substantially free of all foreign material;for example,copper
sulfate,dirt,grea,and oil.
9.Sampling
9.1For routine sampling of cathodes for analysis,the
method of sampling shall be at the discretion of the sampler.
9.2In ca of dispute concerning sampling for chemical
composition,or electrical resistivity,or both,the method of
sampling shall be in accordance with Annex A1.
9.3In ca of special requirements specified in the purcha
order or contract,the method of sampling shall be as agreed
between the supplier and the purchar.
10.Number of Tests and Retests
10.1Tests :
10.1.1Chemical composition shall be determined as the per
element mean of at least two replicate analys of each sample.
10.1.2Electrical resistivity shall be determined as the mean
of results from four specimens.
10.2Retests :
10.2.1In the ca of compositional or resistivity dispute,
retests may be made under the conditions of 9.2.
10.3Umpire Test :
10.3.1In the ca in which retest does not ttle the dispute,
further retest may be made by a qualified third-party laboratory
agreeable to both parties.This provision does not preclude
other contractual agreements.
11.Specimen Preparation
11.1For routine testing,specimen preparation shall be at the
discretion of the preparer.
11.2In the ca of special requirements specified in the
purchar order or contract,specimen preparation shall be as
agreed between the supplier and the purchar.
11.3In the ca of dispute concerning specimen preparation
for chemical composition specified in Table 1or electrical
resistivity,specimen preparation shall be in accordance with
Annex A1.
12.Test Methods
12.1Chemical Composition :12.1.1For routine analysis of Grade 1and Grade 2cathode,the methods of analysis ud shall be at the discretion of the analyst.12.1.2In the ca of dispute concerning the chemical composition,the methods of analysis shall be in accordance with Annex A2,except for copper in Grade 2cathode.12.1.3In the ca of dispute concerning copper content of Grade 2cathode,the method of analysis shall be in accordance with Methods E 53.12.1.4In the ca of dispute concerning special require-ments stated in the purcha order or contract,the methods of analysis ud shall be as agreed between the supplier and the purchar.12.2Electrical Resistivity :12.2.1In the ca of dispute concerning electrical resistiv-ity,the method of testing shall be in accordance with Test Method B 193.13.Significance of Numerical Limits 13.1Calculated values shall
be rounded to the desired number of places as directed in Practice E 29.14.Inspection 14.1The producer shall inspect the product and conduct such tests as are necessary to verify that the requirements of this specification are met.15.Rejection and Rehearing 15.1Rejection :15.1.1Product that fails to conform to the requirements of this specification may be rejected.15.1.2Rejection shall be reported to the producer or sup-plier promptly and in writing.15.1.3In the ca of disagreement or dissatisfaction with the results of the test upon which rejection was bad,the producer or supplier may make claim for a rehearing.15.2Rehearing :15.2.1As a result of product rejection,the supplier may make claim for retest to be conducted by the producer or supplier and the purchar.Samples of the rejected product shall be taken in accordance with this specification and tested by both parties as directed in this specification,or,alterna-tively,upon agreement between both parties,an independent laboratory may be lected for the tests using the test methods prescribed in this specification.16.Packaging and Package Marking 16.1Packaging :16.1.1Cathodes,whether full size or cut,shall be asmbled in bundles or containers of suitable weight for handling and shall be prepared for shipment in such a manner as to ensure acceptance by common carrier for transportation and to afford protection from normal hazards of transportation.16.2Package Marking :16.2.1Each cathode bundle or container shall be marked to identify source and grade.16.2.2When ud,metallic identifying markers shall be firmly attached only to the strapping or shipping container.
TABLE 1Chemical Composition
Element Grade 1A Grade 2A
Percent,%
Copper 99.95,min B
ppm C
Selenium,max 210
Tellurium,max 25
Bismuth,max 1.03
Group total,
Antimony,max 415
Lead,max 540
Arnic,max 515
Iron,max 1025
Nickel,max 1020
Tin,max 510
Sulfur,max 1525
Silver,max 2570
Maximum allowable
A Measurement error is not incorporated in the maximum limits,refer to 10.1.1.
B Including silver.
C Determined from a melted
sample.
17.Keywords
17.1cathode;copper;electrolytic copper;electrorefined
copper;electrowon copper
ANNEXES
(Mandatory Information)
A1.SAMPLING AND SPECIMEN PREPARATION OF ELECTROLYTIC CATHODE COPPER FOR DETERMINATION OF COMPLIANCE WITH SPECIFICATION REQUIREMENTS
A1.1Scope
A1.1.1This practice establishes a procedure for the sam-pling and specimen preparation of electrolytic copper cathodes, Grades1and2,for the determination of conformance with specification requirements.
A1.1.2Units
The values stated in inch-pound units are the standard.The values given in parenthes are mathematical conversions to SI units,which are provided for information only,and are not considered the standard.
A1.1.3This standard does not purport to address the safety concerns,if any,associated with its u.It is the responsibility of the ur of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to u.
A1.2Terminology
A1.2.1Definitions of Terms Specific to This Standard:
A1.2.1.1lot—One shipment,or part of one shipment,pro-duced by one refiner.For u other than continuous cast rod production,shipments greater than200tons short shall be subdivided into lots not exceeding200tons each for sampling purpos.
A1.2.1.2gross sample—The total number of test pieces lected from a lot and considered reprentative of the lot. A1.2.1.3test piece—An individual cathode,or cathode part, randomly lect
ed from the lot.
A1.2.1.4sample—A portion prepared from the gross sample and considered reprentative of the gross sample.
A1.2.1.5specimen—Reprentative fraction taken from the sample for test.
A1.3Selection of Cathode
A1.3.1Nodules shall not be considered a sample repren-tative of the lot.
A1.3.2Cathodes for Continuous Rod Casting:
A1.3.2.1The cathodes shall be available in the original packing for examination.
A1.3.2.2The quantity of cathodes required shall be that necessary toflush the system plus1h of melting furnace operation.
A1.3.2.3All cathode bundles shall be numbered and a random number generator shall be ud to determine which bundles shall be lected for the gross sample.
A1.3.2.4Should there be an insufficient quantity of cath-odes to comply with A1.3.2.2,then the procedure described in A1.3.3shall apply.
A1.3.3Cathodes for Other Us:
A1.3.3.1Not less than25%of the original lot weight or25 tons,whichever is the larger,shall be available in the original packing for examination.
A1.3.3.2A gross sample of24cathodes,or the equivalent in sheared cathode pieces,shall be lected from a lot.To guarantee random lection,all cathodes,or sheared cathode pieces,of the lot shall be individually numbered,and a random number generator shall be ud to lect the individual test pieces.
A1.3.3.3In the ca of sheared cathodes,24full cathodes; 48half-plate cathodes,24each of tops and bottoms;96 quarter-plate cathodes,and24each of the four quarters,shall be lected.
A1.3.3.4The lection of test pieces of cathode sheared smaller than quarter plate shall be by agreement between the producer,or the supplier,and the purchar.
A1.3.3.5Alternatively,to avoid individual numbering of cathodes,or sheared cathode pieces,in the cas
e of large lots, provided both parties agree,individual bundles,or containers, may be lected on a random basis,and then individual cathodes,or sheared cathode pieces,within each bundle,or container,shall be numbered and test pieces lected,using a random number generator as just described.
A1.4Sample Preparation
A1.4.1Cathode for Continuous Rod Casting:
A1.4.1.1The portion ud forflushing the system shall not be ud for sampling.
A1.4.1.2The remaining gross sample,minimum of one hour’s cast,shall be charged to the melting furnace.The rod coils produced from the caster shall be quentially numbered, excluding any coils with obvious defects normally attributed to the rod casting process.
A1.4.1.3Chemical Composition—Each party shall lect2 coils from which a gment of rod approximately16in.(406 mm)in length shall be cut at the trailing ends of the coils.Each rod gment shall be cut into4portions of approximate equal lengths.The16portions shall be divided into4groups;each group shall contain one portion from each of the4original rod gments.The4group
s of rod portions shall be placed in parate noncontaminating containers,then aled and identi-fied for the supplier,the purchar,contingency,and umpire if
necessary.
A1.4.1.4Electrical Resistivity —Each party shall lect 2
coils from which a rod gment of sufficient length for test
shall be taken from the trailing ends of the coils.Each rod
gment shall be cold drawn into a wire about 0.080in.
diameter (2.0mm)and at least 160in.in length (4m).Each
wire coil shall be cut into 4portions of approximately equal
length,and the 16portions shall be individually identified.The
16wires shall be divided into 4groups of 4wires each,one
from each of the 4original rod gments;one group each for
the producer,the purchar,and the umpire,if necessary.
A1.4.2Cathodes for Other Us :
A1.4.2.1Chemical Composition :
(a )From each cathode,or sheared cathode piece,of the gross
sample a vertical strip shall be cut in such a position (e Fig.A1.1)that the collection of the strips so cut reprents all points of the cathode,or sheared cathode piece,including the loops (hangers)for full cathode.All vertical ctions shall be approximately the same width and cut quentially from left to right in the same order as that in which the cathodes were lected.(b )The strips lected shall be immerd in 10%volume/volume (v/v)hydrochloric acid at approximately 20°C for 15min and then removed and washed in distilled or deionized water until all visible extraneous contamination has be
en removed.(c )Where excessive copper sulfate surface contamination is evident,the parties shall confer to determine the extent of
washing.
N OTE 1—Repeat for cond t of twelve cathodes.
FIG.A1.1Vertical Strip Sampling Pattern (Refer to A1.4.2.1(a )of
text)
(d )An electric induction or resistance furnace equipped with a graphite,or other noncontaminating crucible and a clo-fitting lid of the same material with provision for an inert atmosphere within the crucible shall be ud for melting the lected strips.
(e )The crucible shall first be cleaned by melting in it a quantity of copper from the lot in question.The melt shall be discarded.
(f )The prepared cathode strips shall be melted in the cleaned crucible under an inert atmosphere.The molten metal shall be thoroughly stirred with a clean graphite or other noncontaminating rod.
(g )Where the available crucible is not large enough to melt the composite sample,the 24strips shall be grouped into 2or more batches of approximately equal weight for melting.In such cas,the metal from each melt shall be parately sampled.
(h )The metal shall be sampled by one of the following methods:
(1)Ingots:Equal portions of the molten metal shall be cast into graphite ingot moulds at the beginning,middle,and end of the casting operation.The moulds shall provide ingots that are at least 3⁄4by 3⁄4in.(20by 20mm)in cross ction and 4to 8in.(100to 200mm)in length.A sufficient number of ingots shall be cast to provide in excess of 28oz (800g)of small chips when drilled,milled,or sawn,using carbide-tipped tools.The surplus metal not cast into ingots may be discharged by any convenient means.
(2)Shot:Remove a portion of the molten metal using a ladle coated with a noncontaminating mould wash.The molten metal shall be poured into a container of deionized or distilled water until shot in excess of 28oz (800g)has been produced.The depth of the water shall be such that the metal will not adhere to the container.Before sampling,the ladle shall be brought to the molten metal temperature,and the pouring rate shall be such that no metal will solidify in the ladle.The surplus met
al may be discharged by any convenient means.(3)Pin Samples —Take in excess of 28oz (800g)from the molten metal by using either commercially available evacuated glass tubes of veral millimetres in diameter and 100to 120mm in length,or the equipment shown in Fig.A1.2.The latter equipment can be made by attaching a copper tube approxi-mately 9.5-mm diameter and 400-to 500-mm length,to a spring-loaded vacuum pump.The pin may be removed by cutting away that portion of the tube that obviously had been under the molten metal surface,then splitting the tube using a small,sharp,chil and a light hammer.N OTE A1.1—If the vacuum pump method is elected,it is recommended that the ur ensure the cleanliness of the copper tube,and the level of the impurities,if any,in the tube metal be determined to avoid potential specimen contamination.(4)Divide the sample taken into 4portions of approximately 7oz (200g)each and aled in a noncontaminating package and individually identified;one each for the producer,the purchar,contingencies,and the umpire,if necessary.A1.4.2.2Electrical Resistivity :(a )A minimum of 4castings shall be made by pouring the molten metal from (f )in A1.4.2.1into a chill cast mould of sufficient size to produce a wire approximately 0.080in.in diameter (2.0mm)and at least 160in.(approximately 4m)in length.(b )Alternatively,the disputing parties may agree to obtain a sample by drilling lected cathodes along the diagonals to obtain a total of about 140-oz (4000-g)drillings.The drillings shall be melted as described in (d )through (f )of A1.4.2.1and chill cast as described in the preceding paragraph.(c )The cast form may be hot worked initially,provided
care
FIG.A1.2Pin Sampling
Device