 1. a) Licensee

b)IS 14543:2004 Packaged Drinking Water (Other Than Packaged Natural Mineral Water)/ IS 13428:2005 Packaged Natural Mineral Water

Type, Material & Capacity of containers covered under licence c) Other license(s) held CM/L . . . . .. . . . . IS Product

4 Special inspection charges, if applicable, with details of realization 3. Date(s) of inspection 4. Person(s) contacted 5. Change in Management, if any 6. Previous inspection a) Date(s) b) Conducted by c) Conclusion and Recommendations d) Details of last 2 factory samples Sl. No. Date of drawl Mode & Date Status of sample Pass/Fail of sample of dispatch (whether report recd.) (if applicable) ---------------------------------------------------------------------------------------------------------------- 1. 2. --------------------------------------------------------------------------------------------------------------- 7. ACTION ON ADVICE RENDERED IN PREVIOUS INSPECTION OR OTHERWISE ASKED FOR WHILE GRANTING LICENCE /RENEWAL OF THE LICENCE _______ REMARKS OF THE REVIEWING OFFICER ON PERFORMANCE OF LICENSEE KEEPING IN VIEW THE PAST PERFORMANCE (ON IRS, TRS , GENERAL ETC)

SIGNATURE & DATE

63

(2)

CM/L - …………… 8. Source of Raw Water

a) Own Bore well/Municipality/Other Source Supply (specify) b) Whether source changed from declared earlier c) If yes, compliance to STI d) Whether records of testing maintained as per STI

9. Packaging Material (Jar/Bottle/Cup/Glass/ Caps/Closures/Pouch-Give details in each case) a) Details of Receipt Container Name of the Supplier Whether BIS Whether recd.with Whether tested Certified test certificate in-house Type Material Capacity b) Whether packing is done in approved container(s)? If not, give details c) Whether records being maintained in accordance with STI 10. PRODUCTION DETAILS a) Whether Water being produced/packed at the time of inspection b) Whether any change in the process of manufacturing & disinfection from that declared earlier? If yes, give details (Disinfection of natural mineral water is not permitted) c) Production Controls (Satisfactory/Unsatisfactory)

e) Production & supply since last periodic inspection (enclose details for completed month)

i) Quantity produced ii) Quantity marked iii) Quantity unmarked and manner of disposal iv) Reason for not marking v) Parties supplied to (Give complete address):

64

(3) CM/L -………………

11. Storing, Packing and marking of BIS certified material a) Material held in stock b) Packing and marking on packages c) At what stage marking is done (After or before test results are known) d) Any change in the marking procedure from approved one e) Compliance to Labeling Prohibitions 12. TESTING ARRANGEMENTS & TESTING a) Details of change(s) in Testing Personnel, if any since previous inspection b) Competence of new Testing Personnel c) Are the frequencies of tests and records testing being maintained satisfactorily vis-à-vis the STI d) Variation in factory test result Enclose Report in Annexure – 7A e) Details of testing got done from Enclose Report in Annexure - 7B outside laboratory f) Details of failure reported, if any and corrective actions taken for the same g) Are all required instruments available and in working order? If No, give details h) Change/addition in testing facilities/arrangement i) Details of calibration of Balance, Thermometers& pressure gauge 13 Testing in factory Description of the sample (Type, Material, Capacity of containers and B.No./Mfg.Date): Sl.No.Requirements Tested Value Obtained Value Recorded Remark

65

(4) CM/L………………….

14. Samples for Independent Tests a) From where sampled (Stock/production line)? b) Details of sample (Batch/Lot No., Date of Mfg. Shelf-Life and Type, Material and Capacity c) Test record of the batch from which sample is drawn Report in Annexure - 7A d) Give details of packing, labeling, coding, sealing of the sample e) Mode of dispatch and laboratory to which sample will be tested f) Details of the counter sample left with the firm 15. HYGIENIC CONDITIONS a) Availability of responsible/designated hygiene control incharge b) Overall compliance to Annex B of IS 13428/IS 14543 Satisfactory/Unsatisfactory as verified as per the check-list attached 16. CONCLUSION AND RECOMMENDATIONS a) Assessment of performance since last inspection Satisfactory /Unsatisfactory b) If operated unsatisfactorily, give reasons (Also indicate whether the discrepancies were conveyed to the licensee through D/V Report, if so enclose copy) c) Any discussion with the firm for difficulties, in production, testing, operation of Scheme and actions proposed, if any for the difficulties observed d) Recommendation for action to be taken f) Any other observation/comments for better appraisal of the report Signature: No. of Encl.: Inspected by: (Name) Designation: Station: Date:

66

CM/L …………….

ANEXURE – 7A ASSESSMENT OF COMPLIANCE TO IS 13428 FOR PNMW/IS 14543 FOR PDW

LIMIT Sl.

No. REQUIREMENT

PDW PNMW VARIATIONS FROM RECORDS

BATCH DRAWN FOR IT

FOUR HOURLY 1. Description To comply 2. Colour 2 Max 2 Max 3. Odour Agreeable Agreeable 4. Taste Agreeable Agreeable 5. Turbidity 2 NTU,

Max 2 NTU, Max

6. pH 6.5 to 8.5 6.5 to 8.5 EACH CONTROL UNIT 1. Total Dissolved Solids 500 mg/l,

Max 150–700 mg/l, Max

2. Chlorides 200 mg/l, Max

200 mg/l, Max

3. Sulphate 200 mg/l, Max

200 mg/l, Max

4. Alkalinity 200 mg/l, Max

75–400 mg/l

5. Residual Free Chlorine 0.2 -- 6. Escherichia coli Absent Absent 7. Coliform bacteria Absent Absent 8. Sulphite reducing

anaerobes Absent Absent

9. Pseudomonas aeruginosa

Absent Absent

10. Aerobic Microbial Count

a) 20/ ml, Max at 370C & b) 100/ml, Max at 20-220C

--

11. Yeast & Mould Count Absent Absent ONCE IN A WEEK 1. Barium 1 mg/l,

Max 1 mg/l, Max

2. Copper 0.05 mg/l, Max

1 mg/l, Max

3. Iron 0.1 mg/l, Max

0.1 mg/l, Max

67

4. Manganese 0.1 mg/l, Max

2.0 mg/l, Max

5. Nitrate 45 mg/l, Max

50 mg/l, Max

6. Nitrite 0.02 mg/l, max

0.02 mg/l, Max

7. Zinc 5 mg/l, Max

5 mg/l, Max

8. Aluminium 0.03 mg/l, Max

0.03 mg/l, Max

9. Calcium 75 mg/l, Max

100 mg/l, Max

10. Magnesium 30 mg/l, Max

50 mg/l, Max

11. Anionic Surf. Act. Agents

0.2 mg/l, Max

Not detectable

12 Sulphide 0.05mg/l Max

0.05mg/l Max

68

CM/L……………….. ANNEX - 7B

DETAILS OF TESTING GOT DONE FROM OUTSIDE LABORATORY (PROGRESS SINCE LAST PERIODIC INSPECTION)

YEAR MONTHLY,

B.NO./TR NO. 3 MONTHLY, B.NO./TR NO.

6 MONTHLY, B.NO./TR NO.

YEARLY, B.NO./TR NO.

Sl.No

MONTH (RESULT/SENT) (RESULT/SENT) (RESULT/ SENT) (RESULT/SENT) 1 JAN

2 FEB

3 MAR 4 APR 5 MAY 6 JUN 7 JUL 8 AUG 9 SEP 10 OCT 11 NOV 12 DEC

TWO YEARLY TEST:

69

ANNEX 8 (Clause 5.2)

HYGIENE CHECK LIST ( VERIFICATION DURING PERIODIC INSPECTION/ SURVEILLANCE VISIT OF

PACKAGED DRINKING WATER / PACKAGED NATURAL MINERAL WATER AT BIS LICENCED UNIT)

CM/L- DATE OF VISIT: NAME OF THE UNIT:

Particulars Requirements Observation

Remarks, if any

Extraction/Collection The source of extraction is well protected from Contamination and unauthorized access

Yes/No

Raw Water Storage Storage tank for raw water is clean and cleaning schedule is being followed.

Yes/No

Processing Area - Processing area is clean and adequately closed. - Adequate ventilation and lighting facilities available and working - Wire mesh/glass provided on windows - Walls and ceiling are well painted and clean. - Flooring is smooth, sloped, clean and free from cervices. - Freedom from insects, rodent and birds, animals etc. - Fly-catchers provided. - Not being used for storage purposes. - Drains are clean and well covered. - Doors are self closing/close fitting type with air-curtains

Yes/No Yes/No Yes/No Yes/No Yes/No Yes/No Yes/No Yes/No Yes/No Yes/No

Hygienic Facilities - No over flow/ dripping from processing vessels. - Cleaning schedule of equipment is adequate and is being followed. - Proper disinfection of containers and caps is being ensured. - Washing and disinfection of reusable jars is being done adequately and absence of

Yes/No Yes/No Yes/No Yes/No

70

residual cleaning chemicals ensured. - Changing facilities are clean and not being used as store. - Toilets are clean and away from processing area. - Protective clothing being used by workers coming in contact with the product. - Medical examination of workers is being done periodically and affected personnel are not allowed to work. - Adequate hand washing facilities are available and notices to this effect are displayed. - Personnel are being trained in food handling, processing and personal hygienic.

Yes/No Yes/No Yes/No Yes/No Yes/No Yes/No

Raw Material

- The raw material including bottles, caps, etc. are properly stored and free from probable contamination. - TC of R/M is available consignment wise.

Yes/No Yes/No

Finished Product

- Finished product pipeline and storage tank is of inert material and is clean and free from corrosion. - Cleaning schedule being followed and supervised by identified personnel. - Inspection screen is provided and is well lit.

Yes/No Yes/No Yes/No

Storage of finished product

- The packed material is stored adequately under hygienic conditions, free from chances of contamination.

Yes/No

OVERALL ASSESSMENT OF HYGIENIC CONDITIONS: SATIS./NOT SATIS. Signature of I.O._______________ Name:________________________ Date:___________________

71

ANNEX – 9

LIST OF TEST FACILITIES

A- ORGANOLEPTIC AND PHYSICAL REQUIREMENTS

Sl. No.

(1)

Tests

(2)

Clause Ref. of IS 14543:2004

or IS 13428:2005

(3)

Referred Method of Test

& Limit of

Detection (4)

Test Equipment/Apparatus

(5)

Chemicals/Reagents

(6)

1. Colour 5.2, Sl No. i) of Table 1

IS 3025 (P 4):1983 with Am. 1

i) Platinum cobalt (Visual comparison method)

ii) Spectrophoto-

metric method

Nessler cylinders,50 ml Centrifuge or filter assembly, functional pore

size 0.45µm

Spectrophotometer,400-700 nm with 10 mm absorption cell

Filteration system consisting of filteration flask with side tubes crucible holder Micrometallic filter crucible, pore 40 µm Calcined filter aid (Celite 505 or equivalent Vacuum system Refrigerator (recommended) pH meter Centrifuge

Potassium chloroplatinate Cobaltous chloride, crystalline Conc. Hydrochloric acid Distilled water

● Conc. Sulphuric acid

● Sodium hydroxide

72

2. Odour 5.2, Sl No. ii) of Table 1

IS 3025 (P 5):1983 Wide mouth glass stoppered bottles (approx. 1 lit. capacity)

● Odour free distilled water (or distilled water and column of granulated activated carbon)

● Hydrochloric acid

3. Taste 5.2, Sl No. iii) of Table 1

IS 3025 (P 8):1984 Breaker (50 ml) Water bath Thermometer

Taste and Odour free water 2000 mg/l solution of sodium chloride

4. Turbidity 5.2, Sl No. iv) of Table 1

IS 3025 (P 10): 1984

Sample tubes Turbidimeter Volumetric flasks (100 ml) Membrane filter with pore size not more than

0.45 µm

Distilled water Hexamethylene Tetramine Hydrazine sulphate

5. Total dissolved solids

5.2,Sl No. v) of Table 1

IS 3025 (P 16): 1983 with Am. 1

Filter: Filtering Assembly (suitable for type of filter

selected) Drying oven (180 ± 2˚C) Desiccator Analytical balance (200 g capacity, l.c. 0.1

mg) Pipettes Evaporating dish Magnetic stirrer, recommended

73

pH 5.2,Sl No. vi) of Table 1

IS 3025 (P 11): 1983

i) Electrometric method

ii) Colorimetric Method

pH meter – with glass and reference electrode (saturated calomel) l.c 0.1

Magnetic stirrer with polytetrafluoro ethylene coated stirring bar

Thermometer (l.c. 0.5°C) Beakers

Hard glass tubes

Standard pH Buffer solutions/tablets (Minimum two different values) OR

Distilled water Borax (for Borax buffer) Potassium dihydrogen phosphate, Sodium hydrogen phosphate and oven (for phosphate buffer) Potassium hydrogen tartarate (for Tartarate

buffer) Potassium hydrogen phthalate (for Phthalate

buffer) Potassium tetraoxalate dihydrate (for

Calcium hydroxide buffer) Calcium Carbonate Platinum dish, Muffle furnace, Hot Plate, Fritted glass filter of medium porosity, polyethylene bottle, Suction pump & fritted glass funnel (for Tetra oxalate buffer)

Methyl orange, methyl red, bromothymol blue, phenolphthalein and alcohol (66%) (for universal indicator)

Thymol blue indicator (acid range) Bromophenol blue indicator Bromocresol green indicator Methyl red indicator Bromocresol purple indicator Bromothymol blue indicator Phenol Red indicator Cresol Red indicator Thymol Blue (alkali range) indicator Thymolphthalein indicator Thymol violet indicator Different buffer solutions of known pH

74

B - CHEMICAL REQUIREMENTS

Sl. No.

(1)

Tests

(2)

Clause Ref. of IS

14543:2004 or IS

13428:2005 (3)

Referred Method of Test &

Limit of Detection

(4)

Test Equipment/Apparatus*

(5)

Chemicals/Reagents

(6) 1. Barium 5.2, Sl. No i)

of Table 2

i) Annex F of IS 13428:2005

ii) IS 15302:2003

Filter paper and filtration assembly Hot plate/gas burner

Atomic Absorption Spectrophotometer and Associated equipment (Burner, Readout

mechanism, lamp for Barium, Pressure Reducing valves and vents)

Nitrous oxide burner head T-junction valve or other switching valve

Air Acetylene Gas Nitrous oxide gas

Ammonium Dichromate Ammonium Acetate Ammonium Hydroxide Potassium Iodide Sodium Thiosulphate(0.1N) Hydrochloric Acid Ammonium Chloride Starch indicator

Metal free water Hydrochloric Acid Nitric Acid Sulphuric Acid Hydroflouric Acid Potassium Chloride Standard barium solution 100µg/ml

(Barium chloride, oven, hydrochloric acid)

75

iii) IS 3025 (P 2)

:2004

Induction Coupled Plasma-Atomic Emission Spectrometer

Sample Bottles Glasswares Acid Dispensers Membrane Filtration Equipment and Filters

(0.45µ) Hot Plate Argon Gas

Nitric Acid Hydrogen Peroxide Sulphuric Acid Hydrochloric acid Ammonium Sulfate Stock Solution of Barium

2. Copper 5.2, Sl No. ii) of Table 2

i) IS 3025 (P 42): 1992 with Am 1

a) Neocuproine Method

Detection range 0.05 to 5.0mg/l

b) Atomic Abso- rption Method (Direct)


Spectrophotometer & 1cm cell Hot plate Separating funnels (125 ml) Conical flasks

Atomic Absorption Spectro- photometer with air-acetylene flame & Copper Hollow Cathode lamp

Ammonium Hydroxide Chloroform, AR Grade Hydrochloric acid, Conc. Hydroxylamine Hydrochloride Isopropyl Alcohol Neocuproine Double Distilled water Nitric Acid, Conc. Sulphuric Acid, Conc. Hydrated Sodium Citrate Stock copper (II) solution 200µg/ml

(Pure Copper Metal, hot plate) Hydrogen Peroxide

Hydrochloric Acid, Conc. Nitric Acid, Conc. Dilute Sulphuric Acid Stock copper (II) solution – 1.0mg/ml

(Pure Copper metal & hot plate)

76

c) Atomic Absorption Method (Chelation Extraction)

Detection range 0.002 to 0.5 mg/l

d) Differential Pulse Anodic Stripping Voltametry


ii) IS 3025 (P 2)

:2004

Atomic Absorption Spectrophotometer with

air-acetyleneflame Copper Hollow Cathode Lamp Separating Funnel Volumetric Flasks Distillation Assembly

Polarograph capable of Performing differential pulse work

Hanging Mercury Drop electrode Platinum Counter Electrode Saturated Calomel Reference Electrode Magnetic Stirrer Control unit with Stirring Bar Scrubber Assembly Whatman Filter Paper No. 40 Nitrogen Gas




Hydrochloric Acid, Conc. Nitric Acid, Conc. Pyrrolidine Dithiocarbamic acid Methyl Isobutyl Ketone, AR grade Carbon Disulphide Sodium Hydroxide Distilled water Water Standard MIBK Bromophenol Blue Ethanol or Isopropanol Stock copper (II) solution – 1.0mg/ml

(Pure Copper metal & hot plate)

Hydrochloric Acid Conc. (Spectro Grade)

Nitric Acid-Conc. (Spectro Grade) Sulphuric Acid Conc. Pure Copper Metal Granular Zinc Mercury

Nitric Acid Hydrogen Peroxide Sulphuric Acid Hydrochloric acid Ammonium Sulfate Stock Solution of Copper

77

3.

Iron

5.2, Sl. No iii) of Table 2

i) IS 3025 (P 53) :2003

a) 1,10 Phenanthroline Method

i) Detection range 0.075 to 0.5mg/l

ii)This requirement is not applicable for Packaged Natural Mineral Water

b) Atomic Absorption Method (DIRECT)

Detection range 0.1 to 10 mg/l

Spectrophotometer Std. volumetric glass wares Hot Plate Fuming Hood 0.45µ m Membrane Filter with

Filtration Assembly

Atomic Absorption Spectrophotometer Air Acetylene Flame

Iron Hollow Cathode Lamp or Electrodeless discharge lamp for use at 248.3nm

Volumetric Flasks

Amalgamated Zinc (Granular Zinc and Mercury)

Ammonium Meta Vanadate Distilled water Hydrochloric Acid-Conc. (Containing less than 0.00005% iron)

Hydroxylamine Hydrochloride Ammonium Acetate Glacial Acetic Acid

Sodium Acetate 1,10 Phenanthroline Monohydrate

Stock Iron Solution 1ml=200µg of Fe (Conc. Sulphuric Acid, Ferrous Ammonium Sulphate, Potasssium Permanganate)

Std. Iron Solution (1.0 ml=1.0µg of Iron) Di-isopropyl Ether

Distilled water Hydrochloric Acid, Conc. Nitric Acid, Conc. Sulphuric Acid, Conc. Calcium Chloride Solution (Calcium Carbonate, Hydrochloric acid)

Stock Iron Solution (1.0 ml=100µg of Fe) (Pure iron wire, Hydrochloric acid Nitric Acid)

78

ii) IS 15303:2003

Electrothermal Atomic Absorption Spectrometric Method

Minimum detection limit 0.001mg/l

iii) IS 3025 (P 2):2004

Atomic Absorption Spectrometer Hollow Cathode lamp for Iron Graphite Furnace Readout Mechanism Sample Dispenser Vent for fumes Cooling device Membrane Filter, 0.45µm




Metal free water Hydrochloric Acid, Conc. Nitric Acid, Conc. Matrix Modifier stock solutions (Magnesium Nitrate, Nickel Nitrate,

Phosphoric Acid, Palladium Nitrate & Citric Acid)

Stock iron Solution – 100µg/ml (Iron wire)

Sodium hydroxide 10N Chelating resin

Nitric Acid Hydrogen Peroxide Sulphuric Acid Hydrochloric acid Ammonium Sulfate Stock Solution of Iron

4. Manganese 5.2, Sl. No. iv), Table 2

i) IS 3025:2006 Part 59

a) Periodate Colorimetric Method

Detection limit up to 0.2mg/l

Nessler’s Tubes Beakers Hot Plate Volumetric flask Pipettes Conical Flasks Burette

Sulphuric Acid Hydrogen Peroxide (30%) Nitric Acid, Conc. Stabilized Distilled Water OR Distillation Assembly, OR

Distilled water, Potassium Permanganate and Dil Sulphuric Acid Phosphoric Acid (sp. Gr. 1.75) Potassium Periodate Std. Manganese Solution

(1ml=0.02 mg of

79

b) Formaldoxime Spectrometric Method

Detection limit between 0.01mg/l to 5 mg/l

ii) IS 3025 (P 2):2004

Spectrophotometer Glass Bottle Autoclave

Induction Coupled Plasma-Atomic Emission

Spectrometer Sample Bottles Glasswares Acid Dispensers Membrane Filtration Equipment and Filters


Mn) (Standard 0.1 N Potassium Permanganate solution, saturated solution of sulphur dioxide)

Fluoride Free Water Potassium Peroxodisulphate or Sodium

Peroxodisulphate EDTA Tetrasodium Salt, Solution, c(EDTA) Sodium Hydroxide Hydroxylammonium Chloride Formaldehyde Ammonia Solution Ammonium Iron (II) Sulphate Hexahydrate

Solution Sulphuric Acid, conc. Manganese Monohydrate (for Standard Mn

Solution)

Nitric Acid Hydrogen Peroxide Sulphuric Acid Hydrochloric acid Ammonium Sulfate Stock Solution of Iron

5. Nitrate (as NO3)

5.2, Sl. No. v) of Table 2

IS 3025 (Part 34):1988

i) Cadmium Reduction Method

Reduction Column Colorimeter OR Spectrophotometer OR Filter photometer Glass wool 0.45 µ m pore diameter membrane filter Refrigerator

Distilled water Nitrate free water Cadmium granules (40 – 60 mesh) Hydrochloric Acid (6N) Copper Sulphate Solution Sulphanilamide Conc. Hydrochloric Acid N-(1-napthyl))-Ethylenediamine

80

Detection limit maximum 0.1 mg/l

ii) Chromotropic Acid Method


iii) Devarda’s Alloy Reduction Method

Detection limit minimum 2 mg/l

Spectrophotometer Standard laboratory glasswares

Distillation Assembly (Kjeldahl

Assembly)

Measuring Scoop Spectrophotometer

dihydrochloride (NED) Dihydrochloride) Ammonium Chloride

Disodium Ethylene diamine tetra acetate Ammonia Solution

Copper sulphate Solution – 2% Stock nitrate solution – 100µg/ml (Potassium Nitrate & Chloroform)

Chloroform Stock nitrite solution - 100µg/ml (Potassium Nitrite & Chloroform)

Nitrite free water

Nitrate free water Stock Nitrate Solution - 100µg/ml

(Potassium Nitrate, Chloroform)

Standard Nitrate solution – 10.0µg/ml Sulphite Urea Reagent

(Urea & Anhydrous sodium Sulphite)

Antimony reagent (Antimony metal, Conc. Sulphuric acid)

Chromotropic Acid Reagent (Purified chromotropic Acid crystals, Conc. Sulphuric Acid)

Sulphuric Acid, Conc. Nitrate free

Ammonia Free Water Borate Buffer Solution (0.1N Sodium

Hydroxide, 0.025M Sodium Tetraborate) Sodium Hydroxide – 6 N Devarda’s Alloy – 20 mesh with less than

81

0.005 percent Nitrogen

Mixed indicator Solution (Methyl Red indicator, Ethyl alcohol/Isopropyl alcohol, Methylene Blue)

Indicating Boric Acid Solution (Hydroboric Acid, mixed indicator solution)

Std. Sulphuric Acid Titrant - 0.02 N Nessler’s Reagent (Mercuric Iodide,

Potassium Iodine. Sodium Hydroxide) Stock Ammonia Solution -1.22mg

ammonia/ ml (Anhydrous Ammonium Chloride)

Standard Ammonia Solution 6. Nitrite 5.2, Sl. No.

vi) of Table 2

IS 3025(P 34) :1988 Spectrophotometer / Photometer OR

Nessler’s cylinders method Nessler’s Tubes 0.45 µm Membrane Filter Distillation Assembly (borosilicate)

Nitrite Free water (Distilled water, Potassium Permanganate, Barium

Hydroxide/Calcium Hydroxide Conc. Sulphuric Acid, Manganese Sulphate)

Sulphanilamide Reagent NED Dihydrochloride Hydrochloric Acid Sodium Oxalate – 0.05 N. Ferrous Ammonium Sulphate – 0.05N

(Ferrous Ammonium Sulphate, Conc. Sulphuric Acid, Std. Dichromate solution)

Stock Nitrite Solution - 250µg of nitrogen/ml (Sodium Nitrite, Chloroform, Sodium Oxalate, Std., Potassium Permanganate solution)

Intermediate Nitrite Solution – 50.0µg/ml Standard Nitrite Solution – 0.500µg/ml

82

7. Flouride 5.2, Sl. No. vii) of Table 2

Clause 23 of IS 3025:1964

i) Zirconium alizarin Method

Detection range

0.05 to 1.0 mg/l

Nessler Tubes (100ml) Distillation Apparatus Refrigerator (Recommended) Heating mantle

Sodium Thiosulphate Solution (0.1 N) Standard Sodium Fluoride Solution (1ml =

0.01 mg F) Zirconium Oxychloride OR Zirconium

Oxynitrate Alizarin Sodium Monosulphonate (Alizarin

S) Conc. Hydrochloric Acid Conc. Sulphuric Acid Silver Sulphate Perchloric Acid Phenolphthalein Indicator Sodium Hydroxide Solution

ii) Electro Chemical Probe Method

Detection range

0.2mg to 2.0 g/l

Millivolt Meter

Fluoride Ion – Selective Electrode

Reference Electrode – Either a calomel electrode, filled with saturated Potassium Chloride (KCl) Solution or a Silver / Silver Chloride Electrode

easuring Cells – 100ml(Polypropylene fitted with thermostated jacket )

Water Bath

agnatic Stirrer with a polytetrafluoroethylene(PTFE)

Polyethylene Beaker

pH meter

Standard Volumetric Glasswares

Desiccator

Sodium Hydroxide- 5 M

Total Ionic Strength Adjustment Buffer (TISAB)-[Sodium Chloride, Glacial Acetic Acid, Sodium Hydroxide, CDTA( trans -1,2-diaminocyclohexane – N,N,N’,N’ tetra acetic acid)]

Fluoride, Stock Solution, 1000mg/1 (Sodium Fluoride )

Note :

Purity of the reagent – Unless specified otherwise, only pure chemicals & Fluoride free distilled water shall be used in tests.

83

Screw Capped Polyethylene Container

Plastic Bottle

8.

Zinc 5.2, Sl. No. viii) of Table 2

IS 3025 (P 49): 1994 with Am 1

i) Zincon Method

Detection range 0.02 to 5 mg/l

ii) Atomic Absorption Method (Direct)


iii)Atomic Absorption Method (Chelation –Extraction)


Spectrophotometer (620 nm with 1cm cells)

Atomic Absorption Spectrophotometer with

Air-Acetylene Flame Hollow Cathode Lamp

Or Electrodeless discharge lamp

Atomic Absorption Spectrophotometer with Air-Acetylene Flame

Hollow Cathode Lamp

Sodium Hydroxide Potassium Cyanide Cyclohexanone Distt. Water Zincon Methanol Sodium Ascorbate Borate Buffer Solution (Sodium

Hydroxide, Potassium Chloride, Boric Acid)

Hydrochloric Acid, Conc. Zinc Sulphate

Hydrochloric Acid, Conc. Nitric Acid, conc. Stock Zinc Solution – 1.0mg/ml (Zinc

Granules/Zinc Oxide)

Hydrochloric Acid, Conc. Nitric Acid, Conc.

Pyrrolidine Dithio Carbamic Acid - Chloroform Reagent (Pyrrolidine, Chloroform, Carbon disulphide)

Sodium Hydroxide Chloroform

84

iv) Differential Pulse Anodic Stripping Voltammetry (DPASV)Method


Polarographic Instrumentation

Capable of Performing Differential Pulse Work

Hanging Mercury Drop Electrode Platinum Counter Electrode Saturated Calomel Reference

Electrode Magnetic Stirrer

Bromophenol Blue Indicator (Bromophenol Blue, Ethanol or Isopropanol)

Stock Zinc (II) Solution- 1.0 mg/ml (Zinc Granules or Zinc Oxide, Nitric Acid)

Hydrochloric Acid, Conc. Nitric Acid, Conc Stock Zinc Solution -1.0mg/ml Amalgamated Zinc (Granular Zinc, Conc.

Hydrochloric Acid, Mercury) Purified Nitrogen (Ammonium Meta

Vanadate, Scrubber, Amalgamated Zinc, Nitrogen Gas)

9. Silver 5.2, Sl. No. ix) of Table 2

Annex J of IS 13428:2005

Atomic Absorption Spectrophotometer with Oxidizing Air Acetylene Flame

Deionised Distilled Water (Ion Exchange Column & Distilled Water)

Nitric Acid – Redistilled Hydrochloric Acid – Redistilled Silver Std. Solution (Silver Nitrate) Lanthanum Chloride Lanthanum Stock Solution (Lanthanum

Oxide, Hydrochloric Acid) Ammonium Pyrrolidine Dithiocarbamate

solution) Methyl isobutyl ketone

85

10. Aluminium 5.2, Sl. No. x) of Table 2

i) IS 3025(P 55): 2003

a) Eriochrome Cyanine R Method

i) Detection range 0.02 to 0.3mg/l;

ii) This requirement is not applicable for Packaged Natural Mineral Water

b) Atomic Absorption Method (Direct)

Detection range 5 to 100mg/l

ii) IS 15302:2003 Direct Nitrous Oxide – Acetylene Flame Atomic Absorption Spectrometry

Detection limit 0.1mg/l

Spectrophotometer (535 nm with 1cm Cells) pH Meter Standard Volumetric Glasswares

Atomic Absorption Spectrophotometer with Nitrous Oxide – Acetylene Flame and Hollow-Cathode Lamp

Standard Volumetric Glasswares

Atomic Absorption Spectrometer Burner Read Out Mechanism Lamp (Hollow Cathode or EDL) Pressure Reducing Valves Vent Nitrous Oxide Burner Head T-Junction Valve or Other Switching Valve

Air (Compressor or Bottled Gas) Acetylene, Standard Commercial Grade Nitrous Oxide Gas

Sulphuric Acid – 0.02 N and 6 N Ascorbic Acid Solution Buffer Solution (Sodium Acetate & 1 N

Acetic Acid) Acetic Acid Solution – 1:1 and 1 N Sodium Hydroxide Solution – 0.1 N and

1N Stock Eriochrome Cyanine R Dye Solution Stock Aluminium Solution – 500 µg/l

(Aluminium Potassium Sulphate) Methyl Orange Indicator Solution

Hydrochloric Acid, Conc. Nitric Acid, Conc. Potassium Chloride Solution Stock Aluminium Solution - 500 µg/l

(Aluminium Potassium Sulphate)

Metal Free Meter Hydrochloric Acid – 1 N Nitric Acid, Conc. Sulphuric Acid Hydrofluoric Acid – 1 N Potassium Chloride Aluminium Nitrate Standard Aluminium Solution - 100 µg/l

(Aluminium Metal)

86

11. Chloride 5.2, Sl. No .xi) of Table 2

IS 3025 (P32): 1988

i) Argentometric Method

ii) Mercuric Nitrate Method

iii) Potentiometric Method

Erlenmeyer Flask (250ml) Burette

Erlenmeyer Flask (250 ml) Microburette (5 ml with l.c. 0.01ml) Refrigerator pH meter

Glass and Silver- Silver Chloride Electrodes Electronic Voltmeter Mechanical Stirrer

Potassium Chromate Indicator Solution (Potassium Chromate, Silver Nitrate)

Standard Silver Nitrate Solution – 0.01 N (silver nitrate, sodium chloride)

Standard Sodium Chloride Solution – 0.01 N (Sodium Chloride)

Aluminium Hydroxide Suspension (Aluminium Potassium Sulphate or Aluminium Ammonium Sulphate, Conc Ammonium Hydroxide)

Phenolphthalein Indicator Solution Sodium Hydroxide – 1N Sulphuric Acid – 1N Hydrogen Peroxide – 30%

Standard Sodium Chloride Solution, 0.01N

Nitric Acid, 0.1N Sodium Hydroxide, 0.1N Indicator – Acidifier Reagent (S-

Diphenyl- carbazone, Conc. Nitric Acid, Xylene Cyanol FF, Ethyl Alcohol or Isopropyl Alcohol)

Standard Mercuric Nitrate Solution, 0.01N (Mercuric Nitrate, Conc. Nitric Acid, Sodium Bicarbonate, Std. Sodium Chloride Solution)

Mixed Indicator Reagent (Diphenylcarbazone, Bromo Phenol Blue, Ethyl Alcohol or Isopropyl Alcohol)

Standard Mercuric Nitrate Solution – 0.1N

Standard Sodium Chloride Solution (0.01N)

Nitric Acid-Conc

87

iv) Automated Ferricyanide Method

Automated Analytical Equipment Filters (480nm)

Standard Silver Nitrate Solution (0.01N) Pretreatment Reagent (Sulphuric Acid,

Hydrogen Peroxide, Sodium Hydroxide – 1N)

Stock Mercuric Thiocyanate Solution (Mercuric Thiocynate, Methanol)

Stock Ferric Nitrate Solution (Ferric Nitrate, Conc. Nitric Acid)

Colour Reagent (Poly oxy Ethylene 23 Lauryl Ether)

Sodium Chloride 12 Selenium 5.2, Sl. No.

xii) of Table 2

i) IS 3025 (P56): 2003

a)Spectrophotometric Method

(Diamino naphthalene method)

Detection limit minimum 0.01mg/l

b) Atomic Absorption Spectrometric Method (Hydride Technique)

Spectrophotometer (480nm,light path of 1 cm

Volumetric Glasswares Separating Funnel (250ml) Preferably

Flourocarbon Stopcock Water Bath – Thermostatically Controlled pH Meter Centrifuge Centrifuge Bottles with Flourocarbon Screw

Cap

Atomic Absorption Spectrometer ( 196.0 nm) Fitted with Hydride System and Hollow Cathode Lamp/Electrodeless Discharge Lamp

Gas (Argon or Nitrogen) Glasswares Decomposition Apparatus

(Round Bottom Flask, Reflux Condenser, Condensate Reservoir)

Stock Selenium Solution – 1.0mg/ml (Sodium Selenite, Hydrochloric Acid)

Hydrochloric Acid – 0.1N Ammonium Hydroxide,1:1Cyclohexane 2,3 – Diaminonaphthalene (DAN) Hydroxylamine Hydrochloride Sodium Salt of EDTA Amberlite XAD -8 or Equivalent Resin Hydrochloric Acid, Conc Potassium Hydroxide Nitric Acid Sulphuric Acid Hydrochloric Acid Hydrogen Peroxide Sodium Hydroxide Sodium Tetrahydro borate Selenium Stock Solution (1mg/ml)

(Selenium Dioxide)

88

ii) IS 15303:2003 Electrothermal Atomic Absorption Spectrometric Method

Detection limit minimum 0.002mg/l

Atomic Absorption Spectrometer monochromator or filter and adjustable slit Hollow Cathode Lamp or Electrodeless

Discharge Lamp Graphite Furnace Photoelectric Detector Readout Mechanism Sample Dispenser Vent for Fumes Cooling Device Membrane Filter Apparatus (0.45 µ m)

Argon Gas

Metal Free Water Hydrochloric Acid, Conc Nitric Acid, Conc Matrix modifier Stock Solutions

(Magnesium Nitrate, Nickel Nitrate, Phosphoric Acid, Palladium Nitrate, Citric Acid)

Stock Metal Solution – 1mg/ml (Sodium Selenite)

Chelating Resin – 100 to 200 mesh

13 Sulphate 5.2, Sl. No. xiii) of Table 2

IS 3025 (P24): 1986

i)Gravimetric Method

Detection limit more than 10mg/l

ii) Thorin Method

Detection range 5 to 150mg/l

Steam Bath Drying Oven (thermostatically controlled) Muffle Furnace Desiccator Analytical Balance (l.c.0.1mg) Filter Paper (Preferably Whatman No.42) Silica or Porcelain Crucible (max pore size

of 5 microns) Ion Exchange Column Filter (0.45 µ m) Platinum Dish

White Porcelain Basin Burette Ion Exchange Column Filter – 0.45µm

Methyl Red Indicator Hydrochloric Acid Barium Chloride Silver Nitrate Nitric Acid Ion Exchange Resin (Amberlite IR-120 or

Equivalent)

Ethyl Alcohol Ammonium Hydroxide (Ammonia-Conc and Distilled Water)

Hydrochloric Acid Thorin (2,2 – Hydroxy – 3,6 – Disulpho – 1 – Naphthylazo Benzene Arsenic Acid)

89

iii)Turbidity Method

Detection limit 1 to 40mg/l

Turbidity Meter or Spectrophotometer`(420 nm)

Glass Apparatus Hot Plate Refrigerator (recommended) Filter – 0.45µm

Ion Exchange Resin (Amberlite IR-120 or Equivalent)

Stock Sulphate Solution – 100 mg/l (Anhydrous Sodium Sulphate)

Barium Chloride – Standard Solution (Barium chloride in hydrochloric acid ammonia)

Barium Chloride Gelatin Powder Glycerol Hydrochloric Acid, Conc Sodium Chloride Ethyl or Isopropyl Alcohol Anhydrous Sodium Sulphate Stock sulphate solution – 100mg/l

14 Alkalinity 5.2, Sl. No. xiv) of

Table 2

IS 3025 (P 23): 1986 with Amendment 1& 2

i) Indicator Method

Detection range 0.5 to 500mg/l

ii)Potentiometric Method

Detection range 0.5 to 500mg/l

pH Meter Burette Magnetic Stirrer Assembly Beaker

Potentiometer Glasswares

Distilled Water Sulphuric Acid, Conc Sulphuric Acid, 0.02 N Phenolphthalein Indicator Mixed Indicator Solution (Methyl Red,

Bromocresol Green, Ethyl or Isoprophyl Alcohol)

Standard Sulphuric Acid – 0.02N

90

15 Calcium 5.2, Sl. No. xv) of Table 2

i) IS 3025 (P40): 1991 with Amendment 1

a)EDTA Titrimetric Method

b)Atomic Absorption Spectrometric Method

Detection limit maximum 50mg/l

c) Permanganate Titration Method

Hot Plate Glasswares Polyethylene Bottle

Atomic Absorption Spectrometer (422.7 nm ) with Air/Acetylene or Nitrous Oxide/Acetylene Flame and Hollow Cathode Lamp (Calcium)

Beakers, Cover Glass, and Glass Rod Filtration Set up (Gooch Crucible with

Suction) Hot plate

Sodium Hydroxide Solution – 1N Hydrochloric Acid – 0.1N Indicator Solution:Murexide (Ammonium

Purpurate) Indicator, Absolute Ethylene Glycol Sodium Chloride

OR

Patton and Reeder’s Indicator (Eriochrome Blue Black R, Sodium Sulphate/Potassium Sulphate)

Standard EDTA Solution – 0.01M (Disodium Ethylene Diamine Tetra – Acetate, Standard Zinc Solution, (Or Standard Calcium Solution) Buffer Solution, Eriochrome Black T Indicator Solution

Stock Calcium Solution (Calcium Carbonate, Hydrochloric Acid – 0.1N)

Nitric Acid, Conc

Hydrochloric Acid – 1N and 0.1N Lanthanum Chloride Cesium Chloride Standard Calcium Solution

Hydrochloric Acid – 1N Methyl Red Indicator Solution Ammonium Oxalate Solution Urea Dilute Sulphuric Acid – 1N Sodium Oxalate Standard Potassium Permanganate

Solution (Potassium permanganate, sodium oxalate)

91

ii)IS 3025(Part 2) Inductively Coupled Plasma Atomic Emission Spectroscopy (a e s)

Detection limit

0.1 mg/l

ICP AES ( 315.887 nm) including -

computer controlled a e s with background correction

radio frequency generator

argon gas supply ( welding grade or better)

Sample bottles

Glassware ( beakers, filter funnels, volumetric flasks, pipettes)

acid dispensers

Membrane filtration equipment

filter of pore size 0.45 microns

Nitric Acid Hydrogen Peroxide Sulphuric Acid Hydrochloric Acid Ammonium Sulphate Distilled Water Calcium Stock solution ( 10 mg/l )

16 Magnesium 5.2, Sl No. xvi) of Table 2

i) IS 3025 (P 46): 1994 with Amendment 1 & 2

a)Gravimetric Method

Detection limit more than 1 mg/l

Vacuum Pump Filter Flasks Filter Crucibles ( medium porosity, 30 ml) Muffle Furnace

Methyl Red Indicator Hydrochloric Acid Ammonium Oxalate Ammonium Hydroxide Nitric Acid, Conc Diammonium Hydrogen Phosphate Urea

92

b) Volumetric Method (EDTA)

c)Atomic Absorption Spectrophotometric Method

Detection limit max 5 mg/l

-Hot plate -Volumetric Flasks -Glasswares

Atomic Absorption Spectrophotometer ( 285.2 nm ) with Air-Acetylene Flame or Nitrous Oxide-Acetylene Flame and Hollow Cathode Lamp (Magnesium) Polyethylene Bottles

Indicator Solutions i) Patton and Reeder Reagent, Sodium Chloride/Potassium Chloride

ii)Murexide (Ammonium Purpurate), Absolute Ethylene Glycol, Sodium Chloride

iii)Eriochrome Black T Indicator (EBT Indicator), Hydroxylamine Hydrochloride, Ethanol/Methanol

Standard Zinc Solution – 0.01M (Pure Zinc Dust/Granules – 99.9% Pure; Hydrochloric Acid)

Buffer Solution (Ammonium Chloride, Ammonia, Sodium Hydroxide-1N)

Standard Ethylene Diamine Tetra Acetic Acid (EDTA) Solution – 0.001M (Disodium Ethylene Diamine Tetra Acetate Dihydrate, Standard Zinc Solution)

Triethanolamine Solution – 10% Potassium Cyanide Hydroxlamine Hydrochloride

Hydrochloric Acid – 1N and 0.1N Lanhanum Chloride (Lathanum Oxide, Hydrochloric Acid, Conc)

Cesium Chloride Standard Magnesium Solution (1000mg/l)

(Magnesium Oxide, Hydrochloric Acid)

93

ii) IS 3025(Part 2)

Inductively Coupled Plasma Atomic Emission Spectroscopy

Detection limit

0.03 mg/l

ICP AES (279.079nm) including - computer controlled aes with background correction radio frequency generator argon gas supply ( welding grade or better) Sample bottles Glassware ( beakers, filter funnels, volumetric flasks, pipettes) acid dispensers Membrane filtration equipment

Nitric Acid Hydrogen Peroxide Sulphuric Acid Hydrochloric Acid Ammonium Sulphate Distilled Water Magnesium Stock solution ( 10 mg/l )

17 Sodium 5.2, Sl No. xvii) of Table 2

i) IS 3025 (P45): 1993 with Amendment 1

a)Flame Emission Photometric Method

anyone of the following applicable detection range:(0 to 1)mg/lit(1 to 10)mg/lit (0 to 100)mg/lit

b)Atomic Absorption Spectrometry Method


Flame Photometer (Direct Reading OR Internal Standard Type) OR Atomic

Absorption Spectrophotometer (In Flame Emission Mode)

Glasswares pH meter Weighing balance

Atomic Absorption Spectrophotometer

with Air-Acetylene Flame and Hollow Cathode Lamp (Sodium)

Deionized Distilled Water Stock Sodium Solution – 1mg/ml (Sodium

Chloride) Standard Lithium Solution – 1mg/ml Sodium Chloride Potassium Chloride Stock Sodium Solution – 1mg/ml Stock Potassium Solution – 1mg/ml

94

c)Gravimetric Method

ii) IS 3025(Part 2):2004

Glassware Beakers (20ml, Borosilicate) Fritted Glass Crucible or Porous Porcelain

Crucibles Vacuum Pump or Aspirator

Filter paper Pyrex bottle Stirring rod

Oven Membrane filtration equipment and

filters(0.45µm) Inductively coupled plasma atomic emission

spectrometer; Computer controlled AAS with background correction, Radiofrequency Generator, Argon Gas supply(welding grade or better)

pH meter PTFE container PTFE sample bottles(250 ml or 500ml) Acid dispensers, Variables

Zinc Uranyl Acetate Reagent (Glacial Conc. Acetic Acid, Uranyl Acetate Dihydrate, Zinc Acetate Dihydrate, Sodium Chloride)

Ethyl Alcohol Wash Solution (Ethyl Alcohol, Pure Sodium Zinc Uranyl Acetate, Sodium Chloride, Acetic Acid, Diethyl Ether)

Nitric acid Hydrogen peroxide Sulphuric acid Hydrochloric acid Ammonium sulphate Sodium Stock solution

18 Residual Free Chlorine

5.2, Sl No. xviii) of Table 2

IS 3025 (P 26): 1986 Stabilized Neutral Ortho-Toluidine Method


This requirement is not applicable for PNMW

Spectrophotometer ( w i t h l i g ht p a t h o f 1 c m c e l l or l o n g e r f or ≤ 1 mg/ l )

Magnetic Stirrer Assembly Refrigerator (Recommended)

Distilled Water – Chlorine Demand Free

(Distilled Water, Chlorine)

Neutral Ortho-Toluidine Reagent (Hydrochloric Acid – Conc, Mercuric Chloride, Disodium Salt of EDTA –

95

pH meter

Brown Glass Stoppered Bottles

Dehydrated, Ortho-Toluidine Dihydrochloride Buffer Stabilizer Reagent (Dipotassium Hydrogen Phosphate, Potassium Dihydrogen Phosphate, Di (2-Ethyl Hexyl) Sulphosuccinate, Diethylene Glycol Monobutyl ether

Potassium Iodide Solution (Potassium Iodide

Sulphuric Acid Conc. Sodium Carbonate Sodium Arsenite

Standard Chlorine Solution (Chlorine Gas &

Distilled Water OR Hypochlorite Solution) Sodium Thiosulphate Solution – 0.025N)

20 Mineral Oil 5.2, Sl No .xx) of Table 2

IS 3025 (P 39): 1991 with Amendment 1

Partition Infra-Red Method

Detection limit 0.5 to 100 mg/l

Separating Funnel (1lit) with Teflon or Equivalent Stopcock

Infra-Red Spectrophotometer – Double Beam, Recording type

Cells – Infra-Red, Silica Filter Paper – Whatman No.40 or

Equivalent, 11cm Diameter Analytical Balance

Hydrochloric Acid Hexane Sodium Sulphate, Anhydrous Reference Oil (Iso-Octane, Hexadecane,

Benzene) Trichlorotrifluoroethane

96

21 Anionic Surface Active Agents (as MBAS)

5.2, Sl No. xxi) of Table 2

Annex K of

IS 13428:2005

Detection limit about

0.05 mg/l

pH Meter Spectrophotometer (650 nm) 10mm &

50mm cells Gas Stripping Apparatus (1 lit Capacity) Nitrogen Air (20 ltr/hr to 50 ltr/hr) Reflux Condenser Fume hood

Water bath

Sodium Chloride Ethyl Acetate Al2O3 Chloroform Ethanol Methanol Sulphuric Acid Ethanolic Sodium Hydroxide-0.1

mol/lit (Sodium Hydroxide, Ethanol) Methylene Blue, Neutral Solution Methylene Blue, Acidic Solution Bufer Solution, pH 10 (Sodium

CHydrogen Carbonate, Anhydrous Sodium Carbonate)

Phenolphthalein Indicator, Ethanol Dodecyl Benzene Sulphonic Acid Methyl

Ester (Tetrapropylene Type), Stock Standard Solution

22 Sulphide 5.2, Sl. No. xxii) of Table 2

IS 3025 (P 29): 1986

i) Iodometric Method

Detection limit above 1 mg/l

ii) Methylene blue method

Detection limit upto 20 mg/l

Glass Fibre Filter Paper. Reaction Flask (1 lit capacity with 2

holestopper fitted with gas-diffusion tube.

Absorption flasks (250ml Capacity) (2 No’s)

Nitrogen/Carbon dioxide gas cylinder Or Carbon dioxide gas generator

Spectrophotometer (664 nm) or filterphotometer (600 nm).

Matched test tubes

Zinc acetate solution – 2N Sulphuric Acid, Conc. Standard Iodine solution – 0.025 N

(Potassium Iodide, Iodine) Hydrochloric Acid, Conc. Standard Thiosulphate Solution - 0.025

N (Sodium thiosulphate, Sodium Hydroxide/Chloroform)

Starch indicator solution (Starch, salicylic acid, toluene)

Aluminium Chloride solution – 6N Sodium hydroxide – 6N

N, N-dimethyl-p-Phenylene Diamine oxalate

Sulphuric Acid, Conc. & 1:1 solution

97

Droppers Dark glass bottle.

Ferric Chloride Diammonium Hydrogen Phosphate Methylene Blue Standard Sulphide Solution

Zinc acetate

23 Antimony 5.2 Sl. No. xxiii) of Table 2

i) Annex G of IS 13428:2005

Spectrophoto-metric Method

ii) IS 15303:2003

Electrothermal Atomic Absorption Spectrometric Method

Spectrophotometer (565 nm) Erlenmeyer Flask (125ml) Seperating Funnels (125 ml) with Teflon

Stopcocks Refrigerator Ice Bath Test Tubes Pipettes

Atomic Absorption Spectrometer with

Hollow Cathode Lamp OR Electrodeless discharge lamp (EDL). Graphic Furnace Readout Mechanism Microlitre Pipettes-5 to 100 µl. OR Automatic sampling device designed

for the specific instrument. Vent for Fumes Cooling Device Membrance Filter Apparatus

(0.45µm) or smaller pore diameter membrane filters.

Hydrochloric Acid – 6 N Phosphoric Acid – 3N Rhodamine B

Antimony Standard Solution (100 µg/ml and 1 ug/ml (pure antimony,

sulphuric acid)

Benzene Sulphuric Acid Perchloric Acid

Metal free Water Hydrochloric Acid, Conc. Nitric Acid, Conc. Matrix Modifier Stock Solutions

(Magnesium Nitrate, Nickel Nitrate, Phosphoric Acid, Palladium Nitrate, Citric Acid)

Stock MetalSolution Antimony Solutions (100 µg/m Sb) Iron-100µg Fe Selenam-1.00 mg Sb Chelating Resin Sodium hydroxide -10 N

98

24 Borates 5.2, Sl. No. xxiv) of Table 2

Annex H of IS 13428:2005

Spectrometer (410 – 420nm) Lab Apparatus made of

Polypropylene/Polyethylene/Polytetrafluoro Ethylene

Refrigerator

Azomethine – H, Sodium Salt L + - Ascorbic Acid Buffer Solution (pH 5.9) [Ammonium

Acetate, Sulphuric Acid, Phosphoric Acid, Citric Acid, Disodium Ethylene diamine – Tetraacetic Acid Dihydrate]

Borate Stock Solution - (1mg/ml) (Boric Acid)

Boron Standard Solution - 10µg/ml Calcium Hydroxide

99

C - REQUIREMENTS FOR TOXIC SUBSTANCES

1 MERCURY 5.2, Sl.

No. i) of Table 3

IS 3025 (P 48): 1994 with Amendment 1

i) Cold Vapour Atomic Absorption Spectrophotometry

Detection limit 0.0002 mg/l, Min

ii) Colorimetric Dithizone Method

Detection limit 0.002 mg/l, Min

Atomic Absorption Spectrometer and Associated Equipment (Cold Vapour Technique)

Mercury Vapour Generation Assembly Mercury Hollow Cathode Lamp Recorder/Printer/Display Meter BOD bottle, 300 ml Water bath Equipment assembly as per Fig 1

Spectrophotometer Separating Funnels (250 and 1000ml with PTFE

stopcocks) Glass wares Whatman Filter No. 42

Sulphuric acid, conc. Nitric acid, Conc. Stannous chloride Hydrochloric acid, Conc. Sodium chloride Hydroxylamine sulphate Potassium permanganate Potassium persulphate Mercuric chloride Mercury free distilled water

Redistilled or Deionised Distilled Water (Mercury free)

Mercuric chloride Nitric acid, Conc. Potassium permanganate Potassium persulphate Hydroxylamine hydrochloride Dithiozone solution, 6 µg/ml Sulphuric acid – 0.25 N Potassium bromide Chloroform Disodium hydrogen phosphate Anhydrous potassium carbonate Sodium sulphate, Anhydrous Hydrochloric acid (1:1) Ammonium hydroxide

100

2 CADMIUM

5.2, Sl. No. ii) of Table 3

IS 3025 (P 41): 1992 i) Atomic Absorption Method (Direct) Detection range 0.05 to 2mg/l ii) Atomic Absorption Method (Chelation and Extraction) Detection range 0.005 to 0.2mg/l iii) Differential Pulse Anodic Stripping Voltametry Detection range 0.0001 to 0.1mg/l

Atomic Absorption spectrophotometer with Air-Acetylene Flame

Cadmium Hollow Cathode Lamp or Multi Element Hollow Cathode Lamp for Use at 228.8 nm

Atomic Absorption spectrophotometer with Air-Acetylene Flame

Cadmium Hollow Cathode Lamp or Multi Element Hollow Cathode Lamp for Use at 228.8 nm

Separating funnel pH meter pH paper

Polarograph – Capable of Differential Pulse Work Hanging MercuryDrop Electrode Platinum Counter Electrode Saturated calomel Reference Electrode Magnetic Stirrer Control Unit with Stirring Bar Nitrogen Gas (Cylinder) Scrubber assembly for nitrogen purification Voltametric Cell assembly

Hydrochloric acid, Conc. Nitric acid, Conc. Nitric acid, dilute – 1:499 Pure Cadmium Metal

Hydrochloric acid, Conc. Hydrochloric acid – 1:49 Nitric acid, Conc. Nitric acid, dilute – 1:499 Pure Cadmium Metal Sodium hydroxide Methyl Isobutyl Ketone (MIBK) Bromophenol Blue Ethanol or Isopropanol Pyrrolidine dithiocarbamic acid Carbon Disulphide

Hydrochloric Acid, Conc., spectrograde Nitric Acid, Conc., spectrograde Nitric Acid, dil – 1:1 Hydroxylamine Hydrochloride L-Ascorbic Acid Pure Cadmium Metal Granular Zinc Mercury Ammonium Meta Vanadate

3 ARSENIC

5.2, Sl. No. iii) of Table 3

IS 3025(P 37): 1988 i) Atomic absorp tion method Detection limit 0.001 mg/l

Atomic absorption spectrometer equipped with gas flow meter for Argon or Nitrogen and Hydrogen and with arsenic electrode less discharge lamp

Atomizer Reaction cell for producing arsenic hydride Eye dropper or syringe Refrigerator

Argon or Nitrogen and Hydrogen Sodium borohydride Sodium hydroxide Sodium Iodide Sulphuric acid-18N & 2.5 N Potassium persulphate Nitric acid, conc

101

ii) Silver diethyl dithiocarbamate method (Refree method) Detection limit 0.001 mg/l iii) Mercuric bromide stain method Detection limit 0.001mg /l

Arsine generator & absorption assembly (Fig 2 of IS 3025 Pt 37) Spectrophotometer, 535 nm with 1 cm cells Arsine generator glass assembly (Fig 3 of IS 3025 Pt 37)

Perchloric acid, conc Hydrochloric acid, conc Arsenic trioxide Arsenic pentaoxide Dimethyl arsenic acid/cacodylic acid Calcium chloride

Hydrochoric acid , Conc Potassium Iodide Stannous chloride, arsenic free Lead acetate Ephedrine Pyridine Chloroform Silver diethyl dithiocarbamate Zinc – 20 to 30 mesh, arsenic free Arsenic trioxide Sodium hydroxide

Sulphuric acid (1:1) Nitric acid, conc Roll cotton Lead acetate Arsenic papers Mercuric bromide Ethyl alcohol/isopropanol Potassium iodide Arsenic free stannous chloride Zinc-20 to 30 Mesh, arsenic free Arsenic trioxide Sodium hydroxide

4 CYANIDE 5.2, Sl.

No. iv) of Table 3

IS 3025(P.27): 1986 with

Amendment 1 i) Total cyanide after distillation method

Distillation apparatus consisting of boiling flask, 1l, thistle tube, Allihn water cooled condenser, gas dispersion tube, needle valve, suction flask and

Sodium hydroxide Lead carbonate-powdered Sulphamic acid

102

Detection limit minimum 0.02 mg/l ii) Selective electrode method Detection range 0.05 to 10 mg/l

suction pump (Fig 1 of IS 3025 Pt 27) Heating mantle Gas absorber Ground glass ST joints Spectrophotometer for use at 62 nm with 1-cm cell pH paper Thermometer – 0oC – 1100C, l.c. 1oC

Expanded – scale pH meter or specific Ion meter Cyanide Ion selective electrode Reference electrode, double junction Magnetic mixer with TFE coated stirring Bar

Magnesium chloride Sulphuric acid, conc Acetic acid, glacial Potassium cyanide Silver nitrate Chloramine - T Pyridine Pyrazolone BIS – pyrazolone

Potassium cyanide Silver nitrate Sodium hydroxide Potassium nitrate Potassium hydroxide

5 LEAD

5.2, Sl. No. v) of Table 3

IS 3025(P 47): 1994

with Amendment 1 & 2 i) Atomic absorption method (direct) Detection range 1.0 to 10.0mg/l ii) Atomic absorption method (chelation – extraction) Detection range 0.1 to 1.0 mg/l (with graphite system 0.001 mg/l)

Atomic absorption spectrophotometer with air acetylene flame

Hollow cathode lamp OR Electrodeless Discharge lamp for use at 283.3 nm

Atomic absorption spectrophotometer with air acetylene flame

Hollow cathode lamp OR Electrode less Discharge lamp for use at 283.3 nm

Separatory funnel 0.45µm membrane filter Acid washed filter paper pH meter

Hydrochloric acid, conc Nitric acid, conc. (Lead nitrate Nitric acid, dil (1:499)

Hydrochloric acid, conc Hydrochloric acid, dil (1:2) Hydrochloric acid, dil (1:49) Nitric acid, conc. Pyrrolidine Chloroform Carbon disulphide Sodium hydroxide Bromophenol blue Lead nitrate

103

iii) Differential pulse anodic stripping voltametry (DPASV) Detection range 0.001 to 0.1mg/l iv) Dithizone method Detection limit 0.1 mg/l

Polarograph capable of performing differential pulse work

Hanging mercury drop electrode Platinum counter electrode Saturated calomel reference electrode Magnetic stirrer control unit with stirring bar Scrubber assembly for nitrogen purification Nitrogen gas (cylinder) 0.45µm membrane filter

Spectrophotometer for use at 510 nm with 1-cm cell

pH meter TEF beakers, 100 ml Separating funnels, 250 ml, 500 ml

Lead nitrate Hydrochloric acid, conc. Nitric acid, conc. Nitric acid, dil (1:1) Granular zinc Mercury Ammonium metavandate

Lead free distilled water Lead nitrate Nitric acid, 95% (w/w) Nitric acid, dil 20% (w/w) Nitric acid, dil (1:1) Ammonium hydroxide Conc. (14 N) Ammonium hydroxide, dil. 10% ( v/v) Ammonium hydroxide, dil. 1% v/v) Anhydrous Ammonium Citrate Anhydrous Sodium Sulphite Hydroxylamine hydrochloride Potassium cyanide Dithizone Chloroform Hydrochloric acid (1:1)

6 CHROMIUM

5.2, Sl. No. vi) of Table 3

Annex J of IS 13428:2005

Atomic absorption spectrophotometer with

reducing Air – acetylene flame 0.45µm membrane filter pH meter Centrifuge

Deionised distilled water, Ammonia free Nitric acid, redistilled – 1:1 (v/v) Hydrochloric acid, redistilled – 1:1 (v/v) Chromium oxide Lanthanum chloride Lanthanum oxide , 99.9%, w/w Ammonium pyrrolidine dithocarbamate

104

7 NICKEL

5.2, Sl. No. vii) of Table 3

Annex L of IS 13428:2005

Atomic absorption spectrophotometer with

nebulizer – burner having air- acetylene flame Centrifuge Nickel hollow cathode lamp/electrode less

discharge lamp Separating funnel, 250-ml with PTFE taps pH meter

Nitric acid, conc. – 1.4 g/ml Pure nickel metal Sodium hydroxide Hydrochloric acid, conc. – 1.19 g/ml Methyl isobutyleketone (MIBK) Ammonium 1 – pyrrolidino

carbodithioate Bromophenol blue Ethanol

8

POLY CHLORINATED BIPHENYLE

(PCB)

5.2, Sl. No. viii) of Table 3

Annex M of IS 13428:2005

Gas chromatograph with EC detector & coupled

with printer-plotter-cum- integrator Glass chromatographic column, 300 mm long, 8

mm ID with ground glass socket at the upper end and a stop cock at low end.

Kuderna-Danish type, evaporator Snyder columns Syringe (5 µl) Heating oven Desiccator

Silica gel, 60 – 100 mesh N-hexane-redistilled Potassium hydroxide pellets Sodium hydroxide solution – 5N Diethyl ether, chromatography grade Cotton wool, extracted with hexane and

diethyl ether Acetic acid, glacial, redistilled Chromium trioxide, re-crystallized Apiezon L grease Epikote Resin 1001 – 0.15 % Chromosorb G (acid washed) DMCS

treated, 60 – 80 mesh Silicone gum GE-S-SI – 1.3 %

9 POLYNUCLEAR AROMATIC

HYDROCARBON

5.2, Sl. No. ix) of Table 3 APHA 6440

i) High Performance Liquid Chromatography (HPLC) Method ii) Gas chromatographic (GC) Method

High Performance Liquid Chromatograph

(HPLC) complete with gradient pumping system, reverse phase column and detectors (UV and fluorescence)

Gas Chromatograph (GC) complete with column and flame ionization detector.

Separating funnel (2 l) Evaporative flask Three Ball Synder column Kuderna- Danish Apparatus

Reagent Water Sodium thiosulphate, granular Cyclohexane Methanol Acetone, Methylene chloride Pentane – Pesticide quality or equivalent. Acetonitrile – HPLC quality Sodium sulphate, granular, anhydrous Silica Gel – 100/200 mesh

105

Water bath (60-65˚C)

Stock standard solution Std. PAHs Solutions – (a) 100 µg/ml of naphthalene, acenaphthylene, fluorine, phneanthrene and anthracene. (b) 5µg/ml Benzo (k) fluoranthene

*Note: Besides listed Equipments/Apparatus/Chemicals, following accessories are essential part of a chemical lab:

i) General glass wares like Pipettes Burette, Conical flasks, Beakers, Measuring cylinders, Volumetric flasks, (of different volumes)

ii) Provision for distilled/double distilled water

iii) Fuming Hood and sink with tap in the lab

# The list does not cover the requirements of Pesticide Residues and Radio Active Residues as these requirements are got to be tested from outside approved lab.

106

D - MICROBIOLOGICAL REQUIREMENTS

General microbiological lab equipments **

Hot air oven (capable of 180 ºC). Autoclave (capable of 15 psi/ 121 ºC) of suitable size as per need. Weighing Balance with least count 0.01 g (least count 0.001 g, if Tergitol-7 agar medium or Crystal violet neutral red bile lactose (VRBL) agar is being

prepared in house). pH meter with least count 0.1 pH unit. Laminar air flow chamber OR inoculation room/cabinet fitted with U.V. tube light. Hot plate for media preparation. Membrane filtration assembly (including sterilized membrane filters of 47 mm to 50 mm diameter with 0.45 µm pore size, vacuum pump (for applying

vacuum of about 70 kPa) and forceps with rounded tips). Inoculation loop/needle. Bunsen burner with LPG cylinder. Thermostatically controlled water bath. Air conditioner (recommended) Refrigerator Colony counting equipment (recommended) General glasswares including, petri dishes (made of glass or plastic), volumetric pipettes (of capacity 1 ml and 10 ml), flasks, test tubes, culture bottles,

funnels, glass rod, measuring cylinders. Thermometer with least count 1 °C Filter Paper Cotton

Sl No.

Parameter Clause Ref.

Referred Method of Test

Test Equipment/Apparatus ** Chemicals/Media/Reagents **

(1) (2) (3) (4) (5) (6)

1 Escherichia coli (or thermotolerant bacteria)

5.1.1 of IS 14543 : 2004

6.1.1 of IS

i) Reference method

IS 5887 (Part 1) :

General microbiological lab equipments (as listed above)

Incubator capable of maintaining 37 °C

Distilled water MacConkey broth medium – (Peptone, Sodium

taurocholate or Bile salts, Sodium chloride, Lactose, Neutral red, Ethanol)

107

13428 : 2005

1976

@ Incubator capable of maintaining 44 °C (for test for growth with acid and gas production in MacConkey broth)

@ Glass tubes open at both ends (for motility test)

@ Seitz filtration assembly (for sterilizing solution of urea for preparing medium for urease test)

Durham’s fermentation tubes (for carbohydrate fermentation test)

@ Microscope and Glass slides (for Gram staining)

MacConkey agar medium – (MacConkey Broth, Agar)

Eosin methylene blue lactose agar medium – (Peptone, Dipotassium hydrogen phosphate, Agar, Lactose, Eosin Y, Methylene blue)

Tergitol-7 agar medium – (Proteose peptone, Yeast extract, Lactose, Agar, Tergitol-7, Bromothymol blue)

@ Nutrient broth – (Peptone, Meat extract, Sodium chloride)

@ Nutrient agar – (Nutrient broth, Agar)

@ TSI medium for H2S test – (Meat extract, Yeast extract, Peptone, Glucose, Lactose, Sucrose, Ferrous sulphate, Sodium chloride, Sodium thiosulphate, Agar, Phenol red)

@ Medium for urease test – (Peptone, Sodium chloride, Agar, Potassium dihydrogen phosphate, Phenol red, Glucose, Urea)

@ Protease species as control for urease test (optional)

@ Medium for indole production – (Peptone, Sodium chloride, Strain of bacterium known to produce indole)

@ Kovac’s reagent (for indole test) – (p-Dimethyl-aminobenzaldehyde, Amyl alcohol or Iso-amyl alcohol,

108

Concentrated hydrochloric acid)

@ Medium for methyl red and Voges-Proskauer tests – (Peptone, Dipotassium hydrogen phosphate, Glucose)

@ Methyl red, absolute ethanol (for methyl red test)

@ α-naphthol, ethanol, potassium hydroxide (for Voges-Proskauer Reaction)

@ Simmon’s citrate agar – (Sodium chloride, Magnesium sulphate, Ammonium dihydrogen phosphate, Dipotassium hydrogen phosphate, Sodium citrate, Agar, Bromothymol blue)

@ Peptone water medium (for carbohydrate fermentation test) – (Peptone, Sodium chloride, Andrade’s indicator, Sugar)

@ Andrade’s indicator (for Peptone water medium for carbohydrate fermentation tests) – (Sodium hydroxide, Acid fuschin)

@ Gram stain – (Methyl violet or Crystal violet, Iodine, Potassium iodide; Neutral red, Acetic acid, Ethanol)

@ Lactose (for carbohydrate fermentation test)

109

ii) IS 15185 : 2002

a) Standard Test


Water bath and/or incubator thermostatically controlled (36 ± 2 °C and 44.0 ± 0.5 °C

Membrane filter of 0.2 µm pore size (for sterilizing TTC solution during preparation of Lactose TTC agar)

Distilled water

Lactose TTC agar with sodium heptadecylsulphate – (Lactose, Peptone, Yeast extract, Meat extract, Bromothymol blue, Agar; 2,3,5 Triphenyltetrazolium chloride (TTC), Sodium heptadecylsulphate (Tergitol-7))

Tryptone soy agar (TSA) – (Tryptic digest of casein, Soy peptone, Sodium chloride, Agar)

Tryptone broth – (Tryptic digest of casein, L-tryptophan, Sodium chloride)

Oxidase reagent – (Tetramethyl-p-phenylene diamine hydrochloride)

Kovac’s Reagent – (p-Dimethylaminobenzaldehyde, Amyl or butyl alcohol , Concentrated hydrochloric acid)

b) Rapid test (Optional)


Ultra violet lamp, wavelength 254 nm (low pressure mercury lamp)

Filter pads, with a diameter of at least 47 mm.


Distilled water


Tryptone bile agar (TBA) – (Tryptone, Bile salts, Agar)

Indole reagent – (p-Dimethylaminobenzaldehyde, Concentrated hydrochloric acid)

110

2 Coliform Bacteria

5.1.2 of IS 14543 : 2004

6.1.2 of IS 13428 : 2005

i) Reference method

IS 5401 (Pt. 1) : 2012


Incubator capable of operating at 30 ºC ± 1 ºC or 37 ºC ± 1 ºC

@ Test tubes of dimensions approximately 16 mm x 160 mm

@ Durham tubes of dimensions appropriate for use with the test tubes

Distilled water

Crystal violet neutral red bile lactose (VRBL) agar – (Enzymatic digest of animal tissues, Yeast extract, Lactose, Sodium chloride, Bile salts, Neutral red, Crystal violet, Agar)

@ Brilliant green lactose bile broth – (Enzymatic digest of casein, Lactose, Dehydrated ox bile, Brilliant green)

ii) IS 15185 : 2002

Standard Test



Membrane filter of 0.2 µm pore size (for sterilizing TTC solution during preparation of Lactose TTC agar)

Distilled water Lactose TTC agar with sodium heptadecylsulphate –

(Lactose, Peptone, Yeast extract, Meat extract, Bromothymol blue, Agar; 2,3,5 Triphenyltetrazolium chloride (TTC), Sodium heptadecylsulphate (Tergitol-7))


Tryptone broth – (Tryptic digest of casein, L-tryptophan, Sodium chloride)

Oxidase reagent – (Tetramethyl-p-phenylene diamine hydrochloride)

Kovac’s Reagent – (p-Dimethylaminobenzaldehyde, Amyl or butyl alcohol , Concentrated hydrochloric acid)

111

Rapid test (Optional)


Ultra violet lamp, wavelength 254 nm (low pressure mercury lamp)

Filter pads, with a diameter of at least 47 mm.


Distilled water


Tryptone bile agar (TBA) – (Tryptone, Bile salts, Agar)

Indole reagent – (p-Dimethylaminobenzaldehyde, Concentrated hydrochloric acid)

3 Sulphite reducing anaerobes

5.1.4 of IS 14543 : 2004

6.1.4 of IS 13428 : 2005

Annex C of IS 13428 : 2005


Screw cap bottles or vials and stoppers of boron silicate glass of capacities 200, 100 and 25 ml

Test tubes - 150 mm x 13 mm

Iron wire

Incubator (37 ºC ± 1 ºC)

Anaerobic jar assembly (recommended)

Distilled water

Differential reinforced clostridial medium (DRCM) – (Peptone tryptic digest of meat , Meat extract, Yeast extract, Starch, Hydrated sodium acetate, Glucose, L-cysteine-hydrochloride, Sodium hydroxide)

Sodium sulphite

Iron (III) citrate

4 Pseudomonas aeruginosa

5.1.5 of IS 14543 : 2004

6.1.5 of IS 13428 : 2005

Annex D of IS 13428 : 2005


Screw capped bottles

Incubator (37 ± 1° C)

Distilled water

Medium for determination of presumed Pseudomonas aeruginosa – (DL asparagine, L proline, Anhydrous dipotassium hydrogen phosphate, Magnesium sulphate heptahydrate, Anhydrous potassium sulphate, Ethanol)

@ Confirmatory medium (Milk agar medium) – [Skim

112

UV cabinet fitted with UV lamp emitting light of wavelength 360 ± 20 nm

Magnetic stirrer (recommended)

Cellulose acetate or nitrate membrane of pore size 0.22 µm (for alternate sterilization of ethanol)

@ Incubator, capable of being maintained at 42 ± 0.5° C

milk powder, Bacteriological yeast extract, Peptone, Sodium chloride, Agar hexadecyltrimethyl ammonium bromide (centrimide)]

@ Clause D-10 (NOTE) of IS 13428 : 2005 specifies confirmation of non-pigmented strains as a further step, if required. Annex 2D of IS 13428 : 2005 specifies biochemical characteristics to be tested for this purpose. No specific apparatus, media and reagents have been specified for the same. It is specified that commercially available identification kits may be used for this.

5 Aerobic Microbial Count

This requirement is not applicable for Packaged Natural Mineral Water

5.1.6 of IS 14543 : 2004

IS 5402 : 2012 General microbiological lab equipments (as listed above)

Incubators 21 ºC ± 1 ºC and 37 ºC

Colony counting equipment

Distilled water

Plate count agar (PCA) – (Enzymatic digestion of casein, Yeast extract, Glucose anhydrous, Agar)

Overlay medium (if necessary) – Agar

6 Yeast and Mould

5.1.7 of IS 14543 : 2004

6.1.6 of IS 13428 : 2005

IS 5403 : 1999 General microbiological lab equipments (as listed above)

Incubator (25 ± 1 ºC)

Distilled water

Yeast extract-dextrose-chloramphenicol-agar medium – (Yeast extract, Dextrose, Chloramphenicol or Oxytetracycline hydrochloride, Agar)

113

** NOTES

Note 1 – The list does not cover the following requirements, as these parameters are got to be tested from outside approved lab:

i) Faecal streptococci and Staphylococcus aureus.

ii) Salmonella and Shigella.

iii) Vibrio cholera and V. parahaemolyticus.

Note 2 – General Microbiological Lab Equipments as listed are common for various microbiological tests. Other additional equipments required for specific test methods are indicated against each parameter.

Note 3 – For preparation of culture media and reagents ingredients of uniform quality and chemicals of analytical reagent grade should be used. Alternatively, commercially available media and reagents may be used provided their composition comply with those given in Indian Standards.

Note 4 – Disposable glassware may be accepted as an alternative to re-usable glassware.

Note 5 – All efforts have been made to compile the list as per the respective standards exhaustively covering all the required test equipments, apparatus and chemicals. However, in case any omission or incorrectness is noticed while referring, the same may be conveyed to CMD immediately for suitable actions.

@ The marked equipments/ chemicals and media are required for confirmatory tests of respective microorganisms. The confirmatory test may be dispensed with/omitted, provided the licensee undertakes to start corrective actions based on presumptive presence of microorganisms.

114

E - REQUIREMENTS FOR BOTTLES/CONTAINERS FOR PACKAGED WATER

Sl. No.

Clause No. of IS 15410:2003

Specified Requirement

Test Facility Requirement

Range and Accuracy/ Least Count ( If and as Applicable)

Method of Test/ Remarks (If any)

1 4.1 Material --- ---- Raw Material conformity to ISs is indicated

2 4.2 4.2.1

Design, Shape and Dimensions

Visual -----

3 4.3 4.3.1 4.3.2

Manufacture, Workmanship, Finish and Appearance

Visual

----- -----

To adhere GMP --

4 4.4 Capacity Weighing Balance or Measuring Cylinder

Suitable range with , LC 0.1 g for Balance or 1 ml for Cylinder

Cl 5 of IS 2798

5 4.5 Wall Thickness Micrometer Suitable Range with LC 0.02 mm

Cl 4.5 of IS 2798

6 4.6.2 Transparency Transparency/ Haze Meter Range upto 100 %, LC 1%

Annex A of IS 15410

7 4.6.3 Leakage Test Vibration Leakage Tester as per Cl. 6.2.1 of IS 2798 Reservoir Air Pressure Leakage Tester

- Cl 6 of IS 2798

8 4.6.4 Drop Test Drop Tester with height of 0.5 m Cl 8 of IS 2798 9 4.6.5 Migration Test Oven/Water Bath

Hot Plate Analytical Balance SS Evaporating Dish Dessicator Glass Beaker, pyrex, 1000 ml Pouch Sealing Machine

Capable of maintaining 40+2° C

IS 9845

10 4.6.6 Water Potability Test

Conditioning Chamber Capable of maintaining 38+2° C

Annex B of IS 15410

115

F- REQUIREMENTS FOR POLYETHYLENE FLEXIBLE POUCHES FOR PACKAGED WATER Sl. No.

Clause No.

Specified Requirement

Test Facility Requirement

Range and Accuracy/ Least Count ( If and as Applicable)

Method of Test/ Remarks (If any)

Clause 6.1 Requirements for Films 1 6.1.1 Description Visual ----------------- 2 6.1.2 Film Form Visual ----------------- 3 6.1.3 Winding of Film Visual ----------------- 4 6.1.4 Odour Olfactory ----------------- 5 6.1.5 Thickness

(65± 5µ/ 75± 5µ) Dead Weight Dial Micrometer

Suitable Range with LC 1 µ

A-2 of IS 2508

6 6.1.6 Width (in mm) Scale Suitable Range, LC 1 mm

7 6.1.7 Overall Migration Oven/Water Bath Hot Plate Analytical Balance SS Evaporating Dish Dessicator Glass Beaker, pyrex, 1000 ml Pouch Sealing Machine

Capable of maintaining 40 + 2o C

IS 9845

8 6.1.8

Tensile Strength

Tensile Testing Machine of suitable range

LC 0.01 kN A-4 of IS 9845

9. 6.1.9 Elongation at break

Tensile Testing Machine of suitable range

LC 0.01 kN A-4 of IS 9845

10. 6.1.10 Dart Impact Resistance

Dart Impact Tester with Drop Height of 66 cm

Set of weights (Min. Impact failure load : 2.20 N)

A-6 of IS 9845

Clause 7 Requirements for Pouches 11. 7.1 Vibration

Leakage Test Vibration Table Temp. - Ambient or

Table conforming to IS 7028 (Pt 2)

Annex D of IS 15609

116

27 + 20 C in case of dispute

Frequency of vibration 2 Hz

12. 7.2 Water Potability Test

Oven/Heating Arrangement Pouch Sealing Machine

Capable of maintaining 38 + 2o C

Annex E of IS 15609

13. 7.3 Stack Load Test Flat Wooden Plank Temp. - Ambient or 27 + 20 C in case of dispute

Set of weights for 20 N to 200 N

Annex F of IS 15609

14. 7.4 Drop Test Arrangement for flat drop from 1.2 m height

----------- Annex G of IS 15609

15. 7.5 Ink Adhesion Test for Printed Pouch

Pressure Sensitive Tapes or Cello- Tape

25 mm wide tape Arrangement for pulling tape at 10 mm/s at about 90 o

Annex H of IS 15609

16. 7.6 Product Resistance Test for Printed Pouch

Paper Tissue -------------- Annex J of IS 15609

Clause 8 Construction 17. 8 Construction Visual -----------------

Amendment No.1 to PDW Manual Doc No.SM/IS 14543 & IS 13428/03, JULY 2013

Clause 4.10 - add the following text after Note 1 Note 2 - There may be cases when the sample of container drawn during the preliminary inspection or verification visit (under simplified procedure), before GOL, is found to be failing in ONLY the requirements of: a) wall thickness which is evaluated against a declared value (but passing in the requirement of drop test); or/and b) brimful capacity . As these requirements do not have a bearing on the quality of the container and/or the product for considering GOL, the applicant shall be advised to submit corrective actions and offer improved sample of container for independent testing. In such cases, if the applicant establishes through documentary evidence that the improved container samples are procured from the same supplier and are made from the same source and type of raw material as the container sample earlier offered for independent testing during the preliminary/verification visit and submits the supplier's certificate of conformity to IS 15410, then GOL may be considered based on the conformity of the improved container to the requirements of wall thickness and/or brimful capacity, as the case may be, through independent testing.