Asoma Phoenix Ii: Determination of Conversion Coatings On Steel or Aluminum

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ASOMA

Application Note

PROCESS INSTRUMENTS

ASOMA PHOENIX II

Determination of Conversion Coatings on Steel or Aluminum


Introduction

Summary
All samples were analyzed
using the ASOMA PHOENIX
II XRF Benchtop system.
This report demonstrates the
capability of the PHOENIX
II to analyze conversion
coatings on steel or
aluminium.
Conversion coatings are
used for barrier protection
against oxidation and
corrosion, as a primer for
paint-ing, or as a primer for
optimum tooling and cutting
properties.

The ASOMA PHOENIX II benchtop XRF analyzer offers a fast,


precise, simple and non-destructive analysis technique well suited
for the determination of conversion coatings thickness (as given by
coat weight) on steel or aluminium substrates. Galvanization makes
use of zinc coatings. As hexavalent chromium is being phased
out of use, coatings to replace chromate coatings include titanium,
vanadium and zirconium. Coating used as both a paint primer
and tooling preparation include phosphate compounds and silicon
compounds (silane, silicone, etc.)
The PHOENIX II employs state-of-the-art optics. Polarization
excitation offers unique benefits because it eliminates most of the
back-ground scatter emerging from the X-ray tube before it arrives
at the sample. This results in a dramatic improvement in peak-tobackground signal, especially in highly scattering materials. This
translates to vastly improved precision and lower detection limits than
traditional direct excitation XRF systems can achieve.
The PHOENIX II uses an onboard PC computer with a simple
touch screen interface. Thus, an external computer is not required.
Data handling and results storage can be obtained on a thermal
paper printout and are stored in the hard drive of the PHOENIX II.
The data is readily transferred to a USB thumb-drive or a network
Ethernet connection.

Coatings include Zn, Cr, Ti,


V, Zr, P or Si compounds.
Proper monitoring of coat
weight is important. Over
coating may cause loss of
quality and undue over expense. Under coating causes
loss of quality. ASOMA
coating measurements require
little sample preparation.
Simply cut a sample panel,
place it in the sample chamber
and analyze.
These benefits work
together to maximize quality
and reduce operational costs.

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ASOMA

Calibrations are carried out using assayed


standards. This ensures easy traceability of
results for quality purposes. This initial calibration
process is a once only procedure. Subsequently,
the curve can be re-standardized, if required, by
the touch of a button on the main analysis screen.
The PHOENIX II offers power, versatility and
performance all in a small, compact, easy-to-use
design.

Instrument Configuration
ASOMA PHOENIX II
Excitation: 48 kV 50 W Air-cooled X-ray Tube
Detection: Gas-filled Proportional Counter
Analytes Optimization: X-ray voltage, current and
X-ray filters
Atmosphere: Air
Options: HOPG crystal for polarized X-rays;
Moveable secondary target; Detector filters;
Polypropylene 4 m film

Experimental Portion

Note: No consumable gases required.

Equipment

Typical sample panel shown in analysis position

All measurements were conducted using a


PHOENIX II XRF analyzer. Performance is shown for a
measurement time of 100 seconds, except for Si on
Cr coated Steel, which uses an analysis time of 200
seconds.
Sample Preparation
Simply cut an approximately 3 x 5 inch square or
disk panel and place it coating side down over the
aperture in the sample chamber.
Measurement Parameters
All measurement parameters are easily controlled
through the touch screen on the display panel.
Operators simply choose the correct method from
the analysis screen (there may be more than
one method stored, e.g. to deal with chromate
or titanium) and then press the green ANALYZE
button.

Handy Conversion Factors

The results can be reported using a variety of


different options: results are reported on the display
screen; on a thermal paper printout; on an optional
external printer; and in the database history within
the analyzer.

Note:

1 mg/ft2 = 10.8 mg/m2


1 mg/m2 = 0.001 g/m2
t = (coat weight)/d
t = coating thickness
d = density of coating material

The following results sections show performance


for a few typical coatings. The PHOENIX II is
equipped to measure many others. Please contact
AMETEK Process Instruments if you do not see your
application listed here.

Precision for Cr on Aluminum


10 repeat analyses at 100 seconds per
measurement

Calibration for Cr on Aluminum


Element: Cr
Units: mg/ft2

Std. Error of Estimate: 1.24

Sample

Given

Measured

76.8

76.01

7.4

6.10

9.5

9.78

11.8

12.40

15.0

15.25

22.2

22.02

34.3

31.87

44.4

45.29

59.8

61.35

10

0.0

1.17

Element: Cr

Units: mg/ft2

Sample

Given

Mean

Std.
Dev.

%Rel.

76.8

78.66

0.43

0.6

22.2

22.26

0.19

0.9

15.0

15.61

0.15

1.0

Minimum Detection Limit (MDL)


Cr on Aluminum
The Minimum Detection Limit (MDL) for an element
is determined as three times the standard deviation
of ten analyses of the blank uncoated sample. The
following MDL was derived using this empirical
method and applies to this matrix and coat weight
range.

Correlation Plot
for Cr on Alum inum

Measured ( mg/ft2)

80
70

Element

Count Time

MDL

60

Cr

100 sec

0.7 mg/ft2

50
40
30
20
10
0
0

10

20 30 40 50

60 70 80

Given ( m g/ft2)

ASOMA

Results for Cr on Aluminum

Calibration for Cr on Steel


Element: Cr
Units: mg/ft2

Std. Error of Estimate: 1.45

Sample

Given

Measured

20.a

40.5

41.2

15a

32.1

30.3

7a

21.2

21.6

4a

14.6

16.0

2a

7.2

6.6

Precision for Cr on Steel


10 repeat analyses at 100 seconds per
measurement
Element: Ca

37
29
21
13
5
13

21

29

Sample

Given

Mean

Std.
Dev.

% Rel.

20a

40.5

39.4

1.0

2.6

7a

21.2

21.3

1.0

4.9

2a

7.2

7.00

1.3

18.0

The Minimum Detection Limit (MDL) for an element


is determined as three times the standard deviation
of ten analyses of the blank uncoated sample. The
following MDL was derived using this empirical method
and applies to this matrix and coat weight range.

45

Units: mg/ft2

Minimum Detection Limit (MDL)


Cr on Steel

Correlation Plot
for Cr on Steel

Measured ( mg/ft2)

ASOMA

Results for Cr on Steel

37

45

Given ( mg/ft2)

Element

Count Time

MDL

Cr

100 sec

3.1 mg/ft2

Note:

Precision for Ti on Aluminum


10 repeat analyses at 100 seconds per
measurement

Results for vanadium (V) coatings with be


comparable to titanium (Ti) results.

Element: Ti

Calibration for Ti on Aluminum

Units: mg/ft2

Sample

Given

Mean

Std.
Dev.

% Rel.

1.56

1.584

0.037

2.4

0.92

0.910

0.021

2.4

0.25

0.295

0.034

10.4

Element: Ti
Units: mg/ft2

Std. Error of Estimate: 0.053418

Sample

Given

Measured

1.56

1.585

0.25

0.318

0.00

-0.008

0.51

0.474

0.71

0.729

0.92

0.853

Minimum Detection Limit (MDL)


Ti on Aluminum
The Minimum Detection Limit (MDL) for an element
is determined as three times the standard deviation
of ten analyses of the blank uncoated sample. The
following MDL was derived using this empirical method
and applies to this matrix and coat weight range.

Correlation Plot
for Ti on Aluminum
1.6
Measured ( mg/ft2)

1.4
1.2
1.0
0.8
0.6
0.4
0.2
0.0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6
Given ( mg/ft2)

Element

Count Time

MDL

Ti

100 sec

0.09 mg/ft2

ASOMA

Results for Ti on Aluminum

Precision for Zr on Aluminum


10 repeat analyses at 100 seconds per
measurement

Calibration for Zr on Aluminum


Element: Zr

Units: mg/ft

RMS: 0.009

Std. Error of Estimate: 0.028487

Sample

Given

Measured

4.7

4.70

0.8

0.79

1.5

1.53

10

2.6

2.58

Element: Zr

4
3
2
1
0
1

Sample

Given

Mean

Std.
Dev.

% Rel.

20a

40.5

39.4

1.0

2.6

7a

21.2

21.3

1.0

4.9

2a

7.2

7.00

1.3

18.0

The Minimum Detection Limit (MDL) for an element is


determined as three times the standard deviation of ten
analyses of the blank uncoated sample. The following
MDL was derived using this empirical method and
applies to this matrix and coat weight range.

Units: mg/ft2

Minimum Detection Limit (MDL)


Zr on Aluminum

Correlation Plot
for Zr on Aluminum

Measured ( mg/ft2)

ASOMA

Results for Zr on Aluminum

Given ( mg/ft2)

Element

Count Time

MDL

Zr

100 sec

0.025 mg/ft2

Calibration for P on Steel


Element: P

Precision for P on Steel


10 repeat analyses at 100 seconds per
measurement

Units: mg/ft2

Std. Error of Estimate: 3.04

Sample

Given

Measured

119

119.8

106

105.0

95

95.8

63

61.4

73

70.1

56

59.9

Element: P

Units: mg/ft2

Sample

Given

Mean

Std.
Dev.

% Rel.

119

119.9

0.53

0.44

56

57.6

0.18

0.31

Minimum Detection Limit (MDL)


P on Steel
The Minimum Detection Limit (MDL) for an element
is determined as three times the standard deviation
of ten analyses of the blank uncoated sample. The
following MDL was derived using this empirical method
and applies to this matrix and coat weight range.

Correlation Plot
for P on Steel

Measured ( mg/ft2 )

125

100

75

50
50

75

100

125

Given ( m g/ft2 )

Element

Count Time

MDL

100 sec

1.2 mg/ft2

ASOMA

Results for P on Steel

Determination of Conversion Coatings on Steel or Aluminum

Element: Si

10 repeat analyses at 200 seconds per


measurement

Units: mg/ft

R.M.S.: 0.0010

Element: Si

Std. Error of Estimate: 0.0022716

Sample

Given

Measured

0.26

0.255

0.19

0.191

0.16

0.160

0.15

0.149

0.13

0.131

0.11

0.108

0.08

0.081

0.17

0.169

0.23

0.237

Units: g/m2

Sample

Given

Mean

Std.
Dev.

% Rel.

0.26

0.253

0.001

0.5

0.16

0.161

0.001

0.6

0.08

0.082

0.0005

0.6

Minimum Detection Limit (MDL)


Si on Cr Coated Steel
The Minimum Detection Limit (MDL) for an element is
determined as three times the standard deviation of ten
analyses of the blank uncoated sample. The following
MDL was derived using this empirical method and
applies to this matrix and coat weight range.

Precision for Si on Cr Coated Steel

Correlation Plot
for Si on Cr ocated Steel

Element

Count Time

MDL

Si

200 sec

0.001 g/m2

0.30

Measured ( g/m2 )

0.25

Conclusion

0.20
0.15

As can be seen from the above data, the use


of the PHOENIX II XRF system gives excellent
performance when applied to the determination of
conversion coatings on steel or aluminium. Results
are rapid, precise and analysis is easily carried out,
even by non-laboratory personnel. Because no
consumable chemicals are used, the relative cost
of ownership is much lower than other analytical
techniques.

0.10
0.05
0.00
0.00

0.05

0.10

0.15

0.20

0.25

0.30

Given ( g/m 2)

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Ph. +1-412-828-9040, Fax +1-403-826-0399

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2011, by AMETEK, Inc.


All rights reserved. Printed in the U.S.A.
F-0282 Rev. 2 (0511)

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One of a family of innovative process analyzer solutions from AMETEK Process Instruments.
Specifications subject to change without notice.

ASOMA

Calibration for Si on Cr Coated Steel

Application Note

Results for Si on Cr Coated Steel

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