ASTM D4042-93(2003)e1
(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 2003)
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 D 4042; 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.
´ NOTE—Warning notes were editorially moved into the standard text in June 2003.
1. Scope nonhomogeneous dispersions of rolling mill oils in water from
an operating mill coolant system.
1.1 This test method describes a procedure for sampling and
3.2 Thecollectedsampleanddisposablebagareanalyzedas
testing dispersions of rolling oils in water from operating steel
one for ash and total iron.
rolling mills for determination of ash and total iron content. Its
3.2.1 Ash content is determined gravimetrically by evapo-
purpose is to provide a test method such that a representative
rating all water from the sample bag before heating the residue
sample may be taken and phenomenon such as iron separation,
and bag in a muffle furnace to a constant weight (Test Method
fat-emulsion separation, and so forth, do not contribute to
D 482).
analytical error in determination of ash and total iron.
3.2.2 Total iron content is determined by digesting the iron
1.2 The values stated in SI units are to be regarded as the
in the ashed sample and bag in an acidified solution. The iron
standard. The values given in parentheses are for information
in the solution is reduced with stannous chloride and titrated
only.
with standardized potassium dichromate.
1.3 This standard does not purport to address all of the
3.2.3 The ash and total iron contributed by a sample bag
safety concerns, if any, associated with its use. It is the
alone are determined separately and are subtracted from the
responsibility of the user of this standard to establish appro-
values of bag and sample to obtain the values for the sample
priate safety and health practices and determine the applica-
alone.
bility of regulatory limitations prior to use. For specific
warning statements, see Sections 6 and 7.
NOTE 1—There are a number of alternative methods available for
determining total iron in an ashed solution such as Test Methods D 2795
2. Referenced Documents
and D 1068.
2.1 ASTM Standards:
4. Significance and Use
D 482 Test Method for Ash from Petroleum Products
4.1 The life cycle and cleanliness of a recirculating steel
D 1068 Test Methods for Iron in Water
mill rolling oil dispersion is affected by the amount of iron
D 1193 Specification for Reagent Water
present. This iron consists mainly of iron from acid pickling
D 2795 Test Method for Analysis of Coal and Coke Ash
residues and iron from attrition of the steel sheet or rolls during
E50 Practices forApparatus, Reagents, and Safety Consid-
cold rolling. In sampling rolling oils for total iron it is difficult
erations for Chemical Analysis of Metals, Ores, and
to prevent adherence of iron containing sludge to the sample
Related Materials
container.Thus, the accuracy of a total iron determination from
E 832 Specification for Laboratory Filter Papers
analiquotsampleissuspect.Thispracticeprovidesameansfor
3. Summary of Test Method
ensuring that all iron contained in a sample is included in the
analysis.
3.1 Polyethylene disposable sample bags in a suitable hold-
4.2 Although less significant, the ash content is still an
ing device are used to collect representative samples of
essential part of the procedure for obtaining a total iron
1 analysis. Generally, the ash will be mostly iron, and in many
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum
Products and Lubricants and is the direct responsibility of Subcommittee D02.L0 on cases,couldbeusedasasubstitutefortotalironindetermining
Industrial Lubricants (Joint ASTM-ASLE).
when to change the dispersion.
Current edition approved May 10, 2003. Published July 2003. Originally
approved in 1981. Last previous edition approved in 1998 as D 4042 – 93 (1998).
5. Sampling
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 11.01. 5.1 Apparatus:
Discontinued. See 2000 Annual Book of ASTM Standards, Vol 05.05.
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 14.04.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4042–93 (2003)
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
6.2.2 Remove the bagged sample from its carrier container
177 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—Ahockeystickorsimilarformedapparatusofsteel,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:
filter paper to the sample prior to ashing.
5.2.1 Weigh a number of identified sample bags on an
analytical balance to the nearest 0.1 mg. Record the weight of
NOTE 6—Filter paper should conform to Specification E 832, 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 b
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