ASTM E394-22

Standard Test Method for Iron in Trace Quantities Using the 1,10-Phenanthroline Method

SIGNIFICANCE AND USE
4.1 This test method is suitable for determining trace concentrations of iron in a wide variety of products, provided that appropriate sample preparation has rendered the iron and sample matrix soluble in water or other suitable solvent (see 10.1 and Note 4).  
4.2 This test method assumes that the amount of color developed is proportional to the amount of iron in the test solution. The calibration curve is linear over the specified range. Possible interferences are described in Section 5.
SCOPE
1.1 This test method covers the determination of trace concentrations of iron in the range from 1 to 100 μg/g in a wide variety of products.  
1.2 In determining the conformance of the test results using this method to applicable specifications; results shall be rounded off in accordance with the rounding-off method of Practice E29.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 Consult current OSHA regulations, suppliers’ Safety Data Sheets, and local regulations for all materials used in this specification.  
1.5 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: 31-Aug-2022
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

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: E394 − 22
Standard Test Method for
Iron in Trace Quantities Using the 1,10-Phenanthroline
1
Method
This standard is issued under the fixed designation E394; 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* E180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe-
1.1 This test method covers the determination of trace
3
cialty Chemicals (Withdrawn 2009)
concentrationsofironintherangefrom1to100µg/ginawide
E275 Practice for Describing and Measuring Performance of
variety of products.
Ultraviolet and Visible Spectrophotometers
1.2 In determining the conformance of the test results using
E300 Practice for Sampling Industrial Chemicals
this method to applicable specifications; results shall be
rounded off in accordance with the rounding-off method of
3. Summary of Test Method
Practice E29.
3.1 This test method is based upon a photometric determi-
1.3 The values stated in SI units are to be regarded as
nation of the 1,10-phenanthroline complex with the iron(II)
standard. No other units of measurement are included in this
ion. The sample is dissolved in a suitable solvent and the iron
standard.
is reduced to the divalent state by the addition of hydroxylam-
ine hydrochloride.The color is then developed, by the addition
1.4 Consult current OSHA regulations, suppliers’ Safety
of 1,10-phenanthroline. After a short reaction period, the
Data Sheets, and local regulations for all materials used in this
absorbance of the solution is measured at approximately
specification.
510 nm using a suitable photometer. The absorbance of the
1.5 This international standard was developed in accor-
solution, once the color is developed, is stable for at least
dance with internationally recognized principles on standard-
several months.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4. Significance and Use
mendations issued by the World Trade Organization Technical
4.1 This test method is suitable for determining trace
Barriers to Trade (TBT) Committee.
concentrations of iron in a wide variety of products, provided
that appropriate sample preparation has rendered the iron and
2. Referenced Documents
sample matrix soluble in water or other suitable solvent (see
2
2.1 ASTM Standards:
10.1 and Note 4).
D1193 Specification for Reagent Water
4.2 This test method assumes that the amount of color
D6809 Guide for Quality Control and Quality Assurance
developed is proportional to the amount of iron in the test
Procedures for Aromatic Hydrocarbons and Related Ma-
solution. The calibration curve is linear over the specified
terials
range. Possible interferences are described in Section 5.
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
5. Interferences
E60 Practice for Analysis of Metals, Ores, and Related
4
5.1 Fortune and Mellon have made a comprehensive study
Materials by Spectrophotometry
of the interferences of various inorganic ions in this determi-
nation. Table 1 and Table 2, taken from their report, show the
1
This test method is under the jurisdiction of ASTM Committee D16 on effects of various cations and anions on the determination of
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
2.0 µg/g (ppm) iron. If the maximum level of 500 µg/g (ppm)
bility of Subcommittee D16.04 on Instrumental Analysis.
does not interfere, it is very likely that the ion will not interfere
Current edition approved Sept. 1, 2022. Published September 2022. Originally
approved in 1970. Last previous edition approved in 2015 as E394 – 15. DOI:
10.1520/E0394-22.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM www.astm.org.
4
Standards volume information, refer to the standard’s Document Summary page on Fortune, W. B., and Mellon, M. G., Industrial and Engineering Chemistry,
the ASTM website. Analytical Edition, IENAA Vol 10, 1938, pp. 60–64.
*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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E394 − 22
TABLE 1 Effect of Cations on
...

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: E394 − 15 E394 − 22
Standard Test Method for
Iron in Trace Quantities Using the 1,10-Phenanthroline
1
Method
This standard is issued under the fixed designation E394; 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 trace concentrations of iron in the range from 1 to 100 μg.μg/g in a wide variety
of products.
1.2 This test method is intended to be general for the final steps in the determination of iron and does not include procedures for
sample preparation.
1.2 This test method is applicable to samples whose solutions have a pH less than 2. It is assumed that the pH is adjusted toIn
determining the conformance of the test results using this method to applicable specifications; results shall be rounded off in
accordance with the rounding-off method of Practice E29within this range in the sample preparation.
1.4 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first-aid procedures, handling, and
safety precautions.
1.3 The values givenstated in SI units are the standard. Values in parentheses are for information only.to be regarded as standard.
No other units of measurement are included in this standard.
1.6 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.
1.4 Consult current OSHA regulations, suppliers’ Safety Data Sheets, and local regulations for all materials used in this
specification.
1.5 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:
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.04 on Instrumental Analysis.
Current edition approved Nov. 1, 2015Sept. 1, 2022. Published January 2016September 2022. Originally approved in 1970. Last previous edition approved in 20092015
as E394 – 09.E394 – 15. DOI: 10.1520/E0394-15.10.1520/E0394-22.
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

---------------------- Page: 1 ----------------------
E394 − 22
D1193 Specification for Reagent Water
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E60 Practice for Analysis of Metals, Ores, and Related Materials by Spectrophotometry
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers
E300 Practice for Sampling Industrial Chemicals
3. Summary of Test Method
3.1 This test method is based upon a photometric determination of the 1,10-phenanthroline complex with the iron(II) ion. The
sample is dissolved in a suitable solvent and the iron is reduced to the divalent state by the addition of hydroxylamine
hydrochloride. The color is then developed, by the addition of 1,10-phenanthroline. After a short reaction period, the absorbance
of the solution is measured at approximately 510 nm 510 nm using a suitable photometer. The absorbance of the solution, once
the color is developed, is stable for at least several months.
4. Si
...