Standard Test Methods for Chemical Analysis of Graphite

SIGNIFICANCE AND USE
4.1 These test methods provide a practical way to measure the concentration of certain trace elements in graphite. Many end uses of graphite require that it be free of elements which may be incompatible with certain nuclear applications. Other elemental contamination can affect the rate of oxidative degradation.  
4.2 These test methods allow measurement of trace amounts of contaminants with a minimal amount of costly equipment. The colorimetric procedures used are accessible to most laboratories.  
4.3 Other instrumental analysis techniques are available, capable of simultaneous quantitative analysis of 76 stable elements in a single run, with detectability limits in the parts per million range. Standards are currently being developed for elemental analysis of impurities in graphite using glow discharge mass spectrometry (GDMS), inductively coupled plasma optical emission spectroscopy (ICP-OES), combustion ion chromatography (CIC).
SCOPE
1.1 These test methods cover the chemical analysis of graphite.  
1.2 The analytical procedures appear in the following order:    
Sections    
Silicon by the Molybdenum Blue (Colorimetric) Test Method  
9 to 15  
Iron by the o-Phenanthroline (Colorimetric) Test Method  
16 to 22  
Calcium by the Permanganate (Colorimetric) Test Method  
23 to 29  
Aluminum by the 2-Quinizarin Sulfonic Acid Test Method  
30 to 36  
Titanium by the Peroxide (Colorimetric) Test Method  
37 to 44  
Vanadium by the 3,3′-Dimethylnaphthidine (Colorimetric)
Test Method  
45 to 52  
Boron by the Curcumin-Oxalic Acid (Colorimetric) Test Method  
53 to 60  
1.3 The preferred concentration of sought element in the final solution, the limits of sensitivity, and the precision of the results are given in Table 1.    
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. See 56.1 for specific caution statement.  
1.6 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.

General Information

Status
Published
Publication Date
30-Apr-2020
Current Stage
Ref Project

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Standards Content (Sample)

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: C560 − 20
Standard Test Methods for
1
Chemical Analysis of Graphite
This standard is issued under the fixed designation C560; 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* D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to
1.1 These test methods cover the chemical analysis of
Determine Conformance with Specifications
graphite.
1.2 The analytical procedures appear in the following order:
3. Terminology
Sections
3.1 Definitions:
Silicon by the Molybdenum Blue (Colorimetric) Test Method 9 to 15
Ironbythe o-Phenanthroline (Colorimetric) Test Method 16 to 22
3.1.1 calibration solutions, n—solutions of accurately
Calcium by the Permanganate (Colorimetric) Test Method 23 to 29
known concentrations of the chemical element to be deter-
Aluminum by the 2-Quinizarin Sulfonic Acid Test Method 30 to 36
mined using the calibration curve method.
Titanium by the Peroxide (Colorimetric) Test Method 37 to 44
Vanadium by the 3,3'-Dimethylnaphthidine (Colorimetric) 45 to 52
3.1.2 colorimetric analysis, n—photometric analysis
Test Method
Boron by the Curcumin-Oxalic Acid (Colorimetric) Test Method 53 to 60
method of using absorption of monochromatic light in the
visible spectrum.
1.3 The preferred concentration of sought element in the
final solution, the limits of sensitivity, and the precision of the
3.1.3 photometric analysis, n—analytical chemistry method
results are given in Table 1.
for quantitative chemical analysis based on the relationship
1.4 The values stated in SI units are to be regarded as between solution concentrations and the absorption of mono-
chromatic light, as expressed by the Beer law.
standard. No other units of measurement are included in this
standard.
3.2 Definitions of Terms Specific to This Standard:
1.5 This standard does not purport to address all of the
3.2.1 calibration curve, n—graphical or mathematical rep-
safety concerns, if any, associated with its use. It is the
resentation of the relationship between known concentrations
responsibility of the user of this standard to establish appro-
of an element in a series of standard calibration solutions and
priate safety, health, and environmental practices and deter-
the measured response from the measurement system.
mine the applicability of regulatory limitations prior to use.
See 56.1 for specific caution statement.
4. Significance and Use
1.6 This international standard was developed in accor-
4.1 These test methods provide a practical way to measure
dance with internationally recognized principles on standard-
the concentration of certain trace elements in graphite. Many
ization established in the Decision on Principles for the
end uses of graphite require that it be free of elements which
Development of International Standards, Guides and Recom-
may be incompatible with certain nuclear applications. Other
mendations issued by the World Trade Organization Technical
elemental contamination can affect the rate of oxidative deg-
Barriers to Trade (TBT) Committee.
radation.
2. Referenced Documents
4.2 Thesetestmethodsallowmeasurementoftraceamounts
2
2.1 ASTM Standards:
of contaminants with a minimal amount of costly equipment.
C561 Test Method for Ash in a Graphite Sample
The colorimetric procedures used are accessible to most
laboratories.
1
These test methods are under the jurisdiction of ASTM Committee D02 on
4.3 Other instrumental analysis techniques are available,
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
capable of simultaneous quantitative analysis of 76 stable
tee D02.F0 on Petroleum Products, Liquid Fuels, and Lubricants
elements in a single run, with detectability limits in the parts
Current edition approved May 1, 2020. Published May 2020. Originally
ε1
per million range. Standards are currently being developed for
approved in 1965. Last previous edition approved in 2015 as C560 – 15 . DOI:
10.1520/C0560-20.
elemental analysis of impurities in graphite using glow dis-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
charge mass spectrometry (GDMS), inductively coupled
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
plasma optical emission spectroscopy (ICP-OES), combustion
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. ion chromatography (CIC).
*A Summary of Changes section
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: C560 − 15 C560 − 20 An American National Standard
Standard Test Methods for
1
Chemical Analysis of Graphite
This standard is issued under the fixed designation C560; 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
ε NOTE—Subsection 1.2 was corrected editorially in February 2017.
1. Scope*
1.1 These test methods cover the chemical analysis of graphite.
1.2 The analytical procedures appear in the following order:
Sections
Silicon by the Molybdenum Blue (Colorimetric) Test Method 9 to 15
Iron by the o-Phenanthroline (Colorimetric) Test Method 16 to 22
Calcium by the Permanganate (Colorimetric) Test Method 23 to 29
Aluminum by the 2-Quinizarin Sulfonic Acid Test Method 30 to 36
Titanium by the Peroxide (Colorimetric) Test Method 37 to 44
Vanadium by the 3,3'-Dimethylnaphthidine (Colorimetric) 45 to 52
Test Method
Boron by the Curcumin-Oxalic Acid (Colorimetric) Test Method 53 to 60
1.3 The preferred concentration of sought element in the final solution, the limits of sensitivity, and the precision of the results
are given in Table 1.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. See 56.1 for specific caution statement.
1.6 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.
2. Referenced Documents
2
2.1 ASTM Standards:
C561 Test Method for Ash in a Graphite Sample
D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
3. Terminology
3.1 Definitions:
3.1.1 calibration curve, n—graphical or mathematical representation of the relationship between known concentrations of an
element in a series of standard calibration solutions and the measured response from the measurement system.
3.1.1 calibration solutions, n—solutions of accurately known concentrations of the chemical element to be determined using the
calibration curve method.
3.1.2 colorimetric analysis, n—photometric analysis method of using absorption of monochromatic light in the visible spectrum.
3.1.3 photometric analysis, n—analytical chemistry method for quantitative chemical analysis based on the relationship between
solution concentrations and the absorption of monochromatic light, as expressed by the Beer law.
1
These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and are the direct responsibility of Subcommittee D02.F0
on Petroleum Products, Liquid Fuels, and Lubricants
Current edition approved Oct. 1, 2015May 1, 2020. Published November 2015May 2020. Originally approved in 1965. Last previous edition approved in 20102015 as
ε1
C560 – 88 (2010)C560 – 15 . DOI: 10.1520/C0560-15E01.10.1520/C0560-20.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
1

---------------------- Page: 1 ----------------------
C560 − 20
TABLE 1 Concentration of Elements, Limits of Sensitivity, and
Reproducibility
Concentration Reproducibility,
Range, μg/mL Sensitivity Limit, Relative, %
Element Solution μg/mL Solution (σ/x × 100)
Silicon 10 μg ⁄100 mL to 100 μg/ 1 μg/100 mL ±4
100 mL
Iron 100 μg ⁄100 mL to 600 40 μg/100 mL ±5
μg/100 mL
Calcium 600 μg ⁄100 mL to 3000 50 μg/100 mL ±5
μg/100 mL
Aluminum 10 μg ⁄100 mL to 100 μg/ 2 μg/100 mL ±0.1
100 mL
Titanium 600 μg ⁄100 mL to 3000 200 μg/100 mL ±2
μg/100 mL
Vanadium 10 μg ⁄5
...

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