ASTM D4042-93(1998)
(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
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, etc., 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 hazard statements, see Notes 7, 10, 12, 13, and 14.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
An American National Standard
Designation:D4042–93(Reapproved 1998)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.2 Thecollectedsampleanddisposablebagareanalyzedas
one for ash and total iron.
1.1 This test method describes a procedure for sampling and
3.2.1 Ash content is determined gravimetrically by evapo-
testing dispersions of rolling oils in water from operating steel
rating all water from the sample bag before heating the residue
rolling mills for determination of ash and total iron content. Its
and bag in a muffle furnace to a constant weight (Test Method
purpose is to provide a test method such that a representative
D 482).
sample may be taken and phenomenon such as iron separation,
3.2.2 Total iron content is determined by digesting the iron
fat-emulsion separation, and so forth, do not contribute to
in the ashed sample and bag in an acidified solution. The iron
analytical error in determination of ash and total iron.
in the solution is reduced with stannous chloride and titrated
1.2 The values stated in SI units are to be regarded as the
with standardized potassium dichromate.
standard. The values given in parentheses are for information
3.2.3 The ash and total iron contributed by a sample bag
only.
alone are determined separately and are subtracted from the
1.3 This standard does not purport to address all of the
values of bag and sample to obtain the values for the sample
safety concerns, if any, associated with its use. It is the
alone.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
NOTE 1—There are a number of alternative methods available for
bility of regulatory limitations prior to use. For specific hazard
determining total iron in an ashed solution such as Test Methods D 2795
and D 1068.
statements, see Note 7, Note 10, Note 12, Note 13, and Note
14.
4. Significance and Use
2. Referenced Documents
4.1 The life cycle and cleanliness of a recirculating steel
mill rolling oil dispersion is affected by the amount of iron
2.1 ASTM Standards:
present. This iron consists mainly of iron from acid pickling
D 482 Test Method for Ash from Petroleum Products
residues and iron from attrition of the steel sheet or rolls during
D 1068 Test Methods for Iron in Water
cold rolling. In sampling rolling oils for total iron it is difficult
D 1193 Specification for Reagent Water
to prevent adherence of iron containing sludge to the sample
D 2795 Test Method for Analysis of Coal and Coke Ash
container.Thus, the accuracy of a total iron determination from
E 50 Practices for Apparatus, Reagents, and Safety Precau-
analiquotsampleissuspect.Thispracticeprovidesameansfor
tions for Chemical Analysis of Metals
ensuring that all iron contained in a sample is included in the
E 832 Specification for Laboratory Filter Papers
analysis.
3. Summary of Test Method
4.2 Although less significant, the ash content is still an
essential part of the procedure for obtaining a total iron
3.1 Polyethylene disposable sample bags in a suitable hold-
analysis. Generally, the ash will be mostly iron, and in many
ing device are used to collect representative samples of
cases,couldbeusedasasubstitutefortotalironindetermining
nonhomogeneous dispersions of rolling mill oils in water from
when to change the dispersion.
an operating mill coolant system.
5. Sampling
This practice is under the jurisdiction of ASTM Committee D-2 on Petroleum
5.1 Apparatus:
Products and Lubricants and is the direct responsibility of Subcommittee D02.L on
5.1.1 Disposable Plastic (Polyethylene) Sampling Bags
Industrial Lubricants (Joint ASTM-ASLE).
Current edition approved June 15, 1993. Published June 1995. Originally
177 and 473 cm (6 and 16 oz) complete with closure wire.
published as D 4042 – 81. Last previous edition D 4042 – 87.
5.1.2 Holding Fixture.
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 05.05.
5 7
Annual Book of ASTM Standards, Vol 03.05. Sampling bags (with wires) can be found in most common laboratory supply
Annual Book of ASTM Standards, Vol 14.02. catalogues.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D4042
NOTE 2—A plastic baby bottle holder with an open 177-cm (6-oz)
6.1.4 Analytical Balance, 200-g capacity, accurate to 0.1
sampling bag inserted makes a suitable holder.
mg.
5.1.3 Sampling Cup and Handle. 6.1.5 Top-Loading Balance, 600-g minimum capacity, ac-
curate to 0.01 g.
NOTE 3—Ahockeystickorsimilarformedapparatusofsteel,plastic,or
6.2 Procedure:
wood with or without a separate cup can be used to hold the holding
6.2.1 Heat the empty beaker or evaporating dish at 700 to
fixture or the fixture itself can be attached to the handle (see Fig. 1).
800°C (1240 to 1470°F) for 10 min or more. Cool at room
5.2 Sampling Procedure:
temperature in a suitable container (Note 5) and weigh on an
5.2.1 Weigh a number of identified sample bags on an
analytical balance to the nearest 0.1 mg.
analytical balance to the nearest 0.1 mg. Record the weight of
each as W .
B1 NOTE 5—The container in which the beaker or evaporating dish is
5.2.2 Using a different, preweighed, identified plastic dis- cooled should not contain a desiccating agent.
posable sampling bag for each sample, remove samples from
6.2.2 Remove the bagged sample from its carrier container
the mill only while the coolant is circulating and the mill
and place it, still tied, in the dish. Remove the wire and weigh
running. Take samples from the same location between the
the bag with sample on a top loading balance to the nearest
second and third stand whenever possible. Fill the bag approxi-
0.01 g. Subtract the weight of the beaker or evaporating dish
mately two thirds full to allow for tying of the bag.
and record the weight in grams as W .
S1
NOTE 4—Occasionally, due to mill configuration or other reasons, it
6.2.3 Place the beaker or dish, sample, and bag in an oven
may be advisable to obtain the sample from other points in the mill
at 105°C (221°F) overnight or until the moisture has been
system. If so, record complete details on location and time of sampling.
evaporated from the sample.
5.2.3 Tie and seal each sample with the wire provided in
6.2.4 Cover the beaker or evaporating dish with ashless
another disposable plastic sampling bag 473 cm (16 oz) to
filter paper (Note 6) to prevent loss due to spatter. Add this
prevent loss of material in transit. Individual rigid plastic
filter paper to the sample prior to ashing.
bottles of suitable size are also satisfactory containers for
NOTE 6—Filter paper should conform to Specification E 832, Type II.
shipment and can be substituted for the outer 473-cm (16-oz)
plastic bag.
6.2.5 Place the beaker or evaporating dish containing the
5.2.4 Take extreme care not to soil the exterior of the
dried sample, bag, and filter paper in the muffle furnace.
sampling bag with the dispersion or any foreign material.
Carefully heat the beaker or evaporating dish and sample by
progressively advancing it into the muffle furnace where it will
6. Ash Content
eventually ignite.
6.1 Apparatus: 6.2.5.1 Maintain at such a temperature that the sample
6.1.1 Borosilicate-Glass Beaker, 400-mL, or Evaporating
continues to burn at a uniform and moderate rate, leaving only
Dish, 350-mL, designed for ashing in an electric furnace. Do ash and carbon when burning ceases.
not use platinum crucibles because of the tendency to alloy
NOTE 7—Warning: Fumes from burning polyethylene are hazardous.
with metallic iron.
6.1.2 Electric Muffle Furnace, capable of maintaining a 6.2.6 Heat the residue in the muffle furnace at 775 6 25°C
temperature of 775 6 25°C (14276 45°F), preferably having
(1427 645°F)untilallcarbonaceousmaterialhasdisappeared.
suitable apertures at the front and rear that allow a slow natural
6.2.7 Remove the dish and ashed sample from the furnace
draft of air to pass through.
and cool in a suitable container to room temperature.Weigh on
6.1.3 Oven, capable of maintaining a temperature of 105 6
a 200-g analytical balance to the nearest 0.1 mg.
2°C (221 6 4°F).
6.2.8 Reheat the dish to 775 6 25°C (14276 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 of the evaporating dish (6.2.1) and
record the final ash weight as W .
S2
6.2.10 Place a new, empty polyethylene bag trimmed to the
weight of the original sample bag 60.01 g (5.2.2) in a
preweighed evaporating dish (6.2.1) and reduce to ash follow-
ing the procedure described by 6.2.4, 6.2.5, 6.2.6, 6.2.
...
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