ASTM D6647-18
(Test Method)Standard Test Method for Determination of Acid Soluble Iron via Atomic Absorption
Standard Test Method for Determination of Acid Soluble Iron via Atomic Absorption
SIGNIFICANCE AND USE
5.1 In certain applications, such as acid purification, acidic food or chemical purification or decolorization, or other applications wherein iron may be leached out of the carbon, the use of acid-washed carbons will reduce or eliminate color pickup in the effluent or in the product. The acid soluble iron content is usually specified by the carbon supplier to prevent unacceptable levels of iron leach occurring.
5.2 Detection limits, sensitivity, and optimum ranges will vary with the models of atomic absorption spectrophotometers. General instrumental parameters are as follows:
5.2.1 Iron hollow cathode lamp.
5.2.2 Wavelength: 248.3 nm.
5.2.3 Fuel: acetylene (high purity).
5.2.4 Oxidant: air (from compressed air line, laboratory compressor, or a cylinder of compressed air—all need to be clean and dry).
5.2.5 Type of flame: oxidizing.
5.2.6 The following lines may also be used:
248.8 nm Relative Sensitivity 2
271.9 nm Relative Sensitivity 4
302.1 nm Relative Sensitivity 5
252.7 nm Relative Sensitivity 6
372.0 nm Relative Sensitivity 10
5.3 The method, as written, is intended for carbons having an acid soluble iron content of 0.0030 to 0.050 %. For carbons having higher iron contents, larger dilutions or smaller aliquots may be used.
5.4 The user should validate that there are no interferences from other metals in the sample matrix.
5.5 To prevent erroneous results, the user should ensure that no iron instruments contact any of the sample or the solutions used in this procedure. Only glass, ceramics, or plastic should be allowed to contact the sample or solutions.
SCOPE
1.1 This test method covers the determination of the acid soluble iron content of granular and powdered activated carbons, using an atomic absorption spectroscopy method by direct aspiration. Hydrochloric acid is used to extract the iron. This test method is not directly usable to determine the total iron concentration of a sample.
1.2 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. For a specific hazard statement, see Section 8.
1.3 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
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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: D6647 − 18
Standard Test Method for
1
Determination of Acid Soluble Iron via Atomic Absorption
This standard is issued under the fixed designation D6647; 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.
3
1. Scope 2.2 NIST Publication:
Circular 602 Testing of Glass Volumetric Apparatus
1.1 This test method covers the determination of the acid
soluble iron content of granular and powdered activated
3. Terminology
carbons, using an atomic absorption spectroscopy method by
3.1 Definitions—Terms relating to this standard are defined
direct aspiration. Hydrochloric acid is used to extract the iron.
in Terminology D2652.
This test method is not directly usable to determine the total
3.1.1 atomic absorption—in flame atomic absorption
iron concentration of a sample.
spectrometry, a sample is aspirated into a flame and atomized.
1.2 This standard does not purport to address all of the
A light beam is directed through the flame, into a
safety concerns, if any, associated with its use. It is the
monochromator, and onto a detector that measures the amount
responsibility of the user of this standard to establish appro-
of light absorbed by the atomized element in the flame.
priate safety, health, and environmental practices and deter-
Because each metal has its own characteristic absorption
mine the applicability of regulatory limitations prior to use.
wavelength, a source lamp of that element is used.The amount
For a specific hazard statement, see Section 8.
of energy at the characteristic wavelength absorbed in the
1.3 This international standard was developed in accor-
flame is proportional to the concentration of the element in the
dance with internationally recognized principles on standard-
sample over a limited concentration range.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4. Summary of Test Method
mendations issued by the World Trade Organization Technical
4.1 Arepresentativesampleofthematerialtobeanalyzedis
Barriers to Trade (TBT) Committee.
collected according to Practice E300. A known weight of the
sample is ground until 95 % or more of the sample passes 325
2. Referenced Documents
mesh. The ground sample is oven dried, and then mixed with
2
2.1 ASTM Standards: a dilute hydrochloric acid. The solution is boiled for 5 min to
D1193 Specification for Reagent Water convert the iron into a soluble chloride, and then cooled and
D2652 Terminology Relating to Activated Carbon filtered. The filter cake is washed with water. Then the filtrate
E11 Specification for Woven Wire Test Sieve Cloth and Test is transferred quantitatively to a beaker. The concentration of
Sieves iron in the filtrate is measured by atomic absorption against a
E177 Practice for Use of the Terms Precision and Bias in set of standards. The acid soluble iron concentration is then
ASTM Test Methods calculated against the weight of the original sample.
E287 Specification for Laboratory Glass Graduated Burets
5. Significance and Use
E288 Specification for Laboratory Glass Volumetric Flasks
E300 Practice for Sampling Industrial Chemicals 5.1 In certain applications, such as acid purification, acidic
E691 Practice for Conducting an Interlaboratory Study to food or chemical purification or decolorization, or other
Determine the Precision of a Test Method applicationswhereinironmaybeleachedoutofthecarbon,the
use of acid-washed carbons will reduce or eliminate color
pickup in the effluent or in the product. The acid soluble iron
content is usually specified by the carbon supplier to prevent
1
This test method is under the jurisdiction of ASTM Committee D28 on
unacceptable levels of iron leach occurring.
ActivatedCarbonandisthedirectresponsibilityofSubcommitteeD28.02onLiquid
Phase Evaluation.
5.2 Detection limits, sensitivity, and optimum ranges will
CurrenteditionapprovedMay1,2018.PublishedJune2018Originallyapproved
vary with the models of atomic absorption spectrophotometers.
in 2001. Last previous edition approved in 2011 as D6647 – 01 (2011). DOI:
10.1520/D6647-18.
General instrumental parameters are as follows:
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from National Institute of Standards and Technology (NIST), 100
the ASTM website
...
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.
Designation: D6647 − 01 (Reapproved 2011) D6647 − 18
Standard Test Method for
Determination of Acid Soluble Iron Viavia Atomic
1
Absorption
This standard is issued under the fixed designation D6647; 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
1.1 This test method covers the determination of the acid soluble iron content of granular and powdered activated carbons, using
an atomic absorption spectroscopy method by direct aspiration. Hydrochloric acid is used to extract the iron. This test method is
not directly usable to determine the total iron concentration of a sample.
1.2 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. For a specific hazard statement, see Section 8.
1.3 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:
D1193 Specification for Reagent Water
D2652 Terminology Relating to Activated Carbon
D1193 Specification for Reagent Water
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E287 Specification for Laboratory Glass Graduated Burets
E288 Specification for Laboratory Glass Volumetric Flasks
E300 Practice for Sampling Industrial Chemicals
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 NIST Publication:
Circular 602 Testing of Glass Volumetric Apparatus
3. Terminology
3.1 Definitions—Terms relating to this standard are defined in Terminology D2652.
3.1.1 atomic absorption—in flame atomic absorption spectrometry, a sample is aspirated into a flame and atomized. A light
beam is directed through the flame, into a monochromator, and onto a detector that measures the amount of light absorbed by the
atomized element in the flame. Because each metal has its own characteristic absorption wavelength, a source lamp of that element
is used. The amount of energy at the characteristic wavelength absorbed in the flame is proportional to the concentration of the
element in the sample over a limited concentration range.
4. Summary of Test Method
4.1 A representative sample of the material to be analyzed is collected according to Practice E300. A known weight of the
sample is ground until 95 % or more of the sample passes 325 mesh. The ground sample is oven dried, and then mixed with a dilute
1
This test method is under the jurisdiction of ASTM Committee D28 on Activated Carbon and is the direct responsibility of Subcommittee D28.02 on Liquid Phase
Evaluation.
Current edition approved Sept. 1, 2011May 1, 2018. Published November 2011June 2018 Originally approved in 2001. Last previous edition approved in 20062011 as
D6647 – 01 (2011).(2006). DOI: 10.1520/D6647-01R11.10.1520/D6647-18.
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.
3
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6647 − 18
hydrochloric acid. The solution is boiled for 5 minutesmin to convert the iron into a soluble chloride, and then cooled and filtered.
The filter cake is washed with water. Then the filtrate is transferred quantitatively to a beaker. The concentration of iron in the
filtrate is measured by atomic absorption against a set of standards. The acid soluble iron concentration is then calculated against
the weight of the original sample.
5. Significance and Use
5.1 In certain appli
...
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