ASTM C694-90a(2006)
(Test Method)Standard Test Method for Weight Loss (Mass Loss) of Sheet Steel During Immersion in Sulfuric Acid Solution
Standard Test Method for Weight Loss (Mass Loss) of Sheet Steel During Immersion in Sulfuric Acid Solution
SIGNIFICANCE AND USE
The results of this test method can be used to evaluate the pickle weight-loss (mass loss) characteristics of a given lot of sheet steel in dilute sulfuric acid solution, and may enable the enamel processor to select a pickling time that will provide satisfactory porcelain enamel bond.
The results of this test method can be used to evaluate the effectiveness of the enamel processor’pretreatment system in preparing the steel for porcelain enameling, and may aid the processor in obtaining satisfactory porcelain enamel bond.
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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Designation:C694–90a(Reapproved 2006)
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 C694; 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.
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 periods in a bath of dilute sulfuric acid that has been precon-
ditioned by controlled solution of panels of the same sheet
1.1 This test method covers the evaluation of the weight-
steel. The specimens are rinsed, dried, and reweighed after the
loss (mass loss) characteristics of sheet steel in sulfuric acid
timed exposure.
solution.
3.2 Values of weight loss (mass loss) per unit area are
1.2 This test method provides means of rating the effective-
calculated for the four acid immersion periods and, if desired,
ness of in-plant pretreatment acid solutions in preparing steel
the rate of weight loss (mass loss) per unit area per unit time is
surfaces for porcelain enameling.
calculated.
1.3 The values stated in inch-pound units are to be regarded
as the standard. The values in parentheses are for information
4. Significance and Use
only.
4.1 The results of this test method can be used to evaluate
1.4 This standard does not purport to address all of the
the pickle weight-loss (mass loss) characteristics of a given lot
safety concerns, if any, associated with its use. It is the
of sheet steel in dilute sulfuric acid solution, and may enable
responsibility of the user of this standard to establish appro-
the enamel processor to select a pickling time that will provide
priate safety and health practices and determine the applica-
satisfactory porcelain enamel bond.
bility of regulatory limitations prior to use.
4.2 The results of this test method can be used to evaluate
2. Terminology the effectiveness of the enamel processor’s pretreatment sys-
tem in preparing the steel for porcelain enameling, and may aid
2.1 Definitions:
the processor in obtaining satisfactory porcelain enamel bond.
2.1.1 quarter lines—imaginarylinesparalleltothedirection
of rolling, positioned at a distance from the sheet mill edge
5. Apparatus
equal to one quarter of the sheet width.
5.1 Analytical Balance, accurate to 0.01 g.
3. Summary of Test Method 5.2 Linear Measuring Device.
5.3 Borosilicate Glass Container, having an inside diameter
3.1 Representative sheet-steel specimens are selected, mea-
of about 11 ⁄2 in. (290 mm) and an outside depth of about 11 in.
sured, cleaned, and weighed prior to immersion for measured
(280 mm).
5.4 Water Bath, heated, of sufficient size to immerse the
This test method is under the jurisdiction ofASTM Committee B08 on Metallic
glass container (5.3) to within about 1 in. (25 mm) of its top.
and Inorganic Coatings and is the direct responsibility of Subcommittee B08.12 on
5.5 Glass Plate or Acid-Resistant Porcelain-Enameled Steel
Materials for Porcelain Enamel and Ceramic-Metal Systems.
Sheet, sufficient to cover the container described in 5.3.
Current edition approved April 1, 2006. Published April 2006. Originally
approved in 1971. Last previous edition approved in 2000 as C694 – 90a (2000).
DOI: 10.1520/C0694-90AR06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C694–90a (2006)
5.6 Stainless Steel Jig, for support of test specimens (see 7.1.2 Identify the specimens by steel die stamping.
Fig. 1, Fig. 2, and Fig. 3).
8. Test Specimens
6. Reagents and Materials
8.1 File edges of the eight test specimens lightly to remove
6.1 Distilled Water. shearing burrs.
6.2 Isopropyl Alcohol ((CH ) CHOH). 8.1.1 Punch or drill a hole near one end, at the center of the
3 2
6.3 Methyl Alcohol (CH OH). specimen width.
6.4 Steel Sheet, sufficient in size to provide the panels and 8.1.2 Determine the width, W, and length, L, of the test
strips described in 6.4.1 and 6.4.2, and to provide the test specimens to the nearest 0.01 in. (nearest 1 mm).
specimens described in 7.1 and 7.1.1. 8.1.3 Thoroughly clean the specimens with methyl alcohol.
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 Lof 5 6 0.5 weight (mass)
7.1 Shear eight test specimens, each 4 by 6 in. (102 by 152 percent solution using 53 g of trisodium phosphate per litre of
mm), from within the quarter lines of the sheet or coil. tap water.
7.1.1 Choose specimens from rust-free areas that do not 9.1.1 Control the cleaner temperature at 190 to 195°F (88 to
contain the mill identification stamp. 91°C).
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
...
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