Designation: B 115 – 00 (Reapproved 2004)

Standard Specification for

Electrolytic Copper Cathode1
This standard is issued under the fixed designation B 115; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope* E 53 Test Methods for Determination of Copper in Unal-

1.1 This specification establishes the requirements for elec- loyed Copper by Gravimetry
trolytic copper cathode; electrorefined and electrowon. 3. Terminology
1.2 Units—The values stated in inch-pound units are the
standard. The values given in parentheses are mathematical 3.1 For definition of general terms related to copper and
conversions to SI units that are provided for information only copper alloys, refer to the current editions of Classification
and are not considered standard. B 224 and Terminology B 846.

NOTE 1—Cathode produced to this specification corresponds to the 4. Ordering Information

designation “Cath” as defined in Classification B 224 and may be used to 4.1 Orders for product shall include the following informa-
produce all other coppers listed in Classification B 224 that are normally
produced from “Cath” copper.
tion, as applicable:
NOTE 2—Grade 1 cathode conforms to the chemical compositional 4.1.1 ASTM designation and year of issue (for example,
requirements of Copper UNS No. C11040, except for oxygen, and is B 115 – XX),
suitable for the manufacture of wire rod as designated in Specification 4.1.2 Cathode grade (Table 1),
B 49. 4.1.3 Size; full cathode or cut,
1.3 The following hazard caveat applies to the test methods 4.1.4 Total weight of each size.
described in Annex A2 of this specification: This standard does
5. Chemical Composition
not purport to address all of the safety concerns, if any,
associated with its use. It is the responsibility of the user of this 5.1 The cathode furnished shall conform to the requirements
standard to establish appropriate safety and health practices of Table 1 for the grade specified in the contract or purchase
and determine the applicability of regulatory limitations prior order.
to use. 5.2 These composition limits do not preclude the presence
of other elements. Limits may be established and analysis
2. Referenced Documents required for unnamed elements by agreement between the
2.1 ASTM Standards: 2 supplier and the purchaser and such agreement shall be part of
B 49 Specification for Copper Rod Drawing Stock for the contract or purchase order.
Electrical Purposes
6. Physical Property Requirements
B 193 Test Method for Resistivity of Electrical Conductor
Materials 6.1 Electrical Resistivity:
B 224 Classification of Coppers 6.1.1 The maximum electrical resistivity for product pro-
B 846 Terminology for Copper and Copper Alloys duced from Grade 2 cathode shall be 0.153 28 V·g/m2 (con-
E 29 Practice for Using Significant Digits in Test Data to ductivity 100.0 % minimum IACS) at 20°C (68°F) annealed3
Determine Conformance with Specifications when tested in accordance with Test Method B 193. Measure-
E 50 Practices for Apparatus, Reagents, and Safety Consid- ment error is not included in the maximum/minimum limit.
erations for Chemical Analysis of Metals, Ores, and
7. Dimensions, Mass, and Permissible Variations
Related Materials
7.1 Full-size cathodes or cathodes cut to size may be
supplied as agreed upon between supplier and purchaser.
1
This specification is under the jurisdiction of ASTM Committee B05 on Copper
and Copper Alloys and is the direct responsibility of Subcommittee B05.07 on 8. Workmanship, Finish, and Appearance
Refined Copper.
Current edition approved Oct. 1, 2004. Published October 2004. Originally 8.1 Cathodes shall withstand ordinary handling without
approved in 1938. Last previous edition approved in 2000 as B 115 – 00. breakage or excessive separation of nodules. They shall be
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on NBS Notebook 100 available from National Technical Information Service, 528
the ASTM website. Port Royal Rd., Springfield, VA 22161.

*A Summary of Changes section appears at the end of this standard.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 B 115 – 00 (2004)
TABLE 1 Chemical Composition 12. Test Methods
Element Grade 1A Grade 2A 12.1 Chemical Composition:
Percent,% 12.1.1 For routine analysis of Grade 1 and Grade 2 cathode,
Copper 99.95, minB the methods of analysis used shall be at the discretion of the
ppmC analyst.
Selenium, max 2 10 12.1.2 In the case of dispute concerning the chemical
Tellurium, max 2 5
Bismuth, max 1.0 3
composition, the methods of analysis shall be in accordance
Group total, max 3 ... with Annex A2, except for copper in Grade 2 cathode.
12.1.3 In the case of dispute concerning copper content of
Antimony, max 4 15
Lead, max 5 40
Grade 2 cathode, the method of analysis shall be in accordance
Arsenic, max 5 15 with Test Methods E 53.
Iron, max 10 25 12.1.4 In the case of dispute concerning special require-
Nickel, max 10 20
Tin, max 5 10
ments stated in the purchase order or contract, the methods of
Sulfur, max 15 25 analysis used shall be as agreed between the supplier and the
Silver, max 25 70 purchaser.
Maximum allowable total 65 ...
12.2 Electrical Resistivity:
A
Measurement error is not incorporated in the maximum limits, refer to 10.1.1. 12.2.1 In the case of dispute concerning electrical resistiv-
B
Including silver.
C
Determined from a melted sample. ity, the method of testing shall be in accordance with Test
Method B 193.

substantially free of all foreign material; for example, copper 13. Significance of Numerical Limits
sulfate, dirt, grease, and oil. 13.1 Calculated values shall be rounded to the desired
number of places as directed in Practice E 29.
9. Sampling
9.1 For routine sampling of cathodes for analysis, the 14. Inspection
method of sampling shall be at the discretion of the sampler. 14.1 The producer shall inspect the product and conduct
9.2 In case of dispute concerning sampling for chemical such tests as are necessary to verify that the requirements of
composition, or electrical resistivity, or both, the method of this specification are met.
sampling shall be in accordance with Annex A1.
9.3 In case of special requirements specified in the purchase 15. Rejection and Rehearing
order or contract, the method of sampling shall be as agreed 15.1 Rejection:
between the supplier and the purchaser. 15.1.1 Product that fails to conform to the requirements of
this specification may be rejected.
10. Number of Tests and Retests 15.1.2 Rejection shall be reported to the producer or sup-
10.1 Tests: plier promptly and in writing.
10.1.1 Chemical composition shall be determined as the per 15.1.3 In the case of disagreement or dissatisfaction with the
element mean of at least two replicate analyses of each sample. results of the test upon which rejection was based, the producer
10.1.2 Electrical resistivity shall be determined as the mean or supplier may make claim for a rehearing.
of results from four specimens. 15.2 Rehearing:
10.2 Retests: 15.2.1 As a result of product rejection, the supplier may
10.2.1 In the case of compositional or resistivity dispute, make claim for retest to be conducted by the producer or
retests may be made under the conditions of 9.2. supplier and the purchaser. Samples of the rejected product
10.3 Umpire Test: shall be taken in accordance with this specification and tested
10.3.1 In the case in which retest does not settle the dispute, by both parties as directed in this specification, or, alterna-
further retest may be made by a qualified third-party laboratory tively, upon agreement between both parties, an independent
agreeable to both parties. This provision does not preclude laboratory may be selected for the tests using the test methods
other contractual agreements. prescribed in this specification.

11. Specimen Preparation 16. Packaging and Package Marking

11.1 For routine testing, specimen preparation shall be at the 16.1 Packaging:
discretion of the preparer. 16.1.1 Cathodes, whether full size or cut, shall be assembled
11.2 In the case of special requirements specified in the in bundles or containers of suitable weight for handling and
purchaser order or contract, specimen preparation shall be as shall be prepared for shipment in such a manner as to ensure
agreed between the supplier and the purchaser. acceptance by common carrier for transportation and to afford
11.3 In the case of dispute concerning specimen preparation protection from normal hazards of transportation.
for chemical composition specified in Table 1 or electrical 16.2 Package Marking:
resistivity, specimen preparation shall be in accordance with 16.2.1 Each cathode bundle or container shall be marked to
Annex A1. identify source and grade.

2
 B 115 – 00 (2004)
16.2.2 When used, metallic identifying markers shall be
firmly attached only to the strapping or shipping container.
17. Keywords
17.1 cathode; 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

A1.1 Scope A1.3.2.3 All cathode bundles shall be numbered and a

A1.1.1 This practice establishes a procedure for the sam- random number generator shall be used to determine which
pling and specimen preparation of electrolytic copper cathodes, bundles shall be selected for the gross sample.
Grades 1 and 2, for the determination of conformance with A1.3.2.4 Should there be an insufficient quantity of cath-
specification requirements. odes to comply with A1.3.2.2, then the procedure described in
A1.3.3 shall apply.
A1.1.2 Units
A1.3.3 Cathodes for Other Uses:
The values stated in inch-pound units are the standard. The
A1.3.3.1 Not less than 25 % of the original lot weight or 25
values given in parentheses are mathematical conversions to SI
tons, whichever is the larger, shall be available in the original
units that are provided for information only and are not
packing for examination.
considered standard.
A1.3.3.2 A gross sample of 24 cathodes, or the equivalent in
A1.1.3 This standard does not purport to address the safety sheared cathode pieces, shall be selected from a lot. To
concerns, if any, associated with its use. It is the responsibility guarantee random selection, all cathodes, or sheared cathode
of the user of this standard to establish appropriate safety and pieces, of the lot shall be individually numbered, and a random
health practices and determine the applicability of regulatory number generator shall be used to select the individual test
limitations prior to use. pieces.
A1.3.3.3 In the case of sheared cathodes, 24 full cathodes;
A1.2 Terminology 48 half-plate cathodes, 24 each of tops and bottoms; 96
A1.2.1 Definitions of Terms Specific to This Standard: quarter-plate cathodes, and 24 each of the four quarters, shall
A1.2.1.1 lot—One shipment, or part of one shipment, pro- be selected.
duced by one refiner. For use other than continuous cast rod A1.3.3.4 The selection of test pieces of cathode sheared
production, shipments greater than 200 tons short shall be smaller than quarter plate shall be by agreement between the
subdivided into lots not exceeding 200 tons each for sampling producer, or the supplier, and the purchaser.
purposes. A1.3.3.5 Alternatively, to avoid individual numbering of
A1.2.1.2 gross sample—The total number of test pieces cathodes, or sheared cathode pieces, in the case of large lots,
selected from a lot and considered representative of the lot. provided both parties agree, individual bundles, or containers,
A1.2.1.3 test piece—An individual cathode, or cathode part, may be selected on a random basis, and then individual
randomly selected from the lot. cathodes, or sheared cathode pieces, within each bundle, or
container, shall be numbered and test pieces selected, using a
A1.2.1.4 sample—A portion prepared from the gross
random number generator as just described.
sample and considered representative of the gross sample.
A1.2.1.5 specimen—Representative fraction taken from the A1.4 Sample Preparation
sample for test.
A1.4.1 Cathode for Continuous Rod Casting:
A1.3 Selection of Cathode A1.4.1.1 The portion used for flushing the system shall not
be used for sampling.
A1.3.1 Nodules shall not be considered a sample represen- A1.4.1.2 The remaining gross sample, minimum of one
tative of the lot. hour’s cast, shall be charged to the melting furnace. The rod
A1.3.2 Cathodes for Continuous Rod Casting: coils produced from the caster shall be sequentially numbered,
A1.3.2.1 The cathodes shall be available in the original excluding any coils with obvious defects normally attributed to
packing for examination. the rod casting process.
A1.3.2.2 The quantity of cathodes required shall be that A1.4.1.3 Chemical Composition—Each party shall select 2
necessary to flush the system plus 1 h of melting furnace coils from which a segment of rod approximately 16 in. (406
operation. mm) in length shall be cut at the trailing ends of the coils. Each

3
 B 115 – 00 (2004)
rod segment shall be cut into 4 portions of approximate equal wire coil shall be cut into 4 portions of approximately equal
lengths. The 16 portions shall be divided into 4 groups; each length, and the 16 portions shall be individually identified. The
group shall contain one portion from each of the 4 original rod 16 wires shall be divided into 4 groups of 4 wires each, one
segments. The 4 groups of rod portions shall be placed in from each of the 4 original rod segments; one group each for
separate noncontaminating containers, then sealed and identi- the producer, the purchaser, and the umpire, if necessary.
fied for the supplier, the purchaser, contingency, and umpire if A1.4.2 Cathodes for Other Uses:
necessary. A1.4.2.1 Chemical Composition:
A1.4.1.4 Electrical Resistivity—Each party shall select 2 (a) From each cathode, or sheared cathode piece, of the
coils from which a rod segment of sufficient length for test gross sample a vertical strip shall be cut in such a position (see
shall be taken from the trailing ends of the coils. Each rod Fig. A1.1) that the collection of the strips so cut represents all
segment shall be cold drawn into a wire about 0.080 in. points of the cathode, or sheared cathode piece, including the
diameter (2.0 mm) and at least 160 in. in length (4 m). Each loops (hangers) for full cathode. All vertical sections shall be

NOTE 1—Repeat for second set of twelve cathodes.

FIG. A1.1 Vertical Strip Sampling Pattern (Refer to A1.4.2.1(a) of text)

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 B 115 – 00 (2004)
approximately the same width and cut sequentially from left to (1) Ingots: Equal portions of the molten metal shall be cast
right in the same order as that in which the cathodes were into graphite ingot moulds at the beginning, middle, and end of
selected. the casting operation. The moulds shall provide ingots that are
(b) The strips selected shall be immersed in 10 % volume/ at least 3⁄4 by 3⁄4 in. (20 by 20 mm) in cross section and 4 to 8
volume (v/v) hydrochloric acid at approximately 20°C for 15 in. (100 to 200 mm) in length. A sufficient number of ingots
min and then removed and washed in distilled or deionized shall be cast to provide in excess of 28 oz (800 g) of small
water until all visible extraneous contamination has been chips when drilled, milled, or sawn, using carbide-tipped tools.
removed. The surplus metal not cast into ingots may be discharged by
(c) Where excessive copper sulfate surface contamination any convenient means.
is evident, the parties shall confer to determine the extent of (2) Shot: Remove a portion of the molten metal using a
washing. ladle coated with a noncontaminating mould wash. The molten
(d) An electric induction or resistance furnace equipped metal shall be poured into a container of deionized or distilled
with a graphite, or other noncontaminating crucible and a water until shot in excess of 28 oz (800 g) has been produced.
close-fitting lid of the same material with provision for an inert The depth of the water shall be such that the metal will not
atmosphere within the crucible shall be used for melting the adhere to the container. Before sampling, the ladle shall be
selected strips. brought to the molten metal temperature, and the pouring rate
(e) The crucible shall first be cleaned by melting in it a shall be such that no metal will solidify in the ladle. The
quantity of copper from the lot in question. The melt shall be surplus metal may be discharged by any convenient means.
discarded. (3) Pin Samples—Take in excess of 28 oz (800 g) from the
(f) The prepared cathode strips shall be melted in the molten metal by using either commercially available evacuated
cleaned crucible under an inert atmosphere. The molten metal glass tubes of several millimetres in diameter and 100 to 120
shall be thoroughly stirred with a clean graphite or other mm in length, or the equipment shown in Fig. A1.2. The latter
noncontaminating rod. equipment can be made by attaching a copper tube approxi-
(g) Where the available crucible is not large enough to melt mately 9.5-mm diameter and 400- to 500-mm length, to a
the composite sample, the 24 strips shall be grouped into 2 or spring-loaded vacuum pump. The pin may be removed by
more batches of approximately equal weight for melting. In cutting away that portion of the tube that obviously had been
such cases, the metal from each melt shall be separately under the molten metal surface, then splitting the tube using a
sampled. small, sharp, chisel and a light hammer.
(h) The metal shall be sampled by one of the following NOTE A1.1—If the vacuum pump method is elected, it is recommended
methods: that the user ensure the cleanliness of the copper tube, and the level of the

FIG. A1.2 Pin Sampling Device

5
 B 115 – 00 (2004)
impurities, if any, in the tube metal be determined to avoid potential original castings; one group each for the producer, the pur-
specimen contamination. chaser, contingencies, and the umpire if necessary.
(4) Divide the sample taken into 4 portions of approxi- A1.5 Specimen Preparation
mately 7 oz (200 g) each and sealed in a noncontaminating
A1.5.1 Continuous Cast Rod: Chemical Composition—
package and individually identified; one each for the producer,
Chips, clippings, or drillings shall be taken from the rod sample
the purchaser, contingencies, and the umpire, if necessary.
using a noncontaminating tool.
A1.4.2.2 Electrical Resistivity: A1.5.2 Continuous Cast Rod: Electrical Resistivity—The
(a) A minimum of 4 castings shall be made by pouring the wire specimens shall be annealed in an inert atmosphere at
molten metal from (f) in A1.4.2.1 into a chill cast mould of approximately 500°C (932°F) for 30 min and cooled to
sufficient size to produce a wire approximately 0.080 in. in ambient temperature under inert atmosphere. When cool, the
diameter (2.0 mm) and at least 160 in. (approximately 4 m) in wires are removed and cut to test length.
length. A1.5.3 Cathodes for Others Uses: Chemical Composition:
(b) Alternatively, the disputing parties may agree to obtain A1.5.3.1 Drillings from A1.4.2.1 (see Ingots: (1)) shall be
a sample by drilling selected cathodes along the diagonals to etched in 50 % (v/v) nitric acid until the reaction is clearly
obtain a total of about 140-oz (4000-g) drillings. The drillings visible, then washed four times with distilled or deionized
shall be melted as described in (d) through ( f) of A1.4.2.1 and water, once with alcohol or acetone, and air dried.
chill cast as described in the preceding paragraph. A1.5.3.2 Clean the shot (see Shot: (2)), as described in
(c) The cast form may be hot worked initially, provided A1.5.3.1.
care is taken to avoid contamination, or excessive oxidation, or A1.5.3.3 Extreme care must be exercised in the removal of
both. The external oxide shall be removed and the sample cold all glass from samples taken with evacuated glass tubes to
drawn. Each wire coil shall be cut into 4 portions of approxi- avoid contamination from the glass.
mately equal lengths, the 16 portions thus obtained shall be A1.5.4 Cathodes for Other Uses: Electrical Resistivity—
divided into 4 groups of 4 wires each, one from each of the 4 Prepare as described in A1.5.2.

A2. TEST METHODS FOR DETERMINATION OF COMPLIANCE WITH CHEMICAL COMPOSITION REQUIREMENTS
FOR ELECTROLYTIC COPPER CATHODE

A2.1 Scope A2.4 Reagents and Material

A2.1.1 These test methods establish the procedures for the A2.4.1 Reagents and materials required for each test
chemical analysis of electrolytic copper cathode for the ele- method are listed in a separate section in the test method.
ments with the specified limiting value stated in Table 1 of this
specification. A2.5 Sampling
A2.1.2 These test methods do not purport to address all of A2.5.1 Sampling shall be in accordance with specification
the safety concerns, if any, associated with their use. It is the requirements.
responsibility of the user of these test methods to consult and
establish appropriate safety and health practices and deter- A2.6 Rounding Calculated Values
mine the applicability of regulatory limitations prior to use. A2.6.1 Calculated values shall be rounded to the desired
Special hazard statements are given in A2.10 and A2.22. number of places as directed in Practice E 29.
A2.1.3 The test methods are arranged in the following
order: TEST METHOD A—ANTIMONY, ARSENIC,
BISMUTH, IRON, LEAD, NICKEL, SELENIUM,
Sections
SILVER, TELLURIUM, AND TIN BY
Antimony, arsenic, bismuth, iron, lead, nickel, A2.7-A2.17 ELECTROTHERMAL ATOMIZATION ATOMIC
selenium, silver, tellurium, and tin by electro-
thermal atomization atomic absorption spectrometry
ABSORPTION SPECTROSCOPY
Sulfur by combustion and infrared detector A2.18-A2.29
A2.7 Scope
A2.2 Significance and Use A2.7.1 This test method covers the determination of anti-
A2.2.1 These test methods are intended to test electrolytic mony, arsenic, bismuth, iron, lead, nickel, selenium, silver,
copper cathode for compliance with chemical composition tellurium, and tin in electrolytic cathode copper.
requirements of Specification B 115.
A2.8 Summary of Test Method A
A2.3 Apparatus A2.8.1 The test sample is dissolved in nitric acid and the
A2.3.1 Apparatus required for each determination is listed solution diluted to a known volume. An aliquot is introduced
in separate sections preceding the procedure. into an electrothermal atomic absorption spectrometer with

6
 B 115 – 00 (2004)
background correction capability. The absorption of the reso- discharge lamps. Follow the manufacturer’s manual for instal-
nance line energy from the spectrum of the element is lation and system operation.
measured and compared with that of calibration solutions of A2.12.2 Graphite Tubes—Pyrolytically coated graphite
the same element in a matched matrix. tubes and L’vov platforms for use in the electrothermal
atomizer.
A2.9 Significance and Use A2.12.3 Micropipets—5 to 250 µL.
A2.9.1 This test method is intended to test electrolytic A2.12.4 Operating Parameters—Determine the sample size
cathode copper for compliance with antimony, arsenic, bis- and optimum electrothermal atomizer parameters for the type
muth, iron, lead, nickel, selenium, silver, tellurium, and tin of atomizer used as recommended by the instrument manufac-
requirements of the specification. turer. The analytical lines are as follows:
Element Wavelength, nm
A2.10 Interferences Antimony 217.6
A2.10.1 Elements normally present in electrolytic cathode Arsenic 193.9
Bismuth 223.0
copper do not interfere. Iron 248.3
Lead 283.3
A2.11 Hazards Nickel 232.0
Selenium 196.0
A2.11.1 Warning—The ultraviolet radiation must be Silver 328.1
shielded at all times to prevent eye damage. Tellurium 214.3
Tin 224.6
A2.11.2 Arsenic trioxide (As2O3) is a hazardous reagent and
may be fatal if swallowed. Inhalation and prolonged or A2.13 Reagents and Materials
repeated skin contact are to be avoided.
A2.13.1 Acids—Acids, hydrochloric and nitric, should be
A2.11.3 Tellurium and tellurium compounds are hazardous
carefully checked for purity to ensure they do not contaminate
reagents and may be fatal if ingested. Avoid inhalation and
the analysis.
prolonged or repeated skin contact.
A2.13.2 Water—The quality of the water should be care-
A2.11.4 Selenium and selenium compounds are potentially
fully checked for purity to ensure it does not contaminate the
hazardous reagents. Avoid ingestion, inhalation, or prolonged
analysis.
and repeated skin contact.
A2.13.3 Argon—Purity: 99.98 %, min.
A2.11.5 For other specific precautions, refer to Practice
A2.13.4 Copper Solution (1 mL = 50-mg Cu)—Transfer 10
E 50.
g of certified high purity copper (NBS SRM 393 or equivalent)
A2.11.6 Technical Hazards—Warnings
into a 250-mL beaker. Add 25-mL water and 25-mL HNO3 in
A2.11.6.1 It is essential that acids and water be carefully
5-mL increments. After the last increment addition, heat gently
checked for purity to avoid contamination from this source.
to dissolve the copper and expel the brown fumes. Cool,
A2.11.6.2 Laboratory glassware should be thoroughly
transfer to a 200-mL volumetric flask, dilute to volume with
cleaned, soaked in 9 % by volume HNO3 for several hours, and
50 % by volume HNO3 and mix.
rinsed before use. Previously etched glassware should be
A2.13.4.1 Known impurities in the copper metal must be
avoided.
considered when determining specific element ppm concentra-
A2.11.6.3 Effects of nonspecific absorption and light scat-
tion in Table A2.1 and Table A2.2.
tering must be compensated by matrix matching of calibration
A2.13.5 Antimony Standard Solution (1 mL = 0.10-mg
solutions and background correction.
Sb)—Dissolve 0.2740 g of potassium antimony tartrate
A2.11.6.4 Matrix Modifiers—The copper matrix reduces
(KSbC4H4O7·1/2H2O; purity: 99.9 %, min) with water in a
loss for most elements during the char step. Modifiers such as
250-mL beaker. Transfer to a 500-mL volumetric flask, dilute
magnesium nitrate may be found useful to stabilize further
to volume and mix.
elements like nickel and tin.
A2.13.6 Arsenic Standard Solution (1 mL = 0.10-mg As)—
A2.11.6.5 Should lack of homogeneity be suspect in the test
Dissolve 0.1320 g of arsenic trioxide (As2O3; purity: 99.9 %,
material, a 10-g sample, weighed to the nearest 1 mg should be
min) in a 100-mL beaker with one or two pellets of potassium
taken and diluted to 1 L with the appropriate amount of acid.
hydroxide (KOH) in 50 mL of water. Heat gently to dissolve
A2.11.6.6 The lower limit of elemental determination is
the salt. Transfer to a 500-mL volumetric flask. Add 50-mL
affected by the residual level of the element in the copper.
HNO3, dilute to volume and mix.
A2.11.6.7 Optimum settings for operating parameters vary
instrument to instrument and must be experimentally estab-
lished for a particular instrument. TABLE A2.1 Calibration Solution
ppm: As, Sb, Bi, Fe, Pb,
Flask No. µL
Ni, Ag, Se, and Te
A2.12 Apparatus
1 5 0.5
A2.12.1 Atomic Absorption Spectrometer and Electrother- 2 10 1.0
mal Atomizer—The instrument shall be equipped with a 3 25 2.5
background corrector and high speed readout electronics or a 4 50 5.0
5 100 10.0
high-speed recorder, or both. The instrument should be capable 6 250 25.0
of using single-element hollow cathode lamps or electrodeless

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 B 115 – 00 (2004)
TABLE A2.2 Calibration Solution A2.14.2.1 Set the required instrument parameters and align
Flask No. µL
ppm: As, Sb, Bi, Fe, Pb, Ni, the electrothermal atomizer according to the manufacturer’s
Se, Sn, and Te recommendation.
7 5 0.5 A2.14.2.2 Determine the optimum electrothermal atomizer
8 10 1.0
9 25 2.5
parameters for the particular type atomizer and sample size as
10 50 5.0 recommended by the instrument manufacturer.
11 100 10.0 A2.14.3 Spectrometry:
12 250 25.0
A2.14.3.1 Zero the instrument or set the base line on the
recorder, or both.
A2.14.3.2 Check the zero stability and lack of spectral
A2.13.7 Bismuth Standard Solution (1 mL = 0.10- mg Bi)— interference within the atomization system by running the
Dissolve 50 mg of bismuth (Bi; purity: 99.90 %, min) in 10 mL preset heating program for blank firing of the electrothermal
of 25 % by volume HNO3. Heat gently to dissolve the metal atomizer. Repeat to ensure baseline stability.
and expel the brown fumes. Cool, transfer to a 500-mL A2.14.3.3 Inject and atomize the calibration solutions in the
volumetric flask. Add 50-mL HNO3, dilute to volume and mix. order of increasing concentrations. Inject each solution three
A2.13.8 Iron Standard Solution (1 mL = 0.10-mg Fe)— times and record the readings. Should good replication not be
Dissolve 50 mg of iron (Fe; purity: 99.9 %, min) in 10-mL achieved, repeat the process.
HNO3. Heat gently to dissolve the iron and expel the brown A2.14.3.4 Check for memory effects by running the blank
fumes. Cool, transfer to a 500-mL volumetric flask. Add 50-mL firing program and reset the zero, or baseline, if necessary.
HNO3, dilute to volume and mix. A2.14.3.5 Plot the average reading from each calibration
A2.13.9 Lead Standard Solution (1 mL = 0.10-mg Pb)— versus concentration of the analyte in the calibration solution.
Dissolve 50-mg lead (Pb; purity: 99.9 %, min) in 10 mL of A2.14.3.6 For systems with direct instrument calibration,
25 % by volume HNO3. Heat gently to dissolve the lead and ensure that a sufficient number of each calibration solutions is
expel the brown fumes. Cool, transfer to a 500-mL volumetric injected and atomized to determine that proper calibration is
flask. Add 50-mL HNO3, dilute to volume and mix. achieved.
A2.13.10 Nickel Standard Solution (1 mL = 0.10-mg Ni)—
Dissolve 50-mg nickel (Ni; purity: 99.9 %, min) in 20 mL of A2.15 Procedure
50 % by volume HNO3. Heat gently to dissolve the nickel and A2.15.1 Dissolve a 1-g sample, weighed to the nearest 1
expel the brown fumes. Cool, transfer to a 500-mL volumetric mg, in a 100-mL beaker with 20 mL of 50 % by volume HNO3.
flask. Add 50-mL HNO3, dilute to volume and mix. Heat gently to dissolve the copper and expel the brown fumes.
A2.13.11 Selenium Standard Solution (1 mL = 0.10-mg Transfer to a 100-mL volumetric flask. Cool, dilute to volume,
Se)—Dissolve 70.3-mg selenium dioxide (SeO2; purity; and mix.
99.0 %, min) in 50-mL water. Transfer to a 500-mL volumetric A2.15.2 Ensure that the test solution is within 1°C of the
flask. Add 50-mL HNO3, dilute to volume and mix. calibration solutions. Inject and atomize the test solution for
A2.13.12 Silver Standard Solution (1 mL = 0.10-mg Ag)— three readings and record the observations.
Dissolve 50-mg silver (Ag; purity: 99.9 %, min) in 20 mL of
50 % by volume HNO3. Heat gently to dissolve the silver and A2.16 Calculations
expel the brown fumes. Cool, transfer to a 500-mL volumetric
flask. Add 50-mL HNO3, dilute to volume and mix. A2.16.1 Calculate the concentration of each element to be
A2.13.13 Tellurium Standard Solution (1 mL = 0.10-mg determined using the analytical curves prepared in A2.14.3.5.
Te)—Dissolve 50-mg tellurium (Te; purity: 99.9 %, min) in A2.16.2 Systems with direct reading capability will provide
10-mL HNO3. Heat gently to dissolve the tellurium and expel results in the calibration concentration units.
the brown fumes. Cool, transfer to a 500-mL volumetric flask.
Add 50-mL HNO3, dilute to volume and mix. A2.17 Precision and Bias
A2.13.14 Tin Standard Solution (1 mL = 0.10-mg Sn)— A2.17.1 Precision—It is not possible to specify the preci-
Dissolve 50-mg tin (Sn; purity: 99.9 %, min) in 75 mL of 33 % sion of this test method but it is dependent upon the care given
by volume HCl. Heat gently to dissolve the tin. Cool, transfer to sample preparation of the calibration solutions as well as the
to a 500-mL volumetric flask, dilute to volume and mix. purity of the reagents.
A2.17.2 Bias—No information can be presented on the bias
A2.14 Calibration of this test method but it is dependent on the care given to the
A2.14.1 Calibration Solutions—Using micropipets, transfer preparation of the calibration solutions as well as the purity of
to individual 100-mL volumetric flasks the volume of each the reagents.
standard solution as indicated in Table A2.1 and Table A2.2:
A2.14.1.1 Add 20 mL of the copper standard solution to TEST METHOD B—SULFUR BY COMBUSTION AND
each flask in both tables, dilute to volume and mix. Known INFRARED DETECTOR
impurities in the copper standard solution must be considered
when determining final specific element ppm concentration in A2.18 Scope
both tables. A2.18.1 This test method covers the determination of sulfur
A2.14.2 Instrument Parameters: in electrolytic cathode copper.

8
 B 115 – 00 (2004)
A2.19 Summary of Test Method B A2.24 Preparation of Apparatus
A2.19.1 The sulfur is converted to sulfur dioxide (SO2) by A2.24.1 Assemble the apparatus and test the apparatus as
combustion in a stream of oxygen and the SO2 is measured by recommended by the manufacturer.
infrared absorption. A2.25 Sample Preparation
A2.19.2 This test method is written for use with commercial
A2.25.1 The sample should be uniform in size but not finer
analyzers equipped to carry out the operations automatically.
than 40 mesh.
A2.20 Interferences A2.26 Calibration
A2.20.1 The elements ordinarily present do not interfere. A2.26.1 Calibration Reference Materials—Select a mini-
mum of two reference materials with sulfur content near the
A2.21 Apparatus mid-point and high limit.
A2.26.2 Instrument Calibration—Calibrate according to the
A2.21.1 Combustion and Analyzing Instrumentation, ca- manufacturer’s instructions.
pable of making the required measurements.
A2.27 Procedure
A2.22 Reagents and Material A2.27.1 Stabilize the furnace and analyzer according to the
A2.22.1 Reagents: manufacturer’s instruction.
A2.27.2 Transfer the weight of sample recommended by the
A2.22.1.1 Accelerator—Use the accelerator recommended
manufacturer into a crucible and the add same amount of
by the instrument manufacturer which, for copper, should be
accelerator used in the calibration. Proceed as directed by the
sulfur and tin free.
manufacturer’s instructions.
A2.22.1.2 Oxygen, ultra high purity (purity: 99.95 % min):
Other grades of oxygen may be used if sulfur free, or the A2.28 Calculations
oxygen may be purified as described in Practice E 50. A2.28.1 Since most commercially available instruments
A2.22.2 Materials: calculate percent concentrations directly, including corrections
A2.22.2.1 Crucibles—Use crucibles recommended by the for blank and sample weight, calculations by the analyst are not
manufacturer, or equivalent. required.
A2.22.2.2 Crucible Tongs, capable of handling recom- A2.29 Precision and Bias
mended crucibles.
A2.29.1 Precision—It is not possible to specify the preci-
sion of this test method but it is dependent upon the care given
A2.23 Hazards
to sample preparation and the preciseness of calibration.
A2.23.1 For precautions to be observed in the use of certain A2.29.2 Bias—No information can be presented on the bias
reagents in this test method refer to Practice E 50. of this test method but it is dependent on the care given to the
A2.23.2 Use care when handling hot crucibles and operat- preparation and analysis of the sulfur standards as well as their
ing the furnace to avoid burns and electrical shock. homogeneity.

SUMMARY OF CHANGES

This section identifies the location of selected changes to this specification that have been incorporated since
the 1995 issue as follows:

(1) Changed title of specification. Tests and Retests, Rejection and Hearing, Packaging and
(2) Updated the following sections: Scope, Referenced Package Marking, Keywords, Annex A1, Annex A2, and
Documents, Terminology, Ordering Information, Number of Summary of Changes.

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