ASTM D4042-93(2009)
(Test Method)Test Method for Sampling and Testing for Ash and Total Iron in Steel Mill Dispersions of Rolling Oils
Test Method for Sampling and Testing for Ash and Total Iron in Steel Mill Dispersions of Rolling Oils
SIGNIFICANCE AND USE
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.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Sections 6 and 7.
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Designation: D4042 − 93(Reapproved 2009)
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 3. Summary of Test Method
3.1 Polyethylene disposable sample bags in a suitable hold-
1.1 This test method describes a procedure for sampling and
ing device are used to collect representative samples of
testing dispersions of rolling oils in water from operating steel
nonhomogeneous dispersions of rolling mill oils in water from
rolling mills for determination of ash and total iron content. Its
an operating mill coolant system.
purpose is to provide a test method such that a representative
sample may be taken and phenomenon such as iron separation,
3.2 Thecollectedsampleanddisposablebagareanalyzedas
fat-emulsion separation, and so forth, do not contribute to
one for ash and total iron.
analytical error in determination of ash and total iron.
3.2.1 Ash content is determined gravimetrically by evapo-
rating all water from the sample bag before heating the residue
1.2 The values stated in SI units are to be regarded as the
and bag in a muffle furnace to a constant weight (Test Method
standard. The values given in parentheses are for information
D482).
only.
3.2.2 Total iron content is determined by digesting the iron
1.3 This standard does not purport to address all of the
in the ashed sample and bag in an acidified solution. The iron
safety concerns, if any, associated with its use. It is the
in the solution is reduced with stannous chloride and titrated
responsibility of the user of this standard to establish appro-
with standardized potassium dichromate.
priate safety and health practices and determine the applica-
3.2.3 The ash and total iron contributed by a sample bag
bility of regulatory limitations prior to use. For specific
alone are determined separately and are subtracted from the
warning statements, see Sections 6 and 7.
values of bag and sample to obtain the values for the sample
alone.
2. Referenced Documents
NOTE 1—There are a number of alternative methods available for
2.1 ASTM Standards: determining total iron in an ashed solution such as Test Methods D2795
and D1068.
D482 Test Method for Ash from Petroleum Products
D1068 Test Methods for Iron in Water
4. Significance and Use
D1193 Specification for Reagent Water
4.1 The life cycle and cleanliness of a recirculating steel
D2795 Test Methods for Analysis of Coal and Coke Ash
mill rolling oil dispersion is affected by the amount of iron
(Withdrawn 2001)
present. This iron consists mainly of iron from acid pickling
E50 Practices for Apparatus, Reagents, and Safety Consid-
residues and iron from attrition of the steel sheet or rolls during
erations for Chemical Analysis of Metals, Ores, and
cold rolling. In sampling rolling oils for total iron it is difficult
Related Materials
to prevent adherence of iron containing sludge to the sample
E832 Specification for Laboratory Filter Papers
container.Thus,theaccuracyofatotalirondeterminationfrom
analiquotsampleissuspect.Thispracticeprovidesameansfor
ensuring that all iron contained in a sample is included in the
This test method is under the jurisdiction of ASTM Committee D02 on
analysis.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.L0.04 on Metal Deformation Fluids and Lubricants.
4.2 Although less significant, the ash content is still an
Current edition approved April 15, 2009. Published July 2009. Originally
essential part of the procedure for obtaining a total iron
ϵ1
approved in 1981. Last previous edition approved in 2003 as D4042–93(2003) .
analysis. Generally, the ash will be mostly iron, and in many
DOI: 10.1520/D4042-93R09.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or cases,couldbeusedasasubstitutefortotalironindetermining
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
when to change the dispersion.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
5. Sampling
The last approved version of this historical standard is referenced on
www.astm.org. 5.1 Apparatus:
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4042 − 93 (2009)
6.1.2 Electric Muffle Furnace, capable of maintaining a
temperature of 775 6 25°C (1427 6 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 105 6
2°C (221 6 4°F).
6.1.4 Analytical Balance, 200-g capacity, accurate to 0.1
mg.
6.1.5 Top-Loading Balance, 600-g minimum capacity, ac-
curate to 0.01 g.
6.2 Procedure:
6.2.1 Heat the empty beaker or evaporating dish at 700 to
800°C (1240 to 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.
FIG. 1 Possible Holding Fixture and Assembly System
NOTE 5—The container in which the beaker or evaporating dish is
cooled should not contain a desiccating agent.
5.1.1 Disposable Plastic (Polyethylene) Sampling Bags 177
6.2.2 Remove the bagged sample from its carrier container
and 473 cm (6 and 16 oz) complete with closure wire.
and place it, still tied, in the dish. Remove the wire and weigh
5.1.2 Holding Fixture.
the bag with sample on a top loading balance to the nearest
NOTE 2—A plastic baby bottle holder with an open 177-cm (6-oz)
0.01 g. Subtract the weight of the beaker or evaporating dish
sampling bag inserted makes a suitable holder.
and record the weight in grams as W .
S1
5.1.3 Sampling Cup and Handle.
6.2.3 Place the beaker or dish, sample, and bag in an oven
at 105°C (221°F) overnight or until the moisture has been
NOTE 3—Ahockey stick or similar formed apparatus of steel, plastic, or
wood with or without a separate cup can be used to hold the holding evaporated from the sample.
fixture or the fixture itself can be attached to the handle (see Fig. 1).
6.2.4 Cover the beaker or evaporating dish with ashless
filter paper (Note 6) to prevent loss due to spatter. Add this
5.2 Sampling Procedure:
5.2.1 Weigh a number of identified sample bags on an filter paper to the sample prior to ashing.
analytical balance to the nearest 0.1 mg. Record the weight of
NOTE 6—Filter paper should conform to Specification E832, Type II.
each as W .
B1
6.2.5 Place the beaker or evaporating dish containing the
5.2.2 Using a different, preweighed, identified plastic dis-
dried sample, bag, and filter paper in the muffle furnace.
posable sampling bag for each sample, remove samples from
Carefully heat the beaker or evaporating dish and sample by
the mill only while the coolant is circulating and the mill
progressively advancing it into the muffle furnace where it will
running. Take samples from the same location between the
eventually ignite.
second and third stand whenever possible. Fill the bag approxi-
6.2.5.1 Maintain at such a temperature that the sample
mately two thirds full to allow for tying of the bag.
continues to burn at a uniform and moderate rate, leaving only
NOTE 4—Occasionally, due to mill configuration or other reasons, it
ash and carbon when burning ceases. (Warning—Fumes from
may be advisable to obtain the sample from other points in the mill
burning polyethylene are hazardous.)
system. If so, record complete details on location and time of sampling.
6.2.6 Heat the residue in the muffle furnace at 775 6 25°C
5.2.3 Tie and seal each sample with the wire provided in
(1427 645°F)untilallcarbonaceousmaterialhasdisappeared.
another disposable plastic sampling bag 473 cm (16 oz) to
6.2.7 Remove the dish and ashed sample from the furnace
prevent loss of material in transit. Individual rigid plastic
and cool in a suitable container to room temperature.Weigh on
bottles of suitable size are also satisfactory containers for
a 200-g analytical balance to the nearest 0.1 mg.
shipment and can be substituted for the outer 473-cm (16-oz)
6.2.8 Reheat the dish to 775 6 25°C (1427 6 45°F) in the
plastic bag.
muffle furnace for 30 min, and cool to room temperature in a
5.2.4 Take extreme care not to soil the exterior of the
suitable container and reweigh, as in 6.2.6. Repeat the heating,
sampling bag with the dispersion or any foreign material.
cooling, and weighing until consecutive weighings differ by
not more than 0.5 mg.
6. Ash Content
6.2.9 Subtract the weight of the evaporating dish (6.2.1) and
6.1 Apparatus:
record the final ash weight as W .
S2
6.1.1 Borosilicate-Glass Beaker, 400-mL, or Evaporating
6.2.10 Place a new, empty polyethylene bag trimmed to the
Dish, 350-mL, designed for ashing in an electric furnace. Do
weight of the original sample bag 60.01 g (5.2.2)ina
not use platinum crucibles because of the tendency to alloy
preweighed evaporating dish (6.2.1) and reduce to ash follow-
with metallic iron.
ing the procedure described by 6.2.4, 6.2.5, 6.2.6, 6.2.7, and
6.2.8.
6.2.11 Record the final ash weight in grams to the nearest
Sampling bags (with wires) can be found in most com
...
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:D 4042–93 (Reapproved 2003)
Test Method for Designation:D4042–93 (Reapproved 2009)
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
superscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval. ´ NOTE—Warningnoteswereeditoriallymoved
into the standard text in June 2003.
1. Scope
1.1 This test method describes a procedure for sampling and testing dispersions of rolling oils in water from operating steel
rollingmillsfordeterminationofashandtotalironcontent.Itspurposeistoprovideatestmethodsuchthatarepresentativesample
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific warning statements, see Sections 6 and 7.
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
E50 PracticesforApparatus,Reagents,andSafetyConsiderationsforChemicalAnalysisofMetals,Ores,andRelatedMaterials
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 D 482D482).
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 D 2795 and D
1068D2795 and D1068.
This practice test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.L0 on Industrial Lubricants (Joint ASTM-ASLE).
Current edition approved May 10, 2003. Published July 2003. Originally approved in 1981. Last previous edition approved in 1998 as D 4042–93 (1998).on Petroleum
Products and Lubricants and is the direct responsibility of Subcommittee D02.L0.04 on Metal Deformation Fluids and Lubricants.
´1
Current edition approved April 15, 2009. Published July 2009. Originally approved in 1981. Last previous edition approved in 2003 as D4042–93(2003) . DOI:
10.1520/D4042-93R09.
Annual Book of ASTM Standards, Vol 05.01.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4042–93 (2009)
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,theashwillbemostlyiron,andinmanycases,couldbeusedasasubstitutefortotalironindeterminingwhentochange
the dispersion.
5. Sampling
5.1 Apparatus:
5.1.1 Disposable Plastic (Polyethylene) Sampling Bags 177 and 473 cm (6 and 16 oz) complete with closure wire.
5.1.2 Holding Fixture.
NOTE 2—A plastic baby bottle holder with an open 177-cm (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 .
B 1
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 cm (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-cm (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, or Evaporating Dish, 350-mL, designed for ashing in an electric furnace. Do not use
platinum crucibles because of the tendency to alloy with metallic iron.
Annual Book of ASTM Standards, Vol 11.01.
Sampling bags (with wires) can be found in most common laboratory supply catalogues.
FIG. 1 Possible Holding Fixture and Assembly System
D4042–93 (2009)
6.1.2 Electric Muffle Furnace, capable of maintaining a temperature of 775 6 25°C (1427 6 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 105 6 2°C (221 6 4°F).
6.1.4 Analytical Balance, 200-g capacity, accurate to 0.1 mg.
6.1.5 Top-Loading Balance, 600-g minimum capacity, accurate to 0.01 g.
6.2 Procedure:
6.2.1 Heattheemptybeakerorevaporatingdishat700to800°C(1240to1470°F)for10minormore.Coolatroomtemperature
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) 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 E 832E832, Type II.
6.2.5 Placethebeakerorevaporatingdishcontainingthedriedsample,bag,andfilterpaperinthemufflefurnace.Carefullyheat
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 6 25°C (1427 6 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-g analytical balance to the nearest 0.1 mg.
6.2.8 Reheat the dish to 775 6 25°C (1427 6 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 by not more than
0.5 mg.
6.2.9 Subtract the weight o
...
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