ASTM E1915-20

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1915 − 20
Standard Test Methods for
Analysis of Metal Bearing Ores and Related Materials for
Carbon, Sulfur, and Acid-Base Characteristics
This standard is issued under the fixed designation E1915; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.4 The values stated in SI units are to be regarded as
standard.
1.1 These test methods cover the determination of total
1.5 This standard does not purport to address all of the
carbon, sulfur, and acid-base characteristics in metal bearing
safety concerns, if any, associated with its use. It is the
ores and related materials such as leach residues, tailings, and
responsibility of the user of this standard to establish appro-
waste rock within the following ranges:
priate safety, health, and environmental practices and deter-
Analyte Application Range, % Quantitative Range, %
mine the applicability of regulatory limitations prior to use.
TotalCarbon 0to10 0.08to10
Total Sulfur 0 to 8.8 0.023 to 8.8
Specific warning statements are given in Section 6.
1.6 This international standard was developed in accor-
NOTE 1—The test methods were tested over the following ranges:
dance with internationally recognized principles on standard-
Total Carbon 0.01 % to 5.87 %
Total Sulfur 0.0002 % to 4.70 % ization established in the Decision on Principles for the
Residual Carbon from Pyrolysis 0.002 % to 4.97 %
Development of International Standards, Guides and Recom-
Residual Sulfur from Pyrolysis 0.014 % to 1.54 %
mendations issued by the World Trade Organization Technical
Pyrolysis Loss Sulfur 0 % to 4.42 %
Hydrochloric Acid Insoluble Carbon 0.025 % to 0.47 % Barriers to Trade (TBT) Committee.
Hydrochloric Acid Loss Carbon 0 % to 5.78 %
Hydrochloric Acid Insoluble Sulfur 0.012 % to 4.20 %
2. Referenced Documents
Acid Neutralization Potential Acidity Titration -1.0 % to 100 %
Acid Neutralization Potential Acidity Titration Low Range -1.0 % to 2 % CaCO
2.1 ASTM Standards:
Nitric Acid Insoluble Sulfur 0.006 % to 0.924 %
D1067 Test Methods for Acidity or Alkalinity of Water
Nitric Acid Loss Sulfur -0.08 % to 4.19 %
Sodium Carbonate Insoluble Sulfur 0.007 % to 3.78 %
D1193 Specification for Reagent Water
D1976 Test Method for Elements in Water by Inductively-
1.2 The quantitative ranges for the partial decomposition
Coupled Plasma Atomic Emission Spectroscopy
test methods are dependent on the mineralogy of the samples
D5673 Test Method for Elements in Water by Inductively
being tested. The user of these test methods is advised to
Coupled Plasma—Mass Spectrometry
conduct an interlaboratory study in accordance with Practice
D5744 Test Method for Laboratory Weathering of Solid
E1601 on the test methods selected for use at a particular
Materials Using a Humidity Cell
mining site, in order to establish the quantitative ranges for
D6234 Test Method for Shake Extraction of Mining Waste
these test methods on a site-specific basis.
by the Synthetic Precipitation Leaching Procedure
1.3 The test methods appear in the following order:
E29 Practice for Using Significant Digits in Test Data to
Sections
Determine Conformance with Specifications
Carbon and Sulfur, Total 10.1 – 10.9
E50 Practices for Apparatus, Reagents, and Safety Consid-
Carbon and Sulfur, Residual from Pyrolysis 10.10 – 10.18
erations for Chemical Analysis of Metals, Ores, and
Carbon and Sulfur, Hydrochloric Acid Insoluble 10.19 – 10.27
Acid Neutralization Potential Acidity Titration 10.28 – 10.36
Related Materials
Acid Neutralization Potential Acidity Titration Low Range 10.37 – 10.46
E135 Terminology Relating to Analytical Chemistry for
Sulfur, Nitric Acid Insoluble 10.47 – 10.55
Sulfur, Sodium Carbonate Insoluble 10.56 – 10.64 Metals, Ores, and Related Materials
E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
E1019 Test Methods for Determination of Carbon, Sulfur,
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2020. Published August 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1997. Last previous edition approved in 2013 as E1915 – 13. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1915-20. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1915 − 20
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt most decomposition occurs above 550 °C; (3) dolomite decom-
Alloys by Various Combustion and Inert Gas Fusion poses at 800 °C to 900 °C (Hammack, 1994, p. 440).
Techniques
4.2 These test methods also may be used for the classifica-
E1601 Practice for Conducting an Interlaboratory Study to
tion of rock to be used in construction, where the potential to
Evaluate the Performance of an Analytical Method
generate acid under environmental conditions exists.
E1950 Practice for Reporting Results from Methods of
4.3 It is assumed that the users of these test methods will be
Chemical Analysis
trained analysts capable of performing common laboratory
E2242 Test Method for Column Percolation Extraction of
procedures skillfully and safely. It is expected that work will be
Mine Rock by the Meteoric Water Mobility Procedure
performed in a properly equipped laboratory and that proper
waste disposal procedures will be followed. Appropriate qual-
3. Terminology
ity control practices such as those described in Guide E882
3.1 Definitions—For definitions of terms used in these test
must be followed.
methods, refer to Terminology E135.
5. Reagents and Materials
3.2 Definitions of Terms Specific to This Standard:
3.2.1 accuracy, n—qualitative term that involves precision
5.1 Purity of Reagents—Reagent grade chemicals shall be
and bias. The closeness of agreement between a measured
used in all tests. Unless otherwise indicated, it is intended that
quantity value and a true quantity value of a measurand.
all reagents conform to the specifications of the Committee on
3.2.2 standardization, v—analysis of samples with known Analytical Reagents of the American Chemical Society where
values or known additions, prior to and within groups of test such specifications are available. Other grades may be used,
samples to assure accuracy. provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
3.2.3 standardization sample, n—calibration mixtures or
the determination.
samples with known values or known additions that are
analyzed with test samples to assure accuracy of analysis.
5.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined
4. Significance and Use in Type I of Specification D1193.
4.1 These test methods are primarily intended to test mate-
6. Hazards
rials for compliance with compositional specifications and for
monitoring. 6.1 For hazards to be observed in the use of reagents and
apparatus in these test methods, refer to Practices E50. Use
4.1.1 The determination of carbon and sulfur and acid
neutralization potential in ores and related materials is neces- care when handling hot crucibles or boats and when operating
furnaces to avoid personal injury by either burn or electrical
sary to classify ores for metallurgical processing and to classify
waste materials from the mining and processing of ores such as shock.
leach residues, waste rock, and tailings according to their
7. Rounding Calculated Values
potential to generate acid in the environment. This information
is useful during mine development to assist in mining and
7.1 Rounding of test results obtained using this Test Method
mineral processing operations and for proper disposal of waste
shall be performed as directed in Practice E29 Rounding
materials.
Method, unless an alternative rounding method is specified by
4.1.1.1 The use of the acid neutralization potential titration
the customer or applicable material specification.
low range method is most useful where acidity is present in the
samples and when acid potential by titration is desired in the
8. Interlaboratory Studies
uncertain range below 2 % CaCO .
8.1 These test methods have been evaluated in accordance
4.1.2 These test methods are also used to isolate minerals
with Practice E1601 unless otherwise noted in the precision
based on carbon and sulfur contents of metal-bearing ores and
and bias section. The lower limit in the scope of these test
related materials so that acid-base accounting can be performed
methods specifies the lowest analyte content that may be
(that is, carbonate mineral acid neutralization potential (ANP)
analyzed with an acceptable error. A warning statement is
minus sulfide-sulfur mineral acid generation potential (AGP) =
included in the scope for test methods not observing this
net calcium carbonate (NCC)).
convention.
4.1.3 Additionally, the carbon hydrochloric acid insoluble
test method has utility to identify the amount of organic carbon
contained in gold ores so that potential for preg-robbing can be
Hammack, R. W., “Evolved-Gas Analysis: A Method for Determining Pyrite,
identified and rectified through established pretreatment meth-
Marcasite, and Alkaline-Earth Carbonates,” Environmental Geochemistry of Sulfide
ods prior to cyanidation. Warning—Pyrolysis pretreatment at
Oxidation, Alpers, C., and Blowes, D., eds., Chapter 28, ACS Symposium Series
550 °C has a potential to thermally decompose some carbonate
550, American Chemical Society, Washington, D.C., 1994, pp. 431–444.
Reagent Chemicals, American Chemical Society Specifications, American
minerals: (1) transition metal carbonates (for example, siderite,
Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the
FeCO , and rhodochrosite, MnCO ) decompose, yielding car-
3 3
testing of reagents not listed by the American Chemical Society, see the United
bon dioxide (CO ) in the range of 220 °C to 520 °C; (2) calcite
2 States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,
decomposes slightly between 300 °C and 500 °C, although Inc. (USPC), Rockville, MD, http://www.usp.org.
E1915 − 20
8.2 Site-Specific Quantitative Ranges—An interlaboratory 10.4.1.1 Barium Sulfate (BaSO ), Anhydrous, contains
study may be conducted in accordance with Practice E1601 to 13.74 % sulfur (purity 99.9 % minimum). Dry 100 g at 120 °C
establish quantitative ranges for the partial decomposition test for 2 h and store in a 250-mL glass bottle.
methods selected for a particular site. Test samples shall be 10.4.1.2 Blank Reference Sample—Prepare a blank refer-
selected for each alteration or lithologic unit, or both, contain-
ence sample by pulverizing or grinding 100 g of SiO (see
ing high and low contents of carbon and sulfur minerals. Each 10.4.1.6), to pass through a 150-µm (No. 100) sieve, mix, and
test sample must be analyzed in rapid succession for total
store in a 250-mL glass bottle. This blank contains 0.00 %
carbon and sulfur followed by the different partial decompo- carbon and 0.00 % sulfur.
sition treatments selected in order to minimize the between-
10.4.1.3 Calcium Carbonate (CaCO ), Anhydrous, contains
method variation. 12.00 % carbon (purity 99.9 % minimum). Dry 100 g for 2 h at
120 °C and store in a 250-mL glass bottle.
9. Sampling and Sample Preparation
10.4.1.4 Calibration Mixture A—(1 g = 20 mg C and
9.1 Materials Safety—Samples must be prepared, stored, 20 mg S)—Combine 16.67 g CaCO , 14.56 g BaSO , and
3 4
and disposed of in accordance with the materials and safety 68.77 g SiO in a ring and puck grinding mill or equivalent
guidelines in Practices E50. device. Grind until 100 % passes through a 150-µm (No. 100)
sieve, pass the mixture through the screen to break up any
9.2 Prepared Sample—Dry a representative portion of the
lumps, mix, and store in a glass bottle. This mixture contains
gross sample at 80 °C to constant mass in order to minimize
2.00 % carbon and 2.00 % sulfur. Alternatively, grind the
sulfide mineral oxidation. Pulverize or grind the laboratory
reagents separately, mix, and pass through the screen prior to
sample until 100 % passes a 150-µm (No. 100) sieve.
final mixing.
NOTE 2—Results from the interlaboratory study suggest that it may be
10.4.1.5 Calibration Mixtures—Transfer 4.00 g, 10.00 g,
necessary to grind samples to pass a 75-µm (No. 200) sieve in order to
20.00 g, and 30.00 g of Calibration Mixture A to ring and puck
improve precision for samples containing low contents of carbon or sulfur.
grinding mills or equivalent devices. Add the amount of dried
9.3 Diluted Sample—If the content of sulfur in the test
SiO needed to bring the total mass to 40.0 g in each mill, grind
material exceeds 1.75 % for the minimum range instrument,
to 100 % passing a 150-µm (No. 100) sieve, pass the mixture
prepare a diluted sample as in 9.3.1.
through the screen, mix, and store in 250-mL glass bottles.
9.3.1 Weigh 10.0 g 6 0.1 g prepared sample and combine
These mixtures contain: 0.2 %, 0.5 %, 1.0 %, and 1.5 % for
with 40.0 g 6 0.1 g dry silica (SiO ). Grind the mixture in a
both carbon and sulfur. Alternatively, grind the reagents
ring and puck mill, or equivalent, until 100 % will pass through
separately, mix, and pass through the screen prior to final
a 150-µm (No. 100) sieve; mix, and store in a 250-mL glass
mixing. Commercially-produced calibration mixtures, which
bottle.
meet these specifications, may also be used.
10.4.1.6 Silica (SiO ) (purity 99.9 % minimum), Ottawa
NOTE 3—Dry alumina (Al O ) can be used provided proper verification
2 3
of analysis is used.
sand, washed and ignited, containing less than 0.01 % carbon
and 0.01 % sulfur. Dry at 120 °C for 2 h and store in a 250-mL
10. Procedures
glass bottle.
10.4.1.7 Tungstic Acid (H WO ) (purity 99 % minimum).
TOTAL CARBON AND SULFUR 2 4
10.4.1.8 Vanadium Pentoxide (V O ) (purity 99 % mini-
2 5
10.1 Scope—This test method covers the determination of
mum).
total carbon in the content range between 0.1 % and 10 % and
10.4.2 Materials:
total sulfur contents in the range between 0.1 % and 8.8 %.
10.4.2.1 Crucibles or boats, suitable for combustion analy-
10.2 Summary of Test Method:
ses.
10.2.1 The carbon in the test sample is converted to carbon
10.5 Calibration and Standardization:
dioxide (CO ) and the sulfur to sulfur dioxide (SO)by
2 2
10.5.1 Apparatus—Operate and calibrate the instrument in
combustion in a stream of oxygen.
accordance with the manufacturer’s instructions. Resistance
10.2.2 The amount of carbon dioxide (CO ) and sulfur
furnace instruments require the use of V O or H WO for the
2 5 2 4
dioxide (SO ) are measured by infrared absorption.
determination of sulfur in this test method. Use a 0.200 g 6
10.3 Apparatus:
0.01 g mass for all calibration mixtures, reference materials,
10.3.1 Combustion-InfraredAnalyzer, equipped with a com-
blank reference materials, test samples, and diluted test
bustion chamber, oxygen carrier stream, and infrared absorp-
samples in this test method.
tion detector, suitable for analysis of sulfur in a minimum range
10.5.1.1 Certain instruments may require different sample
instrument from 0.1 % to 1.75 % or in a maximum range
masses for certain content ranges, which is permissible as long
instrument from 0.1 % to 8.8 % and carbon in the range of
as the precision and bias requirements of these test methods are
0.1 % to 10 %, using 0.2-g test portions of ores and related
fulfilled.
materials. Instruments, such as those presented in Test Methods
10.5.2 Heat/bake the crucibles or boats for test samples and
E1019 that can be shown to give equivalent results may also be
standard samples in a muffle furnace for 1 h at 550 °C 6 10 °C.
used for these test methods.
10.5.3 Laboratory Test Method Performance
10.4 Reagents and Materials: Demonstration—A demonstration of laboratory test method
10.4.1 Reagents: performance must be performed before this test method may be
E1915 − 20
TABLE 1 Calibration Mixture 95 % Confidence Limits from
analysis of test samples and discard the results since the last
Interlaboratory Testing
acceptable quality control sample result had been obtained.
Mixture Min, % Max., % Min, % Sulfur Max., %
10.5.4.3 Reference Sample—Analyze a reference sample,
Carbon Carbon Sulfur
certified for total carbon and total sulfur before analysis of test
0.0 -0.02 0.04 -0.01 0.01
samples for total carbon and sulfur and within each group of
0.2 0.16 0.25 0.12 0.26
0.5 0.44 0.55 0.42 0.55
fifty test samples. If the difference of the reference sample and
1.0 0.92 1.08 0.85 1.14
the reference value for the reference sample exceeds the limits
1.5 1.42 1.59 1.34 1.62
2.0 1.87 2.13 1.78 2.16 shown in Table 1 for materials of comparable content, correct
BaSO . . 12.4 14.5
any instrumental problems and repeat the analysis of the
CaCO 10.9 12.8 . . . . . .
reference material and discard the results since the last accept-
able quality control sample result had been obtained.
10.5.4.4 Control Sample—Analyze the 0.2 % calibration
mixture prior to and within each group of fifty test samples. If
the result for the control sample exceeds the limits shown in
used in a laboratory for the first time. This demonstration is
Table 1 for the 0.2 % calibration mixture, correct any instru-
particularly important if the laboratory needs to modify the test
mental problems and repeat the analysis of the control sample
method in any way. The demonstration must be repeated
before proceeding with analysis of test samples and discard the
whenever the test method is significantly modified.
results since the last acceptable quality control sample result
10.5.3.1 Linearity Verification—Measure total carbon and
had been obtained.
sulfur for the blank reference sample, calibration mixtures,
10.5.4.5 Spike Addition Sample—Analyze a spike addition
BaSO , and CaCO in increasing order using the same mass of
4 3
sample prior to analysis of each group of fifty test samples by
calibration mixtures selected for test samples, in accordance
preparing a duplicate of the first test sample in the group and
with the manufacturer’s instructions. Record the calibration
adding an equal mass of the 0.5 % calibration mixture just prior
mixture masses used and the carbon and sulfur results from the
to determination of carbon and sulfur. Calculate the reference
instrument. Check for linearity by linear regression or by a
values for the spike addition sample by adding 0.5 % to the
graphical method to meet a deviation less than 10 % relative
carbon and sulfur results for the test sample performed without
for each of the calibration material results at or above a content
the spike addition and divide the sum by two. If the difference
of 0.2 % carbon and 0.2 % sulfur and a correlation coefficient
of any result for the spike addition sample and the reference
of at least 0.99. Correct any problems with the instrument
value exceeds the limits shown in Table 1 for materials of
before proceeding with the analysis of test samples.
comparable content, correct any instrumental problems and
NOTE 4—Linearity may also be verified by the use of BaSO and
repeat the spike addition sample analysis before proceeding
CaCO masses equivalent to the content of the calibration mixtures.
with analysis of test samples, and discard the results since the
10.5.3.2 Blank Sample Precision Verification—Analyze ten
last acceptable quality control sample result had been obtained.
replicates of the blank reference sample. If the standard
10.6 Interferences—The elements normally present in ores
deviation of the replicate analyses exceeds 0.02 % for carbon
and related materials do not interfere with this test method.
or 0.01 % for sulfur, correct any instrumental problems and
10.7 Procedure:
repeat the blank sample precision verification before proceed-
10.7.1 Ignite the crucibles or boats for test samples and
ing with test method implementation.
standardization samples in a muffle furnace for 1 h at 550 °C 6
10.5.3.3 Low Calibration Mixture Precision Verification—
10 °C. See 10.5.2.
Analyze four replicates of the 0.2 % calibration mixture. If any
10.7.2 Test Samples—Transfer test samples, diluted test
result for the 0.2 % calibration mixture exceeds the limits
samples and standardization samples using 0.200 g 6 0.01 g
shown in Table 1, correct any instrumental problems and repeat
the low calibration mixture precision verification before pro- into the crucible or boat used for instrumental analysis and
record the mass. Use of a different sample mass may be
ceeding with test method implementation.
10.5.4 Method Quality Control: required on some instruments for some samples (see 10.5.1.1).
10.7.3 Duplicate Test Sample—Analyze a duplicate test
10.5.4.1 Calibration Verification—Analyze a calibration
mixture with a content greater than or equal to 0.5 % carbon sample within each group of fifty test samples. If the difference
of the duplicate results exceeds the limits shown in Table 1 for
and 0.5 % sulfur prior to and within each group of fifty test
samples. If the calibration mixture result exceeds the limits in a material of comparable content, discard the results since the
last acceptable quality control sample result had been obtained,
Table 1, correct any instrumental problems and repeat the
linearity verification before proceeding with analysis of test correct any sample preparation or instrumental problems, and
repeat the analyses from 10.7.2.
samples and discard the results since the last acceptable quality
control sample result had been obtained. 10.7.4 Analysis:
10.5.4.2 Blank Reference Sample—Analyze a blank refer- 10.7.4.1 Analyze quality control samples before each batch
ence sample before analysis of test samples and within each of test samples and within each group of ten test samples as
group of fifty test samples. If the result for the blank reference directed in 10.5.4. Measure the carbon and sulfur contents for
sample exceeds the limits in Table 1 for the 0.0 % calibration quality control samples, test samples, and diluted test samples
mixture, correct any instrumental problems and repeat the in percent in accordance with the instrument manufacturer’s
analysis of the blank reference sample before proceeding with instructions, and record the measurements.
E1915 − 20
TABLE 2 Statistical Information—Total Carbon TABLE 3 Statistical Information—Total Sulfur
Min, SD Reproducibility Min, SD Reproducibility
Number of Carbon
Test Material (S , Practice Index (R, Prac- R ,% Number of Sulfur (S , Index (R,
M rel M
Laboratories Found, % Test Material R ,%
rel
E1601) tice E1601) Laboratories Found, % Practice Practice
E1601) E1601)
Blank 7 0.012 0.004 0.034 300
Ottawa Sand 10 0.021 0.011 0.0477 230 Blank 7 0.0002 0.002 0.010 5000
(D) Ottawa Sand 11 0.004 0.003 0.0133 312
Inert Diorite (K) 7 0.050 0.005 0.037 74 (D)
Inert Andesite 7 0.090 0.004 0.054 59 Diorite Gneiss 11 0.014 0.007 0.039 283
(J) (F)
Calibration 7 0.095 0.004 0.024 25
Autoclave 10 0.086 0.016 0.115 133
Feed Ore Mixture 0.1
(A) Inert Andesite 7 0.176 0.005 0.095 54
Calibration 7 0.117 0.007 0.049 42 (J)
Mixture 0.1 Inert Diorite (K) 7 0.190 0.004 0.081 43
Duluth Waste 10 0.142 0.017 0.112 79 Pit Rock (G) 11 0.285 0.014 0.068 24
Rock (B) Spiked Andes- 6 0.336 0.005 0.055 16
Spiked Andes- 6 0.292 0.008 0.051 17 ite
ite Vinini Waste 11 0.761 0.019 0.269 35
Reclamation 10 0.462 0.025 0.223 48 Rock (E)
Tailings (C) Refractory 11 1.50 0.052 0.326 22
Vinini Waste 10 0.771 0.024 0.180 23 Gold Ore (I)
Rock (E) Duluth Waste 11 1.57 0.024 0.186 12
Pit Rock (G) 10 0.800 0.025 0.117 15 Rock (B)
Diorite Gneiss 10 1.04 0.032 0.170 16 Zinc Plant Tail- 11 3.79 0.072 0.423 11
(F) ings (H)
Zinc Plant Tail- 10 5.87 0.055 0.494 8 Reclamation 11 4.04 0.053 0.462 11
ings (H) Tailings (C)
Refractory 10 5.70 0.038 0.478 8 Autoclave 11 4.70 0.067 0.648 14
Gold Ore (I) Feed Ore
(A)
TABLE 4 Bias Information—Total Carbon
10.7.4.2 Continue analysis until the batch of test samples is
Reference Difference
Test Material Source Description
completed, or until a quality control sample or duplicate test
Carbon, % Carbon, %
sample result deviates more than the limits shown in Table 1,
Diorite Gneiss 1.0±0.1 0.040 CANMET SY-4 Diorite gneiss
(F) Provisional
for a material of comparable content. If the difference of the
results exceeds the limits shown in Table 1 for a material of
comparable content, discard the results since the last accept-
TABLE 5 Bias Information—Total Sulfur
able quality control sample result had been obtained, correct
Reference Sulfur, Difference
any sample preparation or instrumental problems and repeat Test Material Source Description
% Sulfur, %
the analyses from 10.7.4.2.
Diorite Gneiss 0.015 ± 0.004 –0.001 CANMET SY-4 Diorite
(F) Provisional gneiss
10.8 Calculation:
Pit Rock (G) 0.298 ± 0.015 –0.013 CANMET NBM-1 pit rock
10.8.1 Calculate the total carbon and sulfur contents for the
Recommended
Refractory Gold 1.466 ± 0.044 0.034 NIST NIST-886
test samples in accordance with the manufacturer’s instruc-
Ore (I) Certified refractory gold
tions.
ore
10.8.2 Round the results above 0.1 % to the nearest 0.01 %
and record as total carbon or sulfur. Enclose results from
0.03 % to 0.1 % in parentheses and below 0.03 % in parenthe-
reference materials to verify that this test method is performing
ses followed by an asterisk in accordance with Practice E1950.
10.8.3 Over-Range Results—If the sulfur result exceeds accurately in their laboratory.
CAUTION—The user of this test method is cautioned that
1.75 % for the minimum range instrument, discard the result
and repeat the procedure with the diluted sample. Multiply the the method may not be quantitative for reporting above a
reproducibility index (R) of 50 % relative, in accordance with
diluted test sample result by five and round to the nearest
0.1 %. Practice E1601. The user is advised to take this into account, in
addition to the mineralogy of the sample, when interpreting the
10.8.3.1 Alternatively, use a lower sample mass for the
analysis as specified in 10.5.1.1. results for this test method.
10.9 Precision and Bias:
RESIDUAL CARBON AND SULFUR FROM
10.9.1 Precision—Eleven laboratories cooperated in testing
PYROLYSIS
this test method, providing ten sets of data for carbon and
10.10 Scope—This test method covers the determination of
eleven sets of data for sulfur, and obtained the precision data
residual carbon from pyrolysis in the content range between
summarized in Tables 2 and 3.
0.1 % and 10 % and residual sulfur from pyrolysis contents in
10.9.2 Bias—The accuracy of this test method for carbon
the range between 0.1 % and 8.8 %.
and sulfur is deemed satisfactory based on the values in Tables
4 and 5. Users are encouraged to employ these or similar 10.11 Summary of Test Method:
E1915 − 20
10.11.1 The test sample is ignited in a muffle furnace prior linearity verification before proceeding with analysis of test
to instrumental analysis where the carbon in the test sample is samples and discard the results since the last acceptable quality
converted to carbon dioxide (CO ) and the sulfur to sulfur control sample result had been obtained.
dioxide (SO ) by combustion in a stream of oxygen.
10.14.4.2 Blank Reference Sample—Analyze a blank refer-
10.11.2 The amount of carbon dioxide (CO ) and sulfur ence sample before analysis of test samples and within each
dioxide (SO ) are measured by infrared absorption.
group of fifty test samples. If the result for the blank reference
sample exceeds the limits in Table 1 for the 0.0 % calibration
10.12 Apparatus:
mixture, correct any instrumental problems and repeat the
10.12.1 Combustion-Infrared Analyzer, equipped with a
analysis of the blank reference sample before proceeding with
combustion chamber, oxygen carrier stream and infrared ab-
analysis of test samples and discard the results since the last
sorption detector, suitable for analysis of sulfur in a minimum
acceptable quality control sample result had been obtained.
range instrument from 0.1 % to 1.75 % or in a maximum range
10.14.4.3 Reference Sample—Analyze a reference sample,
instrument from 0.1 % to 8.8 % and carbon in the range of
certified for total carbon and total sulfur before analysis of test
0.1 % to 10 %, using 0.2-g test portions of ores and related
samples for and within each group of fifty test samples and a
materials. Instruments, such as those shown in Test Methods
reference sample certified for pyrolysis residual carbon or
E1019 that can be shown to give equivalent results may also be
sulfur from pyrolysis, if available. If the difference of the
used for these test methods.
reference sample and the reference value for the reference
10.13 Reagents and Materials:
sample exceeds the limits shown in Table 1 for materials of
10.13.1 Reagents:
comparable content, correct any instrumental problems and
10.13.1.1 Barium Sulfate (see 10.4.1.1).
repeat the analysis of the reference material and discard the
10.13.1.2 Blank Reference Sample (see 10.4.1.2).
results since the last acceptable quality control sample result
10.13.1.3 Calcium Carbonate (see 10.4.1.3).
had been obtained.
10.13.1.4 Calibration Mixture A (see 10.4.1.4).
10.14.4.4 Control Sample—Analyze the 0.2 % calibration
10.13.1.5 Calibration Mixtures (see 10.4.1.5).
mixture prior to and within each group of fifty test samples. If
10.13.1.6 Silica (see 10.4.1.6).
the result for the control sample exceeds the limits shown in
10.13.1.7 Tungstic Acid (see 10.4.1.7).
Table 1 for the 0.2 % calibration mixture, correct any instru-
10.13.1.8 Vanadium Pentoxide (see 10.4.1.8).
mental problems and repeat the analysis of the control sample
10.13.2 Materials:
before proceeding with analysis of test samples and discard the
10.13.2.1 Cruciblesorboats, suitable for combustion analy- results since the last acceptable quality control sample result
ses. had been obtained.
10.14.4.5 Spike Addition Sample—Analyze a spike addition
10.14 Calibration and Standardization:
sample prior to analysis of each group of fifty test samples by
10.14.1 Apparatus: Operate and calibrate the instrument in
preparing a duplicate of the first test sample in the group and
accordance with the manufacturer’s instructions. Resistance
adding an equal mass of the 0.5 % calibration mixture just prior
furnace instruments require the use of vanadium pentoxide or
to determination of carbon and sulfur. Calculate the reference
H WO for the determination of sulfur in this test method. Use
2 4
values for the spike addition sample by adding 0.5 % to the
a 0.200 g 6 0.01 g mass for all calibration mixtures, reference
carbon and sulfur results for the test sample performed without
materials, blank reference materials, test samples, and diluted
the spike addition and divide the sum by two. If the difference
test samples in this test method.
of any result for the spike addition sample and the reference
10.14.1.1 Certain instruments may require different sample
value exceeds the limits shown in Table 1 for materials of
masses for certain content ranges, which is permissible as long
comparable content, correct any instrumental problems and
as the precision and bias requirements of these test methods are
repeat the spike addition sample analysis before proceeding
fulfilled.
with analysis of test samples, and discard the results since the
10.14.2 Ignite the crucibles or boats for test samples and
last acceptable quality control sample result had been obtained.
standard samples as described in 10.5.2.
Add the 0.5 % calibration mixture after the pyrolysis procedure
10.14.3 Laboratory Test Method Performance
but before the analysis step.
Demonstration—A demonstration of laboratory test method
performance must be performed before this test method may be 10.15 Interferences—The elements normally present in ores
used in a laboratory for the first time. This demonstration is and related materials do not interfere with this test method. Use
particularly important if the laboratory needs to modify the test of adequate draft in the muffle furnace is necessary to avoid
method in any way. The demonstration must be repeated excessive adsorption of sulfur gasses on the solid phase of the
whenever the test method is significantly modified. Conduct test samples, leading to low sulfur loss by pyrolysis.
the performance demonstration as described in 10.5.3.
CAUTION—SO (g) can be adsorbed by carbonate minerals
10.14.4 Method Quality Control:
within a sample and from other samples in a batch, resulting in
10.14.4.1 Calibration Verification—Analyze a calibration low pyrolysis loss estimates for sulfide. Pyrolysis pretreatment
mixture with a content greater than or equal to 0.5 % carbon at 550 °C has a potential to thermally decompose some
and 0.5 % sulfur prior to and within each group of fifty test carbonate minerals:
samples. If the calibration mixture result exceeds the limits in (1) Transition metal carbonates (for example, FeCO and
Table 1, correct any instrumental problems and repeat the MnCO ) decompose, yielding CO , in the range of 220 °C to
3 2
E1915 − 20
TABLE 6 Residual Carbon From Pyrolysis
520 °C;
(2) calcite decomposes slightly between 300 °C and 500 °C, Min, SD Reproducibility
Number of Carbon
Test Material (S , Practice Index (R, Prac- R ,%
M rel
although most decomposition occurs above 550 °C;
Laboratories Found, %
E1601) tice E1601)
(3) dolomite decomposes at 800 °C to 900 °C.
Ottawa Sand 7 0.002 0.014 0.053 2449
(D)
10.16 Procedure:
Inert Diorite (K) 7 0.011 0.006 0.061 530
10.16.1 Heat/bake the crucibles or boats for test samples
Autoclave 7 0.024 0.009 0.051 210
Feed Ore
and standardization samples in a muffle furnace for 1 h at
(A)
550 °C 6 10 °C (see 10.5.2).
Inert Andesite 7 0.030 0.009 0.061 204
10.16.2 Test Samples—Transfer test samples, diluted test
(J)
Duluth Waste 7 0.107 0.009 0.071 66
samples, and standardization samples using 0.200 g 6 0.01 g
Rock (B)
into the crucible or boat used for instrumental analysis and
Vinini Waste 7 0.131 0.009 0.087 67
record the mass. Use of a different sample mass may be
Rock (E)
Reclamation 7 0.216 0.011 0.101 47
required on some instruments for some samples (see
Tailings (C)
10.14.1.1).
Pit Rock (G) 7 0.359 0.010 0.261 73
10.16.3 Pre-bake—Heat the crucibles or boats containing Diorite Gneiss 7 0.931 0.015 0.125 13
(F)
the test samples, blank, reference samples for pyrolysis re-
Refractory 7 4.84 0.076 0.752 16
sidual carbon and sulfur from pyrolysis and spike addition
Gold Ore (I)
Zinc Plant Tail- 7 4.97 0.047 1.82 37
samples in a muffle furnace for 1 h at 550 °C 6 10 °C. Add the
ings (H)
calibration mixture portion for the spike addition sample after
pyrolysis and cooling, then mix.
10.16.4 Duplicate Test Sample—Analyze a duplicate test
sample within each group of fifty test samples. If the difference
below the lower scope limits enclosed in parentheses and
of the duplicate results exceeds the limits shown in Table 1 for
below the null limit followed by an asterisk in accordance with
a material of comparable content, discard the results since the
Practice E1950.
last acceptable quality control sample result had been obtained,
10.17.4 Over-Range Results—If the sulfur result exceeds
correct any sample preparation or instrumental problems and
1.75 % for the minimum range instrument, discard the result
repeat the analyses from 10.16.2.
and repeat the procedure from with the diluted sample.
10.16.5 Analysis:
Multiply the diluted test sample result by five and round to the
10.16.5.1 Analyze quality control samples before each
nearest 0.1 %.
batch of test samples and within each group of ten test samples
10.17.4.1 Alternatively, use a lower sample mass for the
as directed in 10.14.4. Measure the carbon and sulfur contents
analysis as specified in 10.14.1.1.
for quality control samples, test samples and diluted test
10.18 Precision and Bias:
samples in percent in accordance with the instrument manu-
10.18.1 Precision—Nine laboratories cooperated in testing
facturer’s instructions and record the measurements.
this test method, providing seven sets of data for carbon and
10.16.5.2 Continue analysis until the batch of test samples is
nine sets of data for sulfur, and obtained the precision data
completed, or until a quality control sample or duplicate test
summarized in Tables 6-8.
sample result deviates more than the limits shown in Table 1
10.18.2 Bias—No information on the bias of this test
for a material of comparable content. If the difference of the
method is known because at the time of the interlaboratory
results exceeds the limits shown in Table 1 for a material of
study, suitable reference materials were not available. The user
comparable content, discard the results since the last accept-
of this test method is encouraged to employ accepted reference
able quality control sample result had been obtained, correct
materials, if available, to determine the presence or absence of
any sample preparation or instrumental problems, and repeat
bias.
the analyses from 10.16.2.
CAUTION—The user of this test method is cautioned that
10.17 Calculation:
the method may not be quantitative for reporting above a
10.17.1 Calculate the residual carbon and sulfur from py-
reproducibility index (R) of 50 % relative, in accordance with
rolysis contents for the test samples in accordance with the Practice E1601. The user is advised to take this into account, in
manufacturer’s instructions.
addition to the mineralogy of the sample, when interpreting the
results for this test method.
10.17.2 Calculate the pyrolysis loss sulfur, % A, as follows:
A 5 B 2 C (1)
HYDROCHLORIC ACID INSOLUBLE CARBON AND
SULFUR
where:
B = total sulfur result, %, and
10.19 Scope—This test method covers the determination of
C = residual sulfur from pyrolysis result, %.
HCl insoluble carbon in the content range of 0.1 % to 10 % and
HCl insoluble sulfur contents in the range of 0.1 % to 8.8 %.
10.17.3 Round the results to the nearest 0.01 % and record
as residual carbon from pyrolysis, residual sulfur from 10.20 Summary of Test Method:
pyrolysis, or pyrolysis loss sulfur, at or above the lower scope 10.20.1 The test sample is partially decomposed with HCl
limit established during interlaboratory testing. Report results prior to instrumental analysis, where the carbon in the test
E1915 − 20
TABLE 7 Residual Sulfur From Pyrolysis
10.22.1 Reagents:
Min, SD Reproducibility
10.22.1.1 Barium Sulfate (see 10.4.1.1).
Number of Sulfur
Test Material (S , Practice Index (R, Prac- R ,%
M rel
Laboratories Found, % 10.22.1.2 Blank Reference Sample (see 10.4.1.2).
E1601) tice E1601)
10.22.1.3 Calcium Carbonate (see 10.4.1.3).
Ottawa Sand 9 0.014 0.009 0.029 204
(D) 10.22.1.4 Calibration Mixture A (see 10.4.1.4).
Diorite Gneiss 9 0.107 0.038 0.164 153
10.22.1.5 Calibration Mixtures (see 10.4.1.5).
(F)
Inert Andesite 8 0.196 0.019 0.176 90 10.22.1.6 Silica (see 10.4.1.6).
(J)
10.22.1.7 Tungstic Acid (see 10.4.1.7).
Pit Rock (G) 9 0.229 0.037 0.187 82
10.22.1.8 Vanadium Pentoxide (see 10.4.1.8).
Inert Diorite (K) 9 0.244 0.016 0.187 77
Autoclave 9 0.288 0.022 0.323 112
10.22.2 Materials:
Feed Ore
10.22.2.1 Cruciblesorboats, suitable for combustion analy-
(A)
Vinini Waste 9 0.425 0.015 0.162 38
ses.
Rock (E)
10.22.2.2 Glass Filters—Fine-porosity glass micro filters,
Refractory 9 0.710 0.032 0.244 34
carbon content must be less than 0.15 %, sulfur content must
Gold Ore (I)
Duluth Waste 9 0.714 0.056 0.275 38
be less than 0.05 % and the filter mass must be less than 0.2 g.
Rock (B)
Zinc Plant Tail- 9 1.24 0.042 1.45 117
10.23 Calibration and Standardization:
ings (H)
10.23.1 Apparatus—Operate and calibrate the instrument in
Reclamation 9 1.54 0.025 0.435 28
accordance with the manufacturer’s instructions. Resistance
Tailings (C)
furnace instruments require the use of V O or H WO for the
2 5 2 4
determination of sulfur in this test method. Use a 0.200 g 6
TABLE 8 Pyrolysis Loss Sulfur
0.01 g mass for all calibration mixtures, reference materials,
Min, SD Reproducibility blank reference materials, test samples and diluted test samples
Number of Sulfur
Test Material (S , Practice Index (R, Prac- R ,%
M rel
Laboratories Loss, % in this test method.
E1601) tice E1601)
10.23.1.1 Certain instruments may require different sample
Diorite Gneiss 9 - 0.106 0.038 0.197 -186
masses for certain content ranges, which is permissible as long
(F)
Inert Diorite (K) 9 - 0.063 0.015 0.143 -224
as the precision and bias requirements of these test methods are
Inert Andesite 8 - 0.041 0.018 0.165 -406
fulfilled.
(J)
Ottawa Sand 9 - 0.017 0.009 0.070 -420 10.23.2 Ignite the crucibles or boats for test samples and
(D)
standardization samples as described in 10.5.2.
Pit Rock (G) 9 0.042 0.035 0.225 536
10.23.3 Laboratory Test Method Performance
Vinini Waste 9 0.322 0.024 0.248 77
Rock (E)
Demonstration—A demonstration of laboratory test method
Refractory 9 0.763 0.059 0.373 49
performance must be performed before this test method may be
Gold Ore (I)
used in a laboratory for the first time. This demonstration is
Duluth Waste 9 0.863 0.058 0.384 44
Rock (B)
particularly important if the laboratory needs to modify the test
Reclamation 9 2.50 0.062 0.599 24
method in any way. The demonstration must be repeated
Tailings (C)
whenever the test method is significantly modified. Conduct
Zinc Plant Tail- 9 2.53 0.082 1.21 48
ings (H)
the performance demonstration as described in 10.5.3.
Autoclave 9 4.42 0.076 0.696 16
10.23.4 Method Quality Control:
Feed Ore
(A)
10.23.4.1 Calibration Verification—Analyze a calibration
mixture with a content greater than or equal to 0.5 % carbon
and 0.5 % sulfur prior to and within each group of fifty test
samples. If the calibration mixture result exceeds the limits in
sample is converted to carbon dioxide (CO ) and the sulfur to
Table 1, correct any instrumental problems and repeat the
sulfur dioxide (SO ) by combustion in a stream of oxygen.
linearity verification before proceeding with analysis of test
10.20.2 The amount of carbon dioxide (CO ) and sulfur
samples and discard the results since the last acceptable quality
dioxide (SO ) are measured by infrared absorption.
control sample result had been obtained.
10.21 Apparatus:
10.23.4.2 Blank Reference Sample—Analyze a blank refer-
10.21.1 Combustion-Infrared Analyzer, equipped with a
ence sample before analysis of test samples and within each
combustion chamber, oxygen carrier stream, and infrared
group of fifty test samples. If the result for the blank reference
absorption detector, suitable for analysis of sulfur in a mini-
sample exceeds the limits in Table 1 for the 0.0 % calibration
mum range instrument from 0.1 % to 1.75 % or in a maximum
mixture, correct any instrumental problems and repeat the
range instrument from 0.1 % to 8.8 % and carbon in the range
analysis of the blank reference sample before proceeding with
of 0.1 % to 10 %, using 0.2-g test portions of ores and related
analysis of test samples and discard the results since the last
materials. Instruments, such as those shown in Test Methods
acceptable quality control sample result had been obtained.
E1019 that can be shown to give equivalent results may also be
10.23.4.3 Reference Sample—Analyze a reference sample,
used for these test methods.
certified for total carbon and total sulfur before analysis of test
10.22 Reagents and Materials: samples for total carbon and sulfur and within each group of
E1915 − 20
fifty test samples and a reference sample certified for hydro- of the duplicate results exceeds the limits shown in Table 1, for
chloric acid insoluble carbon or sulfur, if available. If the a material of comparable content, discard the results sin
...