ASTM C560-15

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  
8 to 14  
Iron by the o-Phenanthroline (Colorimetric) Test Method  
15 to 21    
Calcium by the Permanganate (Colorimetric) Test Method  
22 to 28    
Aluminum by the 2-Quinizarin Sulfonic Acid Test Method  
29 to 35  
Titanium by the Peroxide (Colorimetric) Test Method  
36 to 43    
Vanadium by the 3,3′-Dimethylnaphthidine (Colorimetric)
Test Method  
44 to 51    
Boron by the Curcumin-Oxalic Acid (Colorimetric) Test Method  
52 to 59  
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 and health practices and determine the applicability of regulatory limitations prior to use. See 56.1 for specific caution statement.

General Information

• Status: Historical
• Publication Date: 30-Sep-2015
• ICS: 71.060.10 - Chemical elements
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.F0 - Manufactured Carbon and Graphite Products

Relations

• Replaces: ASTM C560-88(2010)e1 - Standard Test Methods for Chemical Analysis of Graphite
• Effective Date: 01-Oct-2015
• Replaced By: ASTM C560-15e1 - Standard Test Methods for Chemical Analysis of Graphite
• Effective Date: 01-Oct-2015

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: C560 − 15 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. Scope* 3.1.1 calibration curve, n—graphical or mathematical rep-
resentation of the relationship between known concentrations
1.1 These test methods cover the chemical analysis of
of an element in a series of standard calibration solutions and
graphite.
the measured response from the measurement system.
1.2 The analytical procedures appear in the following order:
3.1.2 calibration solutions, n—solutions of accurately
Sections
Silicon by the Molybdenum Blue (Colorimetric) Test Method 8 to 14 known concentrations of the chemical element to be deter-
Ironbythe o-Phenanthroline (Colorimetric) Test Method 15 to 21
mined using the calibration curve method.
Calcium by the Permanganate (Colorimetric) Test Method 22 to 28
Aluminum by the 2-Quinizarin Sulfonic Acid Test Method 29 to 35
3.1.3 colorimetric analysis, n—photometric analysis
Titanium by the Peroxide (Colorimetric) Test Method 36 to 43
method of using absorption of monochromatic light in the
Vanadium by the 3,3'-Dimethylnaphthidine (Colorimetric) 44 to 51
Test Method visible spectrum.
Boron by the Curcumin-Oxalic Acid (Colorimetric) Test Method 52 to 59
3.1.4 photometric analysis, n—analytical chemistry method
1.3 The preferred concentration of sought element in the
for quantitative chemical analysis based on the relationship
final solution, the limits of sensitivity, and the precision of the
between solution concentrations and the absorption of mono-
results are given in Table 1.
chromatic light, as expressed by the Beer law.
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 These test methods provide a practical way to measure
1.5 This standard does not purport to address all of the
the concentration of certain trace elements in graphite. Many
safety concerns, if any, associated with its use. It is the
end uses of graphite require that it be free of elements which
responsibility of the user of this standard to establish appro-
may be incompatible with certain nuclear applications. Other
priate safety and health practices and determine the applica-
elemental contamination can affect the rate of oxidative deg-
bility of regulatory limitations prior to use. See 56.1 for
radation.
specific caution statement.
4.2 Thesetestmethodsallowmeasurementoftraceamounts
2. Referenced Documents
of contaminants with a minimal amount of costly equipment.
2
2.1 ASTM Standards:
The colorimetric procedures used are accessible to most
C561 Test Method for Ash in a Graphite Sample
laboratories.
D1193 Specification for Reagent Water
4.3 Other instrumental analysis techniques are available,
E29 Practice for Using Significant Digits in Test Data to
capable of simultaneous quantitative analysis of 76 stable
Determine Conformance with Specifications
elements in a single run, with detectability limits in the parts
3. Terminology
per million range. Standards are currently being developed for
elemental analysis of impurities in graphite using glow dis-
3.1 Definitions:
charge mass spectrometry (GDMS), inductively coupled
plasma optical emission spectroscopy (ICP-OES), combustion
1
These test methods are under the jurisdiction of ASTM Committee D02 on
ion chromatography (CIC).
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
tee D02.F0 on Petroleum Products, Liquid Fuels, and Lubricants
Current edition approved Oct. 1, 2015. Published November 2015. Originally
5. Reagents
ε1
approved in 1965. Last previous edition approved in 2010 as C560 – 88 (2010) .
DOI: 10.1520/C0560-15.
5.1 Purity of Reagents—Reagent grade chemicals shall be
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in all tests. Unless otherwise indicated, it is intended that
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
all reagents shall conform to the specifications of the Commit-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tee onAnalytical Reagents of theAmerican Chemical Society,
*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

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C560 − 15
TABLE 1 Concentration of Eleme
...

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 − 88 (Reapproved 2010) C560 − 15 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—Updated 57.1 editorially in May 2010.
1. Scope 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 8 to 14
Iron by the o-Phenanthroline (Colorimetric) Test Method 15 to 21
Calcium by the Permanganate (Colorimetric) Test Method 22 to 28
Aluminum by the 2-Quinizarin Sulfonic Acid Test Method 29 to 35
Titanium by the Peroxide (Colorimetric) Test Method 36 to 43
Vanadium by the 3,3'-Dimethylnaphthidine (Colorimetric) 44 to 51
Test Method
Boron by the Curcumin-Oxalic Acid (Colorimetric) Test Method 52 to 59
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 and health practices and determine the applicability of regulatory
limitations prior to use. See 56.1 for specific caution statement.
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.
3.1.2 calibration solutions, n—solutions of accurately known concentrations of the chemical element to be determined using the
calibration curve method.
3.1.3 colorimetric analysis, n—photometric analysis method of using absorption of monochromatic light in the visible spectrum.
3.1.4 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 Products, Liquid Fuels, and Lubricants
Current edition approved May 1, 2010Oct. 1, 2015. Published May 2010November 2015. Originally approved in 1965. Last previous edition approved in 20052010 as
ε1
C560 – 88 (2005)(2010) . DOI: 10.1520/C0560-88R10E01.10.1520/C0560-15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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

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C560 − 15
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 to 100 μg/100 mL 1 μg/100 mL ±4
Iron 100 to 600 μg/100 mL 40 μg/100 mL ±5
Calcium 600 to 3000 μg/100 mL 50 μg/100 mL ±5
Aluminum 10 to 100 μg/100 mL 2 μg/100 mL ±0.1
Titanium 600 to 3000 μg/100 mL 200 μg/100 mL ±2
Vanadium 10 to 130 μg/50 mL 5 μg/50 mL ±5
Boron 0.5 to 1.4 μg/50 mL 0.1 μg/50 mL ±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 m
...