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“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 13228 (2006): Corrugated fibreboard boxes for packingand transportation [CHD 15: Paper and its products]

IS 13228:2006

af%JTmW@

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Indian Standard

CORRUGATED FIBREBOARD BOXES FORPACKING AND TRANSPORTATION — SPECIFICATION

Ju@ 2006

(First Revision)

ICS 55.160; 85.060

0 BIS 2006

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Price Group 7

(Reaffirmed - 2012)

Paper and Its Products Sectional Committee, CHD 15

FOREWORD

This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the drafi finalized by thePaper and Its Products Sectional Committee had been approved by the Chemical Division Council.

This standard was first published in 1991. in this revision, tolerance on dimension of assembled box, Cobb value ofcorrugated fibreboard boxes and minimum grarnmage of kraft paper used in linear and partition are modified. Requirementof mould inhibitor has been deleted. Marking clause has also been modified.

The general requirements of corrugated fibrebo-ard boxes for transportation of goods have been covered inIS 2771 (Part 1): 1990 ‘Corrugated fibreboard boxes — Specification: Part 1General requirements (second revision)’.in this standard, emphasis has been laid on the performance requirements of the boxes rather than the specifications ofthe raw materials such as krat?paper, adhesives, etc, which go into makiig of a box. As such, ultimate strength requirementsof the fibreboard box have been specified in this standard.

A scheme for labelling environment friendly products known as ECO-Mark has been introduced at the instince of theMinistry of Environment and Forests (MEF). The ECO-Mark would be administered by the Bureau of Indian Standards(BIS) under the BE Act, 1986 as per the Resolution No. 71 dated 20 February 1991, published in the Gazette of theGovernment of India. For a product to be eligible for ECO-Mark it shall also carry Standard Mark of BIS for quality, inaddition to the compliance with the optional environment tliendly (EF) requirements. For this purpose, the StandardMark of BIS would be a single mark being a combination of the 1S1Mark and the ECO logo. Requirements to besatisfied for a product to quali~ for the BIS Standard Mark for ECO friendliness, will be optional; manufacturing unitswill be free to opt for the 1S1Mark alone also.

The composition of the Committee responsible for formulation of this standard is given in Annex B.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observedor calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS 2: 1960 ‘Rules forrounding off numerical values (revised)’. The number of significant places retained in the rounded off value should bethe same as that of the specified value in this standard.

Indian Standard

CORRUGATED FIBREBOARD

IS 13228:2006

BOXES FORPACKING AND TRANSPORTATION — SPECIFICATION

(First Revision)

1 SCOPE

This standard covers requirements and methods ofsampling and test for corrugated fibreboard boxes forpackaging and transportation of various items such asapples, butter packed in primary cartons, canned/frozensea foods, cigarettes, soaps and jars/bottles of processedfoods.

2 REFERENCES

The standards listed below contain provisions whichthrough reference in this text, constitute provisions of thisstandard. At the time of publication, the editions indicatedwere valid.All standards are subject to revision, and partiesto agreements based on this standard are encouraged toinvestigate the possibility of applying the most recenteditions of the standards indicated below:

Is No.

1060 (Part 1):1966

2771 (Part 1):1990

4006 (Part 1):1985

4006 (Part 2):1985

4261:2001

6481:1971

7028 (Part 6):1987

7063 (Part 2):1976

7186:1973

Title

Methods of sampling and test for paperand allied products: Part 1 (revised)

Corrugated fibreboard boxes –Specification: Part 1 Generalrequirements (second-revision)

Methods of test for paper and pulpbased packaging materials: Part 1@strevision)

Methods of test for paper and pulpbased packaging materials: Part 2 (firstrevision)

Glossary of terms relating to paper andpulp based packaging materials (firstrevision)

Guide for principal uses and styles offibreboard containers

Performance tests for complete, filledtransport packages: “Part 6Compression test (fhsf revision)

Method of test for corrugatedfibreboard: Part 2 Edgewise crushresistance of board

Glossary of terms relating to paper andflexible packagrng

3 TERMINOLOGY

For the purpose of thiswandard, the terms and definitionsgiven in IS 2771 (Part 1), IS 4261 andIS7186 shall apply.

4 MATERIAL

4.1 The fibreboard shall be manufactured fi-omfibre basedpaper/paper board such as krafl paper, krafi liner, duplexboard, pulp board, etc, in suitable combination. This mayalso include coated, impregnated, waxed, laminated orbituminized paper or paperboard so as to satis~ therequirements of this standard.

4.2 Adhesive

Any suitable adhesive capable of firmly adhering thevarious plies together may be used. Sodium silicate or anyother highly alkaline adhesive shall not be used.

4.3 Staple Wire

Unless otherwise specified by the purchaser, galvanizedmild steel wire not less than 0,51 mm thick and 2.20 mmwide shall be used for stapling the manufacturer’s joint.

4.4 Linear and Partition

For packaging of glassjars and bottles filled-withprocessedfood, the side, top, bottom liners, centre layers and slottedpartitions, if required, shall be made from double wallboard of AB or AA flutting with all plies of minimumgrammage of150 g/m2of krafi paper.

5 STYLE

The boxes, with/without interior fitments shall conformto the appropriate styles, giveninIS6481, depending uponthe end use. Some of these are mentioned in Table 1.

6 MANUFACTURE, WORKMANSHIP AND FINISH

6.1 The boxes shall be manufactured from not more thantwo pieces offibreboard, scored and slotted to.form a bodypiece having 4 flaps for closing each of the opposite ends.The flaps along the longer edge shall form the outer flapsand those along the shorter edge shall form inner flaps.All flaps shall be of equal length and the outer flaps shallmeet when closed.

1

IS 13228:2006

6.2 The blanks shall beproperly creased andslotted, sothat when the box is assembled, there shall be no holes atthe comers. The flaps of the box shall be capable of beingfolded 180° along the line of creasing without fracture ofthe board or facings.

6.3 The body joint shall be lapped and lapping shall notbe less than 30 mm. The manufacturer’s joint shall besecured by staples, taping or glueing which shall be freefrom rust and not protruding. Each piece shall not havemore than two body joints,

8.2.3 The adhesive applied shall be in a strip not less than15 mm.

8.2.4 Tle adhesive shall be applied not nearer to a cutedge than 3 mm, and not nearer to a crease at the ends ofthe lap than 12 mm,

9 PERFORMANCE REQUIREMENTS

9.1 The corrugated fibreboard boxes shall comply withthe performance requirements given in Table 1.

7 DIMENSIONS AND TOLERANCES 9.1.1 Flat Crush Resistance

The flat crush resistance shall be applicable to 3 ply7,1 The internal dimensions of the assembIed box shallbe as agreed to between the purchaser and the supplier.

corrugated fibreboard boxes for packing of frozen seafoods and ilog legs, When tested as Ver 6 of IS 7063

It shall always be stated in the sequence of length (L) x (pm 2), its value shall not be less than 2,5 k~cmz.width (W) x height (1-f).

7.2 Normal manufacturing tolerances on the individualordered dimensions of the assembled boxes shall be asunder:

a) +3 mm for 3-ply boxes,

b) *5 mm for 5-ply boxes, and

c) +7 mm for 7-ply boxes.

8 MANUFACTURER’S JOINT

The manufacturer’s joint shall be stitched or glued asfollows.

9.1.2 Compression Test

The complete empty boxes used for packing of cigarettes,soaps and apples, conditioned at a temperature of 27 +2° C and 65 ● 5 percent relative humidity shall be testedin assembled condition for compression strength as permethod given in IS 7028 (Part 6). The average compressionstrength of the empty box at a deflection not more than20 mm shall not be less than 1kg/cm of base. However, incase of Type 1 boxes for cigarettes (for defence purposeonly) it shalI be minimum 2 k#cm of base.

9.1.3 Printability of Outer Surface

8.1 Stitched Joint The condition of the outer surface of the box shall be suchas to allow the marking, stamping or stenciling of the box

8,1.1 Stitching Lap with the type of ink normally used-for the purpose. The

The stitching lap shall be not less than 30 mm wide, and ink should not smudge or.discolour and itshould be water

may be inside or outside the box. resistant.

8.1.2 Spacing of Stitches 10 PACKING AND MARKING

The centre-to-centre spacing of stitches shall not exceed50 mm The clear distance tiom a cut edge of the fibreboard 10.1 Packing

to any stitch shall be not less than 6 mm and not more than Boxes shall be supplied in collapsed condition in bundles25 mm. The stitches shall be made at an angle of 45° to of 20 or as agreed to between the purchaser and thethe cut edge. supplier.

8.L3 Rows ofStitches 10.2 MarkingRows of stiches shall be used as ordered by the purchaser.

10.2.1 Each box shall be legibly and indelibly marked on8.2 Glued Joint the outside with the following particulars:

8.2.1 The glueing lap shall be not less than 30 mm wide. a) Indication of the source of manufacture,

b) Batch or lot number, and8.2.2 The adhesive used for the joint shall be waterresistant type. c) Any other information as required by the purchaser.

2

IS 13228:2006

Table 1 Performance Requirements for Corrugated Fibreboard Boxes

(Clauses 5 and 9.1)

S1No. Product to be Box Style Content Bursting Puncture Cobb-Value, Packed Weight Strength, JWin Resistance, A4in Max

kglcm’ kgf.cm(1) (2) (3) :) (5) (6) (7)

O

ii)

iii)

iv)

v)

vi)

vii)

Frozensea foodsand froglegs

Canned sea foods (exp)

Processedfoods in glassjarsand bottles

Cigarettes

Type 1

Type 2

Soaps

Apples

Butter

02010201

2030

1214

1215

101214

175200

8080

2030

175200

8080

02040204

0201 or0204

152030

— —

0201 or I 0000Cigarettes

30.5 100—

0202 61

120

240

200

100

80

80

100

—

160r20

25

6.5

15

14

—

0320

0201 or0204

Methods of Test — . 12.5 of 1S 1060 8 of IS4006 6 of IS4006(Part 1) (Part 2) (Part 1)

(Protection) Act, 1986 and the Rules made thereunder,while applying for ECO-Mark. Additionally themanufacturers shall also comply with the provisions underPrevention of Food Adulteration Act, 1954 and the Rulesmade thereunder, wherever necessary.

11.2 Specific Requirements

11.2,1 The material shall be of the following two typesdepending on the raw material used in the manufacture:

.10.2.2 BIS Certl~cation Mark

Each box may also be marked with the Standard Mark.

1-0.2.2.1 The use of the Standard Mark is governed by theprovisions of the Bureau of Indian Standards Act, 1986and the Rules and Regulations made thereunder. Thedetails of conditions under which the Iicence for the useof Standard Mark may be granted to manufacturers orproducers may be obtained from the Bureau of IndianStandards.

a)

b)

TypeA — Manufactured from-pulp containing notless than 60 percent by mass of pulp made tlommaterials other than bamboo, hardwood, soflwoodand reed.

TypeB — Manufactured from pulp made from 100

11 ADDITIONAL REQUIREMENTS FORECO-MARK

11.1 General Requirements

11.1.1 The product shall conform to the requirements forquality and performance prescribed under 4 to 9.

11,1.2 The manufacturer shall produce to BIS, theenvironmental consent clearance from the concerned StatePollution Control Board as per provisions of Water(Prevention and Control of Pollution) Act, 1974 and Air(Prevention and Control ofPollution) Act, 1981 along withthe authorization, if required under the Environment

percent waste paper or agricul&ral/industrial waste.

11.2.2 The material, if used for the packaging of foodmaterials, shall be manufactured from virgin pulp and shallbe free from dioxins. Printed surface of the paper shallnot come into contact with the food and the maximumamount of contaminants in paper intended to come intocontact with food shall not exceedlhe limitsTrescribed inTable 2 when tested according to the methods given inAnnex A.

3

IS 13228: 2i106

Table 2 Limits of Contaminants in Paper(Clause 11.2.2)

SI Contaminant Paper Intended to Paper Intended to Paper forNo. Come into Contact Come into Contact Filtration

with Dry Food with Wet Food andFood with Fatty Surface

(mg/kg of paper) (mg/kg of paper) (m#kg of paper)(1) (2) (3) (4) (5)

i) Cadmium (Cd) — 0.5 0.5

ii) Chromium (Cr ‘+) — 0.1 0.1

iii) Lead (Pb) — 3.0 3.0

iv) Mercury (Hg) — 0.3 0.3

v) Pentachlorophenol(PCP) 0.05 0.05 0.05

vi) Polychlorinatedbiphenyls (PCBS) 2.0 2.0 0.5

11.2.3 The corrugated fibreboard boxes for packing andtransportation may display in brief the criteria based onwhich the product has heen Iabelled as environmentfriendly.

11.2.4 The corrugated fibreboard boxes for packing andtransportation shall be sold along with instruction forproper use and mode of safe disposal so as to maximiseits performance and minimise wastage.

11.2.5 It shall be suitably marked that ECO-Mark label isapplicable only to the corrugated fibreboard boxes forpacking and transportation if content is not separatelycovered under the ECO-Mark scheme.

NOTE — It may be stated that the ECO-Mark is applicable tothe productor packaging material or both,

11.2.6 For ECO-Mark, corrugated fibreboard boxes forpacking and transportation shall be packed in suchpackages which shall be recyclable/reusable orbiodegradable.

12 SAMPLING, CONDITIONING AND TESTING

12.1 The boxes shall be sampled and tested within20 days of their receipt by the purchaser. From eachconsignment of 10000 boxes or part thereof, 20 boxesshall be selected for testing as follows:

a) If the boxes are bundled, 20 bundles shall beselected at random and from each bundle soselected one box shal) be selected at random fortesting, and

b) If the boxes are not bundled, 20 boxes shall beselected at random from the total consignment.

12.2 Conditioning

The sample of 20 boxes so selected sha[l be deemed torepresent the whole consignment of boxes and shall beconditioned for testing by the method prescribed in 5 ofIS 1060 (Part 1).

12.3 Testing

12.3.1 The types of tests and selection of boxes fortesting shall be as irrdicated in Table 3.

12.3.1.1 The requirements for the material of constructionof box as well as method of test for evaluating theserequirements shall be as given in relevant clauses and inTable 3.

12.4 Acceptance and Retesting

12.4.1 Acceptance

The consignment of boxes shall be deemed to comply withthe test requirements of the standard if after the specifiednumber of boxes fi-omthe test samples as given in Table 3have been tested as required in relevant clauses and allthe boxes pass the test.

12.4.2 Retests

If only one box from the test sample fails to meet one ormore of the tests, fimtherboxes shall be selected at randomfrom the consignment of boxes for testing for the defectiveproperty or properties. The number of additional boxes tobe tested shall be twice the number specified in Table 3for the test or tests in which the%ox tlom the original testsample failed.

4

IS 13228:2006

Table 3 Testing of Boxes(C/auses -12.3.1, 12.3.1.1, 12.4.1 and 12.4.2)

S1No. ~pe of Test No. of Boxes No. of Test No. of Tests on Method of TestSelected from Specimens. Each Specimen Ref to

Sample for Obtained from ClauseTesting Each Box

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

O Burstingstrength 3 1

ii) Punctureresistance 3 4(2 each for

CD and MD)

iii) Water absorption, 30 min Cobb test 3 2(One from (On external

outer box andone frominner box)

iv) Compressionstrengthtest 5 1

10 12.5 of IS 1060(5 each side) (Part 1)

1 8 of IS 4006(Part 2)

6 of IS 4006(Pi 1)

surfaceof theouter piece ofthe box andon internal

surfaceof theinner pieceof the box )

1 IS 7028 (Part 6)

ANNEX A(Clause 11.2.2)

DETERMINATION OF CHROMIUM, LEAD, MERCURY, CADMIUM, PENTACHLOROPHENOLAND POLYCHLORINATED BIPHENYLS

A-1 -DETERMINATION OF CHROMIUM (as Cr 6+)

A-1.1 Principle

The hexavalent chromium is determined colorimetrictilIyby reaction with diphenylcarbazide in acid solution at awavelength of 550 nm.

A-1.2 Apparatus

A-1.2. 1 Spectrophotometer

Any spectrophotometer suitable for measurementat a wavelength of about 550 nm or photoelectricabsorptiometer fitted with filters giving maximumtransmission near 550 nm.

A-1.2.2 Shaker

Any shaker suitable for rotating/moving at30 ● 2 rev/ min.

A-1.3 Reagents

A-1.3. 1 Extraction Fluid— Mix 5.7 ml of acetic acid indistilled water.

5

A-1.3.2 Nitric Acid, concentrated.

A-1.3.3 Sulphuric Acid, approximately 0.2 N.

A-1.3.4 Diphenylcarbaziz.ie Solution — Dissolve 0.25 gof diphenylcarbazide in 50 ml acetone. Store in a brownbottle. Discard when solution becomes discolored.

A-1.3.5 Stock Chromium Solution — Dissolve O.141 gK2Cr207 in distilled water and dilute to 100 ml. Onemillilitre of this solution contains 500 ~g of chromium(as Cr b+).

A-1.3.6 Intermediate Chromium Solution — Take 10 mlof stock chromium solution and dilute to 1 000 ml withdistilled water. One millilitre of this solution contains 5.00pg of chromium (as Cr 6+).

A-1.3.7 Standard Chromium Solution — Take 10 ml ofintermediate chromium solution and dilute to 1 000 mlwith distilled water. One millilitre ofthis solution contains0.05 pg of chromium (as Cr 6+).

A-1 .3.8 Indicator Paper — Covering the pH range0.5 to 1.5.

IS 13228:2006

A-1.4 Procedure A-1.4.2.3 According totheexpected chromium content,take an aliquot portion of the test solution containing

A-1,4.1 Preparation of Calibration Curve 10 to 100 pg of chromium to a‘100-ml volumetric flask.

Into each of a series often 250-ml volumetric flasks, place Adjust thepH of the solution to 1.0 + 0.3 by adding 0.2 N

the quantities of standard Chromium solution as indicated sulphuric acid. Dilute to 100 ml. Add 2 ml

below: diphenylcarbazide solution, mix thoroughly, and wait for10 min.

Standard Chromium Solution Corresponding to Cr b+ml 1% .A-.I.4.2.4 Photometric measurement

1.0 0.05 Carry out the photometric measurements of thetest solution

2.0 0.10according-to the methods given in A-1.4.1.1.

3.0 0.15 A-1.4.3 Calculation4.0 0.20 By means of the calibration curve (see A-1.4.1.3)5.0 0.25 determine the quantity of chromium present:

6.0

7.0

0.30

0.35mxD

Chromium (as Cr 6+),ppm = ~

8.0 0.40 where9.0 0.45

m = mass of chromium determined in the aliquot of10.0 0.50 the sample solution, in ~g;

A-1.4.1.1 Add sulphuric acid to adjust the solution pH to D = ratio of the volume of test solution to the volume

1.0 * 0.3 in each flask and dilute to 100 ml. Add 2.0 ml of aliquot portion taken for the colour

diphenylcarbazide solution, mix thoroughly and wait for development and

10 min. M= mass of paper sample taken for testing, in g.

A-1.4.1.2 Carry out the measurement on the A-2 DETERMINATION OF MERCURY (as Hg)spectrophotometer or on a photoelectric calorimeter usingappropriate filter with a 1 cm cell at a wavelength of A-2,1 PrinciPle550 nm. As references use extraction fluid, correct theabsorbance readings of standard solution by subtracting

The flameless atomic absorption procedure is a physical

absorbance of a reagent blank carried through the abovemethod based on the absorption of radiation at 253.7 runby mercury vapour. The mercury is reduced to the

method.elemental state and aerated from solution in a closed

A-1 .4.1.3 Construct a calibration curve by plottingsystem. The mercury vapour passes through a cell

corrected absorbance values against chromium content inpositioned in the light path of mercury hallow cathode lamp

microgram per 102 ml.of an atomic absorption spectrophotometer. Absorbance(peak height) is measured as a function of mercury

A-1.4.2 Determinationconcentration and record,

A-1.4.2.1 Sample preparation

Tear the air dry sample into pieces of suitable size. Do notuse cut or punched edges or other parts where metalliccontamination may have occurred.

A-1.4.2.2 Preparation of test solution

Weigh to the nearest 0.01 g about 20 g of paper, leach thepaper with about 200 ml of extraction fluid for 18+2 husing shaker rotating/moving at 30 * 2 rev/rein. Filter theextract through glass fibre filter with 0.45 micron poresize. Add sufilcient amount of aluminium sulphate andfilter, if any precipitate appears. Transfer the solutionquantitatively to a volumetric flask of suitable capacity,dilute to the mark and mix.

A-2.2 Apparatus

A-2.2. 1 Atomic Absorption Spectrometer (AAS) andAssociated Equipment — Instrument settingsrecommended by the manufacturer shall be followed.Instruments designed specifically for the measurement ofmercury using the cold vapour technique may besubstituted for the AAS.

A-2.-2.2 Mercury Vapour Generation Assembly —Consists of an absorption cell, peristaltic pump, flow meter,aeration tubing and a drying tube containing magnesiumperchlorate.

A-2.2.3 A4ercwy Hollow Cathode Lamp

6

A-2.2.4 Recorder/Printer/Display Meter — Anymulti-range variable recorder that is compatible with theUV detection system is suitable,

A-2.3 Reagents

A-2.3.1

A-2.3.2

A-2.3.3

Sulphuric Acid concentrated.

Nitric Acid concentrated.

Stannous Chloride Solution — Dissolve 25 g ofstannous chloride (SnClz) in water containing 50 ml of-concentrated hydrochloric acid and dilute to 250 ml. If asuspension forms, stir reagent continuously during use.

A-2.3.4 Sodium Chloride — Hydroxylamine SulphateSolution — Dissolve 12 g of-sodium chloride and 12 g.ofhydroxylamine sulphate ,@IHzOFI)zHZSOain distilled waterand dilute to 100 ml.

A-2.3.5 Potassium Pi?rmanganate Solution — Dissolve5 g of potassium permanganate in distilled water anddilute to 100 ml.

-A-2.3.+ Potassium Persulphate Solution — Dissolve 5 gof potassium persulphate in distilled water and dilute to100 ml.

A-2.3.7 Stock Mercwy Solution — Dissolve 1.354 g ofmercuric chloride in about 700 ml of distilled water. Add10 ml of concentrated nitric acid and make up to 1000ml. One millilitre of the solution contains 1mg of mercuryas Hg.

IS 13228:2006

A-2.3.8 Standard Mercury Solution

Prepare a series of standard mercury solutions containingOto 5@l by appropriate dilution of stock mercury solution(see A-2.3.7) with water containing 10 ml of concentratednitric acid per Iitre. Prepare standards daily.

NOTE — Use mercwy free distilled waterfor the preparationofreagentsand standards.

A-2.4 Procedure

A-2.4.1 Instrument Operation

Follow the procedure of the manufacturer’s operatingmanual. Connect the mercury vapour generating assemblyas shown in Fig. 1.

A-2.4.2 Standardization

Transfer 100ml of each of the 1.0,2.0 and.5.Opg/1standardmercury solution and a blank of 100 ml water to 300 ml+30D bottles. Add 5 ml of concentrated sulph~ic acid and2.5 ml of concentrated nitric acid to each bottle. Add 15‘mlof potassium permanganate solution to each .bottle andlet stand for at least 15 min. Add 8 ml of potassiumpersulphate (KZS208)solution to each bottle and heat for2 h in a water bath at 95”C. Cool and add 6 ml of sodiumchloride-hydroxy lamine sulphate solution to reduce theexcess permanganate. After decolourization add 5 ml ofstannous chloride solution and attach the bottleimmediately to the aeration apparatus forming a closedsystem. As mercury is volatilized and carried into theabsorption cell, absorbance will increase to a maximumwithin a few seconds. As soon as recorder returns

ro-1 DIR PUMP

DES=~

i

RECORDER HOLLOW

: .Y

m ‘E RABSORPTION CELL

AA DETECTORBUBBLER P

SAMPLE SOLUTION SCRUBBER CONTAINING A

IN BOD BOl_fLE MERCURY ABSORBING MEDtA

FIG.’1 SCHEMATICARRANGEMENTOF EQUIPMENTFORMEASUREMENTOF

MERCURY BY COLD VAPGURATOMIC ABSORPTIONTECHNIQUE

7

IS 13228:2006

approximately to the base line, remove stopper holdingthe aeration fi-itfrom the reaction bottle and replace witha bottle containing distilled water. Flush the system for afew seconds and run the next standard in the same manner.Construct a standard calibration curve by plottingabsorbance (peak height) versus mercury concentrationin pg.

A-2,4.3 Determination

A-2.4.3. 1 Sample preparation

Tear the air dry sample into pieces of suitable size. Do notuse cut or punched edges or other parts where metalliccontamination may have occurred.

A-2.4.3.2 Preparation oftest solution

Weigh to the nearest 0.01 g about 20 g of paper, leach thepaper with about 200 ml of extraction fluid for 18+2 husing shaker rotating/moving at 30 + 2 rev/rein. Filter theextract through glass flbre filter with 0.45 micron pore.size. Transfer the solution quantitatively to a volumetricflask of suitable capacity, dilute to the mark and mix.

A-2.4.3.3 According to the expected mercury content, takean aliquot portion of the test solution containing motmorethan 5 I.@ of mercury to a 300 ml BOD bottle and treat asin A-2.4.2.

A-2.5 Calculation

Determine peak height of sample from recorder chart, readmercury value from standard curve and determine themercury content of the sample using the following formula:

CxvMercury (as Hg), ppm = ~ ~ ~ 000

where

C = concentration of mercury from the calibrationcurve;

V = volume of test solution prepared, ml; and

M= mass of paper sample taken for testing, g.

A-3 DETERMINATION OF LEAD (AS Pb)

A-3.1 Principle

The lead content of the sample is determined byelectrothermal atomic absorption spectrometric method.

A-3.2 Apparatus

A-3.2.1 Atomic Absorption Spectrometer with graphiteoven technique in place of conventional burner assembly.

A-3.2.2 Lead Hollow-Cathode Lamp or MultielementHollow-Cathode Lamp, for use at 283.3 nm.

1

4-3.2.3 Hot Plate

4-3.3 Reagents

A-3.3.1

4-3.3.2

4-3.3.3

A-3.3.4

Nitric Acid, concentrated.

Nitric Acid 1:1.

Dilute Nitric Acid 1:499.

Stock Lead Solution

Dksolve 1.5999 g of Pb (IW3)2 in a mixture of 10 ml ofconcentrated HN03 and 100 ml of water and dilute to oneIitre.One millilitre of this solution contains 1.0mg of lead[as Pb).

A-3.3.5 Intermediate Lead Solution

A-3.3.6 Standard Lead Solution

Dilute 100 ml of intermediate lead solution to one litrewith dilute nitric acid (1 : 499). One milliliter+,of thissolution contains 0.1 mg of lead (as Pb).

A-3.4 Procedure

A-3.4. 1 Sample Preparation

Tear the air dry sample into pieces of suitable size. Do notuse cut or punched edges or other parts where metalliccontamination may have occurred.

A-3.4.2 Preparation of Test Solution

Weigh to the nearest 0.01 g about 20 g of paper, leach thepaper with about 200 ml of extraction fluid for 18+2 husing shaker rotatingjmoving at 30 * 2 rev/rein. Filter theextract through glass tibre .tilter with 0.45 micron poresize.

A-3.4.3 Transfer the extract to a 250-ml conical flask,Add 5 ml concentrate nitric acid and a few boiling chipsor glass beads, Slowly evaporate on a hot plate-to about10 to 20 ml. Continue heating and adding concentratednitric acid until digestion is complete. Wash down withwater and then filter, if necessary. Quantitatively transferfiltrate to a 100-ml volumetric flask, dilute to the markand mix thoroughly,

A-3.4.4 Inject a measured portion of the digested solutioninto the graphite oven. Dry, char and atomize accordingto the preset programme. Measure the absorbance.

A-3.4.5 Prepare a reagent blank and sufficient standardscontaining 5.0, 7.5 and 10.0 mg/1 of lead by dilutingsuitable volume of the standard lead solution with nitricacid (1 : 499) and repeat as above (see A-3.4.3). Inject asuitable portion of each standard solution in order of

8

increasing concentration. Analyze each standard solutionand measure the absorbance.

A-3.4.6 Calculation

, Construct a standard calibration graph by plotting theabsorbance versus lead concentration of each standard inmilligram. Read the concentration of the sample flom thegraph and determine the lead content of the sample fromthe calibration graph using the following formula:

Lead (as Pb), ppm =CXFX1O()

M

where

C = concentration of lead from the calibration curve;

F = dilution factor; and

M = mass of paper sample taken for testing, in g.

A-4 DETERMINATION OF CADMIUM (AS Cd).

A-4. 1 Principle

The cadmium content of the sample is determined byelectrothermal atomic absorption spectrometric method.

A-4.2 Apparatus

A-4.2. 1 Atomic Absorption Spectrometer with graphiteoven technique in place of conventional burner assembly.

A-4.2.2 Cadmium.HolIow-Cathode Lamp or MultielementHollow-Cathode Lamp, for use at 228.8 nm.

A-4.2.3 Hot Plate

A-4.3 Reagents

A-4.3.1 Ntric Acid concentrated.

A-4.3.2 Nitric Acid, 1:1.

A-4.3.3 Dilute Nitric Acid, 1:499.

A-4.3.4 Stock Cadmium Solution — Dissolve 1.0 g ofpure cadmium metal in minimum quantity of concentratednitric acid and dilute to one litre with distilled water. Onemillilitre of this solution contains 1 mg of cadmium(as Cd).

A-4.3.5 Intermediate Cadmium Solution — Add 1 ml ofconcentrated nitric acid to 50 ml of stock solution anddilute to one Iitre with distilled water. One millilitre ofthis solution contains 50 ~g of cadmium (as Cd).

A-4.3.6 Standard Cadmium Solution — To 10 ml ofcadmium intermediate solution add 1 ml of concentrated

IS 13228:2006

nitric acid and dilute to one litre with distilled water. Onemillilitre of this solution contains “0.5 pg of cadmium(as Cd).

A-4.4 Procedure

A-4.4. 1 Sample Preparation

Tear the air dry sample into pieces of suitable size. Do notuse cut or punched edges or other parts where metalliccontamination may have occurred,

A-4.4.2 Preparation of Test Solution

Weigh to the nearest 0.01 g about 20 g of paper, leach thepaper with about 200 ml of extraction fluid for 18+2 husing shaker rotating/moving at 30 * 2 Fev/min.Filter theextract through glass fibre filter with 0.45 micron poresize,

A-4.4.3 Transfer the extract to a 250-ml conical flask.Add 5 ml concentrate nitric acid and a few boiling chipsor glass beads. Slowly evaporate on a hot plate to about10 to 20 ml. Continue heating and adding concentratednitric acid until digestion is complete. Wash down withdistilled water and then filter if necessary, Quantitativelytransfer filtrate to a 100-ml volumetric flask, dilute to themark and mix thoroughly.

A-4.4.4 Inject a measured portion of the digested solutioninto the graphite oven. Dry, char and atomize accordingto the preset prograrnrne. Measure the absorbance.

A-4.4.5 Prepare a reagent blank and sufficient standardscontaining 5.0,7.5 and 10.0 mg/1of cadmium by dilutingsuitable volume of the standard cadmium soluticm withnitric acid (1 : 499). Inject a suitable portion of eachstandard solution in order of increasing concentration.Analyze each standard solution and measure the ‘absorbance.

A-4.4.6 Calculation

Construct a standard calibration graph by plotting theabsorbance versus mg of cadmium concentration of eachstandard. Read the concentration of the sample from thegraph and determine the cadmium content of the sampleI?om the calibration graph using the following formula

CXFX.1OOCadmium (as Cd), ppm = M

where

C = concentration of cadmium from the calibrationcurve;

F= dilution facto~ and

M= mass of paper sample taken for testing, in.g,

9

IS 13228:2006

A-5 13ETERM1NATION OF PENTACHLOROPHENOL (PCP)

A-5.1 Principle

PCP is extracted with acetone by Soxhlet extraction.Acetone extract is evaporated to dryness and subjected toacetylation. The acetylated PCP is determinedquantitatively by Gas “Chromatograph-Electron CaptureDetector (GC-ECD).

A-5.2 Apparatus

A-5.2.1

A-5.2.2

A-5.2.3

A-5.2.4

A-5.2.5

Round Bottom Flask, 250 ml.

Soxhlet Extractor

Water Bath

Separating Funnels, 60 ml and 100 ml.

Injection Syringes, 1 pl, 5 V1and 10 pl.

A-5.2.6 Gas Chromatography with ECD, capillary

columns.

A-5.2.7 Glass Columns — Length 20 cm, internal diameter12 mm filled with 5 cm of silica gel having particle size63 pm x 200 ~m.

A-5.3 Reagents

A-5.3. 1 Acetone

A-5.3.2 n-Hexane

A-5.3.3 Acetic Anhydride

A-5.3.4 Sodium Sulphate Anhydrous

A-5.3.5 PCP Stock Solution — Dissolve 10 mg ofpentachlorophenol in 100 ml of acetone. One millilitre ofthis solution contains 0..1mg of pentachlorophenol.

A-5.3.6 PCP Standard Solution — Dilute 10 ml of stocksolution with acetone to 100 ml. One millilitre of thissolution contains 0.01 mg of pentachlorophenol.

A-5.3.7 .Internal StandardStock Solution — Dissolve 1gof 2, 4 dibromophenol in 1 1of acetone. One millilitre ofthis solution contains 1 mg of dibromophenol.

A-5.3.8 Internal Standard Solution — Dilute 1 ml of thestock solution (see A-5.3.7) with acetone to 100 ml. Onemillilitre of this solution contains 10 ~g of dibromophenol.

A-5.4 Procedure

A-5.4.1 Determine the moisture content of the sample asgiven in 9 of IS 1060 (Part 1).

A-5.4.2 Weigh accurately about 1 g of the paper samplepieces up to two decimal places and put into a thimble.Extract with about 150 ml of acetone by Soxhlet extractionfor 6 h. Filter the acetone extract, dry over anhydroussodium sulphate, and evaporate under vacuum to a smallvolume approximately to 5 ml and cool.

A-5.4.3 Clean-Up

Transfer the extract (see A-5.4.2) to the silica gel packedcoloumn and elute with about 25 ml of n-hexane at therate of 2 ml/min. Collect the eluent in a flask. Dry overanhydrous sodium sulphate and evaporte nearly to dryness.

A-5.4.4 Treat the residue (see A-5.4.3) with 1ml of aceticanhydride, and heat on a water bath for about 30 min.Remove the flask from the water bath and cool theacetylated product. Transfer the content in a separatingfunnel and add 10 ml of hexane and 5 ml distilled water.Shake well for 2 min and let the layers be separated. Collectthe hexane layer, dry cwer anhydrous sodium sulphate andevaporate nearly to dryness. Cool for at least 10 rein, add1 ml of internal standard solution and adjust the volumeto 5.0 ml with n-hexane.

A-5.4.5 Inject 2 pl of the solution into the gaschromatography. Record the peak size in area and peakheight units. If peak response exceeds linear range of thesystem, dilute the concentration of the extract andreanalyze.

A-5.4.6 Calibration

Prepare three calibration standards from the PCP standardsolutions. Add 1ml of internal standard solution and followthe steps as above (see A-5.4.3 to A-5.4.5), Tabulate peakheight or.area responses against calculated equivalent massof underivatized pentachlorophenol injected. Prepare acalibration curve.

A-5.5 Calculation

Determine the PCP content of the sample from thecalibration graph using the following formula:

PCP content, mg/kg

,4x~xqx loo”on dry matter=

~xcxv,x(loo-~

where

A = PCP content from the graph, in pg;

B = total volume of hexane extract beforederivetization, in ml;

V,= volume of eluent injected, in ml;

10

M-=mass of the paper sample taken for testing, in g;

C = volume of hexane extract carried throughderivatization, in ml;

~= volume of total eluent, in ml; and

X= moisture content, percent by mass.

A-6 DETERMINATION OF POLYCHLORINATEDBIPHENYLS (PCBS)

A-6.1 Principie

PCB is extracted with boiling etharmlic potassiumhydroxide soiuticm.An aiiquot of the extract is mixed withdistiiled water and subjected to extraction with hexane.The PCB content is determined quantitativeiy by GC-ECDby comparing the pattern of the peaks with the pattern ofa suitabie technicai PCB.

A-6.2 Apparatus

A-6.2.1

A-6.2.2

A-6.2.3

A-+.2.4

Erlenm~er Flask, 200 mi.

Water Bath

Separating Funnels, 60 mi and 100 ml.

Injection ‘syringes, 1 pi, 5“pi and 10 PI.

A-6,2.5 Gas Chromatography with ECD, capiiiarycolumns.

A-6.2.6 Glass Columns — Length 20 cm, intemai diameter12 mm fiiled with 5 cm of silica gei having particie size63 pm x 200 pm.

A-6.3 Reagents

A-6.3. 1 Ethanolic Potassium Hydroxide Solution —Prepare 1 N ethanolic potassium hydroxide solution bydissolving the required amount of potassium hydroxide inabsoiute ethanoi that has been purified as foiiows:

Dissoive 1,5 g of siiver nitrate in 3 ml of water andadd it to one litre;of alcohol. Dissolve 3 g of potassiumhydroxide in the smallest amount ofhot distiiied water,cooi, and add it to the silver nitrate solution. Shakethoroughly, aliow the soiution to stand for at least24 h, fiiter and distiil.

NOTE — Absolutealcohol denaturedwith 10 percentby volumeof methanolmay also be used.

A-6.3.2

A-6.3.3

A-6.3.4

n-Hexane

Sodium Sulphate Anhydrous

PCB Stock Solution — Dissoive 10 mg of any

IS 13228:2006

PCB technical in i 00 ml of hexane. One miiiilitre of thissoiution contains 0.1 mg of PCB.

A-6.3.5 PCB Standard Solution — Diiute 10 mi of stocksoiution with hexane to 100 ml. One millilitre of thissolution contains 0.01 mg of PCB.

A-6.3.6 Internal Standard Stock Solution — Dissoive 1 g ‘of2,4 dibromophenol in 1 i ofn-hexane. One miliiiitre ofthis soiution contains 1 mg of dibromophenoi.

A-6.3.7 Internal Standard Solution — Dilute i mi of thestock solution (see A-6.3.6) with hexane to 100 mi, Onemiliilitre of this solution contains 10 pg of dibromophenol,

A-6.4 Procedure

A-6,4.1 Determine the moisture content of the sampie asgiven in 9 of IS 1060 (Part 1).

A-6.4,2 Weigh accurately about 1 g of the paper sampiepieces up to two decimal piaces and take into a 200-miErienmeyer flask. Add 50 ml of ethanolic potassiumhydroxide soiution and heat under reflux condenser for4 h, fiiter and dilute to the mark with alcohoi in a 250-mlvolumetric flask. Take an aliquot portion of the test solutionin a separating funnel, add sufficient distiiied water and15 ml hexane. Shake weii for 5 min and wait fori 5 min. Coiiect the hexane phase.

A-6.4.3 Fiiter the hexane extract. Dry the filtrate overanhydrous sodium sulphate, and evaporate under vacuumto approximately 5 ml. Take the residue for clean-up.

A-6.4.4 Clean-Up

Transfer the hexane extract (see A-6.4.3) to the silica geipacked coiumn and elute with about 25 ml of n-hexane atthe rate of 2 ml/min, Collect the eluent in a flask andevaporate to a smaii volume. Add 1mi of intemai standardsolution and make up to 10 mi with hexane.

A-6.4.5 Inject 2 pl of the solution to the gaschromatography. From the peaks obtained, PCB andinternal standard are -identified by their retention times asweil as reiative.retention time.

A-6.4.6 Calibration

Prepare three calibration standards from the PCB standardsolutions and foiiow the steps as above (A-6.4.3to A-6.4.5). Tabuiate peak height or area responsesagainst calculated equivalent mWs of underivatizedpentachlorophenoi injected. Prep&e a calibration curve.

A-65 Caicuiation

Determine the PCB content of the sample from thecalibration graph using the foiiowing formuia

-11

IS 13228:2006

PCB content, mglkgAxv, xloo”

on dry matter=&fx Vtx(]()()-x)

where

A = PCB content from the graph, in ~g

V,= volume of eluent injected, in ml;

M= mass of the paper. sample taken for testing, in g;

~ = volume of total eluent, in ml; and

X= moisture content, percent by mass,

ANNEX B(Foreword)

COMMITTEE COMPOSITION

Paper and Its Products Sectional Committee, CHD 15

Organization

Central Pulp & Paper ResearchInstitute, Saharanpur

All India Federationof Master Printers, New Delhi

B&A Multiwall Packaging Ltd, Kolkata

Ballarpur IndustriesLtd, New Delhi

CentralForerrsicScienceLaboratory,NewDelhi

CenturyPulpandPaperMills,Nainital

CentralPulp&PaperResearchInstitute, Saharanpur

Central RevenuesControl Laboratory,New Delhi

Crop Care Federationof India, New Delhi

Dcfence Materials& Stores,R & D Establishment,Kanpur

Departmentof Industrial Policy& Promotion, New Delhi

Directorate General of Supplies& Disposals,New Delhi

Directorate of Printing (Ministry of Urban Development), New Delhi

Federationof Corrugated Box Manufacturers of hsdirt,Mumbai

Federationof PaperTradersAssociationof Indi% Mumbai

ForestResearchInstitute, Debra Dun

Hindustan Lever Limited. “Mumbai

Hindustan PaperCorporation Ltd, Kolkata

Representative(s)

DRA. G KULKARNI(Chahnan)

SHRIS. R. SHARMA

SHRIV. K. MALIK(Alternate)

SHP.-RONODURJOYROYCHOUOHURY

DR S. C. SHENOY

SHRIK. D. PRASA~(Affernde)

SHRJS. L. kfUKHI

SHIUD. P, CHANOARANA

DR S. K, KAPOORDRY V. SOOD(Alternate)

DRY. K. S. RATHOIWSHRII. C. VARSHNEV(Alternate)

DR D. K. JAIN

SHRIS. P. BAJPAISHRIV. K. SKWH(Alternate)

SHRIP. K. JmNDR K. R. MURTHV(A2/ernate)

SHRIH. M. RATHI

SHSUJAGSNOERSIFWH

SHRIPANKAJD. SHAHSHRIM. L. MEHRA(Ahernale)

SHRISATYAPALGUPTASHIUBADALCHAUDHURI(A/ternate)

DR K. S. BHANOARS

SHRIM. V. PRABHAXAIMNSHRIM. K. LAHnu(Alternate)

SHN RAJ1PHILIPSHRIJ. D. FERNANDSS(Alternate)

12

IS 13228:2006

Organization Representative(s)

hrdia Security Press,Nasik SHRISWAPANKUMARGHOSHSHIUMANISHSHANKAR(Alternate)

Indian Paper ManufacturersAssociation, New Delhi SHRIR. VARDHANSHRIR. N. MOORTHY(Ahernafe)

Indian Pulp and PaperTechnical Association, Saharanpur SHIUANILKUMARDR M. PATEL(AIternate)

Indian Instituteof Packaging, Mumbai SHRIRAJIVDHARSHRIK. B. GUPTA(Ahernare)

Indian Institute of Technology,Roorkee Campus, %haranpur DR J. S. UPADHVAYADR A. K, R.m(Ahernare)

Indian Recycled Paper Mills Association, Delhi SHIUR. C. RASTOGI

JK Paper Ltd, New Delhi SHIUS. C. MAJUMDAR

Ministry of Defence (DGQA), New Delhi SHRIK. N. PATILSHP.IP. H. KULKARNI(Alternate)

NEPA Limited, Nepanagar SHIUMANURASTOGISHRINIAZIR./% KHAN(~/~ernU?e)

Regional ResearchLaboratory (CSIR), Jorhat SHIUS. K. GHOSHDR FARIDALI (Alternafe)

Security Printing Press,Hyderabad SHIUP. N. RADKARSHRIS. G. K. ACHARYULU(,4/ierrrafe)

StationeryOfTice,Government of [ndi% Kolkata SfiRIR. K. ROY

Voluntary Organization in Interest of Consumer Education (VOICE), REPRESENTATIVE

New Delhi

INS Directorate General DR U. C. Sruv.wm%,Director&Head(Chem)[RepresentingDirector General (Ex-oficio)]

MemberSecretarySHRI S, N. CHATJERJEE

Director (Chem), BIS

13

.-

Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standar& Act, 1986 to promoteharmonious development of the activities of standardization, marking and quality certification of goods andattending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced in any formwithout the prior permission in writing of BIS. This does rrot preclude the fkeeuse, in the course of implementingthe standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating tocopyright be addressed to the Director (Publications), 131S. r

Review of Indian Standards

Amendments are issued to standards as the.need arises on the basis of comments. Standards are also reviewedperiodically; a standard along with amendments is reatl%med when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision, Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Dot: NO. CHD 15 (1344),

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS

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Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002Telephones: 23230131,23233375,2323 9402 website: wvvw.bis.org.in

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