2£! - BISbis.org.in/sf/fad/FAD15(2815-2822)_26022015.pdf · 6 FAD 15 (2820 )C Prerequisite...
Transcript of 2£! - BISbis.org.in/sf/fad/FAD15(2815-2822)_26022015.pdf · 6 FAD 15 (2820 )C Prerequisite...
तकनीक समितत, एफ ए डी 15 रषिती
क खाय व छता, सरषा रबधन एव अ य त र षविय समितत, एफएडी 15 क
अ यष एव सि त सस य। ख खाय एव कषि षवभाग पररिस, एफ ए डी सी क सि त सस य । ग चि रखन वाल सभी तनकाय ।
िहोसय/िहोसया आपक अवलोकन हत तन नमलिखत रलख सलन ह र. स.
रलख स या विषय
1 एफएडी 15 (2815) सी खाय खला की सष ा वषवकी - सष ा ीव गणना की षवतत षवचध - भाग 1 पोर लत तकनीक वारा ° स. पर कॉलोनी गणना (आई एस ओ 4833-1:2013 का अगीकरण)
2 एफएडी 15 (2816)सी खाय खला की सष ा वषवकी - सष ा ीव गणना की षवतत षवचध - भाग 2 सतह लतग तकनीक वारा स. पर कॉलोनी गणना (आई एस ओ 4833-2:2013 का अगीकरण)
3 एफएडी 15 (2817) सी खाय एव पश आहार की सष ि वषवकी – रीयल ताईि पोमलिर खला रततरिया (पी.सी.आर.) पर आधाररत -- खाय तनत रोगाणओ को ञात करन की पधतत - शीगा तॉससन को पवसा करन वाल एिररमशया कोलाई (एस ती ई सी) को ञात करन की षवतत षवचध और O157, O111, O26, O103 तथा O145 सीरो रप का तनधाारण (आई एस ओ/ती एस 1 1 6:2012 का अगीकरण)
4 एफएडी 15(2818) सी खाय एव पश आहार की सष ि वषवकी – रीयल ताईि आर ती - पी सी आर का उपयोग करत हए खाय पसाथ ि हपताईतस ए वाइरस और नोरावाइरस ञात करन की षवतत षवचध - भाग1
रलख रषण सञापन सदभ ददनाक
एफ ए डी 15/ टी 25/02/2015
यापक पररिालन िस सा
रिाराकरण की षवचध (आई एस ओ/ती एस 15216-1:2013 का अगीकरण)
5 एफएडी 15(2819) सी खाय एव पश आहार की सष ि वषवकी – रीयल ताईि आर ती - पी सी आर का उपयोग करत हए खाय पसाथ ि हपताईतस ए वाइरस और नोरोवाइरस ञात करन की षवतत षवचध - भाग 2 गणा िक पहिान की षवचध (आई एस ओ/ती एस 15216-2 : 2013 का अगीकरण)
6 एफएडी 15(2820) सी खाय सरषा का पवाापषण कायािि - भाग 2 कतररग (आई एस ओ/ती एस 22002-2 : 2013 का अगीकरण)
7 एफएडी 15(2821) सी खाय सरषा का पवाापषण कायािि - भाग 4 खाय पवकबसी तनिााण (आई एस ओ/ती एस 22002-4 : 2013 का अगीकरण)
8 एफएडी 15(2822) सी खाय सरषा रब ध पधततयॉ - खाय सरषा रब ध पधततय का सपरीषण एव रिाणन रसान करन वाल तनकाय की अपषाऍ (आई एस ओ/ती एस 22003 का प हला पनरीषण तथा आई एस ओ/ती एस 22003 2 1 का अगीकरण)
कपया इन रलख का अवलोकन कर अपनी स िततयॉ य बतात हए भ रक यस अतत य िस स रारीय िानक क प ि रकामशत हो ाए तो इन पर अिल करन ि आपक यवसाय अथवा कारोबार ि स या कानाइया आ सकती ह । स िततया कपया सल न राप ि अधोह ताषरी को भ ।
स िततया नन क तति ततथि : 27/04/2015 यस कोई स ितत रा त नही होती हव अथवा स ितत ि कवल भािा सब धी रत हई तो
उपरोस त रलख को यथावत अतति प सया ायगा । यस कोई स ितत तकनीकी रकतत की हई तो षविय समितत क अ यष क परािशा स अथवा उनकी इ छा पर आग की कायावाही क मलए षविय समितत को भ ान क बास रलख को अतति प स सया ायगा ।
य रलख हिारी वबसाईत www.bis.org.in पर भी उपल ध ह । ध यवास,
भवसीय, )किार अतनल)
रतत उपररमलिखत ववञातनक एफ एव रिख (खाय एव कषि षवभाग)
ई -िल [email protected]
TECHNICAL COMMITTEE: FAD 15
ADDRESSED TO:
1. The Chairperson & all the Members of Food Hygiene, Safety Management and Other
Systems Sectional Committee, FAD 15
2. All members of FADC
3. All interested
Dear Madam/Sir (s),
Please find enclosed the following documents:
Sl
No.
Doc No. Title
1 FAD 15 (2815)C Microbiology of the food chain — Horizontal method for the
enumeration of microorganisms — Part 1: Colony count at 30°C by
the pour plate technique (Adoption of ISO 4833-1:2013)
2 FAD 15 (2816)C Microbiology of the food chain — Horizontal method for the
enumeration of microorganisms — Part 2: Colony count at 30°C by
the surface plating technique (Adoption of ISO 4833-2:2013)
3 FAD 15 (2817)C Microbiology of food and animal feed — Real-time polymerase
chain reaction (PCR)-based method for the detection of food borne
pathogens — Horizontal method for the detection of Shiga toxin-
producing Escherichia coli (STEC) and the determination of O157,
O111, O26, O103 and O145 serogroups (Adoption of ISO/TS
13136:2012)
4 FAD 15 (2818)C Microbiology of food and animal feed — Horizontal method for
determination of hepatitis A virus and norovirus in food using real-
time RT-PCR — Part 1: Method for quantification (Adoption of
ISO/TS 15216-1:2013)
5 FAD 15 (2819)C Microbiology of food and animal feed — Horizontal method for
determination of hepatitis A virus and norovirus in food using real-
time RT-PCR — Part 2: Method for qualitative detection (Adoption
of ISO/TS 15216-2:2013)
WIDE CIRCULATION
DRAFTS
DOCUMENT DISPATCH ADVICE
Our Ref: Date
FAD 15/T 25/02/2015
6 FAD 15 (2820)C Prerequisite programmes on food safety —Part 2:Catering
(Adoption of ISO/TS 22002-2:2013)
7 FAD 15 (2821)C Prerequisite programmes on food safety —Part 4: Food packaging
manufacturing (Adoption of ISO/TS 22002-4:2013)
8 FAD 15 (2822)C Food safety management systems — Requirements for bodies
providing audit and certification of food safety management
systems (First Revision of ISO/TS 22003 and Adoption of ISO/TS
22003:2013)
Kindly examine these draft standards and forward your views stating any difficulties
which you are likely to experience in your business or profession, if these are finally adopted
as Indian Standards. Comments if any, may please be made in the format as given overleaf
and mailed to the undersigned at the above address.
Last date for comments : 27/04/2015
In case no comments are received or comments received are of editorial nature, you
will kindly permit us to presume your approval for the above documents as finalized.
However, in case comments of technical nature are received, then these may be finalized
either in consultation with the Chairman, Sectional Committee or referred to the Sectional
Committee for further necessary action, if so desired by the Chairman, Sectional Committee.
The documents are also hosted on BIS Website www.bis.org.in.
Thanking you,
Yours faithfully,
(Kumar Anil )
Encl: As above. Scientist ‘F’ & Head (Food & Agri)
E-mail: [email protected]
Draft for Comments Only Doc No. : FAD 15 (2815) C
Draft Indian Standard
MICROBIOLOGY OF THE FOOD CHAIN — HORIZONTAL METHOD FOR
THE ENUMERATION OF MICROORGANISMS — PART 1: COLONY COUNT
AT 30 °C BY THE POUR PLATE TECHNIQUE (Adoption of ISO 4833-1:2013)
ICS No. 07.100.30 Not to be reproduced without the permission Last Date for Comments :
of BIS or used as standard. 27 04 2015
Food Hygiene, Safety Management and Other Systems Sectional Committee, FAD 15
NATIONAL FOREWORD
(adoption clause will be added later)
This Indian Standard is identical to "ISO 4833-1:2013 Microbiology of the food chain —
Horizontal method for the enumeration of microorganisms — Part 1: Colony count at
30 °C by the pour plate technique", issued by International Organization for
Standardization
The text of ISO standard has been approved as suitable for publication as an Indian
Standard without deviations. Certain conventions are however not identical to those used
in Indian Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard,
they should be read as ‘Indian Standard’.
b) Comma(,) has been used as a decimal marker while in Indian Standards, the
current practice is to use a point (.) as the decimal marker.
In this adopted standard, reference appears to the following International Standards for
which Indian Standards also exist. The corresponding Indian Standards which are to be
substituted in their respective places are listed below along with their degree of
equivalence for the edition indicated:
International Standard Corresponding
Indian Standard
Degree of
Equivalence
ISO 6887-1:1999 Microbiology
of food and animal feeding stuffs
-- Preparation of test samples,
initial suspension and decimal
dilutions for microbiological
examination -- Part 1: General
rules for the preparation of the
initial suspension and decimal
IS 10232:2003 General rules for
the preparation of initial
suspension and decimal dilutions
for microbiological examination
of foods (first revision)
Identical
dilutions
ISO 6887-2:2003 Microbiology
of food and animal feeding stuffs
-- Preparation of test samples,
initial suspension and decimal
dilutions for microbiological
examination -- Part 2: Specific
rules for the preparation of meat
and meat products
ISO 7218:2007 Microbiology of
food and animal feeding stuffs --
General requirements and
guidance for microbiological
examinations
IS 15990:2012 Microbiology of
food and animal feeding stuffs --
Preparation of test samples,
initial suspension and decimal
dilutions for microbiological
examination -- Part 2: Specific
rules for the preparation of meat
and meat products
IS 16122:2013 Microbiology of
food and animal feeding stuffs -
General requirements and
guidance for microbiological
examinations
Identical
Identical
The technical committee responsible for the preparation of this standard may also review
the provisions of the following ISO Standards and decide if they are acceptable for use in
conjunction with this standard:
International Standard Title
ISO 6887-3:2003
ISO 6887-4:2003 ISO 6887-5:2010 ISO 6887-6:2013
Microbiology of food and animal feeding stuffs -- Preparation
of test samples, initial suspension and decimal dilutions for
microbiological examination -- Part 3: Specific rules for the
preparation of fish and fishery products
Microbiology of food and animal feeding stuffs -- Preparation
of test samples, initial suspension and decimal dilutions for
microbiological examination -- Part 4: Specific rules for the
preparation of products other than milk and milk products,
meat and meat products, and fish and fishery products
Microbiology of food and animal feeding stuffs -- Preparation
of test samples, initial suspension and decimal dilutions for
microbiological examination -- Part 5: Specific rules for the
preparation of milk and milk products
Microbiology of food and animal feed -- Preparation of test
samples, initial suspension and decimal dilutions for
microbiological examination -- Part 6: Specific rules for the
preparation of samples taken at the primary production stage
In reporting the result of a test or analysis made in accordance with this standard, if the
final value, observed or calculated, is to be rounded off, it shall be done in accordance
with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’.
‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO 4833-1:2013’
For obtaining a hard copy of the complete document please contact/write to:
Scientist – F & Head
Food and Agriculture Department
Bureau of Indian Standards
Manak Bhavan,
9 Bahadur Shah Zafar Marg,
New Delhi – 110 002
Telefax: 011 23231128
Email: [email protected]
Draft for Comments Only Doc No. : FAD 15 (2816) C
Draft Indian Standard
MICROBIOLOGY OF THE FOOD CHAIN — HORIZONTAL METHOD FOR
THE ENUMERATION OF MICROORGANISMS — PART 2: COLONY COUNT
AT 30 °C BY THE SURFACE PLATING TECHNIQUE
(Adoption of ISO 4833-2:2013)
ICS No. 07.100.30 Not to be reproduced without the permission Last Date for Comments :
of BIS or used as standard. 27 04 2015
Food Hygiene, Safety Management and Other Systems Sectional Committee, FAD 15
NATIONAL FOREWORD
(adoption clause will be added later)
This Indian Standard is identical to "ISO 4833-2:2013 Microbiology of the food chain —
Horizontal method for the enumeration of microorganisms — Part 2: Colony count at
30°C by the surface plating technique", issued by International Organization for
Standardization
The text of ISO standard has been approved as suitable for publication as an Indian
Standard without deviations. Certain conventions are however not identical to those used
in Indian Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard,
they should be read as ‘Indian Standard’.
b) Comma(,) has been used as a decimal marker while in Indian Standards, the
current practice is to use a point (.) as the decimal marker.
In this adopted standard, reference appears to the following International Standards for
which Indian Standards also exist. The corresponding Indian Standards which are to be
substituted in their respective places are listed below along with their degree of
equivalence for the edition indicated:
International Standard Corresponding
Indian Standard
Degree of
Equivalence
ISO 6887-1:1999 Microbiology
of food and animal feeding stuffs
-- Preparation of test samples,
initial suspension and decimal
dilutions for microbiological
examination -- Part 1: General
rules for the preparation of the
initial suspension and decimal
IS 10232:2003 General rules for
the preparation of initial
suspension and decimal dilutions
for microbiological examination
of foods (first revision)
Identical
dilutions
ISO 6887-2:2003 Microbiology
of food and animal feeding stuffs
-- Preparation of test samples,
initial suspension and decimal
dilutions for microbiological
examination -- Part 2: Specific
rules for the preparation of meat
and meat products
ISO 7218:2007 Microbiology of
food and animal feeding stuffs --
General requirements and
guidance for microbiological
examinations
IS 15990:2012 Microbiology of
food and animal feeding stuffs --
Preparation of test samples,
initial suspension and decimal
dilutions for microbiological
examination -- Part 2: Specific
rules for the preparation of meat
and meat products
IS 16122:2013 Microbiology of
food and animal feeding stuffs -
General requirements and
guidance for microbiological
examinations
Identical
Identical
The technical committee responsible for the preparation of this standard may also review
the provisions of the following ISO Standards and decide if they are acceptable for use in
conjunction with this standard:
International Standard Title
ISO 6887-3:2003
ISO 6887-4:2003 ISO 6887-5:2010 ISO 6887-6:2013
Microbiology of food and animal feeding stuffs -- Preparation
of test samples, initial suspension and decimal dilutions for
microbiological examination -- Part 3: Specific rules for the
preparation of fish and fishery products
Microbiology of food and animal feeding stuffs -- Preparation
of test samples, initial suspension and decimal dilutions for
microbiological examination -- Part 4: Specific rules for the
preparation of products other than milk and milk products,
meat and meat products, and fish and fishery products
Microbiology of food and animal feeding stuffs -- Preparation
of test samples, initial suspension and decimal dilutions for
microbiological examination -- Part 5: Specific rules for the
preparation of milk and milk products
Microbiology of food and animal feed -- Preparation of test
samples, initial suspension and decimal dilutions for
microbiological examination -- Part 6: Specific rules for the
preparation of samples taken at the primary production stage
In reporting the result of a test or analysis made in accordance with this standard, if the
final value, observed or calculated, is to be rounded off, it shall be done in accordance
with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’.
‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO 4833-2:2013 ’
For obtaining a hard copy of the complete document please contact/write to:
Scientist – F & Head
Food and Agriculture Department
Bureau of Indian Standards
Manak Bhavan,
9 Bahadur Shah Zafar Marg,
New Delhi – 110 002
Telefax: 011 23231128
Email: [email protected]
Draft for Comments Only Doc No. : FAD 15 (2817) C
Draft Indian Standard
MICROBIOLOGY OF FOOD AND ANIMAL FEED — REAL-TIME
POLYMERASE CHAIN REACTION (PCR)-BASED METHOD FOR THE
DETECTION OF FOOD BORNE PATHOGENS — HORIZONTAL METHOD
FOR THE DETECTION OF SHIGA TOXIN-PRODUCING ESCHERICHIA COLI
(STEC) AND THE DETERMINATION OF O157, O111, O26, O103 AND O145
SEROGROUPS
(Adoption of ISO/TS 13136:2012)
ICS No. 07.100.30 Not to be reproduced without the permission Last Date for Comments :
of BIS or used as standard. 27 04 2015
Food Hygiene, Safety Management and Other Systems Sectional Committee, FAD 15
NATIONAL FOREWORD
(adoption clause will be added later)
An ISO Technical Specification (ISO/TS) represents an agreement between the members
of a technical committee and is accepted for publication if it is approved by 2/3 of the
members of the committee casting a vote, whereas International Standard (ISO) requires
approval by at least 3/4 of the member bodies casting a vote. An ISO/TS is reviewed after
three years in order to decide whether it will be confirmed for a further three years,
revised to become an International Standard, or withdrawn.
This Indian Standard is identical to "ISO/TS 13136:2012 Microbiology of food and
animal feed — Real-time polymerase chain reaction (PCR)-based method for the
detection of food borne pathogens — Horizontal method for the detection of Shiga toxin-
producing Escherichia coli (STEC) and the determination of O157, O111, O26, O103
and O145 serogroups", issued by International Organization for Standardization
The text of ISO standard has been approved as suitable for publication as an Indian
Standard without deviations. Certain conventions are however not identical to those used
in Indian Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard,
they should be read as ‘Indian Standard’.
b) Comma(,) has been used as a decimal marker while in Indian Standards, the
current practice is to use a point (.) as the decimal marker.
In this adopted standard, reference appears to the following International Standards for
which Indian Standards also exist. The corresponding Indian Standards which are to be
substituted in their respective places are listed below along with their degree of
equivalence for the edition indicated:
International Standard
Corresponding
Indian Standard
Degree of
Equivalence
ISO 7218:2007 Microbiology of
food and animal feeding stuffs --
General requirements and
guidance for microbiological
examinations
ISO 20838:2006 Microbiology of
food and animal feeding stuffs —
Polymerase chain reaction (PCR)
for the detection of food-borne
pathogens — Requirements for
implification and detection for
qualitative methods
ISO 22174:2005 Microbiology of
food and animal feeding stuffs —
Polymerase chain reaction (PCR)
for the detection of food-borne
pathogens — General
requirements and definitions
IS 16122:2013 Microbiology of
food and animal feeding stuffs -
General requirements and
guidance for microbiological
Examinations
DOC.FAD 15(2551) Draft
Indian Standard - Microbiology
of food and animal feeding stuffs
-- Polymerase chain reaction
(PCR) for the detection of food-
borne pathogens -- Requirements
for amplification and detection
for qualitative methods
DOC.FAD 15(2559) Draft
Indian Standard - Microbiology
of food and animal feeding stuffs
-- Polymerase chain reaction
(PCR) for the detection of food-
borne pathogens -- General
requirements and definitions
Identical
Identical
Identical
In reporting the result of a test or analysis made in accordance with this standard, if the
final value, observed or calculated, is to be rounded off, it shall be done in accordance
with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’.
‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO/TS 13136:2012’
For obtaining a hard copy of the complete document please contact/write to:
Scientist – F & Head
Food and Agriculture Department
Bureau of Indian Standards
Manak Bhavan,
9 Bahadur Shah Zafar Marg,
New Delhi – 110 002
Telefax: 011 23231128
Email: [email protected]
Draft for Comments Only Doc No. : FAD 15 (2818) C
Draft Indian Standard
MICROBIOLOGY OF FOOD AND ANIMAL FEED — HORIZONTAL
METHOD FOR DETERMINATION OF HEPATITIS A VIRUS AND
NOROVIRUS IN FOOD USING REAL-TIME RT-PCR — PART 1:
METHOD FOR QUANTIFICATION
(Adoption of ISO/TS 15216-1:2013)
ICS No. 07.100.30 Not to be reproduced without the permission Last Date for Comments :
of BIS or used as standard. 27 04 2015
Food Hygiene, Safety Management and Other Systems Sectional Committee, FAD 15
NATIONAL FOREWORD
(adoption clause will be added later)
An ISO Technical Specification (ISO/TS) represents an agreement between the members of a
technical committee and is accepted for publication if it is approved by 2/3 of the members of
the committee casting a vote, whereas International Standard (ISO) requires approval by at
least 3/4 of the member bodies casting a vote. An ISO/TS is reviewed after three years in
order to decide whether it will be confirmed for a further three years, revised to become an
International Standard, or withdrawn.
This Indian Standard is identical to " ISO/TS 15216-1:2013 Microbiology of food and animal
feed — Horizontal method for determination of hepatitis A virus and norovirus in food using
real-time RT-PCR — Part 1: Method for quantification", issued by International Organization
for Standardization
The text of ISO standard has been approved as suitable for publication as an Indian Standard
without deviations. Certain conventions are however not identical to those used in Indian
Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard, they
should be read as ‘Indian Standard’.
b) Comma(,) has been used as a decimal marker while in Indian Standards, the current
practice is to use a point (.) as the decimal marker.
In this adopted standard, reference appears to the following International Standard for which
Indian Standard also exists. The corresponding Indian Standard which is to be substituted in
its respective places is listed below along with its degree of equivalence for the edition
indicated:
International Standard Corresponding
Indian Standard
Degree of
Equivalence
ISO 22174:2005 Microbiology of
food and animal feeding stuffs —
Polymerase chain reaction (PCR)
for the detection of food-borne
pathogens — General
requirements and definitions
DOC.FAD 15(2559) Draft
Indian Standard - Microbiology
of food and animal feeding stuffs
-- Polymerase chain reaction
(PCR) for the detection of food-
borne pathogens -- General
requirements and definitions
Identical
In reporting the result of a test or analysis made in accordance with this standard, if the final
value, observed or calculated, is to be rounded off, it shall be done in accordance with IS 2 :
1960 ‘Rules for rounding off numerical values (revised)’.
‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO/TS 15216-1:2013'
For obtaining a hard copy of the complete document please contact/write to:
Scientist – F & Head
Food and Agriculture Department
Bureau of Indian Standards
Manak Bhavan,
9 Bahadur Shah Zafar Marg,
New Delhi – 110 002
Telefax: 011 23231128
Email: [email protected]
Draft for Comments Only Doc No. : FAD 15 (2819) C
Draft Indian Standard
MICROBIOLOGY OF FOOD AND ANIMAL FEED — HORIZONTAL
METHOD FOR DETERMINATION OF HEPATITIS 'A' VIRUS AND
NOROVIRUS IN FOOD USING REAL-TIME RT-PCR — PART 2:
METHOD FOR QUALITATIVE DETECTION
(Adoption of ISO/TS 15216-2:2013)
ICS No. 07.100.30
Not to be reproduced without the permission Last Date for Comments :
of BIS or used as standard. 27 04 2015
Food Hygiene, Safety Management and Other Systems Sectional Committee, FAD 15
NATIONAL FOREWORD
(adoption clause will be added later)
An ISO Technical Specification (ISO/TS) represents an agreement between the members of a
technical committee and is accepted for publication if it is approved by 2/3 of the members of
the committee casting a vote, whereas International Standard (ISO) requires approval by at
least 3/4 of the member bodies casting a vote. An ISO/TS is reviewed after three years in
order to decide whether it will be confirmed for a further three years, revised to become an
International Standard, or withdrawn.
This Indian Standard is identical to " ISO/TS 15216-2:2013 Microbiology of food and animal
feed — Horizontal method for determination of hepatitis A virus and norovirus in food using
real-time RT-PCR — Part 2: Method for qualitative detection", issued by International
Organization for Standardization
The text of ISO standard has been approved as suitable for publication as an Indian Standard
without deviations. Certain conventions are however not identical to those used in Indian
Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard, they
should be read as ‘Indian Standard’.
b) Comma(,) has been used as a decimal marker while in Indian Standards, the current
practice is to use a point (.) as the decimal marker.
In this adopted standard, reference appears to the following International Standard for which
Indian Standard also exists. The corresponding Indian Standard which is to be substituted in
its respective places is listed below along with its degree of equivalence for the edition
indicated:
International Standard Corresponding
Indian Standard
Degree of
Equivalence
ISO 22174:2005 Microbiology of
food and animal feeding stuffs —
Polymerase chain reaction (PCR)
for the detection of food-borne
DOC.FAD 15(2559) Draft
Indian Standard - Microbiology
of food and animal feeding stuffs
-- Polymerase chain reaction
Identical
pathogens — General
requirements and definitions
(PCR) for the detection of food-
borne pathogens -- General
requirements and definitions
In reporting the result of a test or analysis made in accordance with this standard, if the final
value, observed or calculated, is to be rounded off, it shall be done in accordance with IS 2 :
1960 ‘Rules for rounding off numerical values (revised)’.
‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO/TS 15216-2:2013’
For obtaining a hard copy of the complete document please contact/write to:
Scientist – F & Head
Food and Agriculture Department
Bureau of Indian Standards
Manak Bhavan,
9 Bahadur Shah Zafar Marg,
New Delhi – 110 002
Telefax: 011 23231128
Email: [email protected]
Draft for Comments Only Doc No. : FAD 15 (2820) C
Draft Indian Standard
PREREQUISITE PROGRAMMES ON FOOD SAFETY —PART 2:CATERING
(Adoption of ISO/TS 22002-2:2013)
ICS No. 67.040 Not to be reproduced without the permission Last Date for Comments :
of BIS or used as standard. 27 04 2015
Food Hygiene, Safety Management and Other Systems Sectional Committee, FAD 15
NATIONAL FOREWORD
(adoption clause will be added later)
An ISO Technical Specification (ISO/TS) represents an agreement between the members of a
technical committee and is accepted for publication if it is approved by 2/3 of the members of
the committee casting a vote, whereas International Standard (ISO) requires approval by at
least 3/4 of the member bodies casting a vote. An ISO/TS is reviewed after three years in
order to decide whether it will be confirmed for a further three years, revised to become an
International Standard, or withdrawn.
This Indian Standard is identical to " ISO/TS 22002-2:2013 Prerequisite programmes on
food safety —Part 2:Catering ", issued by International Organization for Standardization.
The text of ISO standard has been approved as suitable for publication as an Indian Standard
without deviations. Certain conventions are however not identical to those used in Indian
Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard, they
should be read as ‘Indian Standard’.
b) Comma(,) has been used as a decimal marker while in Indian Standards, the current
practice is to use a point (.) as the decimal marker.
In this adopted standard, reference appears to the following International Standard for which
Indian Standard also exists. The corresponding Indian Standard which is to be substituted in
its respective places is listed below along with its degree of equivalence for the edition
indicated:
International Standard Corresponding
Indian Standard
Degree of
Equivalence
ISO 22000:2005, Food safety
management systems —
Requirements for any
organization in the food chain
ISO 22000:2005, Food safety
management systems —
Requirements for any
organization in the food chain
Identical
The technical committee responsible for the preparation of this standard may also review the
provisions of the following ISO Standard and decide if it is acceptable for use in conjunction
with this standard:
International Standard Title
ISO 21469:2006 Safety of machinery — Lubricants with incidental
product contact — Hygiene requirements
In reporting the result of a test or analysis made in accordance with this standard, if the final
value, observed or calculated, is to be rounded off, it shall be done in accordance with IS 2 :
1960 ‘Rules for rounding off numerical values (revised)’.
‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO/TS 22002-2:2013'
For obtaining a hard copy of the complete document please contact/write to:
Scientist – F & Head
Food and Agriculture Department
Bureau of Indian Standards
Manak Bhavan,
9 Bahadur Shah Zafar Marg,
New Delhi – 110 002
Telefax: 011 23231128
Email: [email protected]
1
For BIS use only
DRAFT FOR COMMENTS ONLY Doc: No. FAD 09(2721)C
Draft Indian Standard
SPICES AND CONDIMENTS — RAW MANGO (MANGIFERA INDICA LINN.)
POWDER (AMCHUR) AND SLICES — SPECIFICATION
(First Revision of IS 13242) ICS No. 67.220.10
Not to be reproduced or used as
STANDARD without permission of BIS
Last date for comments: April 30, 2015
Spices and Condiments Sectional Committee, FAD 9
FOREWORD
(Adoption clause would be added later)
Amchur, the powdered form of raw mango is a popular condiment especially in the northern part of the country
in the various food preparations for imparting special aroma and taste. Amchur is generally prepared from
unripe, wind-fallen sour mangoes (Mangifera indica Linn.). As the production of this product is fast getting
organised, this standard is expected to help in the quality control of the product for its home consumption.
The requirements for the characteristics as provided in the standard are in consonance with the requirements
provided in the Grading and Marking Rules by the Directorate of Marketing and Inspection, wherever
applicable.
This standard was first published in 1991 under the title 'Spices and Condiments — Amchur, Raw Mango
(Mangifera Indica Linn.) Powder — Specification'. This revision is being undertaken to incorporate the
requirements of raw mango slices also, modify the title accordingly and align the requirement of acidity of
Amchur powder with the specifications laid down in the Food Safety and Standards (Food Products Standards
and Food Additives) Regulations, 2011 and include requirements for aflatoxins, total viable count, E. coli,
mould and Salmonella in line with Sundried Raw Mango slices and Powder Grading and Marking Rules, 2003
issued by Directorate of Marketing and Inspection.
In the formulation of this standard, due consideration has been given to the provisions of the Food Safety and
Standards Act, 2006 and the Rules and Regulations framed thereunder and the Legal Metrology (Packaged
Commodities) Rules, 2011. However, this standard is subject to the restrictions imposed under these, wherever
applicable.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.
1 SCOPE
This standard prescribes the requirements for raw mango (Mangifera indica Linn.) powder (Amchur) and slices
(Khatai).
2 REFERENCES
The standards given below contain provisions which, through reference in this text, constitute provisions of this
standard. At the time of publication, the editions indicated were valid. All standards are subject to revision and
parties to agreements based on this standard are encouraged to investigate the possibility of applying the most
recent editions of these standards.
IS No. Title
460 (Part 1) : 1985 Test sieves : Part 1 Wire cloth test sieves (third revision)
1070 : 1992 Reagent grade water Specification (third revision)
1797 : 2015 Methods of test for spices and condiments (third revision) (under print)
2
5402 : 2012 Microbiology of food and animal feeding stuffs Horizontal method for the
/ISO 4833 : 2003 enumeration of microorganisms Colony count technique at 30 degree C
(second revision)
5403 : 1999 Method for yeast and mould count of food stuffs and animal feeds (first revision)
5887 Methods for detection of bacteria responsible for food poisoning
(Part 1) : 1976 Isolation, identification and enumeration of Escherichia Coli
(Part 3) : 1999 General guidance on methods for detection of SALMONELLA (second revision)
/ISO 6579 : 1993
13145 : 2014 Spices and Condiments Methods of sampling (second revision)
14216 : 1994 Code for hygienic practice for spices and condiments processing units
Doc: No. FAD 28(2609)F Draft Indian Standard Foodstuffs Determination of aflatoxin B1, and the total
content of aflatoxins B1, B2, G1 and G2 in cereals, nuts and derived products
High-performance liquid chromatographic method (Adoption of ISO 16050 : 2003)
(under print)
3 TERMINOLOGY
For the purpose of this standard, the following definitions shall apply.
3.1 Inorganic Extraneous Matter Metallic pieces, sand, gravel, dirt, stone, lumps of earth, clay and mud.
3.2 Organic Extraneous Matter Chaff, stem and straw.
3.3 Seed Coating Exterior covering of the seed.
3.4 Damaged and Discoloured Slice Slices that are eaten by weevils or other insects and including slices
internally damaged by fungus, moisture or heating.
4 REQUIREMENTS
4.1 Description
4.1.1 The Amchur powder shall be prepared by grinding peeled clean and dried raw mango slices Mangifera
indica (Linn.).
4.1.2 Khatai (raw mango slices) shall be dried wholesome, edible part of raw mango fruit with or without the
outer skin.
4.2 Colour, Taste and Flavour
The product shall have the characteristic colour, taste and flavour. It shall be free from musty odour. It shall be
free from extraneous matter, added colouring matter, flavouring matter and preservatives.
4.3 Freedom from Moulds, Insects, etc
The product shall be free from dirt, mould growth and insect infestation and/or fungus contamination.
4.4 The product shall not contain any preservative except edible common salt which may be added to the extent
of 5 percent by weight on dry basis (see 16 of IS 1797).
4.5 Fineness
The Amchur powder shall be ground to such a fineness that not less than 97 percent by weight passes through a
500 μm IS Sieve [see IS 460 (Part 1)].
4.6 The Amchur powder and Khatai (raw mango slices) shall also comply with the requirements given in
Table 1 and Table 2, respectively.
4.7 The product shall be manufactured and packed under hygienic conditions (see IS 14216).
3
4.8 The pesticide residues, heavy metals, toxins (aflatoxins and other naturally occuring toxins), if any, in the
product shall not exceed the limits as prescribed in the Food Safety and Standards (Contaminants, Toxins and
Residues) Regulations, 2011.
Table 1 Requirements for Amchur Powder
(Clause 4.6)
Sl
No.
Characteristic Requirement
Method of test, Ref to
(1) (2) (3) (4)
i) Moisture, percent by weight, Max 10.0 9 of IS 1797
ii) Total ash (on dry basis), percent by weight,
Max
4.8 6 of IS 1797
iii) Acid insoluble ash, percent by weight, Max 1.0 8 of IS 1797
iv) Crude fibre, percent by weight, Max 3.5 13 of IS 1797
v) Acidity, as anhydrous tartaric acid acid, percent
by weight
12.0 to 26.0 Annex A
vi) Aflatoxin, g/kg, Max 30 Doc: No. FAD 28(2609)F
vii) Total viable count, per g, Max 106 IS 5402
viii) E. coli, per g, Max 10 IS 5887 (Part 1)
ix) Moulds, per g, Max 104 IS 5403
x) Salmonella, in 25 g Absent IS 5887 (Part 3)
Table 2 Requirements for Khatai (Raw Mango Slices)
(Clause 4.6)
Sl
No.
Characteristic Requirement
Method of test, Ref to
(1) (2) (3) (4)
i) Colour White to brown ii) Extraneous matter, percent by weight, Max
a) Inorganic
b) Organic
0.5
1.0
4 of IS 1797
iii) Slices below 15 mm in length, percent by
weight, Max
4.01)
Physical separation and
weighing
iv) Seed coating, percent by weight, Min (see 3.3) 3.0 Physical separation and
weighing
v) Damaged and discoloured slices, percent by
weight, Max (see 3.4)
3.0 Physical separation and
weighing
vi) Moisture, percent by weight, Max 10.0 9 of IS 1797
vii) Aflatoxin, g/kg, Max 30 Doc: No. FAD 28(2609)F
viii) Total viable count, per g, Max 106 IS 5402
ix) E. coli, per g, Max 10 IS 5887 (Part 1)
x) Moulds, per g, Max 104 IS 5403
xi) Salmonella, in 25 g Absent IS 5887 (Part 3)
1)shall be measured from one end to the other end of the slice.
5 PACKING AND MARKING
5.1 Packing
The product shall be packed in clean, sound and dry container made of metal, glass, food grade polymers, wood
or jute bags. The wooden boxes or jute bags shall be suitably lined with moisture proof lining which shall not
impart any foreign smell to the product. The packing material shall be free from any fungal or insect infestation
and should not impart any foreign smell. Each container shall be securely closed and sealed.
5.2 Marking
5.2.1 The following particulars shall be marked or labelled on each container/bag:
a) Name and address of the manufacturer or packer;
4
b) Name of the material;
c) Trade name of brand name, if any;
d) Batch or code number;
e) Net quantity;
f) Month and year of packing;
g) Best before (month and year); and
h) Any other information required under the Legal Metrology (Packaged Commodities) Rules, 2011 and
the Food Safety and Standards (Packaging and Labelling) Regulations, 2011.
5.2.1.1 If the containers are packed in cases, each case shall also be marked with the particulars (a) to (h) in
5.2.1.
5.2.2 BIS Certification Marking
The product may also be marked with the Standard Mark.
5.2.2.1 The use of standard mark is governed by the provisions of the Bureau of Indian Standards Act, 1986 and
the Rules and regulations made there under. The details of conditions under which a license for the use of the
Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian
Standards.
6 SAMPLING
Representative samples for testing the conformity of the final product to this specification shall be drawn
according to IS 13145.
7 TESTS
7.1 The sample of raw mango (Mangifera indica Linn.) powder (Amchur) and slices (Khatai) shall be tested for
ascertaining conformity of the material to the requirement of this specification by the methods of test referred to
in col 5 of Table 1.
7.2 Quality of Reagents
Unless specified otherwise, pure chemicals shall be employed in tests and distilled water (see IS 1070) shall be
used where the use of water as reagent is intended.
NOTE — 'Pure chemicals' shall mean chemicals that do not contain impurities which affect the test results.
ANNEX A [Table 1, Sl No. (v)]
DETERMINATION OF ACIDITY
A-1 REAGENTS
A-1.1 Sodium Hydroxide Solution — 0.1 N.
A-1.2 Phenolphthalein Indicator —1 percent (in alcohol).
A-2 PROCEDURE
Weigh about 0.5 g of sample in a 250 ml conical flask. Add about 100 ml of distilled water. Heat on a steam-
bath for about 15-20 minutes. Cool and titrate with 0.1 N NaOH using 2-3 drops of phenolphthalein indicator to
a pale pink end point. Note the titre value and calculate as follow.
A-3 CALCULATION
Acidity as anhydrous tartaric acid, percent by weight, (w/w) = 64 x titre x normality of NaOH x 100
1000 weight of sample
1
For BIS use only
DRAFT FOR COMMENTS ONLY Doc: No. FAD 09(2722)C
Draft Indian Standard
GARAM MASALA — SPECIFICATION
(First Revision of IS 13545) ICS No. 67.220.10
Not to be reproduced or used as
STANDARD without permission of BIS
Last date for comments: April 30, 2015
Spices and Condiments Sectional Committee, FAD 9
FOREWORD
(Adoption clause would be added later)
Spices and condiments and their blends are extensively used for culinary purposes in India and the neighbouring
countries. Garam masala is a blend of selected spices and aromatic herbs. It is used to garnish vegetarian and
non-vegetarian dishes to enhance flavour and aroma.
This standard was first published in 1992. This revision is being undertaken to align product description and
requirement of salt content with special grade of Agmark standard for garam masala and to include the
requirements for aflatoxin, total viable count, E. coli, moulds and Salmonella in line with Agmark standard.
In the formulation of this standard, due consideration has been given to the provisions of the Food Safety and
Standards Act, 2006 and the Rules and Regulations framed thereunder and the Legal Metrology (Packaged
Commodities) Rules, 2011. However, this standard is subject to the restrictions imposed under these, wherever
applicable.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.
1 SCOPE
This standard prescribes the requirements and methods of sampling and test for garam masala.
2 REFERENCES
The standards given below contain provisions which, through reference in this text, constitute provisions of this
standard. At the time of publication, the editions indicated were valid. All standards are subject to revision and
parties to agreements based on this standard are encouraged to investigate the possibility of applying the most
recent editions of these standards.
IS No. Title
1070 : 1992 Reagent grade water Specification (third revision)
1797 : 2015 Methods of test for spices and condiments (third revision) (under print)
5402 : 2012 Microbiology of food and animal feeding stuffs Horizontal method for the
/ISO 4833 : 2003 enumeration of microorganisms Colony count technique at 30 degree C
(second revision)
5403 : 1999 Method for yeast and mould count of food stuffs and animal feeds (first revision)
5887 Methods for detection of bacteria responsible for food poisoning
(Part 1) : 1976 Isolation, identification and enumeration of Escherichia Coli
(Part 3) : 1999 General guidance on methods for detection of SALMONELLA (second revision)
/ISO 6579 : 1993
13145 : 2014 Spices and Condiments Methods of sampling (second revision)
14216 : 1994 Code for hygienic practice for spices and condiments processing units
2
Doc: No. FAD 28(2609)F Draft Indian Standard Foodstuffs Determination of aflatoxin B1, and the total
content of aflatoxins B1, B2, G1 and G2 in cereals, nuts and derived products
High-performance liquid chromatographic method (Adoption of ISO 16050 : 2003)
(under print)
3 REQUIREMENTS
3.1 Description
3.1.1 Garam masala powder shall be obtained by grinding clean, dry and wholesome spices and condiments. It
shall contain minimum 90 percent of spices, It may contain added starch, pulses, edible oil and edible common
salt.
3.1.2 Garam masala shall be free from dirt, insect infestation, rodent excreta and hair, mould growth, when
examined with naked eye (corrected, if necessary, for abnormal vision) or with such magnification as may be
necessary. If the magnification exceeds 10 X, this fact shall be stated in the test report.
3.2 Taste and Flavour
The taste and flavour of garam masala shall be fresh and pleasant.
3.3 Garam masala shall also comply with the requirements given in Table 1.
Table 1 Requirements for Garam Masala
(Clause 3.3)
Sl
No.
Characteristic Requirement
Method of test, Ref to
(1) (2) (3) (4)
i) Moisture, percent by weight, Max 10.0 9 of IS 1797
ii) Total ash (on dry basis), percent by weight,
Max
7.0 6 of IS 1797
iii) Acid insoluble ash (on dry basis), percent by
weight, Max
1.0 8 of IS 1797
iv) Non-volatile ether extract (on dry basis),
percent by weight, Min
15.0 14 of IS 1797
v) Volatile oil (on dry basis), ml/100 g, Min 1.5 15 of IS 1797
vi) Crude fibre (on dry basis), percent by weight,
Max
15.0 13 of IS 1797
vii) Salt (as NaCl) (on dry basis), percent by
weight, Max
5.0 16 of IS 1797
viii) Lead (as Pb), (on dry basis), mg/kg, Max 5.0 Annex A
ix) Chromium salts Absent Annex B
x) Aflatoxin, g/kg, Max 30 Doc: No. FAD 28(2609)F
xi) Total viable count, per g, Max 106 IS 5402
xii) E. coli, per g, Max 103 IS 5887 (Part 1)
xiii) Moulds, per g, Max 104 IS 5403
xiv) Salmonella, in 25 g Absent IS 5887 (Part 3)
3.4 Garam masala shall be ground and packed under hygienic conditions (see IS 14216).
3.5 The pesticide residues, heavy metals, toxins (aflatoxins and other naturally occuring toxins), if any, in the
product shall not exceed the limits as prescribed in the Food Safety and Standards (Contaminants, Toxins and
Residues) Regulations, 2011.
4 PACKING
Garam masala shall be packed in scaled, clean and sound tinplate or glass containers or paper cartons properly
lined with water-proof paper or in moisture-proof bags made of a material which does not impart any smell to
the garam masala. The product shall be packed in quantities as stipulated under the provisions of the Legal
Metrology (Packaged Commodities) Rules, 2011. A suitable number of such containers/cartons shall be packed
in cardboard cases.
3
5 MARKING
5.1 The following particulars shall be marked or labelled on each container/carton in English/Russian/
French/Hindi:
a) Name of the material and trade name or brand name, if any;
b) Name and address of the manufacturer;
c) Batch or code number;
d) Net quantity;
e) The names of spices and condiments in descending order by weight;
f) Date of manufacture;
g) Best before date;
h) Directions for use; and
j) Any other information required under the Legal Metrology (Packaged Commodities) Rules, 2011 and
the Food Safety and Standards (Packaging and Labelling) Regulations, 2011.
5.2 Each case shall also be marked with the particulars (a) to (j) in 5.1.
5.3 If glass containers are used, each case shall be marked, in addition, with the words ‘Glass, Handle with care '.
5.4 BIS Certification Marking
The product may also be marked with the Standard Mark.
5.4.1 The use of standard mark is governed by the provisions of the Bureau of Indian Standards Act, 1986 and
the Rules and regulations made thereunder. The details of conditions under which a license for the use of the
Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian
Standards.
6 SAMPLING
Representative samples of garam masala for testing the conformity to this specification shall be drawn
according to IS 13145.
7 TESTS
7.1 The samples of garam masala shall be tested for ascertaining conformity of the material to the requirements
of this specification by the methods of test referred to in col 4 of Table 1.
7.2 Quality of Reagents
Unless specified otherwise, pure chemicals shall be employed in tests and distilled water (see IS 1070) shall be
used where the use of water as reagent is intended.
NOTE — 'Pure chemicals' shall mean chemicals that do not contain impurities which affect the test results.
ANNEX A
[Table 1 Sl No. (viii)]
DETERMINATION OF LEAD CONTENT
A-l PRINCIPLE
The sample is ashed and the acid solution of ash is neutralised with ammonia in the presence of citrate. Several
other interfering elements are complexed with cyanide and lead is isolated as lead dithizonate into chloroform.
The chloroform layer is shaken again with dilute nitric acid and chloroform layer is discarded. The aqueous
phase is buffered to pH 9.5 to 10 0 and lead is re-extracted with dithizone in chloroform. The colour produced
is read at 510 nm and is compared with standard.
4
A-2 REAGENTS
A-2.1 Lead Standard Solution
A-2.1.1 Stock Solution (1 mg lead/ml in 1 percent nitric acid) Dissolve 1.598 5 g of pure lead nitrate
[Pb (NO3)2] crystals in 1 percent nitric acid and dilute to 1 litre.
A-2.1.2 Working Solution Prepare as needed by diluting stock solution suitably with 1 percent nitric acid
solution.
A-2.2 Nitric Acid (1 percent) Dilute 10 ml of fresh, colourless nitric acid (sp gr 1.40) to 1 litre with
redistilled water. If acid is redistilled, boil off nitrous fumes before diluting.
A-2.3 Citric Acid Solution (Concentrated Lead Free Solution) Prepare the solution so that 1 ml of
solution contains about 0.5 g of citric acid.
A-2.4 Dithizone Solution [1 mg/ml in Chloroform (CHCl3)] Dissolve 100 mg of purified dithizone in
chloroform and dilute to 100 ml. Prepare dilute solution as needed by diluting stock solution suitably with
chloroform.
A-2.5 Potassium Cyanide Solution (10 percent, w/v) Dissolve 25 g of recrystallised, phosphate free
potassium cyanide (KCN) in water and dilute to 250 ml.
A-2.6 Ammonia-Cyanide Mixture To 100 ml of 10 percent potassium cyanide solution in a 500 ml
volumetric flask, add enough ammonium hydroxide (NH4OH) solution to introduce 19.1 g of ammonia (NH3)
and dilute to volume with water.
A-2.7 Washed Filter Paper Soak 9 cm quantitative papers overnight in 1 percent nitric acid. Wash with
large volumes of water on Buchner funnel to remove acid and any traces of lead.
A-3 PROCEDURE
A-3.1 Preparation of Sample
A-3.1.1 Accurately weigh representative sample of 5 to 100 g depending upon amount of sample available and
expected lead content, into a clean silica dish. Dry wet samples on steam bath or in oven.
A-3.1.2 Char the sample carefully over burner. Do not let the material to ignite. Charring of sample is carried
out by means of a soft flame to volatilize as much as possible of the organic matter. Materials being ashed must
not be allowed to ignite during any phase of ashing.
A-3.1.3 When the sample is dry and charred, place it in a temperature controlled muffle furnace and raise
temperature slowly without ignition. Cover the floor of furnace with a piece of asbestos board or silica plate so
that sample receives most of its heat by radiation and not by conduction. Ash the sample at temperatures not
exceeding 500°C for about 8 to 10 hours. If ashing is not complete after 30 minutes, remove the dish, cool and
cautiously add 2 to 3 ml nitric acid. Dry again and place in furnace and continue ashing until practically carbon-
free ash is obtained.
A-3.1.4 When clean ash is obtained, cool, cover the dish with watch glass and cautiously add 15 to 20 ml
concentrated hydrochloric acid (HCl). Rinse down the watch glass with water and heat on steam bath. If clear
solution is not obtained evaporate to dryness and repeat addition, of HCl. Dilute the clear solution with water to
a definite volume (filter solution if necessary, wash the insoluble material on filter successively with few
millilitre of hot HCl, hot citric acid solution and hot 40 percent ammonium acetate solution and make up to
100 ml). Prepare a sample blank solution using exactly the same amounts of reagents including water and
exposing the sample blank in furnace or on steam bath for the same length of time and giving identical treatment
as given in case of sample.
A-3.2 Isolation and Determination of Lead
A-3.2.1 Transfer suitable aliquot of ash solution of sample to a 250 ml separatory funnel and add citric acid
reagent and mix well equivalent to 10 g of citric acid and mix well.
5
A-3.2.2 Make slightly alkaline to litmus with ammonium hydroxide keeping the solution to cool, swirl gently
and let it stand for 1-2 minutes. At this stage, the solution should be clear without any precipitate. If precipitate
forms, redissolve with hydrochloric acid. Transfer the solution to a stoppered conical flask and adjust to pH 3.0
to 3.4 (bromophenol blue) with ammonium hydroxide. If enough iron is present to colour solution strongly,
adjust with the help of spot plate. Dissolve any precipitate, if formed, by shaking and cooling. If amount of lead
expected is small, add 5 to 10 mg of pure copper sulphate (CuSO4.5H2O) to solution. Pass hydrogen sulphide
until the solution is saturated (3 to 5 minutes) and immediately filter with suction. Dissolve the residue of
precipitated sulphides without previous washing, with 5 ml of hot nitric acid drawing solution through into
original flask, wash with hot water. Stopper the flask, shake the nitric acid and water, wash well and boil the
solution to remove hydrogen sulphite. Transfer this solution to separator funnel and add citrate solution
equivalent to 5 g of citric acid, make amoniacal.
A-3.2.3 To the clear solution add 5 ml of 10 percent potassium cyanide solution (more may be necessary if large
amounts of Zn, Cu, Cd etc, are present ). Shake and check the pH of the solution by adding a drop of thymol
blue indicator solution (pH should be preferably be 8.5 to 9.5, blue green to blue colour with thymol blue).
A-3.2.4 Immediately add 20 ml of dithizone solution (in this step usually solution of 8 mg dithizone/litre of
chloroform is adequate), shake for 20 to 30 seconds and let the layers to separate. Transfer the chloroform layer
to a small separatory funnel containing 25 ml of 1 percent nitric acid. Repeat, and continue extractions till the
chloroform layer is distinctly green. Drain all the extracts into the small separatory funnel containing 1 percent
nitric acid. Shake combined extracts well and drain the green dithizone layer into another separatory funnel
containing additional 25 ml portion of 1 percent nitric acid. Shake the contents and let the layers to separate and
discard the organic layer. Filter the acid extracts containing lead, in succession through small pledget of wet
cotton inserted in stem of a small funnel, into a 50 ml flask using second acid extract to rinse the separatory
funnel in which first extraction was made. Make up any slight deficiency in volume with 1 percent nitric acid
and mix.
A-3.2.5 Take suitable aliquot (or entire volume if needed) of the 50 ml of 1 percent nitric acid solution
containing lead to make total volume to 50 ml. Add 10 ml of ammonia-cyanide mixture and mix (pH is about
9.7). Immediately add appropriate volume of dithizone solution of suitable concentration, and shake for
1 minute and let the layers to separate. The appropriate volume and concentration of dithizone solution can be
chosen as per information provided in Table 2.
A-3.2.6 Drain the lower dithizone layer into a clean and dry tube and read the absorbance at 510 nm against a
reagent blank prepared by following all the steps as was done for sample but substituting the aliquot of ash
solution taken with same volume of 2 N HCl. Carry out isolation and determination of lead content in sample
blank solution in identical manner to that of sample solution.
Table 2 Range of Estimated Content, Concentration and Volume of Dithizone Solution
(Clause A-3.2.5)
Sl
No.
Lead Range Concentration of Dithizone in Chloroform
(mg of Dithizone/litre Solution)
Volume of Dithizone
Solution to be taken in ml
(1) (2) (3) (4)
i) 0 to 10 8 5
ii) 0 to 50 10 25
iii) 0 to 200 20 40
A-3.3 Preparation of Standard Curve
Prepare working curve of required range (to be decided basing on lead content of samples), starting with blank
to final standard of range with four intermediate increment.
A-3.3.1 Pipette appropriate amounts of lead solution into series of separatory funnels and add 1 percent nitric
acid solution so that total volume in each funnel is always 50 ml. Add the required volume of acid solution first
and then the proposed volume of standard solution.
A-3.3.2 Add 10 ml 6f ammonia-cyanide mixture and mix (resultant pH will be 9.7).
A-3.3.3 Develop the colour immediately by shaking for 1 minute with proper quantity of dithizone solution
(see Table 2). Let the layer to separate.
6
A-3.3.4 Drain the lower chloroform layer into a clean and dry tube. Read absorbance ‘A’ of each standard
extract against the extract of zero lead content (reagent blank of standards). Plot ‘A’ against g of lead.
NOTE Standard lead and 1 percent nitric acid solutions used in preparation of standard curve should be saturated with chloroform
before use, by shaking those solutions with clear chloroform discarding the organic layer.
A-4 CALCULATION
A-4.1 Convert absorbance ‘A’ to g of lead from the calibration curve.
A-4.2 Subtract the lead content obtained for sample blank solution from that of sample solution to get actual
lead content of sample and calculate the lead content of sample.
ANNEX B
[Table 1, Sl No. (ix)]
DETERMINATION OF CHROMIUM SALTS
B-1 PRINCIPLE
Chromates give violet colour with diphenyl carbazide reagent.
B-2 REAGENTS
B-2.2 Dilute Sulphuric Acid (1 : 7 v/v)
B-2.2 Diphenyl Carbazide Solution (0.2 percent w/v) in ethyl alcohol.
B-3 PROCEDURE
Ash about 2 g of the sample. Dissolve the ash in 4 to 5 ml of dilute sulphuric acid in a test tube and add 1 ml of
diphenyl carbazide solution. The presence of chromate is indicated by violet colour.