इंटरनेट मानक

Disclosure to Promote the Right To Information

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

“जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न' 5 तरफ”

Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 1060-2 (1960): Methods of sampling and test for paper

and allied products: Part 2 [CHD 15: Paper and its
products]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 IS : 1060 (Part II) - 1960
( Reaffirmed 1997 )
Indian Standard
METHODS OF SAMPLING AND TEST FOR
PAPER AND ALLIED PRODUCTS, PART II
( Tenth Reprint NOVEMBER 1996 )

UDC 676.017

0 Copyright 1960
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAII ZAFAR MARG
NEW DELHI 1100(~:

Gr7 December 1960

 IS: lOSO(PartII)-1960

Indian Standard
METHODS OF SAMPLING AND TEST FOR
PAPER AND ALLIED PRODUCTS, PART II

Paper Sectional Committee, CDC 15

Chainon

SHBI C. A. SUBBAHYANYAX Ministry of Works, Housing & Supply

Members
Da. J. C. AWABWAL Bengal Paper Mill Co Ltd , Calcutta
Suar N. J. ABDE~HIR All India Federation of Master Printers
Saer S. C. GHOSEJ ( A&emote )
SIIBI TBIDIBESE BASU Publishers’ Association of West Bengal, -&lcutta
SEBI S. N. BHANDARY Sirpur Paper Mills Ltd , Sirpur
SHBI A. P. BHARQAVA Stationery & Office Equipment Association of India,
Calcutta
SRIU R. K. BATRA ( Alfern&)
Sanr M. P. BEAROAVA Rohtas Industries Ltd , Dalmianagar
SHBI S. P. GOYAL ( Alfemafe)
Sm R. P. BHARQAVA Indian Paper Mills Association, Calcutta
SHFLI S. P. MISRA ( Alternafe )
SHEI B.B. CEAUDHURI Ministry of Defence (R & D )
DE A. N. NAYER ( Alfcmatc )
DB S. R. D. GUHA Forest Research Institute and Colleges, Dehra Dun
SRBI S. N. GUHA RAY Association of Master Printers of West Bengal,
Calcutta
SHRI M. L. DUTT ( Alfernafc )
SHBI N. K. S. IYENGAR Development \Ving, Ministry of Commerce &
Industry
SHRI N. NA~AS~YHAN ( AlfernateJ
MAJOR N. V. R. IYENQAR Central Food Technological Research Institute,
Mysore
SHRI MOHAN LAL Jaswant Sugar Mills Ltd , h&xrut
SHRI MAEAVIR KAPOOR ( Altcrnotc )
SHRI C. C. MUKHERJEE Calcutta Paper Traders’ Association, Calcutta
SHRI N. L. DUTTA ( .4fternate )
SHRI S. P. MULLICE Government Test House, Calcutta
SHRI S. K. BoSE ( Alternafc )
SERI P. K. NANDA Indian Paper Makers’ Association, Calcutta
SHXU M. A. JOOLEKAR ( Alternafc )

( Continued on page 2 )

BUREAU OF ISDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NSW D”.T FTT ll(1002
Is:1060(Purxr)-1960
(CIJiraridfiompcyr 1)
M8l&r5
SHEI K. NAEENDEA Indian & Eastern Newspaper Society, New Delhi
Sam S. S. L. ROHAT~I Directorate General of Supplies & Disposah
( Ministry of Works, Housing & Supply )
DB P. N. SAHAI Printing & Stationery Department, Government of
India
SHEI M. A. JHANOIANI ( Al&mate )
Sasr R. B. SILVER Titaghur Paper Mills Co Ltd , Calcutta
SHBI W. G. W. WAEEEN Imperial Tobacco Company of India Ltd , Calcutta
Sslu S. K. KESHAVA ( Al&mate )
DE LAL C. VERUAN ( Ex-oficio) Director, ISI
DE SADOOPAL( Altemafc) Deputy Director ( Chcm ), ISI

Sccrcta~
SEEI S. K. SEN Deputy Director ( Metric Ccli ), IS1

Methods of Test Subcommittee, CDC 15 : 2

conunw
DE P. N. SAHAI Printing & Stationery Dcptrtmcnt, Government of
India

Members
DB J. C. AOQABWAL Bengal Paper Mill Co Ltd., Calcutta
SEEI B. B. CHAUDHUBI Ministry of Dcfcncc ( R & D )
DE A. N. NAYEB ( Al&ma&)
DE S. R. D. GUHA Forest &search Institute and Collcgcs, Debra Dun
SEEI S. P. MIERA Orient Paper Mills Ltd , Brajrajnagar

2
 ISt1060(PartlI)-1960

Indian Statidard
METHODS OF SAMPLING AND TEST FOR
PAPER AND ALLIED PRODUCTS, PART TT

4). FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards Institution
on 7 June 1960, after the draft finalized by the Paper Sectional Committee
had been approved by the Chemical Division Council.
0.2 A number of test methods for paper and allied products has been
prescribed in*IS : 1060 ( Part I )-1956 Methods of Sampling and Test for
Paper and Allied Products, Part I. They cover the more general types
of tests required for paper and allied products. Tests included in this
standard are for special purposes.
0.3 This standard has been based partly on the standards now in use in
Defence Laboratories. Note has also been taken of the data available with
the Governn\ent of India Stationery Office, and the Cellulose and Paper
Branch of the Forest Research Institute. Due weightage had to be given
to the need for international co-ordination. among standards prevailing in
different countries of the world, and these considerations led the Sectional
Committee responsible for the preparation of this standard also to draw
upon the methods of tests prescribed by the British Standards Institution,
the American Society for Testing Materials and the Technical Association
of the Pulp and Paper Industry, USA.
0.4 This general standard of test methods is a necessary adjunct tostandard
specifications for individual types of paper and allied products.
0.4.1 Test methods not included in this standard and not o:herwise pro-
vided in the individual detailed standards shall be subject to agreement
between the-purchaser and the vendor.
0.5 This standard requires reference to the following Indian Standards:
*IS : 250-1953SPECIFICATIONFORPOTASSIUM
BICHROMATE,
TECHNICAL
AND ANALYTICALREAGENT
*IS : 266-1950 SPECIFICATION
FOR SULPHURIC ACID
IS : 376-1952 SPECIFICATION
FOR SODIUM HYDROXIDE, ANALYTICAL
REAGENT
*IS : 460-1953 SPECIFKXTIONFOR TEST SIEVES ( WITH AMENDMENT
No. 1, NOVEMBER1955 )

*Sina &sai.

3
IS:106O(PartII)-1960

‘IS : 1060 ( PART I )-1956

METHODSOF SAMPLINGAND TEST FORPAPZR
AND ALLIED PRODUCTS,PART I
IS : 1070- 1960 SPECIFICATION
FOR WATER, DISTILLED QUALITY (Revised)
0.5.1 Wherever a reference to any Indian Standard mentioned in 0.5 or
otherwise, except IS : 460-1953:appears in this standard, it shall be taken
as a reference to the latest version of the standard.
0.6 In reporting the results 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 ). The number of significant places retained i
the rounded off value should be the same as that of the specified value 1*a
the standard, it being understood that the analyst will carry out his deter-
mination to at least one place more than in the specified value.

1. SCOPE
1.1 This standard prescribes methods of tests for paper for special purposes
not covered in IS : 1060 ( Part I )-1956: The tests prescribed are:
4 Bursting strength, wet;
b) Tensile strength, wet;
c) Bending test;
4 Cupping test;
e) Exudation test;
f) Bleeding resistance;
9‘) Fastness to-light;
h) Brightness;
3 Water vapour permeability;
k) Estimation of alpha cellulose content;
ml Estimation of lead and lead compounds;
n) Estimation of chIorides ( water soluble );
P) Estimation of sulphates ( water soluble );
q) Estimation of fatty and/or rosin acid extractable by ether;
r) Estimation of matter soluble in ether; and
s) Estimation of bcnzx ne soluble matter.
1.2 Should any inconsistency exist between the requirements of this
standard and those of the standard for an individual material, the latter
shall prevail.
-
*Since revised.

4
2. TERMINOLOGY
2.1 For thepurpose of this standard, definitions given in 1s : 1060 ( Part I )-
1956*shall apply.

3. SAMPLING
3.1 Representative samples for test shall be drawn as prescribed in 3 of
IS : 1060 ( Part I )-19561‘

4. CONDITIONING
4.1 Conditioning of test specimens shall be carried out in accordance
with 5 of IS : 1060 ( Part I )-1956:

5. QUALITY OF REAGENTS
5.1 Unless otherwise specified, pure chemicals and distilled water ( see
IS : 1070-1960 ) freshly boiled and cooled, shall be employed in tests.
NOTE - ‘Pure chemicals ’ shall mean chemicals that do not contain impurities
which affect the results of analysis.

6. BURSTING STRENGTH, WET

6.1 General - The popularity of bursting strength test depends not only
on the ease with which the test is made, but also on the combination of
strength, ‘ give ’ and toughness which it measures and which serve as a
measure of the serviceability of paper in various applications. It has the
disadvantage, however, that it depends in a complicated way on the machine
direction tensile strength, stretch and the size of the burst area. Also it
does not give any indication of cross direction tensile strength.
6.2 Equipment - A tester in which testing is done by hydraulic pressure
communicated through the medium of glycerine or compressed air to a pure
gum rubber diaphragm of thickness 0.85 -& 0.05 mm in contact with the
paper shall be used. The gauge used shall be so chosen that the individual
reading shall not be less than 25 percent or more than 75 percent of the total
indicated capacity of the gauge. The gauge should be of the maximum
reading type and should be calibrated not less frequently than once every
six months.
6.3 Procedure-Immerse the test piece in water at 27” f 2°C for four
hours. Remove and place it flat and straight on a pad of four thicknesses
of dry blotting paper and cover it with a similar pad. Roll a metal cylinder
weighing 500 f 5 g and having a diameter of about 50 mm steadily over the
top blotter to remove the surface moisture as quickly as possible. Imme-
diately clamp the test specimen firmly ( without slippage during the test )
over the diaphragm, between two annular plane unpolished ( matte) surfaces
yince revised.
5
IS:1060(PartII)-1960

of 30.0 f 0.5 mm internal diameter. Run the machine so that the pressure
increases at a.uniform rate of approximately 0.75 kg/cm2 per second until
the test piece bursts. Note from the pressure gauge the pressure in kg/cm2
at which the test piece bursts. Take one reading with the wire side upper-
most and one with the top side uppermost with each sample sheet.
NOTE-A rate of 120 revolutions per minute in glycerine-operated machine is
usually satisfactory.

6.4Report - Report the type of tester used and give the average, maxi-
mum and minimum values of the reading for each side separately.
6.5 Burst Factor - Used for comparing two papers with regard to their
bursting strength:

Burst Factor = _______~_

Bursting ~_~~
strength
._
in g/cm2 ~~~~~~
Substance in g/m2 [see 6 of IS : 1060( Part I )-1956’1

7. TENSILE STRENGTH, WET

7.1 General - This method of test covers a procedure for determining the
tensile strength of paper and paper products after wetting with water or
other liquid. It is of special usefulness in evaluating the performance
characteristics of paper and paper products subjected to stress during pro-
cessing or use, while wet. Depending on the requirement in use, the test
piece may be immersed in the appropriate liquid for a given time and tested
whether it is completely saturated or not. However, unless otherwise
specified, the wet tensile strength test is assumed to be performed on the
test piece after complete saturation in water.
7.2 Test Piece - Prepare a sufficient number of test pieces cut from each
principal direction of the paper, excluding watermarks, creases or other
visible imperfections. The pieces shall be clean-cut to within plus or minus
one percent of their nominal widths, with edges parallel, and shall be long
enough to be inserted in the jaws of the clamps of the testing apparatus
without handling the section under test. The width of the test pieces shall
not exceed 37.5 mm nor shall be less than 12.5 mm.
NOTE-Varying the width of the test pieces between 12.5 and 37.5. mm,
with a proportionate change in the rate of loading, does not, in general, make
much difference in the proportionate test results except for unbeaten long-fibre
papers, when the difference may be appreciable.

7.3 Procedure

7.3.1 Use the testing machine referred to in 12.4 of IS : 1060 ( Part I )-

1956’and calibrate as follows:
Accurately level the apparatus in both its principal directions and
make the mechanism move freely. Apply weights of known value
to the upper clamp so that it moves in the same direction and plane
~-
*Since revised.
6
 IS: 1060( Portrx)-1888

as when testing. Disengage the pawls of the pendulum, suspend the

test weight by a flexible connection from the centre of the upper clamp,
release the latch holding the pendulum at zero indication, and allow the
pendulum to come slowly to equilibrium. Note the indicated scale
reading for each load applied and record all test data. It is recommend-
ed that readings be taken at not less than three distributed points on the
scale of the instrument.
7.3.2 Immerse the test piece in the specified liquid till saturated. Nor-
mally 4 hours’ immersion in water will be adequate for most papers. Unless
otherwise required, the liquid shall be maintained at 27” & 2°C.
7.3.3 At the end of the immersion time and before placing the test piece
in the tensile testing machine, place it flat and straight on a pad of four
thicknesses of dry blotting paper and cover it with a similar pad. Roll a
metal cylinder weighing 500 f 5 g and having a diameter of about 50 mm
steadily over the top blotter, taking about 2 seconds for the operation.
7.3.4 Immediately after blotting, place the test piece loosely in the jaws
of the clamps, align it squarely, then tighten the upper clamp, take up the
slack, and finally tighten the lower clamp, without touching the portion
under test. Then apply the load as follows:
For weak papers breaking below 2.5 kg per 15 mm width, adjust
the loading so that fracture. occurs in not less than 5 nor more than
15 seconds. For all other papers, adjust the rate of loading so that
the lower clamp moves at a rate of 30.0 f 1.5 cm/min.
7.3.5 At least ten test pieces from each direction of the sheet shail be
tested.
7.4 Report - Report the average, maximum and minimum values of the
test results. Express the tensile strength, wet, in kg/cm width to three
significant figures and also as a percentage of the dry tensile strength,
Express the stretch in each direction separately as percentage elongation
correct to one place of decimal. The exact width of the test piece and the
initial distance between the jaws shall be reported with the results.

8. BENDING TEST
8.1 General - This test is applicable to paperboards.
8.2 Procedare -Fold a square test piece at least 60 x 60 mm by fingers
along the diagonal so that the inner surfaces are in contact completely.
Unfold and repeat the folding along the same crease in the opposite direction
until the other surfaces are in contact completely. Repeat the test with a
second test piece.
8.2.1 Record any visible fibrous breaks or cracks on the surface of the
folded test piece after each crease is made. Report the average number and
length of the visible breaks on the surface and, if coated, the appearance of
IS: mO(PartII)-1960

the folded surface resulting from the test. If no break is more than 6 mm
long, the board may be classified as fair. If the board shows no fibrous
break, it is classified as good.

9. CUPPING TEST

9.1 General - This test is applicable to paperboards.

9.2 Procedure - Cut out a disc from each test piece. Damp the disc by
dipping momentarily in water and then air dry for 5 to 10 minutes till all
surface moisture is removed but the paper remains just damp. Then press
the disc into a cup-shap, .I mould of diameter approximately 9 mm to form
a cup 3 mm deep. The radius of curvature of the plunger shall be 0 5 mm.
9.2.1 The cup so produced must be free from chipping and cracks at the
bottom where the material is turned up.

10. EXUDATION TEST

10.1 General -This method of test is applicable in the case of bitumen
or pitch coal tar impregnated papers.
10.2 Procedure - Place the test piece of suitable size over and in contact
with a clean white filter paper and apply a load of 6.4 kg through a flat
metal plate of 45 ems area. Maintain a temperature of 72” f 2°C.
10.2.1 There should be no exudation of the impregnating material or
staining of the filter paper at the end of two hours.

11. BLEEDING RESISTANCE TEST

11.1 General -This method covers the test for determining the degree of
bleeding resistance which is a measure of the ability of bitumen or asphalt
laminated or similarly treated case-liners or baling paper to avoid staining
the contents of a case or bundle.
11.2 Apparatus - The apparatus shall consist of the following:
a>kgwith
Pressure Block -A
a smooth,
block of metal 75 x 75 mm weighing about 2
flat under-surface. A wooden knob fastened to
the top of the block conveniently serves as a handle.
b) Bed Plate - A piece of metal 75 x 75 mm and about 6 mm thick,
having a smooth, flat upper surface.
4 Plate Guide - A guide for the pressure block which may conveni-
ently be made from 115x 115 mm sheet metal with the corners
turned up vertically.
4 Metal Separators - 75 x 75 mm made from thin, flat aluminium
sheet or heavy aluminium foil.

8
 18:1060(P4utIl)-1360

e) I’ujwr&eLr- 75 x 75 mm cut from smooth, white imitation

art paper.
f) Oven - capable of maintaining the test assembly at a constant
temperature of 66”f 2°C.
11.3 Test Piece -The test piece shalI_be 75 x 75 mm cut in such a way
as to be representative of the sample to be tested.

11.4 Procedure
11.4.1 Put the test pieces and the disassembled apparatus in the oven
at 66% for a sufficient time for all to reach that temperature. Place a test
piece between the two sheets of white imitation art paper and place the
combination between two aluminium separator sheets. If desired, up to
five of such sandwiches may be laid on one another but separated by single
metal sheets and tested simultaneously.
116.2 Place the sandwiches on the bed plate in the guide and cover with
the pressure block ( which exerts a pressure of O-035 kg/cm* ). Make this
assembly with as little cooling as possible. Leave the assembly in the oven ..
at 66’ f 2°C for 5 hours.
11.4.3 Then remove, separate the sandwiches and examine the white
imitation art paper for staining by the exuded material.
11.3 Report - Report the de of bleeding as follows, disregarding any
staining arising from the cut ecYee
ges of the test piece:
Degree of Bleeding Demipion
a) No bleeding No visible staining
b) Slight bleeding Staining in the form of specks only;
blotches or spots under l-5 mm in
diameter
c) Considerable bleeding Staining in the form of spots and
blotches l-5 mm or more in dia-
meter
NOTE -Care should be taken that radiant heat does not raise the temperature
of the assembly conaidcrably above the indicated temperature of the oven.

12. FASTNESS TO LIGHT

12.1 The fastness to light of the colour of the paper is tested in a Kelvin
fetometer.
12.2 Kelvin Fqgitometer- This comprises a revolving drum which
carries the samples under test in special holders. These sample holders are
suspended from the top of the revolving drum in a constant upward stream

9
IS:1060(PartII)-1960

of air, conditioned to a predetermined humidity and temperature. This is

assured by a horizontal fan which rotates just above the level of the humidi-
fying water in a circular tray at table level. The temperature of this water
is controlled by immersion heaters with thermostatic controls.
12.2.1 The source of fading radiation is the standard carbon arc lamp*
On comparison of spectrum of the fugitometer lamp with that of sunlight,
there is very close resemblance- particularly at the violet end of the
spectrum - and because of the steady and intensive light impinging on the
samples under test, the period of time required to produce results comparable
with natural conditions of sunlight is substantially reduced.
12.3 Procedure - Expose the test piece in the fugitometer for the period
specified in the specification for the individual material. The test piece
passes the test if no fading occurs.

13. BRIGHTNESS

13.1 General-This method is intended for determining the 45” -0’

directional reflectance of uncoloured paper for blue light. In the paper
trade, this quantity is known as ‘brightness’.
NOTE- Brightness, as determined by this test is primarily a measure of frec-
dom from yellowness arising in pulp and paper from the presence of lignin and
other so-called inlpurities left by incomplete bleaching. It thus differs from
luminous ( visible ) reflectance. Blue light is used for the measurement of
brightness, whereas light of all colours, with major weight given to the green is used to
measure luminous reflectance.

13.2 Apparatus - The apparatus shall consist of a reflectometer, either

visual or photo-electric type, having such source, filter, and receptor charac-
teristics that it Will measure, for undyed papers and pulps, 45” -0O”
directional reflectance for blue light as herein described, accurate within
l-0 percent. The apparatus shall have the following characteristics:
a) Speclral Characferistics - The product of spectral energy of source,
spectral transmission of any filters through which light must pass,
and spectral response of receptor shall be equivalent to the product
of the z function of the standard observer and calorimetric co-
ordinate system recommended by the International Commission on
Illuminationt multiplied by theenergy distributionofthe Commis-
sion’s standard illuminant A ( representative of incandescent lamp
light ). Such a combination will have a maximum spectral res-
ponse to energy at about 460 millimicrons.
-
*Electrical particulars of a typical fugitomclcr arc:
Power supply . 50 cycles ac Arc voltage ... 120-145 V
Line voltage . 200-250 V Arc current ... 15-17 A
tprocecdings of eighth session of the International Commission on Illumination,
Cambridge, England, Scptem bcr 193 I.

10
 IS: 1060 (PartII)-1960

b) Geometric Characteristics - Rays incident on the test piece shall

spread no more than 4” from the axis ofthe incident beam; rays
accepted for measurement shall spread no more than 15” from the
axis of the viewed beam. Rays in the incident and viewing beams
shall be symmetrically arranged with respect to their respective
axes. The above directions ofilluminating and viewing may be
inter-changed, giving the equivalent 0” - 45” conditions.

13.3 Standards
13.3.1 Primary Standard - The primary standard of 45” - 0” directional
reflectance shall be a layer ( at least 0.5 mm in thickness ) of magnesium
oxide freshly prepared by collecting the smoke from burning magnesium
ribbon or turnings on a suitable surface in accordance with Appendix A.
13.3.2 Working Standards - Either of two types of working standards
may be used for day-to-day operatian of the instrument : (a) pieces of paper
carefully measured on an instrument known to be in good adjustment, and
(b) ceramic tiles or porcelain-enamelled plaques carefully measured on an
\ instrument known to be in good adjustment and to possess essentially the
same geometry as the device with which they are to be used. Calibrated
pieces of paper shall be used for only a short period following their calibra-
tion, and soiled pieces shall be discarded. Ceramic tiles and porcelain
enamelled plaques, usually can be cleaned without alteration of their reflec-
tive properties. Nevertheless, working standards of this second type should
be checked from time to time for assigned values of reflectance for blue
light. The assigned reflectance for blue light of the working standard shall
be calculated as follows:

RI=; x 100

where
R, = assigned reflectance of the working standard, in percent;
b = average reading for working standard; and
a = average reading for primary standard.
13.4 Test Piece -Test pieces shall be handled carefully to avoid soiling,
and care shall be taken not to touch the areas tested. A pad of test pieces
shall be used for the measurement, so thick that doubling the number of
sheets does not cause change in the measured reflectance.

13.5 Procedure
13.5.1 When available, a working standard of abqut the same reflectance
for blue light as the test pieces shall be used. The reflectance ofthis working
standard shall be read both before and after readings of reflectance of the

11
IStlMO(PartII)-1960

testpieces are made. Readings shall be made on at least five separate test
pieces in each pad. To average out any effects of rotatio?, equal number
of readings shall be taken along and across the machine dlrection.
13.5.2 The 45” - 0” directional reflectanceshall be calculated as follows:

R =+xRl

where
R = 45” - 0” directional reflectance for blue light of the sample,
in percent;
c = average reading for test pieces;
b = average reading for working standard; and
R 1= assigned reflectance of working standard; in percent.
13.6 Report - Values of 45” - 0” directional reflectance for blue light shall
be reported for the wire and felt sides separately, to the nearest one percent.
The report shall state that this method was used.
NoTE - Because of the variability of standard magnesium oxide aurkca,
possible inaccuracies of photometera, possible inaccurate I tral conditiona,
geometric conditions, etc, it is felt that results accurate to Cc ttcr th8n &out
phu or minus one percent are not obtainable. However, where parties ioterutcd
in a test arc willing to accept valuer assigned to a workng rtandard aa accurate
to plus or minur @l percent, results can be obtained that can be reproduad to
plus or minus 0+2 percent, or even 01 percent.

14. WATER VAPOUR PE RMEABILITY TFST

14.1 Gtntd -This method is for the determination of water vapour

permeability of paper and board under 3 mm thickness, under prescribed
conditions of temperature and humidity. A quantity of desiccant, enclosed
in a dish sealed by a sheet of the material, is stored in a conditioned atmos-
phere and the rate of water vapour transmission is computed from the rate
of increase in weight of the dish assembly.
14.2 Apparatam - The apparatus shall consist of the following:
a) Test Dishes - Shallow aluminium dishes of as large a diameter as
can conveniently be accommodated on the balance, should be used.
The test dishes shall be designed so that the area of a test piece is
accurately defined and a wax seal between the test piece and the
dish satisfactorily prevents the transmission of water vapour at or
through the edges of the sheet. Figure 1 shows a suitable design of
dish and templates for cutting and sealing the test pieces. Using
the dimensions shown, test areas of 50 ms and 25 cm’ are obtain-
ed. The dishes and their covers may be manufactured from
@900 mm deep drawing quality alyninium sheet.

12
 IS:HMO(PartII)-1960

b) Weighing Covers- If the test dishes are removed from the cabinet
or room for weighing, an aluminium lid ( see Fig. 1 ) should be pro-
vided to fit each dish in order to minimize changes in weight while
the test pieces are out of the controlled atmosphere.

(A CUTTING TEMPLATE

t0 WAXING TEMPLATE

fC LID

99 (72) .-y
r61-
I
________ L_____-l
4 L-f
I \ - ___“f---__ J
I

ID SHALLOW DISH FOR MATERIALS

OF NORMAL PERMEABILITY

1C DEEP DISH FOR MATERIALS OF

PERMEABILITY GREATER THAN
I009 per sq m per 24 HOURS
TAPERED TO NEST

All dimensions in millimetru.

NOTNS- 1. Dimensions are shown for test areas of 50 ems and 25 cm’, the
latter in brackets.
2. Figures for dishes and lids show inside dimensions, except the
overall diameter of the dishes, which is an outside dimension.

FIO. 1 DIAWSAY or DISHIS AND TXMPLATIUJ

13
IS:HMO(PartII)-1960

4 Balance -The balance used shall be accurate to O*OOO5 g.

4 Humid+ Cabinet -The cabinet shall have racks to support the
dishes and means of circulating air-conditioned at:
65 & 2 percent relative humidity and 27” f 2”C, or
90 f 2 percent relative humidity and 38” f 1°C
continuously over the test pieces. The air circulation shall be
sufficiently rapid to maintain the specified humidity at the surface
of test piece. The design of the cabinet shall be such that no con-
densation of moisture takes place in the vicinity of the test pieces
during the test. Care shall be taken to ensure that the cabinet is
not loaded to such an extent that the rate of moisture up-take
reduces the relative humidity below the lower limit specified.
e) Desiccant - The desiccant used shall be such that the relative
humidity within the dish does not rise above 2 percent during the
determination. Anhydrous calcium chloride and magnesium per-
chlorate are suitable and shall be used in the forrn of small lumps
passipg through IS Sieve 240 ( 2 399 & 91 microns, see IS : 460-
1953 ) but free from fines passing through 1s Sieve 60 ( 592 f 33
microns, see IS : 460- 19533.
f) Wax -The wax compound used for sealing shall adhere firmly
both to the surfaces of the test piece and to the dish and shall not
be brittle at room temperatures. It is important that the wax be
relatively stable and non-absorbent to water vapour ; the weight
change on an area of 50 cm2 of wax surface exposed for 24 hours
at 90 percent relative humidity and 38” & 1°C shall be less than
0.001 g.
14.3 Test Piece - The sides of the test piece shall be designated I and II
respectively, side I being that side which in use is exposed to the higher
humidity whether this be inside or outside the package. Where the condi-
tions of use of the material are unknown, side I shall be that side which faces
outwards. If the material is coated on one side only, the word coated shall
be added to the designation, for example, Side I ( coated ).
14.3.1 The determination shall be made with test pieces as follows:
a) Uncreased with side I exposed to the high humidity,
b) Uncreased with side II exposed to the high humidity,
c) Creased with side I exposed to the high humidity, and
d) Creased with side II exposed to the high humidity.
A total area of not less than 100 cm* made up of at least two test pieces
shall be examined for each of the four types of tests listed above. The
minimum area of a test piece shall be 25 cm*.
-_-
*Since revised.

14
 IS : 1060 ( Part II ) - 1960

14.4 Creasing

14.4.1 Creasing shall be done in the conditioning atmosphere ( 27’ 1 2°C

and 65 f 2 percent RH ) or immediately after removal therefrom.

14.4.2 Cut square samples and, after conditioning, crease to give two sets
of pleats, equal in number, along the two principal directions of the sheet.
Use a Aat plate as the creasing bed and make the creases by a loaded platen
whose width is about 2 cm greater than the length of the sample to be
creased. The creasing load shall be one kilogram per centimetre of crease
and shall be applied for 10 to 15 seconds. The total length of crease in
centimetres shall be equal to the effective area of the test piece in square
centimetres.

14.4.3 Creases shall be made one at a time and immediately unfolded,

adjacent creases being made on opposite sides of the sheet so that the final
effect is a set of pleats. The process shall be repeated to produce a similar
set of pleats at right angles to the first. A circular test piece shall tllen be
cut from the square creased sample.

14.4.4 The sparing between adjacent creases shall be as below:

1.85 cm for an effective test area of 25 cm2, and ir:
2.10 cm for an effective test area of 50 cm2. &

14.5 Procedure

14.5.1 Cut the test piece using a template which is of such diameter- tliat
the edge of the test piece covers half the annular recess of the dish. Fill 111e
dish with desiccant to within 1 to 2 mm of the supporting ring. Place the
test piece on the supporting ring and centre ( see Fig. 2 ). Place the \~axirlg
template centrally over the dish and tcrt piece, and rrm molten l\.ax into the
annular recess until the \vax is level with the top surf;tce of the tcmlilatc.
Break any air bubbles in the wax with a small gas jet, allow the i\ax to
’ harden and remove the template. Inspect the tli\h ro yn\ure that the seal
is satisfactory and remove any wax on the outside. It is important that the
filling and sealing of the dish is carried out as rapidly as l~~ss~l~le 50 11lat the
destccant absorbs a minimum of water vapour from the ;Itmo~pl~crc. (Lre
must be taken not to damage the test area during the operation or to allf~
the desiccant to come into contact with it. To facilitate the removal of the
template from the wax, apply a thin film of petroleum jelly to the l~evellcd
edge before sealing; remove any surplus on the lower surface.
14.5.2 Prepare the required number of dishes and place in the lrrrmidity
cabinet. Make successive weighings at suitable intervais which must be
sufficiently frequent to complete the test before the relative humidity in the
dish rises above 2 percent. Plot the cumulative weight increase of each dish
in milligrams against the total time of exposure in the cabinet. When
at least three, but preferably four, points lie on a straight liue, a constant

15
IS:106O(PartII)-1960

rate of gain has been attained and the experiment may be discontinued.
The weighings should be made to an accuracy of one percent of the weight
change between two successive weighings or WOO1 g \vhichever is larger.

Fro. :! CESTRIM SAMPLE ON DISH

14.5.3 If the samples are exposed in a cabinet from which the\- are removed
for weighing, precautions must be taken to ensure that the dishes are out of
the cabinet for the same period and under the same conditions at each suc-
cessive weighing. The following procedure is recommended. About eight
dishes are removed from,the cabinet at a time and immediately covered with
their respective lids. The dishes should be allowed to cool until their tem-
perature is not appreciably different from that of the room. At the com-
pletion of the weighings, the lids are removed and the samples immediately
replaced. Precisely the same routine and time schedule must be followed in
detail at each successive weighing interval. Where possible, the cabinet and
balance should be kept in a room having constant humidity and temperature.

14.6 Report
14.6.1 Report the water vapour permeability as g/m* per 24 hours at the
temperature and relative humidity specified for the material.

16
 14.6.2 Calculate the permeability from the slope of the graph which has
been obtained by plotting the cumulative weight increase of each dish in
milligrams against the total time of exposure in the cabinet. The required
slope is that of the best straight line drawn through those pcints which
represent the constant rate of gain. If it is such that x mg is the weight
increase over a period ofy hours for an exposed area of A cm?, the permeabi-
lity is ?% g/m2 per 24 hours.
AU
14.6.3 The average, maximum and minimum values for each type of test
made as in 14.3.1 shall be reported to two significant figures or the nearest
0.2 g/m2 per 24 hours, whichever is larger.

15. ALPHA-CELLULOSE CONTENT

15.1 General - Alpha-cellulose is taken as the fraction that can be filtered

out of a mixture consisting of the fibrous material and sodium hydroxide
solution of maximum dissolving power ( 7.3 percent, W/W ), after the fibres
have previously been swelled with sodium hydroxide solution ( 17.5 percent,
W/W or 5.24 & 0.05 N ). After separation, the alpha-cellulose is determined
either by drying and weighing, or volumetrically by oxidation with potas-
sium dichromate. Both methods are capable of the same reproducibility
and give practically the same values. In the volumetric method, no mois-
ture or ash determinations are made and a much smaller sample is used,
res_ulting in a shorter and more rapid procedure.
15.2 Apparatus - consisting of the following:

4 Grinder - A Koerner or equivalent type grinder that will comple-

tely disintegrate the paper without heating or contaminating it.
b) Mixer - A device with which uniform mixture of the ground mate-
rial can be secured. A mixer is easily constructed by fitting a crock
or bell jar, of approximately equal diameter and depth, with a
wooden lid through which runs theshaft of an electric fan, vanes
being properly placed to produce turbulence. Mixing for 20 to
40 seconds at full speed normally suffices; longer periods result
in separation of the light material from the heavy.
4 Bath - A water-bath that can be maintained at 20.0” f 0*1X.
4 Electrometric X&ration Apparatus - For the estimation of dichromate,
an indicator may be used as descrjbed in 15.3(e), but for rapid,
accurate analysis! an electrometric apparatus is recommended. Any
ordinary potentiometric circuit with a platinum wire electrode
and calomel half-cell is suitable. A suitable arrangement is shown
in Fig. 3. The potentiometric arrangement may consist of a galvano-
meter with a sensitivity of 0.5 to 1.0 microampere per millimetre
scaledivision, a dry cell, and a sliding-contact rheostat having a

17
IS : 1060 ( Part II ) - 1960

total resistance of approximately 400 ohms. Smaller rheostats

-will suffice but they drain the dry cell more quickly. The large
deflection at the end point is unmistakable from possible slow creep-
ing during the titration. The galvanometer is adjusted to zero by
varying the resistance at the beginning of the titration.

Fm. 3 AURAXQEMENT FOB ELECTROMETRICTITRATION

15.3 Reagents - consisting of the following:
a) Sodium Hydroxide Solution ( 17.5 percent, w/w or 5.24 N) - Allow a
50 percent solution of sodium hydroxide ( conforming to IS : 376-
1952 ) to stand about one week in a stoppered vessel to permit iettl-
ing of sodium carbonate. Draw off 2.0 ml of the supernatant liquid
with a pipette, andabout 50 ml of distilled water and 1 ml of3N
barium chloride to lessen the effect of carbon dioxide on the end
point, and titrate with standard 1 N hydrochloric acid, using phe-
nolphthalein as indicator. Knowing the approximate normality of
the concentrated sodium hydroxide, dilute it with distilled water
to 5.24 f 0.05 N, checking’the diluted sodium hydroxide by titrat-
ing 10.0 ml of it as before, and diluting further, if necessary, to
obtain the normality specified.
b) Potassium Dichromate Solution - Dissolve 90.0 g df oven-dry ( 100’
to 105°C ) potassium dichromate ( conforming to IS : 250-1953.) in
*Since revised.
18
 IS: 106o(PartII)-1960

hot water ( 70’ to 90% ), and dilute to one iitre after allowing
the solution to cool.
cl Ferrous Ammonium Sulphate Solution - Dissolve 195 g of ferrous
ammonium sulphate crystals in,water containing 10 ml ofsulphuric
acid ( sp gr 1.84 ) and dilute to one litre. If the solution is kept out
of contact with oxygen, for example, by means of a slow, continuous
stream of hydrogen, its strength will remain quite constant. The
amount of hydrogen thus used is about one-fifth of a 5 m3 cylinder
per year. This precaution is not necessary, but reduces the fre-
quency with which the potassium dichromate-ferrous ammonium
sulphate ratio must be determined from once a day to two or
three times a month.
4 Acetic Acid Solution for Gravimetric Procedure - Prepare a solution
of acetic acid approximately 10 percent by weight.
e>Bichromate Indicator -
solve 0.3 g of barium
If electrometric apparatus is not available,dis-
diphenylamine sulfonate and O-5 g of sodium
sulphate in 100 ml of water. Use 5 to 10 drops in a solution suffi-
ciently dilute for good observation of the end point, which is shown
by a change of colour from red to green. As an alternative, the
outside indicator, potassium ferricyanide solution, may be placed
in drops upon white porcelain. The end point occurs when a drop
of the solution being titrated turns a drop of the ferricyanide indi-
cator blue.
f-1Barium Chloride ( 3 N) - Dissolve 37 g of barium chloride crystals
in water and dilute to 100 ml.
g) Sufphuric Acid ( 24 N) - Cautiously add three vo!umes of sulphuric
acid of sp gr 1.84 ( conforming to IS : 266-1950 ) to two volumes
of water in a heat-resistant flask, cool by tap water, and add the
acid in small portions, shaking after each addition. The acid will
then be approximately 72 percent by weight.
h) Sufphuric Acid ( 6 N) - Dilute one volume of the 24 N sulphuric
acid to 3.5 volumes in a graduated cylinder. After mixing, standar-
diae against the 5.24 N sodium hydroxide and then dilute to
6.0 -& 0 1 N.
15.4 Test Piece - The test piece shall be cut from the specimen obtained
as in 3 of IS : 1060 ( Part I )-1956*m such a way as to be representative of
the lot. It shall be reduced to cotton-like form in the disintegrator and then
thoroughly mixed.. If the paper is mineral-coated, the coating shall be
removed before grinding.
15.5 Test Temperature - Perform all operations ( except weighing
in 15.6.1 ) and keep all liquids at 20.0” & O*l”C.
*Since revised.

19
ISr1060(PartII)-1960
15.6 Volumetric Method
15.6.1 Weigh 0.30 f 0.01 g of the disintegrated test piece in a lOO-ml
beaker. Add 20-O ml of sodium hydroxide ( 17.5 percent ), macerate until
the fibres are uniformly wet and dispersed, and let it stand for 10 minutes
from the time of addition of sodium hydroxide. Then add 33 ml of water,
stir the mixture thoroughly, and let it stand for one hour more, stirring once
during the interval. After stirring once more, pour about 5 ml of the un-
settled mixture on a copper or brass *wire screen of 0.177 f 0.011 mm aper-
ture ( IS Sieve 18, see IS : 460-1953 ) fitted into a Gooch crucible. The
crucible and ring are supported by a funnel fitted into the neck of a loo-ml
volumetric flask with a rubber stopper through which passes a glass tube for
suction ( pressure differential 10 to 20 mm of mercury ). Avoid excessive
packing of the fibres, as this retards filtering, It may be necessary to re-
filter the first filtrate, but loss of small amounts of alpha-cellulose to the
filtrate does not affect the results appreciably. Pour the remainder of the
mixture on the mat and, before the last ofthe liquid has run through, wash
the beaker and the mat with 35 ml of water.
15.6.2 Moisten the residue of alpha-cellulose with water and remove it
from the crucible. Place the crucible upright in a 400-ml beaker, fill it with
25 ml of 24 N sulphuric acid at room temperature, and rinse it after a few
minutes with 50 ml more of the acid. Disintegrate the alpha-cellulose pad
in the acid, using a stirring rod. Add to the alpha-cellulose solution, with
a pipette, 25.0 ml of the potassium dichromate solution, and heat at 140” to
150°C for 10 minutes. Bubble air in a finestream through the solution
to prevent bumping, and keep the beaker covered with a watch glass, notched
to permit entrance of a thermometer and the bubbling tube. After the solu-
tion has cooled to 13O”C, add 50 ml of water, rinse the thermometer, bub-
bling tube, etc, and cool the solution to 60°C or lower. Titrate the rernain-
ing potassium dichromate with the ferrous ammonium sulphate solution.
15.6.3 Pipette exactly half of the filtrate from the alpha-cellulose, after _
all fibres present have settled, into a 400-ml beaker containing 50 ml of
potassium dichromate solution. If the paper contains oxidizable fillers,
such as zinc sulphide pigment or calcium sulphite, filter the filtrate once
through a thick pad of asbestos in a Gooch crucible before taking the
portion for analysis. ( Such fillers remaining with the alpha-cellulose may
cause some error, but this is usually slight. ) Caunously, while stirring
constantly, pour 50 ml of sulphuric acid ( sp gr 1.84 ) down the side of the
beaker containing the portion of the filtrate for analysis, then heat and
titrate as described in 15.6.2 for the alpha-cellulose solution.
15.6.4 Culculution- Calculate the percentage of alpha-cellulose from the
following equations, except that when rosin, starch, or glue are present,
corrections shall be made in accordance with 15.6.4.1:
A-25-(I’rxr)
B=2x (5-Vsxr) ::: ::: I:;‘
*Since revised.

20
 IS: 1060( PartII)-1960

Alpha-cellulose, percent = +B x 100 ... . . . (3)

where
A = volume of potassium dichromate solution in ml required
to oxidize the alpha-cellulose;
B = volume‘of potassium dichromate solution in ml required
to oxidize the filtrate;
V, and V, = volume of ferrous ammonium sulphate solution in ml
required for titration of the potassium dichromate
remaining after oxidation of the alpha-cellulose and
filtrate, respectively; and
7 = volume of potassium dichromate equivalent to one
millilitre of ferrous ammonium sulphate solution
( determined frequently by titrating 5 ml of potassium
dichromate in 100 ml of diluted sulphuric acid ( 1 : 1 ).
15.6.4.1 If rosin, starch, or glue are present, the volumes of potassium
dichromate shall be corrected as follows before calculating the percentage
of alpha-cellulose:
The amounts of sizing materials remaining with the alpha-cellu-
loseare taken as 0.25 percent glue, 0.2 percent starch, and 0.2 percent
rosin, based on the dry weight of the sample ( see Note ). Convert
these values into weights, and then into millilitres of the potassium
dichromate solution by dividing each weight by the corresponding
factors, which are 0.015 4 g/ml for glue, 0.012 9 g/ml for starch, and
0.006 6 g/ml for rosin. Subtract the resulting volumes in millilitres
of the potassium dichromate solution from the volumes of potassium
dichromate consumed by the alpha fraction and substitute the
corrected values in equations 1 and 2.
NOTE -These arc average values but actual amounts have been found to
vary not more than 0.1 percent from them, irrespective of the content of glue, starch,
or rosin in the papers. For example, if a paper were found to contain 3’4 percent
glue, 0.7 percent starch, and 1.1 percent rosin, then the sizing materials remaining in
the beta plus gamma portion would be 3.15, 05, and 0.9 percent respectively.

15.7 Gravimetric Method

15.7.1 Allow the disintegrated test piece to come to moisture equilibrium
with the atmosphere of the balance case. Weigh, to the nearest milligram,
1.5 g of the disintegrated test piece for the alpha.cellulose determination.
Weigh at the same time samples for the moisture and ash determinations,
and also for those determinations of components other than cellulose as
may be found necessary for calculation of the total cellulose content, such
as fillers and sizing materials.

21
 15.7.2 Add 100 ml of sodium hydroxide ( 17.5 percent, w/w ) to the
weighed quantity of the test piece in a 400-ml beaker. Macerate until
uniformly wet and dispersed, and let it stand for 10 minutes from the time
of addition of sodium hydroxide. Dilute with 165 ml of water, stir the
mixture thoroughly, and let it stand for one hour more, stirring once during
the interval. After stirring once more, pour the mixture upon a medium-
weight cotton cloth cut to fit a 75 mm Buckner funnel, the cloth having
been previously washed, and the fitted piece dried to constant weight at
100” to 105°C and weighed in a weighing bottle before use. Remove by
refiltration any fibres passing through the filter. Before the last of the
liquid has run through, add water, break up the pad well with a pointed
stirring rod, and keep it in a loose condition until 200 ml of wash water
have passed through. Then cover the alpha-cellulose with acetic acid
( 10 percent) and allow to soak for 5 minutes after which pass an addi-
tional 500 ml of wash water through while breaking up the pad with a
pointed stirring rod.

15.7.3 Dry the alpha-cellulose on the cloth in the original weighing

bottle overnight at 100” to 105”C, cool, and weigh. Determine the ash
content and correct the weight accordingly. The sizing materials, if any,
remaining with the alpha-cellulose are taken as 0.25 percent glue, O-2
percent starch, and 0.2 percent rosin, based upon the dry weight of the test
piece, and the corresponding weights subtracted from the total.

15.8 Report - The percentage of alpha-cellulose shall be based upon the

total cellulose including pentosans, but excluding moisture, ash, rosin, or
any sizing or other added nonfibrous materials. All determinations of
alpha-cellulose shall be made in duplicate, the results of which shall agree
at least within 0.4 percent of the dry weight of the sample, and the average
shall be expressed to the nearest one percent. The report shall state whether
the volumetric or the gravimetric method was used.
NOTE - The precision of the volumetric method is much greater than these
requirements would indicate. It is felt, however, that the average value of two
determinations which differ by 0.4 when expressed as a percentage, adequately
represents the specimen as prepared for testing. When, however, a given spcci-
men is ground and tested in different laboratories, greater drsagreemcnt may
arise, due to the differences in freeness and extent of fibrillation of the fibres on
the one hand, and individual differences in analysis on the other, added to the
lack of perfect uniformity of the test specimen, and ordinary errors in analysis.
Therefore, the reporting of alpha-cellulose values to the nearest one percent is
more compatible with experience, and is sufhcientrfor the practical usefulness
of the value.

16. ESTIMATION OF LEAD AND LEAD COMPOUNDS

16.1 General -The method of test for the estimation of lead covers all
papers and paper products where lead restriction is specified.

22
 IS:106O(PartII)-1960

16.2 Procedure
165.1 Weigh 20 g of the material into a silica basin and carefully ash.
On no account shall the basin get above a faint red heat, otherwise lead
may be lost by volatilization. Extract the ashed material for one hour with
1 : 3 nitric acid and filter. Now add 2 ml of concentrated sulphuric acid
to the nitric acid solution in a 150-ml beaker and evaporate to fuming on
a hot plate. Add 100 ml of water and keep the beaker on the water-bath
for 15 minutes, then at the room temperature overnight, and filter.
16.2.1.1 The lead sulphate must be separated from other insoluble
material, such as barium sulphate, silica, etc, as in 16.2.2.

16.2.2 Transfer the filter paper and the residue to a small beaker and
cover with about 20 ml of water. Add 1 to 2 g of solid ammonium acetate,
allow to stand on the water-bath for at least half an hour stirring occasion-
ally. Then decant the liquid through a No. 42 Whatman filter paper or
equivalent and repeat the extraction. Wash the beaker into the filter with
warm water a few times to make sure that all the lead solution is extracted.
Collect the filtrate in a 150-m] beaker. Pass hydrogen sulphide for 10 to
15 minutes and filter the lead sulphide at once and wash thoroughly but
quickly with hydrogen sulphide water, the filtrate and washings being
retained. Transfer the precipitate and paper to a tared crucible, carefully
ignite, sulphate the ash, cool and weigh.

16.3 Report - Lead is calculated as below :

A x 0.683
Lead ( as Pb ), percent by weight = pB_. x 100

where
A = weight of lead sulphate residue obtained ; and
B = weight of the material taken for estimation.

Two determinations shall be made and reported.

17. ESTIMATION OF CHLORIDES ( WATER SOLUBLE )

17.1 General -This method is applicable to papers containing small
quantities of chlorides soluble in water. Since the amounts to be determin-
ed are small, it is important that the determinations should be carried in a
chloride free atmosphere.

17.2 Reagents - The following reagents are required:

a) Standard Silvn .h%rate.Solution - Dissolve 2.5 g of silver nitrate and
dilute to one litre. Standardize on 0.03 g portions of sodium chlo-
ride, by dissolving it in water and titrating as described below:
Adjust volume so that one millilitre of silver nitrate solution is
equivalent to O*OOO838 g of sodium chloride.

23
IS:IOGO(PartII)-1960

b) Potassium Chromate Indicator - approximately 5 percent.

17.3 Procedure
17.3.1 Weigh out 5 g of the test piece and transfer to a 500-ml
Erlenmeyer flask. Add 250 ml of boiling distilled water, attach a water or
air condenser to the flask and boil gently for one hour. A ground glass
connection between the condenser and flask should be used to avoid
contamination. Filter the contents of the flask through a Buckner funnel.
Return the paper sample to the flask. Add another 200 ml of boiling water
to the paper and again extract for 15 to 30 minutes. Filter through the same
filter previously used and wash the extracted specimen and filter with 50 ml
of hot water in small portions. Run blanks on the water for each series
of tests at :he same time, putting the blanks through the same operations as
the test pieces.
17.3.2 Combine the filtrates. If the extract is not neutral to litmus,
adjust to neutrality with very dilute nitric acid or chloride-free sodium
hydroxide. Add 5 ml of 5 percent potassium chromate solution as indicator
and titrate with the standard silver nitrate solution to the first, brick red
colour of silver chromate. Carry out a blank determination of the same
amount of water as used ‘in extraction of the paper and subtract the volume
of silver nitrate required for the blank from that used for the titration of
the paper extract. From the difference, calculate the percentage of
chlorides, as sodium chloride, on the ‘conditioned paper.
17.4 Result - Calculate as below:
A x O*OOO838 x loo
Chlorides ( as NaCl ), percent by weight =
B
where
A = volume of silver nitrate in ml required for titration; and
B = weight of the conditioned material taken for test.
Results of duplicate determinations shall be reported.

18. ESTIMATION OF WATER SOLUBLE SULPHATES

18.1 General - This method is applicable to paper containing small quan-

tities of sulphates soluble in water.
18.2 Reagent - The following reagent is required:
aj Barium Chloride Solution- approximately 10 percent.

185 Procedure
18.3.1 Proceed as described in 17.3.1 for estimation of chlorides,

24
 IS:106O(PartII)-1960

18.3.2 To the combined filtrate, add one millilitre of concentrated hydro-

chloric acid, heat to boiling and add dropwise with stirring 5 ml of 10 percent
barium chloride solution. Digest at approximately 80°C for 4 hours or
longer, filter through a No. 42 Whatman filter paper or equivalent and wash
with hot water till free from chlorides.
18.3.3 Transfer the filter paper and contents to a tare-d crucible, ignite
slowly at first with free access ofair to prevent reduction of barium sulphate
by the filter paper and then at 800’-900°C. Cool and weigh. Carry out a
blank test in the same \vay on the same amount of water and reagents, and
subtract any barium sulphate found. Report as sodium sulphate percent.
18.4 Result - Calculate as below:
A x 0.608
Sulphates ( as Sa,SO, ), percent by weight = ~~~ R _ x 100

where
A = weight in g of barium sulphate precipitate, and
B = weight in g of material taken for test (see 17.3.1 ),
Results of duplicate determinations shall be reported.

19. ESTIMATION OF FATTY AND/OR ROSIN ACID

EXTRACTABLE BY ETHER
19.1 General -This method covers the procedure for quantitative
determination of fatty acid or rosin acid extractable by ether.
19.2 Procedure
19.2.1 Extract a representative portion of the sample, 30 g in weight,
with ether in a Soxhlet extraction apparatus for 16 hours. Filter the ether
extract, if necessary, and divide into two portions A and B representing 10
and 20 g of the sample respectively.
19.2.2 Total Acidity Content - Distil off the ether from portion A ‘until
about 10 ml are left. Add 20 ml of alcohol neutralized to phenolphthalein.
Boil the mixture under a reflux condenser for 10 minutes and then titrate
with N/20 sodium hydroxide. Carry out a blank experiment side by side
and apply necessary correction. Express the result as percent oleic acid
present in the sample using the following formula:
Total acidity ( as C,,H,,COOH ),
percent by weight =1 V
~_ x N X.0’282~ x 100
W
where
V = volume in ml of sodium hydroxide solution,
.N = normality of sodium hydroxide solution, and
W = weight in g of the material taken for the test.

25
IS:lO6O(PartlI)-1960

19.23 Rosin Acid Content

19.2.3.1 Distil off the ether from portion B and dry the residue for
30 minutes in a boiling water oven. Add 30 ml ofdry petroleum ether ( BP40”
to 60°C ), boil the mixture under a reflux condenser for 30 minutes and then
filter into a separating funnel, the flask and the filter paper being washed
with petroleum ether. Wash the solution with 3 successive portions of
20 ml water and then transfer the petroleum ether layer to a flask.
19.2.3.2 Dry the residue remaining after the distillation of the petro-
leum ether for 30 minutes in a boiling water oven and then treat with 30 ml
of methyl alcohol to which has been added previously 2 ml of concentrated
sulphuric acid. Boil the mixture under a reflux condenser for exactly
3 minutes. Add 50 ml of 5 percent aqueous sodium chloride solution and
transfer the contents of the flask to a separating funnel. Wash the flask
3 times with 20 ml of ether, adding the washings to the contents of the
separating funnel. Shake the latter vigorously and return the ether extract
layer to the flask.
19.2.3.3 Make two similar extractions of the aqueous portion. Combine
the extracts in a separating funnel and wash successively with 20 ml of
aqueous 5 percent sodium chloride solution until the washing liquid is neutral
to phenolphthalein. Transfer the ether extract to the flask and distil off
the ether until 10 ml is left. Add 20 ml of ethyl alcohol previously neutra-
lized to phenolphthalein, boil under a reflux condenser for 10 minutes and
titrate with N/20 sodium hydroxide solution.
19.2.3.4 Carry out a similar blank and apply necessary correction.
19.2.3.5 Express the result as percent oleic acid present in the sample
using the formula given in 19.2.2.

29. ESTIMATION OF ETHER SOLUBLE MATTER

20.1 General - This method of test covers the procedure for determining
quantitatively the ether soluble matter in paper.
20.2 Procedure - Extract 5 g of the material cut into small pieces with
ethyl ether in a Soxhlet extraction apparatus of approximately 75-m] capa-
city, for 4 hours. The ether should siphon from the Soxhlet apparatus
approximately 18 times per hour. Filter the extract into a weighed flask
and distil off the ether. Dry the residue to constant weight in an oven at
95” to 100°C.
29.3 Result - Calculate the result as percent ether extract on the original
weight of the material. Results of two determinations shall be expressed
as the matter soluble in ether.

21. ESTIMA’l’ION OF BENZENE SOLUBLE MATTER

21.1 General - The method of estimation of benzene soluble matter coven
the range of waterproof papers containing bitumen or pitch.

26
 IS:106O(PartIl)-1960

21.2Test Piece - Cut out a test piece in the form of a rectangle to any
convenient size of not less than 100 cm*. Measure the sides correct to
@5 percent for each dimension. Determine the area of the test piece cor-
rect to the nearest 0.25 percent of the area, Weigh the test piece correct
to 3 significant figures.
213 Procedure -Take three test pieces from different parts of a sheet.
Shred them together and extract with benzene in a Soxhlet extraction
apparatus of 75-ml capacity, for 16 hours. The benzene should siphon from
the Soxhlet apparatus approximately 18 times per hour. Distil off the
benzene and dry the residue to constant weight at 95” to 100°C.
21.4 Results - Calculate the result as grams per square metre of the
original material. At least three determinations shall be made from test
pieces cut from. widely separate portions of the sample and the highest,
lowest and average values reported. The extremes shall not differ from the
average by more than f 5 percent of the average figure.

APPENDIX A
(Chse 13.3.1 )
PREPARATION OF MAGNESIUM OXIDE STANDARD

A-l. GENERAL
A-l.1 This method covers the preparation of a magnesium oxide standard
for calibrating apparatus used in determining the reflectance and spectral
reaectivity of paper and paperboard, The smoke from magnesium freely
burning in air, deposited on a satisfactory base, forms a uniform, fine-
grained, diffusing surface of a high reflectance. This surface of magnesium
oxide ( MgO ) may be made reproducible; hence, it serve-s as a convenient
and reliable standard.

A-2. MATERIALS
A-2.1 The following materials are required:
a) Mugnesium- The magnesium should have high purity and be in
either of the following forms : (1) turnings approximately 0.5 mm
in thickness and 3 mm in width, preferably ofspiral shape, and
containing a minimum of magnesium dust; or (2) magnesium
ribbon 0.15 mm in thickness and 3 mm in width.
NOTX- &gnuium ribbon is prefvrrd for small aurfhca, and magnesium harninp
rotlarge surfaces.

27
lSr1060(PartII)-1960

b) Base - The magnesium oxide shall be deposited on a surface not

affected in air by the heat from the burning magnesium. Asatis-
factory base may be made of aluminium, block porcelain, sheet
steel coated with white vitreous enamel, a baked surface of a
sprayed mixture of magnesium oxide powder and distilled water
or a block of magnesium carbonate. Milk or opal glass is often
unsatisfactory because it easily cracks from heating. Depolished
surfaces are better than polished because the oxide adheres better;
for the same reasqn, metallic surfaces are usually to be preferred
to non-metallic. Surfaces having reflectance high and uniform
throughout the spectrum are better than dark or chromatic sur-
faces, because with the former a thinner layer of oxide is trust-
worthy. The thinner layer is desirable, apart from speed of
preparation, because it does not chip off so readily. A hollow,
tray-like structure is recommended with a flat surface sqd a rim
1 to I.5 mm in height to prevent the edges from chipping.

Aa. PROCEDURE

A-3.1 Combustion of Taraiags - Place about 5 g of the turnings on a

refractory disc approximately 10 cm in diameter and 2.5 cm in thickness
with a recess in the top face; vent holes through the disc may ‘be desirable.
Zirconium silicate and magnesite are suitable refractory materials for the
disc. Ignite the turnings with a hand blow torch or Bunsen burner*. Work
the unignited chips beneath the flame with a silica rod until a slowly burning
ball or clinker is formed; this gives a steady stream of smoke. When the
clinker has to be turned over or broken, in order to permit the magnesium
to burn completely, the surface being coatkd should be temporarily removed,
since the burst of flame is likely to carry/up large dust particles.
A-3.2 Combustion of Ribbon - Cut the magnesium ribbon in a number
of 25-cm lengths. Holding one end of a length of ribbon in pliers, wipe the
ribbon with a freshly laundered cloth to remove surface impurities. Ignite
the free end with a Bunsen burner+ and hold the ribbon in an approximately
horizontal position. When the ribbon has burned to a point within about,
2.5 cm of the pliers, drop it upon a metal or refractory surface below. the
work. Burn additional lengths of ribbon until the coating process is
completed.
A-3.3 Coating - Place the surface to be coated about 8 to 10 cm above the
flame and tilted at 30 degrees to the horizontal. Use of smaller distances
*The operation should be carried out under a well-ventilated hood in order to
dispose of the excess oxide. However, the current of air should not be such as to disturb
either the flame or the stream of smoke arising from the flame. The air of the room in
which the coating is done should be as free as possible of dust and vapours. The operator’s
eyes should be protected from the high intensities of visible and ultraviolet radiant energy
by suitable goggles or other means.

28
 IS:1ofa(PartII)-1960

results in a coarse-grained deposit and risks contamination by possible

impurities in the magnesium. The flame of the burning magnesium should
not be allowed to ‘ lick ’ the oxide surface. Move either the combustion disc
or the surface being coated from side to side in order to obtain a uniform
deposit. Repeat the operation several times until a sufficient deposit is
obtained. The layer should be so thick that further increase produces no
sensible change in reflectance; the critical thickness is about 0.5 mm. Re-
peated deposits of thin coatings rather than the full 0.5 mm deposit at one
time is recommended. Do not attempt to burn a large number of small
charges. In cases where it is inconvenient to measure the thickness of the
coating, place a small dot of India ink on the original surface near the edge,
then deposit magnesium oxide until the spot cannot be seen in good illu-
mination. If the original surface is dark, put on one coat of magnesium
oxide first; a deposit of black smoke ( from a candle or smoky gas flame )
in a small spot near the edge will then supply a similar test.

29
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