Standard Test Method for Sampling and Testing for Ash and Total Iron in Steel Mill Dispersions of Rolling Oils

SIGNIFICANCE AND USE
5.1 The life cycle and cleanliness of a recirculating steel mill rolling oil dispersion is affected by the amount of iron present. This iron consists mainly of iron from acid pickling residues and iron from attrition of the steel sheet or rolls during cold rolling. In sampling rolling oils for total iron it is difficult to prevent adherence of iron containing sludge to the sample container. Thus, the accuracy of a total iron determination from an aliquot sample is suspect. This practice provides a means for ensuring that all iron contained in a sample is included in the analysis.  
5.2 Although less significant, the ash content is still an essential part of the procedure for obtaining a total iron analysis. Generally, the ash will be mostly iron, and in many cases, could be used as a substitute for total iron in determining when to change the dispersion.
FIG. 1 Possible Holding Fixture and Assembly System
SCOPE
1.1 This test method describes a procedure for sampling and testing dispersions of rolling oils in water from operating steel rolling mills for determination of ash and total iron content. Its purpose is to provide a test method such that a representative sample may be taken and phenomenon such as iron separation, fat-emulsion separation, and so forth, do not contribute to analytical error in determination of ash and total iron.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 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 specific warning statements, see Sections 7 and 8.  
1.4 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.

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Publication Date
29-Feb-2024
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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: D4042 − 24
Standard Test Method for
Sampling and Testing for Ash and Total Iron in Steel Mill
1
Dispersions of Rolling Oils
This standard is issued under the fixed designation D4042; 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* D2795 Test Methods for Analysis of Coal and Coke Ash
3
(Withdrawn 2001)
1.1 This test method describes a procedure for sampling and
D4175 Terminology Relating to Petroleum Products, Liquid
testing dispersions of rolling oils in water from operating steel
Fuels, and Lubricants
rolling mills for determination of ash and total iron content. Its
E50 Practices for Apparatus, Reagents, and Safety Consid-
purpose is to provide a test method such that a representative
erations for Chemical Analysis of Metals, Ores, and
sample may be taken and phenomenon such as iron separation,
Related Materials
fat-emulsion separation, and so forth, do not contribute to
E832 Specification for Laboratory Filter Papers
analytical error in determination of ash and total iron.
3. Terminology
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information 3.1 Definitions:
only. 3.1.1 For definitions of terms used in this test method, refer
to Terminology D4175.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Polyethylene disposable sample bags in a suitable hold-
priate safety, health, and environmental practices and deter-
ing device are used to collect representative samples of
mine the applicability of regulatory limitations prior to use.
nonhomogeneous dispersions of rolling mill oils in water from
For specific warning statements, see Sections 7 and 8.
an operating mill coolant system.
1.4 This international standard was developed in accor-
4.2 The collected sample and disposable bag are analyzed as
dance with internationally recognized principles on standard-
one for ash and total iron.
ization established in the Decision on Principles for the
4.2.1 Ash content is determined gravimetrically by evapo-
Development of International Standards, Guides and Recom-
rating all water from the sample bag before heating the residue
mendations issued by the World Trade Organization Technical
and bag in a muffle furnace to a constant weight (Test Method
Barriers to Trade (TBT) Committee.
D482).
4.2.2 Total iron content is determined by digesting the iron
2. Referenced Documents
in the ashed sample and bag in an acidified solution. The iron
2
2.1 ASTM Standards:
in the solution is reduced with stannous chloride and titrated
D482 Test Method for Ash from Petroleum Products
with standardized potassium dichromate.
D1068 Test Methods for Iron in Water
4.2.3 The ash and total iron contributed by a sample bag
D1193 Specification for Reagent Water
alone are determined separately and are subtracted from the
values of bag and sample to obtain the values for the sample
alone.
NOTE 1—There are a number of alternative methods available for
determining total iron in an ashed solution such as Test Methods D2795
1
This test method is under the jurisdiction of ASTM Committee D02 on
and D1068.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.L0.04 on Metal Deformation Fluids and Lubricants.
5. Significance and Use
Current edition approved March 1, 2024. Published March 2024. Originally
approved in 1981. Last previous edition approved in 2019 as D4042 – 93 (2019).
5.1 The life cycle and cleanliness of a recirculating steel
DOI: 10.1520/D4042-24.
mill rolling oil dispersion is affected by the amount of iron
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 The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
*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 ----------------------
D4042 − 24
NOTE 4—Occasionally, due to mill configuration or other reasons, it
present. This iron consists mainly of iron
...

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: D4042 − 93 (Reapproved 2019) D4042 − 24
Standard Test Method for
Sampling and Testing for Ash and Total Iron in Steel Mill
1
Dispersions of Rolling Oils
This standard is issued under the fixed designation D4042; 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 Scope*
1.1 This test method describes a procedure for sampling and testing dispersions of rolling oils in water from operating steel rolling
mills for determination of ash and total iron content. Its purpose is to provide a test method such that a representative sample may
be taken and phenomenon such as iron separation, fat-emulsion separation, and so forth, do not contribute to analytical error in
determination of ash and total iron.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 specific warning statements, see Sections 67 and 78.
1.4 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:
D482 Test Method for Ash from Petroleum Products
D1068 Test Methods for Iron in Water
D1193 Specification for Reagent Water
3
D2795 Test Methods for Analysis of Coal and Coke Ash (Withdrawn 2001)
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E832 Specification for Laboratory Filter Papers
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.L0.04 on Metal Deformation Fluids and Lubricants.
Current edition approved Dec. 1, 2019March 1, 2024. Published December 2019March 2024. Originally approved in 1981. Last previous edition approved in 20142019
as D4042 – 93 (2014).(2019). DOI: 10.1520/D4042-93R19.10.1520/D4042-24.
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
The last approved version of this historical standard is referenced on www.astm.org.
*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 ----------------------
D4042 − 24
4. Summary of Test Method
4.1 Polyethylene disposable sample bags in a suitable holding device are used to collect representative samples of nonhomoge-
neous dispersions of rolling mill oils in water from an operating mill coolant system.
4.2 The collected sample and disposable bag are analyzed as one for ash and total iron.
4.2.1 Ash content is determined gravimetrically by evaporating all water from the sample bag before heating the residue and bag
in a muffle furnace to a constant weight (Test Method D482).
4.2.2 Total iron content is determined by digesting the iron in the ashed sample and bag in an acidified solution. The iron in the
solution is reduced with stannous chloride and titrated with standardized potassium dichromate.
4.2.3 The ash and total iron contributed by a sample bag alone are determined separately and are subtracted from the values of
bag and sample to obtain the values for the sample alone.
NOTE 1—There are a number of alternative methods available for determining total iron in an ashed solution such as Test Methods D2795 and D1068.
5. Significance and Use
5.1 The life cycle and cleanlin
...

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