Standard Test Method for Weight Loss (Mass Loss) of Sheet Steel During Immersion in Sulfuric Acid Solution

SCOPE
1.1 This test method covers the evaluation of the weight-loss (mass loss) characteristics of sheet steel in sulfuric acid solution.
1.2 This test method provides means of rating the effectiveness of in-plant pretreatment acid solutions in preparing steel surfaces for porcelain enameling.
1.3 The values stated in inch-pound units are to be regarded as the standard. The values in parentheses are for information only.
1.4 This standard does not purport to address the safety problems 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.

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ASTM C694-90a(1995) - Standard Test Method for Weight Loss (Mass Loss) of Sheet Steel During Immersion in Sulfuric Acid Solution
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: C 694 – 90a (Reapproved 1995)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Weight Loss (Mass Loss) of Sheet Steel During Immersion
in Sulfuric Acid Solution
This standard is issued under the fixed designation C 694; 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.
INTRODUCTION
In the manufacture of porcelain-enameled ware, formed steel articles are pretreated to ensure
enamel adherence. The pretreatment comprises, in part, of etching the steel surface with sulfuric acid
solution and in depositing nickel on the steel surface from a nickelous sulfate solution. Conditions are
maintained to provide a minimum amount of metal removal (weight loss) (mass loss) in the acid
solution and a minimum amount of nickel deposition. These minimums are particularly critical in
direct-on enameling in which the ground-coat enamel with its adherence-promoting oxides is omitted.
1. Scope calculated for the four acid immersion periods and, if desired,
the rate of weight loss (mass loss) per unit area per unit time is
1.1 This test method covers the evaluation of the weight-
calculated.
loss (mass loss) characteristics of sheet steel in sulfuric acid
solution.
4. Significance and Use
1.2 This test method provides means of rating the effective-
4.1 The results of this test method can be used to evaluate
ness of in-plant pretreatment acid solutions in preparing steel
the pickle weight-loss (mass loss) characteristics of a given lot
surfaces for porcelain enameling.
of sheet steel in dilute sulfuric acid solution, and may enable
1.3 The values stated in inch-pound units are to be regarded
the enamel processor to select a pickling time that will provide
as the standard. The values in parentheses are for information
satisfactory porcelain enamel bond.
only.
4.2 The results of this test method can be used to evaluate
1.4 This standard does not purport to address all of the
the effectiveness of the enamel processor’s pretreatment sys-
safety concerns, if any, associated with its use. It is the
tem in preparing the steel for porcelain enameling, and may aid
responsibility of the user of this standard to establish appro-
the processor in obtaining satisfactory porcelain enamel bond.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Apparatus
2. Terminology 5.1 Analytical Balance, accurate to 0.01 g.
5.2 Linear Measuring Device.
2.1 Definitions:
5.3 Borosilicate Glass Container, having an inside diameter
2.1.1 quarter lines—imaginary lines parallel to the direction
of about 11 ⁄2 in. (290 mm) and an outside depth of about 11 in.
of rolling, positioned at a distance from the sheet mill edge
(280 mm).
equal to one quarter of the sheet width.
5.4 Water Bath, heated, of sufficient size to immerse the
3. Summary of Test Method glass container (5.3) to within about 1 in. (25 mm) of its top.
5.5 Glass Plate or Acid-Resistant Porcelain-Enameled Steel
3.1 Representative sheet-steel specimens are selected, mea-
Sheet, sufficient to cover the container described in 5.3.
sured, cleaned, and weighed prior to immersion for measured
5.6 Stainless Steel Jig, for support of test specimens (see
periods in a bath of dilute sulfuric acid that has been precon-
Fig. 1, Fig. 2, and Fig. 3).
ditioned by controlled solution of panels of the same sheet
steel. The specimens are rinsed, dried, and reweighed after the
6. Reagents and Materials
timed exposure.
6.1 Distilled Water.
3.2 Values of weight loss (mass loss) per unit area are
6.2 Isopropyl Alcohol ((CH ) CHOH).
3 2
6.3 Methyl Alcohol (CH OH).
This test method is under the jurisdiction of ASTM Committee B-8 on Metallic
6.4 Steel Sheet, sufficient in size to provide the panels and
and Inorganic Coatings and is the direct responsibility of Subcommittee B08.12 on
strips described in 6.4.1 and 6.4.2, and to provide the test
Materials for Porcelain Enamel and Ceramic-Metal Systems.
Current edition approved July 27, 1990. Published December 1990. Originally
specimens described in 7.1 and 7.1.1.
published as C 694 – 71 T. Last previous edition C 694 – 90.
C 694
Metric Equivalents
in. ⁄4 45 6
(mm) (6) (102) (127) (127)
NOTE 1—All materials are of Type 316 stainless steel.
FIG. 1 Specimens Suspended from Stainless-Steel Jig
6.4.1 Shear two to four 4 by 6-in. (102 by 152-mm) panels (Thereafter, handle the specimens by the edges with clean
from the steel sheet of 6.4. Use these panels in the precondi- white gloves.)
tioning in accordance with 9.3.3 and 9.3.4. 8.1.4 Dry in still air.
6.4.2 Shear ten to twelve ⁄4 by 5-in. (6 by 127-mm) strips 8.1.5 Store the specimens in a desiccator until ready for
from the steel sheet of 6.4. Fashion these strips into hooks for weighing.
hanging test specimens from the stainless steel jig. 8.2 Determine the initial weight (mass), W , of each test
6.5 Sulfuric Acid (H SO ), American Chemical Society specimen to the nearest 0.01 g.
2 4
(ACS) reagent grade. 8.2.1 Store the specimens in a desiccator until ready to run
6.6 Trisodium Phosphate—(Na PO ·12H O), granular, the test.
3 4 2
technical grade.
9. Preparation of Solutions
7. Sampling
9.1 Cleaner—Prepare at least 19 L of 5 6 0.5 weight (mass)
percent solution using 53 g of trisodium phosphate per litre of
7.1 Shear eight test specimens, each 4 by 6 in. (102 by 152
mm), from within the quarter lines of the sheet or coil. tap water.
9.1.1 Control the cleaner temperature at 190 to 195°F (88 to
7.1.1 Choose specimens from rust-free areas that do not
contain the mill identification stamp. 91°C).
9.2 Cleaner Rinse—At least 19 L of tap water.
7.1.2 Identify the specimens by steel die stamping.
9.2.1 Control the rinse temperature at 170 6 5°F (77 6
8. Test Specimens
3°C).
8.1 File edges of the eight test specimens lightly to remove 9.3 Sulfuric Acid Solution—Add 76
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