ASTM D4042-93(2019)
(Test Method)Standard Test Method for Sampling and Testing for Ash and Total Iron in Steel Mill Dispersions of Rolling Oils
Standard Test Method for Sampling and Testing for Ash and Total Iron in Steel Mill Dispersions of Rolling Oils
SIGNIFICANCE AND USE
4.1 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.
4.2 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 6 and 7.
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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Buy Standard
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: D4042 − 93 (Reapproved 2019)
Standard Test Method for
Sampling and Testing for Ash and Total Iron in Steel Mill
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
(Withdrawn 2001)
1.1 This test method describes a procedure for sampling and
E50 Practices for Apparatus, Reagents, and Safety Consid-
testing dispersions of rolling oils in water from operating steel
erations for Chemical Analysis of Metals, Ores, and
rolling mills for determination of ash and total iron content. Its
Related Materials
purpose is to provide a test method such that a representative
E832 Specification for Laboratory Filter Papers
sample may be taken and phenomenon such as iron separation,
fat-emulsion separation, and so forth, do not contribute to
3. Summary of Test Method
analytical error in determination of ash and total iron.
3.1 Polyethylene disposable sample bags in a suitable hold-
1.2 The values stated in SI units are to be regarded as the
ing device are used to collect representative samples of
standard. The values given in parentheses are for information
nonhomogeneous dispersions of rolling mill oils in water from
only.
an operating mill coolant system.
1.3 This standard does not purport to address all of the
3.2 Thecollectedsampleanddisposablebagareanalyzedas
safety concerns, if any, associated with its use. It is the
one for ash and total iron.
responsibility of the user of this standard to establish appro-
3.2.1 Ash content is determined gravimetrically by evapo-
priate safety, health, and environmental practices and deter-
rating all water from the sample bag before heating the residue
mine the applicability of regulatory limitations prior to use.
and bag in a muffle furnace to a constant weight (Test Method
For specific warning statements, see Sections 6 and 7.
D482).
1.4 This international standard was developed in accor-
3.2.2 Total iron content is determined by digesting the iron
dance with internationally recognized principles on standard-
in the ashed sample and bag in an acidified solution. The iron
ization established in the Decision on Principles for the
in the solution is reduced with stannous chloride and titrated
Development of International Standards, Guides and Recom-
with standardized potassium dichromate.
mendations issued by the World Trade Organization Technical
3.2.3 The ash and total iron contributed by a sample bag
Barriers to Trade (TBT) Committee.
alone are determined separately and are subtracted from the
values of bag and sample to obtain the values for the sample
2. Referenced Documents
alone.
2.1 ASTM Standards:
NOTE 1—There are a number of alternative methods available for
determining total iron in an ashed solution such as Test Methods D2795
D482 Test Method for Ash from Petroleum Products
and D1068.
D1068 Test Methods for Iron in Water
D1193 Specification for Reagent Water
4. Significance and Use
4.1 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
This test method is under the jurisdiction of ASTM Committee D02 on
residues and iron from attrition of the steel sheet or rolls during
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
cold rolling. In sampling rolling oils for total iron it is difficult
Subcommittee D02.L0.04 on Metal Deformation Fluids and Lubricants.
to prevent adherence of iron containing sludge to the sample
Current edition approved Dec. 1, 2019. Published December 2019. Originally
approved in 1981. Last previous edition approved in 2014 as D4042 – 93 (2014). container.Thus,theaccuracyofatotalirondeterminationfrom
DOI: 10.1520/D4042-93R19.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4042 − 93 (2019)
analiquotsampleissuspect.Thispracticeprovidesameansfor 5.2.3 Tie and seal each sample with the wire provided in
ensuring that all iron contained in a sample is included in the another disposable plastic sampling bag 473 cm (16 oz) to
analysis. prevent loss of material in transit. Individual rigid plastic
bottles of suitable size are also satisfactory containers for
4.2 Although less significant, the ash content is still an
shipment and can be substituted for the outer 473 cm (16 oz)
essential part of the procedure for obtaining a total iron
plastic bag.
analysis. Generally, the ash will be mostly iron, and in many
5.2.4 Take extreme care not to soil the exterior of the
cases,couldbeusedasasubstitutefortotalironindetermining
sampling bag with the dispersion or any foreign material.
when to change the dispersion.
6. Ash Content
5. Sampling
6.1 Apparatus:
5.1 Apparatus:
6.1.1 Borosilicate-Glass Beaker, 400 mL, or Evaporating
5.1.1 Disposable Plastic (Polyethylene) Sampling
4 3 3
Dish, 350 mL, designed for ashing in an electric furnace. Do
Bags 177 cm and 473 cm (6 oz and 16 oz) complete with
not use platinum crucibles because of the tendency to alloy
closure wire.
with metallic iron.
5.1.2 Holding Fixture.
6.1.2 Electric Muffle Furnace, capable of maintaining a
NOTE 2—A plastic baby bottle holder with an open 177 cm (6 oz)
temperature of 775 °C 6 25 °C (1427 °F 6 45 °F), preferably
sampling bag inserted makes a suitable holder.
having suitable apertures at the front and rear that allow a slow
5.1.3 Sampling Cup and Handle.
natural draft of air to pass through.
NOTE 3—Ahockey stick or similar formed apparatus of steel, plastic, or 6.1.3 Oven, capable of maintaining a temperature of 105 °C
wood with or without a separate cup can be used to hold the holding
6 2 °C (221 °F 6 4 °F).
fixture or the fixture itself can be attached to the handle (see Fig. 1).
6.1.4 Analytical Balance, 200 g capacity, accurate to
5.2 Sampling Procedure:
0.1 mg.
5.2.1 Weigh a number of identified sample bags on an
6.1.5 Top-Loading Balance, 600 g minimum capacity, accu-
analytical balance to the nearest 0.1 mg. Record the weight of
rate to 0.01 g.
each as W .
B1
6.2 Procedure:
5.2.2 Using a different, preweighed, identified plastic dis-
6.2.1 Heat the empty beaker or evaporating dish at 700 °C
posable sampling bag for each sample, remove samples from
to 800 °C (1240 °F to 1470 °F) for 10 min or more. Cool at
the mill only while the coolant is circulating and the mill
roomtemperatureinasuitablecontainer(Note5)andweighon
running. Take samples from the same location between the
an analytical balance to the nearest 0.1 mg.
second and third stand whenever possible. Fill the bag approxi-
mately two thirds full to allow for tying of the bag.
NOTE 5—The container in which the beaker or evaporating dish is
cooled should not contain a desiccating agent.
NOTE 4—Occasionally, due to mill configuration or other reasons, it
may be advisable to obtain the sample from other points in the mill 6.2.2 Remove the bagged sample from its carrier container
system. If so, record complete details on location and time of sampling.
and place it, still tied, in the dish. Remove the wire and weigh
the bag with sample on a top loading balance to the nearest
0.01 g. Subtract the weight of the beaker or evaporating dish
and record the weight in grams as W .
S1
6.2.3 Place the beaker or dish, sample, and bag in an oven
Sampling bags (with wires) can be found in most common laboratory supply at 105 °C (221 °F) overnight or until the moisture has been
catalogues.
evaporated from the sample.
6.2.4 Cover the beaker or evaporating dish with ashless
filter paper (Note 6) to prevent loss due to spatter. Add this
filter paper to the sample prior to ashing.
NOTE 6—Filter paper should conform to Specification E832, Type II.
6.2.5 Place the beaker or evaporating dish containing the
dried sample, bag, and filter paper in the muffle furnace.
Carefully heat the beaker or evaporating dish and sample by
progressively advancing it into the muffle furnace where it will
eventually ignite.
6.2.5.1 Maintain at such a temperature that the sample
continues to burn at a uniform and moderate rate, leaving only
ash and carbon when burning ceases. (Warning—Fumes from
burning polyethylene are hazardous.)
6.2.6 Heat the residue in the muffle furnace at 775 °C 6
25 °C (1427 °F 6 45 °F) until all carbonaceous material has
FIG. 1 Possible Holding Fixture and Assembly System disappeared.
D4042 − 93 (2019)
6.2.7 Remove the dish and ashed sample from the furnace 7.2.2 Purity of Water—Unless otherwise indicated, refer-
and cool in a suitable container to room temperature.Weigh on ences to water shall be understood to mean reagent water as
a 200 g analytical balance to the nearest 0.1 mg. defined in Specification D1193, Type II.
6.2.8 Reheat the dish to 775 °C 6 25 °C (1427 °F 6 45 °F)
7.2.3 Hydrochloric Acid (HCL) (36 %). (Warning—
in the muffle furnace for 30 min, and cool to room temperature
Poison. Cau
...
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: D4042 − 93 (Reapproved 2019)
Standard Test Method for
Sampling and Testing for Ash and Total Iron in Steel Mill
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
(Withdrawn 2001)
1.1 This test method describes a procedure for sampling and
E50 Practices for Apparatus, Reagents, and Safety Consid-
testing dispersions of rolling oils in water from operating steel
erations for Chemical Analysis of Metals, Ores, and
rolling mills for determination of ash and total iron content. Its
Related Materials
purpose is to provide a test method such that a representative
E832 Specification for Laboratory Filter Papers
sample may be taken and phenomenon such as iron separation,
fat-emulsion separation, and so forth, do not contribute to
3. Summary of Test Method
analytical error in determination of ash and total iron.
3.1 Polyethylene disposable sample bags in a suitable hold-
1.2 The values stated in SI units are to be regarded as the
ing device are used to collect representative samples of
standard. The values given in parentheses are for information
nonhomogeneous dispersions of rolling mill oils in water from
only.
an operating mill coolant system.
1.3 This standard does not purport to address all of the
3.2 The collected sample and disposable bag are analyzed as
safety concerns, if any, associated with its use. It is the
one for ash and total iron.
responsibility of the user of this standard to establish appro-
3.2.1 Ash content is determined gravimetrically by evapo-
priate safety, health, and environmental practices and deter-
rating all water from the sample bag before heating the residue
mine the applicability of regulatory limitations prior to use.
and bag in a muffle furnace to a constant weight (Test Method
For specific warning statements, see Sections 6 and 7.
D482).
1.4 This international standard was developed in accor-
3.2.2 Total iron content is determined by digesting the iron
dance with internationally recognized principles on standard-
in the ashed sample and bag in an acidified solution. The iron
ization established in the Decision on Principles for the
in the solution is reduced with stannous chloride and titrated
Development of International Standards, Guides and Recom-
with standardized potassium dichromate.
mendations issued by the World Trade Organization Technical
3.2.3 The ash and total iron contributed by a sample bag
Barriers to Trade (TBT) Committee.
alone are determined separately and are subtracted from the
values of bag and sample to obtain the values for the sample
2. Referenced Documents
alone.
2.1 ASTM Standards:
NOTE 1—There are a number of alternative methods available for
D482 Test Method for Ash from Petroleum Products determining total iron in an ashed solution such as Test Methods D2795
and D1068.
D1068 Test Methods for Iron in Water
D1193 Specification for Reagent Water
4. Significance and Use
4.1 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
This test method is under the jurisdiction of ASTM Committee D02 on
residues and iron from attrition of the steel sheet or rolls during
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
cold rolling. In sampling rolling oils for total iron it is difficult
Subcommittee D02.L0.04 on Metal Deformation Fluids and Lubricants.
to prevent adherence of iron containing sludge to the sample
Current edition approved Dec. 1, 2019. Published December 2019. Originally
container. Thus, the accuracy of a total iron determination from
approved in 1981. Last previous edition approved in 2014 as D4042 – 93 (2014).
DOI: 10.1520/D4042-93R19.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4042 − 93 (2019)
an aliquot sample is suspect. This practice provides a means for 5.2.3 Tie and seal each sample with the wire provided in
ensuring that all iron contained in a sample is included in the another disposable plastic sampling bag 473 cm (16 oz) to
analysis. prevent loss of material in transit. Individual rigid plastic
bottles of suitable size are also satisfactory containers for
4.2 Although less significant, the ash content is still an
shipment and can be substituted for the outer 473 cm (16 oz)
essential part of the procedure for obtaining a total iron
plastic bag.
analysis. Generally, the ash will be mostly iron, and in many
5.2.4 Take extreme care not to soil the exterior of the
cases, could be used as a substitute for total iron in determining
sampling bag with the dispersion or any foreign material.
when to change the dispersion.
6. Ash Content
5. Sampling
6.1 Apparatus:
5.1 Apparatus:
6.1.1 Borosilicate-Glass Beaker, 400 mL, or Evaporating
5.1.1 Disposable Plastic (Polyethylene) Sampling
4 3 3
Dish, 350 mL, designed for ashing in an electric furnace. Do
Bags 177 cm and 473 cm (6 oz and 16 oz) complete with
not use platinum crucibles because of the tendency to alloy
closure wire.
with metallic iron.
5.1.2 Holding Fixture.
6.1.2 Electric Muffle Furnace, capable of maintaining a
NOTE 2—A plastic baby bottle holder with an open 177 cm (6 oz)
temperature of 775 °C 6 25 °C (1427 °F 6 45 °F), preferably
sampling bag inserted makes a suitable holder.
having suitable apertures at the front and rear that allow a slow
5.1.3 Sampling Cup and Handle.
natural draft of air to pass through.
NOTE 3—A hockey stick or similar formed apparatus of steel, plastic, or 6.1.3 Oven, capable of maintaining a temperature of 105 °C
wood with or without a separate cup can be used to hold the holding
6 2 °C (221 °F 6 4 °F).
fixture or the fixture itself can be attached to the handle (see Fig. 1).
6.1.4 Analytical Balance, 200 g capacity, accurate to
5.2 Sampling Procedure:
0.1 mg.
5.2.1 Weigh a number of identified sample bags on an
6.1.5 Top-Loading Balance, 600 g minimum capacity, accu-
analytical balance to the nearest 0.1 mg. Record the weight of
rate to 0.01 g.
each as W .
B1
6.2 Procedure:
5.2.2 Using a different, preweighed, identified plastic dis-
6.2.1 Heat the empty beaker or evaporating dish at 700 °C
posable sampling bag for each sample, remove samples from
to 800 °C (1240 °F to 1470 °F) for 10 min or more. Cool at
the mill only while the coolant is circulating and the mill
room temperature in a suitable container (Note 5) and weigh on
running. Take samples from the same location between the
an analytical balance to the nearest 0.1 mg.
second and third stand whenever possible. Fill the bag approxi-
mately two thirds full to allow for tying of the bag.
NOTE 5—The container in which the beaker or evaporating dish is
cooled should not contain a desiccating agent.
NOTE 4—Occasionally, due to mill configuration or other reasons, it
may be advisable to obtain the sample from other points in the mill 6.2.2 Remove the bagged sample from its carrier container
system. If so, record complete details on location and time of sampling.
and place it, still tied, in the dish. Remove the wire and weigh
the bag with sample on a top loading balance to the nearest
0.01 g. Subtract the weight of the beaker or evaporating dish
and record the weight in grams as W .
S1
6.2.3 Place the beaker or dish, sample, and bag in an oven
Sampling bags (with wires) can be found in most common laboratory supply at 105 °C (221 °F) overnight or until the moisture has been
catalogues.
evaporated from the sample.
6.2.4 Cover the beaker or evaporating dish with ashless
filter paper (Note 6) to prevent loss due to spatter. Add this
filter paper to the sample prior to ashing.
NOTE 6—Filter paper should conform to Specification E832, Type II.
6.2.5 Place the beaker or evaporating dish containing the
dried sample, bag, and filter paper in the muffle furnace.
Carefully heat the beaker or evaporating dish and sample by
progressively advancing it into the muffle furnace where it will
eventually ignite.
6.2.5.1 Maintain at such a temperature that the sample
continues to burn at a uniform and moderate rate, leaving only
ash and carbon when burning ceases. (Warning—Fumes from
burning polyethylene are hazardous.)
6.2.6 Heat the residue in the muffle furnace at 775 °C 6
25 °C (1427 °F 6 45 °F) until all carbonaceous material has
FIG. 1 Possible Holding Fixture and Assembly System disappeared.
D4042 − 93 (2019)
6.2.7 Remove the dish and ashed sample from the furnace 7.2.2 Purity of Water—Unless otherwise indicated, refer-
and cool in a suitable container to room temperature. Weigh on ences to water shall be understood to mean reagent water as
a 200 g analytical balance to the nearest 0.1 mg. defined in Specification D1193, Type II.
6.2.8 Reheat the dish to 775 °C 6 25 °C (1427 °F 6 45 °F)
7.2.3 Hydrochloric Acid (HCL) (36 %). (Warning—
in the muffle furnace for 30 min, and cool to room temperature
Poison. Causes severe burns. Harmful or fatal if swallowed or
in a suitable container and reweigh,
...
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 2014) D4042 − 93 (Reapproved 2019)
Standard Test Method for
Sampling and Testing for Ash and Total Iron in Steel Mill
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
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific warning statements, see Sections 6 and 7.
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
2.1 ASTM Standards:
D482 Test Method for Ash from Petroleum Products
D1068 Test Methods for Iron in Water
D1193 Specification for Reagent Water
D2795 Test Methods for Analysis of Coal and Coke Ash (Withdrawn 2001)
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E832 Specification for Laboratory Filter Papers
3. Summary of Test Method
3.1 Polyethylene disposable sample bags in a suitable holding device are used to collect representative samples of
nonhomogeneous dispersions of rolling mill oils in water from an operating mill coolant system.
3.2 The collected sample and disposable bag are analyzed as one for ash and total iron.
3.2.1 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).
3.2.2 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.
3.2.3 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.
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 May 1, 2014Dec. 1, 2019. Published July 2014December 2019. Originally approved in 1981. Last previous edition approved in 20092014 as
D4042 – 93 (2009).(2014). DOI: 10.1520/D4042-93R14.10.1520/D4042-93R19.
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.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4042 − 93 (2019)
4. Significance and Use
4.1 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.
4.2 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.
5. Sampling
5.1 Apparatus:
4 3 3
5.1.1 Disposable Plastic (Polyethylene) Sampling Bags 177 and 473 cm177 cm (6 and 16473 cm oz) (6 oz and 16 oz)
complete with closure wire.
5.1.2 Holding Fixture.
NOTE 2—A plastic baby bottle holder with an open 177-cm177 cm (6-oz)(6 oz) sampling bag inserted makes a suitable holder.
5.1.3 Sampling Cup and Handle.
NOTE 3—A hockey stick or similar formed apparatus of steel, plastic, or wood with or without a separate cup can be used to hold the holding fixture
or the fixture itself can be attached to the handle (see Fig. 1).
5.2 Sampling Procedure:
5.2.1 Weigh a number of identified sample bags on an analytical balance to the nearest 0.1 mg. Record the weight of each as
W .
B1
5.2.2 Using a different, preweighed, identified plastic disposable sampling bag for each sample, remove samples from the mill
only while the coolant is circulating and the mill running. Take samples from the same location between the second and third stand
whenever possible. Fill the bag approximately two thirds full to allow for tying of the bag.
NOTE 4—Occasionally, due to mill configuration or other reasons, it may be advisable to obtain the sample from other points in the mill system. If
so, record complete details on location and time of sampling.
5.2.3 Tie and seal each sample with the wire provided in another disposable plastic sampling bag 473 cm473 cm (16 oz) (16 oz)
to prevent loss of material in transit. Individual rigid plastic bottles of suitable size are also satisfactory containers for shipment
and can be substituted for the outer 473-cm473 cm (16-oz)(16 oz) plastic bag.
5.2.4 Take extreme care not to soil the exterior of the sampling bag with the dispersion or any foreign material.
6. Ash Content
6.1 Apparatus:
6.1.1 Borosilicate-Glass Beaker, 400-mL,400 mL, or Evaporating Dish, 350-mL,350 mL, designed for ashing in an electric
furnace. Do not use platinum crucibles because of the tendency to alloy with metallic iron.
FIG. 1 Possible Holding Fixture and Assembly System
Sampling bags (with wires) can be found in most common laboratory supply catalogues.
D4042 − 93 (2019)
6.1.2 Electric Muffle Furnace, capable of maintaining a temperature of 775775 °C 6 25°C (142725 °C (1427 °F 6
45°F),45 °F), preferably having suitable apertures at the front and rear that allow a slow natural draft of air to pass through.
6.1.3 Oven, capable of maintaining a temperature of 105105 °C 6 2°C (2212 °C (221 °F 6 4°F).4 °F).
6.1.4 Analytical Balance, 200-g200 g capacity, accurate to 0.1 mg.
6.1.5 Top-Loading Balance, 600-g600 g minimum capacity, accurate to 0.01 g.0.01 g.
6.2 Procedure:
6.2.1 Heat the empty beaker or evaporating dish at 700700 °C to 800°C (1240800 °C (1240 °F to 1470°F)1470 °F) for 10 min
or more. Cool at room temperature in a suitable container (Note 5) and weigh on an analytical balance to the nearest 0.1 mg.
NOTE 5—The container in which the beaker or evaporating dish is cooled should not contain a desiccating agent.
6.2.2 Remove the bagged sample from its carrier container and place it, still tied, in the dish. Remove the wire and weigh the
bag with sample on a top loading balance to the nearest 0.01 g. Subtract the weight of the beaker or evaporating dish and record
the weight in grams as W .
S1
6.2.3 Place the beaker or dish, sample, and bag in an oven at 105°C (221°F)105 °C (221 °F) overnight or until the moisture has
been evaporated from the sample.
6.2.4 Cover the beaker or evaporating dish with ashless filter paper (Note 6) to prevent loss due to spatter. Add this filter paper
to the sample prior to ashing.
NOTE 6—Filter paper should conform to Specification E832, Type II.
6.2.5 Place the beaker or evaporating dish containing the dried sample, bag, and filter paper in the muffle furnace. Carefully heat
the beaker or evaporating dish and sample by progressively advancing it into the muffle furnace where it will eventually ignite.
6.2.5.1 Maintain at such a temperature that the sample continues to burn at a uniform and moderate rate, leaving only ash and
carbon when burning ceases. (Warning—Fumes from burning polyethylene are hazardous.)
6.2.6 Heat the residue in the muffle furnace at 775775 °C 6 25°C (142725 °C (1427 °F 6 45°F)45 °F) until all carbonaceous
material has disappeared.
6.2.7 Remove the dish and ashed sample from the furnace and cool in a suitable container to room temperature. Weigh on a
200-g200 g analytical balance to the nearest 0.1 mg.
6.2.8 Reheat the dish to 775775 °C 6 25°C (142725 °C (1427 °F 6 45°F)45 °F) in the muffle furnace for 30 min, and cool to
room temperature in a suitable container and reweigh, as in 6.2.6. Repeat the heating, cooling, and weighing until consecutive
weighings differ
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