Reagents of the American Chemical Society.
4
Other grades
may be used, provided it is first ascertained that the reagent is
of sufficiently high purity to permit its use without lessening
the accuracy of the determination.
5.2 Purity of Water—Use distilled or deionized water.
5.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
monium hydroxide (NH
4
OH).
5.4 Ammonium Persulfate—(NH
4
)
2
S
2
O
8
.
5.5 Dimethylglyoxime—Prepare a 1 % solution of dimethyl-
glyoxime in methyl alcohol or a 2.62 % solution of sodium
dimethylglyoximate in water (store in a polyethylene bottle).
5.6 Hydrochloric Acid (1+5)—Dilute 1 vol of concentrated
hydrochloric acid (HCl, sp gr 1.19) with 5 vol of water.
5.7 Nickel Sulfate, Standard Solution—Dissolve 0.448 g of
nickel sulfate (NiSO
4
·6H
2
O) in water. When the material is
completely dissolved, cautiously add 10 mL of concentrated
H
2
SO
4
and transfer the solution to the 1000-mL flask. When
cool, make up to the mark with water. One millilitre of this
standard solution is equivalent to 0.0001 g of nickel per
millilitre.
5.8 Nitric Acid (1+1)—Dilute 1 vol of concentrated nitric
acid (HNO
3
, sp gr 1.42) with 1 vol of water.
5.9 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
(H
2
SO
4
).
6. Sampling
6.1 Sampling frequency shall be consistent with the objec-
tive of control of the nickel dipping operation.
7. Standardization of Photoelectric Photometer
7.1 The photoelectric photometer shall be standardized as
follows:
7.1.1 Using a buret, accurately measure out 2, 4, 8, 12, 16,
and 20 mL portions of nickel sulfate standard solution. These
amounts are equivalent to 0.2, 0.4, 0.9, 1.3, 1.7, and 2.1 g of
nickel per square metre (0.02, 0.04, 0.08, 0.12, 0.16, and 0.20
g of nickel per square foot) of surface when specimens from
the steel surface are obtained as prescribed. (Iron in solution
that is dissolved from the steel surfaces has a negligible effect
on the nickel determinations.) Using the standard analytical
procedures described in 8.2, determine the percent transmis-
sion at a wavelength of approximately 525 nm for each of the
six increments of nickel sulfate standard solution. Then plot a
graph on appropriate graph paper of the percent light transmis-
sion against the known nickel concentration representing 0.2 to
2.1 g of nickel deposit per square metre of surface. The
resulting graph, which should be a straight line, will be used to
obtain nickel-coating masses from light transmission results.
8. Determinations of Nickel Coating Masses
8.1 Sampling a Nickel-Coated Steel Surface:
8.1.1 Place the weighted, rubber ring assembly on the
nickel-coated metal surface. Add 3 mL of warm (approxi-
mately 120°F (50°C)) HNO
3
(1+1). Allow the foaming reaction
to proceed for about 10 s for light nickel coatings and about 15
s for heavier nickel coatings. If the warm acid does not react,
scratch the steel surface or try another spot. After the acid has
foamed for the prescribed time, add 5 mL of HCl (1+5) to stop
the foaming reaction. Withdraw the solution from the steel
surface with the aspirator into the calibrated flask. Rinse the
test area twice with water and retain the washings in the flask.
8.1.2 Alternative methods for determining nickel are de-
scribed in Test Methods E30, Sections 62 to 70 for the
gravimetric method and Sections 71 to 73 for the volumetric
method.
8.2 Analytical Procedure:
8.2.1 Add chemicals in the order given below to the solution
in the flask and mix thoroughly after each addition:
Additions for 23-mm Optical
Path Cell
A
Amount in
Order of Use
Ammonium hydroxide (sp gr 0.90) 50 mL
Ammonium persulfate 4 g
Dimethylglyoxime 10 mL
Dilute with water to 500 mL
A
Cells with other optical path lengths are available.
8.2.2 Filter a portion of the solution. Discard the first 10 to
20 mL from the filter and collect a sufficient amount of filtrate
in the absorption cell for testing. Just before testing, set the
wavelength as determined in accordance with Section 7and
adjust the instrument to 100 % transmission with a cell that
contains only water. Place the cell containing the test solution
in the photometer and read the percent transmission.
9. Calculation and Report
9.1 Refer to the graph developed in Section 7. Determine
the mass of nickel that corresponds to the percent transmission
reading shown by the photometer. Report the results in grams
of nickel per square metre of steel surface.
10. Precision and Bias
10.1 The precision and bias of this test method is believed to
be within 0.000929 g/ft
2
(0.1 g/m
2
). Exact values are difficult to
obtain because of sample inhomogeneity, and the effect of the
acid etch on the rubber ring diameter (see 4.2.1).
4
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
NOTE 1—The outer ring is a steel disk approximately 6 by
1
⁄
2
in. (152
by 13 mm), weighing approximately 3
1
⁄
2
lb (1.58 kg).
FIG. 1 Detailed Drawing of Rubber Ring
C715 − 90 (2016)
2