Klass.-Nr./Class. No.

50 22 1 July 2005
Chrome-Plated Surfaces
Determination of Potential Differences and Layer
Thicknesses of Nickel Coatings
PV
1065
Konzernnorm
Descriptors: potential difference, layer thickness, coating thickness, nickel layer, nickel
coating, bright nickel, semi-bright nickel, nickel coat
Page 1 of 6
Fachverantwortung/Responsibility Normung/Standards (EZTD, 1733)
K-GQL-1/5 Frau Hoffmann Tel.: +49-5361-9-76941 Dr. Schilling Wiesner Tel.: +49-5361-9-29064 Sobanski


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VOLKSWAGEN AG
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1 Scope
This standard describes a procedure to determine potential differences and thicknesses of nickel
coatings.
2 Description
Potential difference acc. to PV 1065
Layer thickness acc. to PV 1065
3 Test method
3.1 Principle
During chrome plating of parts, nickel layers of different electrical potentials are deposited. These
potential differences and layer thicknesses have an influence on corrosion.
The nickel layers shall be separated from the substrate by means of an anodic galvanostatic
separation method (at constant current) within an exactly defined surface. During this process, the
potential course shall be recorded with respect to a reference electrode (Ag/AgCl) and represented
in a potential/layer thickness diagram. On the basis of this diagram the potential differences
between the nickel layers and the layer thicknesses shall be determined.
This measuring procedure is a modification of the coulometric layer thickness measurement acc. to
DIN EN ISO 2177 based on ASTM B 764.
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PV 1065: 2005-07



Legend
1 Start of layer separation
2 Separation of bright nickel layer
3 Separation of semi-bright nickel layer
4 End of separation
5 Bright nickel
6 Semi-bright nickel
7 Copper
8 Cathode (counter electrode)
9 Silver cone (reference electrode)
10 Plastic seal
Figure 1 Test procedure using a double-nickel layer as an example
3.2 Test equipment and auxiliary equipment
Test setup (see Figure 2) consisting of:
! DC power supply source, adjustable from 0 mA to 50 mA
! Electrolyte pump
! Detector
! Measuring cell
! Silver reference electrode
! Counter electrode (cathode)
NOTE: The complete test setup is commercially available in the form of a complete device (e.g.
Couloscope CMS Step by Helmut Fischer GmbH & Co. KG, Sindelfingen, Germany).
3.3 Chemical agents
! Hydrochloric acid, approx. 18%
! Electrolyte consisting of: 300 g/l nickel chloride (NiCl2 x 6 aq), 50 g/l sodium chloride (NaCl)
and 25 g/l boric acid (H3BO3) in de-ionized water. The pH-value shall be monitored; it shall be
pH = 3 0.1. If this is not the case, it shall be brought to the value by adding diluted
hydrochloric acid or sodium lye.
NOTE: Ready-to-use electrolyte is commercially available (e.g. Fischer Elektrolyt F22 by Helmut
Fischer GmbH & Co. KG, Sindelfingen, Germany).
Page 3
PV 1065: 2005-07


Legend
1 Electrolyte pump
2 Measuring cell
3 Working electrode (anode)
4 Specimen
5 Counter electrode (cathode)
6 Silver reference electrode
7 Detector
Figure 2 Determination of the layer thickness
3.4 Procedure
3.4.1 Specimen preparation
The specimens shall be plane and have a size of approx. (3 x 3) cm. Larger components shall be
divided accordingly.
The chrome layer is removed by one of the following methods:
! Chemical separation of the chrome layer in an approx. 18% hydrochloric acid bath, approx.
5 min at room temperature. The potential differences shall be measured no sooner than 24 h
after separation of the chrome layer, as there may be ambiguous differences between
microporous nickel and bright nickel otherwise.
! Electrolytic separation of the chrome layer (e.g. separation during the coulometric layer
thickness measurement acc. to DIN EN ISO 2177). In this case the potential differences may
be measured immediately after the separation of the chrome layer.
Subsequently, the specimens shall be thoroughly cleaned with de-ionized water and dried.
3.4.2 Measurement
Prior to each measurement series, the silver reference electrode shall be conditioned on non-
conductive material (for formation of silver chloride coating). This is to ensure that a current only
occurs between the silver reference electrode and the cathode. The conditioning time shall be 30 s.
In case of longer device downtimes, it may be necessary to repeat conditioning several times.
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PV 1065: 2005-07

The system functional capability shall be checked prior to each measurement series by means of a
known reference setup. At monthly intervals, a calibrated reference standard shall be used for the
comparison measurement (e.g. calibration standard Kalibriernormal Step Ni/Cu by Helmut Fischer
GmbH & Co. KG, Sindelfingen, Germany).
Measuring process:
! Positioning of specimen under the measuring cell
! Grounding of specimen
! Connection of silver reference electrode with detector/evaluation unit
! Separation speed: 5 m/min
! Max. separation voltage: 5 V
! Current density: 2.5925 mA/mm
The following amperages result from this when using the Fischer measuring cell:
3.2 mm (blue seal): 20.85 mA
2.2 mm (green seal): 9.852 mA
1.5 mm (yellow seal): 4.589 mA
! Filling of cell with electrolyte
! Measurement start until complete separation of all nickel layers
After every individual measurement the counter electrode (cathode) shall be cleaned from any films
by means of a soft cloth.
The electrolyte shall be replaced after every measurement.
The separation area shall be evaluated after every measurement. The separation shall be
complete; its diameter shall have the same dimensions as the seal. If this is not the case, the
measurement shall be repeated or the seal shall be replaced.
In order to conserve the silver chloride coating, the reference electrode shall be kept in a closed
container after the measurements in the electrolyte have been finished.
3.5 Evaluation
The measured values shall be represented in a potential/layer thickness diagram (example see
Figure 3). The X axis represents the layer thicknesses, the Y axis the potential differences.
Evaluation may be performed manually or automatically.
3.5.1 Layer thicknesses
The thickness of the individual layers shall be measured between the characteristic curve steps
(example see Figure 3).
3.5.2 Potential differences
The potential differences shall be determined by subtracting the semi-bright nickel layer potential
from the bright nickel layer potential and by subtracting the bright nickel layer potential from the
porous nickel layer potential (example see Figure 4).
If there is a drift in the characteristic curve, the potentials shall be determined by applying a
tangent.
Page 5
PV 1065: 2005-07


Legend
1 Microporous nickel
2 Bright nickel
3 Semi-bright nickel
1.6 m
9.1 m
8.5 m
Figure 3 Determination of the layer thickness

Legend
1 Microporous nickel
2 Bright nickel
3 Semi-bright nickel
4 40 mV difference
5 135 mV difference
6 340 mV absolute
7 300 mV absolute
8 435 mV absolute
Figure 4 Determination of the potential difference
Page 6
PV 1065: 2005-07


Legend
1 Semi-bright nickel potential
2 Bright nickel potential
3 Bright nickel layer thickness (point of reading: upper value)
4 Semi-bright nickel layer thickness (point of reading: lower value)
Figure 5 Determination of layer thickness and potentials in case of a drift in the
characteristic curve
3.6 Test report
See Table 1.
Table 1 Example of a test report (refers to measurement in Figures 3 and 4)
1 Layer thickness of porous nickel in m 1.6
2 Potential step between porous nickel/bright nickel in mV 40
3 Layer thickness of bright nickel in m 9.1
4 Potential step between bright nickel/semi-bright nickel in mV 135
5 Layer thickness of semi-bright nickel in m 8.5
4 Referenced standards
*

DIN EN ISO 2177 Metallic Coatings; Measurement of Coating Thickness; Coulometric Method
by Anodic Dissolution
ASTM B 764 Standard Test Method for Simultaneous Thickness and Electrode Potential
Determination of Individual Layers in Multilayer Nickel Deposit (STEP Test)

*
In this section terminological inconsistencies may occur as the original titles are used.