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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 1817 (1961): Methods of sampling non-ferrous metals for


chemical analysis [MTD 13: Ores and Raw Materials]

“!ा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”

Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
Is:1817-1961
(Reaffirmed 2000)
In&m Standard
METHODS OF SAMPLING NON-FERROUS
METALS FOR CHEMICAL ANALYSIS

( Second Reprint JUNE 1994 )

UDC 669.2/.8:543.05

: @ Cofiyright1961
.f *
AJREAU 0~ INDIAN STANDARDS
MM k BHAVAN, 9 BAHADUR SHAH IsAFAR MARG
t
NEW DELHI 1 lOOK?
/
Cr3 November 1961
IS : 1817- 1961

Indian Standard
METHODS OF SAMPLING NON-FERROUS
METALS FOR CHEMICAL ANALYSIS
Methods of Sampling Sectional Committee, SMDC 4
Chahaa,,
The TataIron .g. Strol Co. Ltd.. Jamsbedp~~,

DR.. N. AHJ.u?EYULV Lead. Zinc, Tin t\ntmwng and Thrtr Alloys Sectional Committrr
(SMDC 12), IS1
DR. T. BANERJEE Methods of Chemical Analysis Sectional Committee (SNDC Z), IS1
SHRI K. K. BHASIX Light Metals and Their .4lloys Sectional Committer (SMDC IO), 151
SHRI A. K. BHATTACHARYA Zlinistrv of Railways
SHRI M. N. BHIDE (AEtntmfe~
DR. M. K. BOSE Precious Jfetals Sectional Committee (SUDC Is), 15.1
SHRI N. G. CHAKRAVARTY Foundry Sectional Committee (SMDC 17), IS1
SHRI K. C. CHOUDHURI Copper and Copper Alloys Sectional Committee (SalDC 11). ISI
SHRI H. R. DEW&N Indian Hureau of Mines (Ministry ot Steel, 3fines & Fuel),
NagpIlr
SHR~ V. K. S. VARAD.AN (dUemuci
Smr D. N. ELCHIDANA It&b Privatr Ltd., Bombay
SHRI S. S. HONAVAR (ALkmu!e) (Calcutta)
SHRX J. P. PATEL (‘4dtn+t&E) (Madras)
SHRI B. B. GHOSHAL lndian Iron & Steel Co. Ltd., Burnpur
SHRI J. N. BAR&IAN(AItwn&)
SHRI D. B. LAHIRl Indiau Statbtical lhtitute, Calcutta
DR. A. MATCHAX(~&vwtc)
SHRI s. c. LAHIRY Inspection Wing, Directorate General of Suppbes & Disposals
(Ministry of Works, Housing, 8: Supply)
SHRI R. D. LALKAKA Pig Iron & Ferro-Alloys Sectional Committee (SMDC ?I), IS1
SHRI D. R. MALIK Directorate General of Ordnance Factories (Ministry of Defence!.
Calcutta
SHRI R. N. DATTA (Alhmle) (Calcutta)
SHRI A. SOUNDRARAJ (dltnmte) (Bombay)
SHRI N. T. MATHEIV
SHRI M. N. BHATTACHARYA (.4llernale)
DR. H. K. MrmA Refractories Sectional Committee (SMDC IS), IS1
SHHI N. C. MITRA Government of India P.fitlt (Ministry of Finance)
DR. M. K. Bose (A&m&)
Smr M. M. .\~OIJDGILI Indian Non-Ferrous Metals Manufacturers Association, Calcutta
SHRI N. MAZVMDAR (Allerrtate)
SHRI S. N. MUKERJI Government Tes! House, Calcutta
SHRI D. S. MURTV Defence Producti& B Inspection Organiration [Ministry of Uelrnw
&GDP) ]
Xethods of Physical Tests SectIonal Committee (SMDC ?), IS1
Ca;&{ron & 3ialIeable Cast Iron Sectional Committee ISMDC $3).
DR. B. C. ROY Ores Br Rw %faterials Sectional Committee (S!dDC IF,). IS1
SHRI J. S. VATCHACANUIY Steel Swtional Committee (SMDC 5), IS1
SHR~ B. N. SINGH, Director, IS1 (Ex~o~cio Monhrr)
Assistant Director (Statistics1

SHRI S. R. Iivw~asn
Ex!ra Assistant Director (Statistics), 151
Subcommittee on Sampling of Non-Ferrous Metals, SMDC 4 : 1
COX%VZW
SHRI ?.I. C. SEX Gu~rn (kxernmnt ‘Test Housr. Calcutt;t
Members
SHRI A. K. BHATTACH~IYA .Ministry of Railway-
SHRI B. B. GHOSHAL Indian Iron J: Sterl Co. Ltd., Bumpur
SHRI N. C. MITRA Government of India Mint (Ministry of Finance)
SHRI D. Y. MOGHE Directorate General of Ordnance Factories (Ministry of Defence),
Calcutta
:;;; x: ;: ;;y$ Indian Non-Ferrous Metals Manufacturers’ Association, Calcutta
Binani Metal Works Private Ltd., Calcutta

BlfJtEAU OF INDIAN STANDARDS


M&K BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
I
NEW DELHI 110002
IS : 1817- 1961

Indian Standard
METHODS OF SAMPLING NON-FERROUS
METALS FOR CHEMICAL ANALYSIS

0. FOREWORD

0.1 This Indian Standard was adopted by t.he Indian Standards Institu-
tion on 14 November 1961, after the draft finalized by the Methods of
Sampling Sectional ,Committce had been approved by the Structural and
Metals Di\Gsion Council.

0.2 The difficulty in obtaining a thoroughly representative sample of non-


ferrous metals or alloys lies iti the fact that the impurities or the alloying
elements tend to segrcgatc in the process of solidification. Hence, while
sampling non-ferrous metals, due regard should be given to the existihg
knowledge of the typr and estcut of segregation likely to occur in the
particular item.

0.3 Taking into consideration the views of producers, testing authorities


and technologists, the Sectional Committee responsible for the preparation
of this standard felt that it should be related to technological and sampling
procedures followed in the country in this field. Furthermore, due
weightagc had to be given to the need for international co-ordination among
standards prevailing in dlffcrrnt countries of the world in this field. These
considerations led the Sectional Committee to derive assistance from the
following publications :
B.S. 1499 : 1949 SABIPLIXGSOS-I;ERROUSMETALS. British Standards
Institution.
AST!U E 55-48 STANDARD W:THOU OF SAMPLIXC WROUGHT Nos-
I$RI<OLXMET:W AXI) AI.J.OYS FOR DETERJIISATIONOF CHEWCAL
COWOSITIOS. American Society for Testing Materials.
ASTM E 88-50T TEE;TATIVEMETHOD 0~ SA~~PLINGNON-FERROUS
METALS AND ALLOYS IN CAST FORM FOR DETERMINATIONOF CHEMICAL
COJIPOSITIOX.American Society for Testing Materials.
.i ‘i
‘a.4 Metric system has been adopted in India and all quan:ities and dimen-
sib s in this standard have been given in this system.
&
, 2
IS : 1817- 1961

0.5 In reporting the result of a test or analysis, if the final value, observed
or calculated, is to be rounded off, it shall be done in accordance with the
latest version of IS : 2-1960 Rules for Rounding Off Sumcrical Values
@eked).
0.6 This standard is intended chiefly to cover the technical provisions
relating to the sampling of non-ferrous metals and alloys, and it does not
include all the necessary provisions of a contract.

1. SCOPE

1.1 This standard lays down the procedure for preparing samples of non-
ferrous metals and alloys, for the detemlination of chemical composition.
1.2 The procedure laid down in this standard covers the general principles
of preparing samples of non-ferrous metals and is not intended to supersed:
or replace existin, n specification requirements for samp1in.g of a particular
material. The number of samples required to be tested from a lot and the
number of .pieces to be sclccted for the preparation of a sample are not
considered in this standard since these will vary with the material and
will be dealt with in appropriate material specifications.

2. TERMINOLOGY

2.0 For the purpose of this standard, the following definitions shall apply.
2.1 Lot - The quantity, of non-ferrous metals and alloys of one typz and
grade produced under uniform conditions of manufacture and offered for
inspection at one time ; a lot may consist of the whole or a part of the
quantity ordered for.
2.2 Melt, Cast or Heat -The product of a single furnace charge.
Sometimes the furnace contents are tapped into two or more ladies when
the product of each ladle may be called a separate cast.

2.2 sample -The quantity of material, in the form of drilling<, sawings,


&apings, etc, for chemical analysis.
2.4 Castigg - An object, produced by pouring molten metal into specially
prepared’&&ls of desired shape and size depending upon the finished
object to be ‘m,a.$e.
/u 3
IS : 1817 - 1961

2.5 Cake -- A casting intended for rolling into plate or sheet.

2.6 Ingot - An open-mould casting of definite size and shape for remelting.

2.7 Slab - A casting in the form of a bar used for rolling into strip.

2.8 Billet - A solid cylindrical casting used for extrusion into rod, bar,
tube, or shape or for hot piercing into tube.

2.9 Wire Bar - A long rectangular cast bar with tapered ends, used for
rolling into rod and wire.

2.10 Plate - A rolled product, of rectangular cross section, having a


width much greater than thickness which is 3 mm or over.

2.11 Sheet-Material, generally flat, of uniform thickness and over


500 mm width.
2.12 Strip - Material, generally coiled, of uniform specified thickness
and under 500 mm width.

2.13 Wire -A solid section, other than strip, supplied in coils or on


spools, reels or bucks. Flat wire, including square, however, may also be
furnished in straight lengths.

2.14 Supplier - The party supplying the material. The supplier may or
may not be the actual manufacturer of the material.

2.15 Purchaser -The party purchasing the material. The term


’ purchaser ’ shall also cover person or persons expressly authorized in
writing hy the purchaser to act on his behalf for inspection of the material.

3. SAMPLING OF MOLTEN METAL

3.1 During the tapping of the molten metal, from each cast or heat, three
heavily chilled ingots shall be prepared out of three spoonfuls of molten
metal collected during the beginning, middle ‘and the end of the tapping
period taking care to avoid dust and slag. The spoon used shah be of
such material which does not contaminate the metal sampled. The
convenient size for such ingots is 150 x 50 x 6 mm. The sample shall be
prepared from these ingots following the appropriate procedures described
under 4.2.1 to 4.2.4.
3.3 If the metal tends to segregate very. much during solidification as an
in& L or if the ingot cannot be satrsfactorrlp machined, a granulated sample
*9
44 4
IS : 1817- 1961

or a splash sample shall bc prepared as give11 below


a) Granulalcd Sample - The three spoonfuls of moltcu metal collected
during the beginning, middle and the end of the tapping period, taking
care to avoid dust and slag, shall be poured in a thin stream into
cold water, adjusting the diameter of stream to produce granules.
A sufficient quantity of the granules so obtained shall be rcduccd in
size by crushing through a jaw crusher or a roll crusher or broken
in a mortar. From this a sample shall be prepared as untltr 5.
b) Splash Sam$e - The three spoonfuls of molten metal collcctcd tluriup
the beginning, middle and the end of the tapping period, taking care to
avoid dust and slag, shall be poured separately on to a clean surface
so as to produce a thin sheet less than one millimetrr thick. The
sheet shall be sampled as under 4.2.7 and further processed as under 5.

4. SAMPLING OF SOLID METAL

4.1 Wherever high accuracy is desired, and provided there is no risk ot


change in the composition of the metal/alloy due to remelting, a sufficient
quantity of the solicl metal should be rcmeltcd and sampled as under 3.
4.2 When solid metal; are to be sampled by machining the preferred
procedure, to yield a repre;entativc sample, ii to collect material from the
whole cross section of the metal and for this purpose milling or sawing is
recommended. In some cases it may be impracticable, uneconomic or
under certain circumstances undesirable to take millings or sawings, in
which case drillings may be taken.
NOTE 1 -The preference for samples representing the whole cross section of a
solid mass is dictated by the knowledge that in most materials and most solid forms
segregation is greatest, if present at all, across a planr at right angles to the longest
axis of the piece. It is important, however, to choose a plane removed from thr
ends of the piece, particularly if the piece is cast, since there may also be segregation
from the end inwards along the major axis. In some cases where the length and
thickness of the piece arc similar, a sample from a single cross-sectional plane ma>
still give a sample not truly representative of the whole but the best result is likely
to be obtained if the plane chosen is distant from one end of the piece by one-quarter
of the length of the piece.
NOTE 2 - When agreed between the purchaser and the supplier, the remaius
of the test pieces subjected to the physical tests may he used conveniently, in place
of specially selected samples, for chemical analysis.

4.2.1 Un-notched Ingot Without Lugs (See Fig. 1) - Un-notched ingots with-
out lugs (see Fig. 1A) shall be s rwn or milled across the whole section of the ingot
along a plane at right angles to the long axis and halfway between the end
of the ingot and the point of maximum shrinkage, that is, at approximately
a of the way along the length of the ingot (see Fig. 1B) from one end.
Alternatively, five holes shall be drilled in the sampling plane as shown
in Fig.,JC. The drilling shall be through the total thickness and, if
necessary~$lrilled from both the directions, top and bottom.
.9
44 5
IS: 1817 - I%1

1A INGOT

i- SAMPLING
PLANE
16 PLANE POSITION FOR SAWING
OR MILLING

.‘__________-______~____;
/
k_ SAMPLING
PLANE
1C PLANE POSIT:3N FOR DRILLING

FIG. 1 SAMPLING OF UN-XOTCHED INGOTS WITHOUT LIJGS

4.2.2 Un-notched Ingot With Lugs (See Fig. 2) -Lugs which are not more
than 25 mm in thickness cool sufficiently rapidly on solidification and will be
free from serious segregation. For sampling un-notched ingots with lugs
(see Fig. 2A) one half of a lug shall be detached by sawing at right angb
to the longer axis of the ingot and milled across the sawn faces of the piece
(&&,,Fig. 2B). Alternatively, five holes shall be drilled through the ‘lug
alor& t$e sampling plane (see Fig. 2C).
IS : 1817- 1961

2A 1NGOT

2B. PLANE POSITION FOR SAWING


OR MILLING

PLANE
2C PLANE POSITION FOR DRILLING
FIG. ‘2 SAMPLING OF UN-NOTCHED INGOTS WITH LUGS

4.2.3 Notched Ingots (Se? Fig. ?) -In notched ingots of the normal type
(see Fig. 3A), the metal immediately above the notch cools rapidly and may
be considered to be free from serious segregation. For sampling, the ingot
shall be broken or sawn across the centre of the notch and milled across the
broken or sawn faces. Milling shall be stopped when the depth of the
ingot faces exposed, is 25 mm (see Fig. 3B). Alternatively, holes shall be
drilled through the thickness of the chilled section immediately above the
notches as shown in Fig. 3C. If this section is very thin or the individual
sections are very small and drilling becomes impracticable, the ingot shall
be- samj$d by milling. Ingots with a single notch and in certain cases
large ingots with two or three notches may be treated as if each section
was an zcn-no&&d ingot without lug.
IS : 1817- t!%if

3A INGOT

;-25mm MAX

38 PLANE POSITION FOR SAWING


OR MliLlNG

iC PLANE POSITION FOR DRfLLlNG

4.2.4 Iqots oj Other Typt~s (.Sl~~zjxs),Casti~lgs uud Cakes --- In sampling


ingots of types other than those referred to under 4.2.1, 4.2.2 and 4.2.3
and in sampling of castings and cakes, due regard should be given to the
existing knowledge of the type and extent of segregation likely to occur in
the particular item. Machinable items shall be milled or sawn at suitable
points to collect the sample ; alternatively, thelV, shall be sampled by drilling
five holes at suitable points.

4.2.5 Slabs -- Where the size of the slab permits, it shall be sawn through
the cross section at ) of the length from one end ; alternatively, one of the
sawn faces shall be milled. Where this is impracticable, say for large slabs,
at least five holes shall be drilled to half the depth of the slab and at regular
inte&als along one of the diagonals of the major faces from both the direc-
tions, togs and bottom.
42.6 Billets and Wire Bais - Billets and wire bars shall be sawn
through the cross section in a plant perpendicular to the longest axis and
approximately,g of the length from one end. Alternatively, they shall be
milled right actoss one of the sawn faces.

4.2.7 Plates, Sheets or Strips-Clippings, millings or sawings repre-


senting the whole cross section along a plane at right angles to the length
in the case of strips and at a convenient angle to the direction of rolling,
normally 45” or less, in the case of sheets shall be taken. Alternatively,
sheets or strips may be folded once or more by bringing the ends together
and closing the bends ; the inside sheared edges may then be milled or flat
surface shall be drilled; special precautions are needed for coated materials.

4.2.8 Wires ‘-- Clippings shall be taken from both ends of the coil.

4.2.9 Metal Scrap - Usually metal scrap will consist of old castings,
sheets, plates, old tubes, wires, bars, etc. For sampling, pieces representing
each type of material in the same proportion as in the scrap shall be
selected. Proportionate quantity of drillings, sawings, millings or clippings
taken from these selected pieces shall be charged into a pre-heated crucible
and melted as rapidly as possible without overheating. The use of a flux,
which might alter the composition by reacting with the melt, shall be
avoided.
NOTE -When testing for the non-ferrous metal contents in metal scraps mixed
with ferrous impurities, the ferrous portion shall be removed by use of strong
magnet and separately accounted for in the analysis.

5. PREPARATION OF SAMPLE AND STORAGE

5.1 Drillings, millings, sawings, clippings, etc., shall be carefully examined


to remove any foreign material. Non-magnetic metals or alloys shall be
carefully treated with a strong magnet to remove any particles of iron
introduced in the process of drilling, milling, etc. They shall be mix,ed
well and reduced to the requisite quantity to constitute a sample. The
weight of the sample shall comply with the sampling requirements of Indian
Standard specification covering that material but shall not be less than
100 g. The sample shall be divided into three approximately equal parts,
each of which shall be placed in a package and scaled for distribution-one
each to the supplier, the purchaser and a referee.

5.2 Samples that are to be stored over long periods or that are oxidized
readily or otherwise altered in composition under varying atmospheric
conditions or that may become seriously contaminated in contact with
paper qf cardboard shall be kept in wide-mouthed and well stoppered glass
bottles. ‘$I other cases tight leakproof paper sample envelopes or card-
board cartonspshall be used to store the sample.
/u
9
1s : 1813 - 1961

6. GENERAL PRECAUTIONS

6.1 The ingot, slab, sheet, etc, to be saInpled shall be clean and frw from
scale, dirt, oil, grease, etc. If necessary, they shall ht. c.lcancd using
suitable solvent, and dried. Scale and dirt may be removed by suitabk
mechanical or chemical treatment ; if chemical methods of cleaning arr
used, such operations should not alter the metal surface in any uay. When
testing for proportion of metal contained, as in the case of scrap)<, the<r.
provisions do not apply as a general rule.

6.2 The saw, drill, cutter or other tools used shall be capable of producing
small .and uniform particles. They shall be thoroughly cleaned befor?
use. Depth of cut, speed of cutting, etc., shall be so regulated that excessivt
heating and consequent oxidation of the snmple shall be avoided. Brittle
metal and alloys shall be pulverized in a suitable percussion mortar.

6.3 Ko lubricant shall be used for drilling, sawing, etc., exc:t.pt in cases
where experience shows that the use of lllbricants dots not vitiate snmpling
and lubrication is necessary to avoid excessive oxidation of ttlc. 5anlp!t*,
* to reduce power requirements, or to save labour and tinlp. 111 SWII CAL.;:+
the use and choice of a satisfactory lubricant shall be agreed upon l~~t\~i~c~n
the supplier and the purchaser. Lubricants selected shall not altcl 01
change the composition of the materials during contact. The lubrica.nts
shall be completely removed as soon 2s possidle after drilling or milimg
operation by the use of suitable so!vents, and d:-ied.

6.4 Drillings, sawings, or clippings of non-magnetic non-ferrous alloys


shall be carefully treated with a strong rnagnct to rerno\.o anv particles ;,f
iron introduced in the operation. Contamination of this l&d 5houid br
avoidtd as far as possible by the 11se o f suitz.blc cutt.ing took. In tht>
case of scme metals, an acid dip n-,ay be r,ecc ssar~ if low iron is critical.

10
BUREAU OF INDIAN STANDARDS

Headquarters :
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