ASTM E1915-99
(Test Method)Standard Test Method for Analysis of Metal Bearing Ores and Related Materials by Combustion Infrared Absorption Spectrometry
Standard Test Method for Analysis of Metal Bearing Ores and Related Materials by Combustion Infrared Absorption Spectrometry
SCOPE
1.1 This test method covers the determination of total carbon and sulfur in metal bearing ores and related materials such as tailings and waste rock within the following ranges:
AnalyteApplication Range, % Quantitative Range, %Total Carbon0 to 10 0.08 to 10Total Sulfur0 to 8.80.023 to 8.8
Note 1--The test methods were tested over the following ranges:
Total Carbon- 0.01 to 5.87 %
Total Sulfur- 0.0002 to 4.70 %
Residual Carbon from Pyrolysis- 0.002 to 4.97 %
Residual Sulfur from Pyrolysis- 0.014 to 1.54 %
Pyrolysis Loss Sulfur- 0 to 4.42 %
Hydrochloric Acid Insoluble Carbon- 0.025 to 0.47 %
Hydrochloric Acid Loss Carbon- 0 to 5.78 %
Hydrochloric Acid Insoluble Sulfur- 0.012 to 4.20 %.
1.2 The quantitative ranges for the partial decomposition test methods are dependent on the mineralogy of the samples being tested. The user of these test methods are advised to conduct an interlaboratory study in accordance with Practice E1601 on the test methods selected for use at a particular mining site, in order to establish the quantitative ranges for these test methods on a site-specific basis.
1.3 The test methods appear in the following order: SectionsCarbon and Sulfur, Hydrochloric Acid Insoluble12.13 - 12.18Carbon and Sulfur, Residual from Pyrolysis12.7 - 12.12Carbon and Sulfur, Total12.1 - 12.6
1.4 The values stated in SI units are to be regarded as standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in Section 7.
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Designation: E 1915 – 99
Standard Test Methods for
Analysis of Metal Bearing Ores and Related Materials by
Combustion Infrared Absorption Spectrometry
This standard is issued under the fixed designation E 1915; 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 882 Guide for Accountability and Quality Control in the
Chemical Analysis of Metals
1.1 This test method covers the determination of total
E 1019 Test Methods for Determination of Carbon, Sulfur,
carbon and sulfur in metal bearing ores and related materials
Nitrogen, Oxygen and Hydrogen in Steel and in Iron,
such as tailings and waste rock within the following ranges:
Nickel and Cobalt Alloys
Analyte Application Range, % Quantitative Range, %
E 1601 Practice for Conducting an Interlaboratory Study to
Total Carbon 0 to 10 0.1 to 10
Total Sulfur 0 to 8.8 0.1 to 8.8
Evaluate the Performance of an Analytical Method
E 1950 Practice for Reporting Results from Methods of
1.2 The quantitative ranges for the partial decomposition
Chemical Analysis
test methods are dependent on the mineralogy of the samples
being tested. The user of these test methods are advised to
3. Terminology
conduct an interlaboratory study in accordance with Practice
3.1 Definitions—For definitions of terms used in these test
E 1601 on the test methods selected for use at a particular
methods, refer to Terminology E 135.
mining site, in order to establish the quantitative ranges for
these test methods on a site-specific basis.
4. Significance and Use
1.3 The test methods appear in the following order:
4.1 These test methods are primarily intended to test mate-
Sections
rials for compliance with compositional specifications and for
Carbon and Sulfur, Residual from Pyrolysis 12.7 — 12.12
Carbon and Sulfur, Total 12 — 12.6
monitoring. The determination of carbon and sulfur in ores and
related materials is necessary to classify ores for metallurgical
1.4 The values stated in SI units are to be regarded as
processing and to classify waste materials from the mining and
standard.
processing of ores such as leach spoils, waste rock and tailings
1.5 This standard does not purport to address all of the
according to their potential to generate acid in the environment.
safety concerns, if any, associated with its use. It is the
This information is useful during mine development to assist in
responsibility of the user of this standard to establish appro-
mining and mineral processing operations and proper disposal
priate safety and health practices and determine the applica-
of waste materials.
bility of regulatory limitations prior to use. Specific warning
4.2 These test methods also may be used for the classifica-
statements are given in Section 7.
tion of rock to be used in construction, where the potential to
2. Referenced Documents
generate acid under environmental conditions exists.
4.3 It is assumed that the users of these test methods will be
2.1 ASTM Standards:
trained analysts capable of performing common laboratory
D 1193 Specifications for Reagent Water
procedures skillfully and safely. It is expected that work will be
E 29 Practice For Using Significant Digits in Test Data to
performed in a properly equipped laboratory and that proper
Determine Conformance With Specifications
waste disposal procedures will be followed. Appropriate qual-
E 50 Practices for Apparatus, Reagents and Safety Precau-
ity control practices such as those described in Guide E 882
tions for Chemical Analysis of Metals
must be followed.
E 135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
5. Apparatus
5.1 Combustion-Infrared Spectrophotometer, equipped with
This test method is under the jurisdiction of ASTM Committee E-1 on
a combustion chamber, oxygen carrier stream and infrared
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal- absorption detector, suitable for analysis of sulfur in a mini-
lurgical Materials.
mum range instrument from 0.1 to 1.75 % or in a maximum
Current edition approved Dec. 10, 1999. Published February 2000. Originally
range instrument from 0.1 to 8.8 % and carbon in the range of
published as E 1915 – 97. Last previous edition E 1915 – 97.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 14.02.
4 5
Annual Book of ASTM Standards, Vol 03.05. Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1915
0.1 to 10 %, using 0.2-g test portions in ores and related 7. Hazards
materials. Instruments, such as those shown in Test Methods
7.1 For hazards to be observed in the use of reagents and
E 1019 and in the section entitled Apparatus for Determination
apparatus in these test methods, refer to Practice E 50. Use care
of Total Carbon by Direct Combustion and the section entitled
when handling hot crucibles or boats and when operating
Apparatus for the Determination of Sulfur by Direct Combus-
furnaces to avoid personal injury by either burn or electrical
tion of Practices E 50, that can be shown to give equivalent
shock.
results may also be used for these test methods.
8. Rounding Calculated Values
6. Reagents and Materials
8.1 Calculated values shall be rounded to the desired num-
6.1 Purity of Reagents—Reagent grade chemicals shall be
ber of places as directed in the Rounding Method of Practice
used in all tests. Unless otherwise indicated, it is intended that
E 29.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
9. Interlaboratory Studies
such specifications are available . Other grades may be used,
9.1 These test methods have been evaluated in accordance
provided it is first ascertained that the reagent is of sufficiently
with Practice E 1601 unless otherwise noted in the precision
high purity to permit its use without lessening the accuracy of
and bias section. The lower limit in the scope of these test
the determination.
methods specifies the lowest analyte content that may be
6.2 Reagents:
analyzed with an acceptable error. A warning statement is
6.2.1 Barium Sulfate (BaSO ), Anhydrous, contains 13.74 %
included in the scope for test methods not observing this
sulfur (purity: 99.9 % minimum). Dry 100 g at 120°C for 2 h
convention.
and store in a 250-mL glass bottle.
9.2 Site-Specific Quantitative Ranges—An interlaboratory
6.2.2 Blank Reference Sample—Prepare a blank reference
study may be conducted in accordance with Practice E 1601 to
sample by pulverizing or grinding 100 g silica (see 6.2.6),
establish quantitative ranges for the partial decomposition test
passing it through a No. 100 (150-μm) sieve, and mixing and
methods selected for a particular site. Test samples shall be
storing it in a 250-mL glass bottle. This blank contains 0.00 %
selected for each lithologic unit containing high and low
carbon and sulfur.
concentrations of carbon and sulfur minerals. Each test sample
6.2.3 Calcium Carbonate (CaCO ), Anhydrous, contains
must be analyzed in rapid succession for total carbon and sulfur
12.00 % carbon (purity: 99.9 % minimum). Dry 100 g for 2 h
followed by the different partial decomposition treatments
at 120°C and store in a 250-mL glass bottle.
selected in order to minimize the between-method variation.
6.2.4 Calibration Mixture A—(1 g 5 20 mg C and 20 mg
S)—Combine 16.67 g CaCO , 14.56 g BaSO and 68.77 g
3 4
10. Sampling and Sample Preparation
SiO in a ring and puck grinding mill or equivalent device.
10.1 Materials Safety—Samples must be prepared, stored
Grind until 100 % passes through a No. 100 (150-μm) sieve,
and disposed of in accordance with the materials and safety
pass the mixture through the screen to break up any lumps, mix
guidelines in Practices E 50.
and store in a glass bottle. This mixture contains 2.00 % carbon
10.2 Prepared Sample—Dry a representative portion of the
and sulfur.
gross sample at 80°C to constant weight. Pulverize or grind the
6.2.4.1 Alternatively, grind the reagents separately, mix, and
laboratory sample until 100 % passes a No. 100 (150-μm)
pass through the screen prior to final mixing.
sieve.
6.2.5 Calibration Mixtures—Transfer 4.00, 10.00, 20.00
and 30.00 g of Calibration Mixture A to ring and puck grinding
NOTE 1—Results from the interlaboratory study suggest that it may be
mills or equivalent devices. Add the amount of dried SiO necessary to grind samples to pass a No. 200 (75-μm) sieve in order to
improve precision for samples containing low concentrations of carbon or
needed to bring the total weight to 40.0 g in each mill, grind to
sulfur.
100 % passing a No. 100 (150-μm) sieve, pass the mixture
through the screen, mix and store in 250-mL glass bottles. 10.3 Diluted Sample—If the concentration of sulfur in the
These mixtures contain: 0.2, 0.5, 1.0, and 1.5 % for both
test material exceeds 1.75 % for the minimum range instru-
carbon and sulfur. ment, prepare a diluted sample as in 10.3.1.
6.2.5.1 Alternatively, grind the reagents separately, mix, and
10.3.1 Weigh 10.0 6 0.1 g prepared sample and combine
pass through the screen prior to final mixing. with 40.0 6 0.1 g dry SiO . Grind the mixture in a ring and
6.2.5.2 Commercially produced calibration mixtures, that
puck mill, or equivalent, until 100 % will pass through a No.
meet the specifications of 6.2.5, may also be used. 100 (150-μm) sieve; mix, and store in a 250-mL glass bottle.
6.2.6 Silica (SiO ), (purity: 99.9 % minimum), Ottawa sand,
11. Calibration and Standardization
washed and ignited, containing less than 0.01 % carbon and
sulfur. Dry at 120°C for 2 h and store in a 250-mL glass bottle.
11.1 Apparatus—Operate and calibrate the instrument ac-
cording to the manufacturer’s instructions. Resistance furnace
instruments require the use of vanadium pentoxide or tung-
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
stenic acid for the determination of sulfur in these test methods.
listed by the American Chemical Society, see Analar Standards for Laboratory
Use a 0.200 6 0.1 g weight for all calibration mixtures,
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
reference materials, blank reference materials, test samples and
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. diluted test samples in these test methods.
E 1915
11.1.1 Certain instruments may require different sample verification before proceeding with analysis of test samples,
weights for certain concentration ranges, which is permissible and discard the results since the last acceptable quality control
as long as the precision and bias requirements of these test sample result had been obtained.
methods are fulfilled. 11.4.2 Blank Reference Sample—Analyze a blank reference
11.2 Ignite the crucibles or boats for test samples and sample before analysis of test samples and within each group
standard samples in a muffle furnace for1hat550 6 10°C. of fifty test samples. If the result for the blank reference sample
11.3 Laboratory Test Method Performance exceeds the limits in Table 1 for the 0.0 % calibration mixture,
Demonstration—A demonstration of laboratory test method correct any instrumental problems and repeat the analysis of
performance must be performed before this test method may be the blank reference sample before proceeding with analysis of
used in a laboratory for the first time. This demonstration is test samples, and discard the results since the last acceptable
particularly important if the laboratory needs to modify the test quality control sample result had been obtained.
method in any way. The demonstration must be repeated 11.4.3 Reference Sample—Analyze a reference sample, cer-
whenever the test method is significantly modified. tified for total carbon and total sulfur before analysis of test
11.3.1 Linearity Verification—Measure total carbon and samples for total carbon and sulfur and within each group of
sulfur for the blank reference sample, calibration mixtures, fifty test samples. If the difference of the reference sample and
barium sulfate and calcium carbonate in increasing order using the reference value for the reference sample exceeds the limits
the same weight of calibration mixtures selected for test shown in Table 1 for materials of comparable concentration,
samples, in accordance with the manufacturer’s instructions. correct any instrumental problems and repeat the analysis of
Record the calibration mixture weights used and the carbon the reference material, and discard the results since the last
and sulfur results measured by the instrument. Check for acceptable quality control sample result had been obtained.
linearity by linear regression or by a graphical method to meet 11.4.4 Control Sample—Analyze the 0.2 % calibration mix-
a deviation less than 10 % relative for each of the calibration ture prior to and within each group of fifty test samples. If the
material results at or above a concentration of 0.2 % carbon result for the control sample exceeds the limits shown in Table
and sulfur and a correlation coefficient of at least 0.99. Correct 1 for the 0.2 % calibration mixture, correct any instrumental
any problems with the instrument before proceeding with the problems and repeat the analysis of the control sample before
analysis of test samples. proceeding with analysis of test samples, and discard the
11.3.1.1 Linearity may also be verified by the use of barium results since the last acceptable quality control sample result
sulfate and calcium carbonate weights equivalent to the content had been obtained.
of the calibration mixtures. 11.4.5 Standard Addition Sample—Analyze a standard ad-
11.3.2 Blank Sample Precision Verification—Analyze ten dition sample prior to analysis of each group of fifty test
replicates of the blank reference sample. If the standard samples by preparing a duplicate of the first test sample in the
deviation of the replicate analyses exceeds 0.02 % for carbon group and adding an equal weight of the 0.5 % calibration
or 0.01 % for sulfur, correct any instrumental problems and mixture just prior to determination of carbon and sulfur.
repeat the blank sample precision verification before proceed- Calculate the reference values for the standard add
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