TS01016D/06/EN/01.

13

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Test specification TS01016

(Previous document no. 123005)

CORE INSTRUCTION
Positive Material Identification (PMI)

A1
A2
A3

Scope
Purpose
Terms and Abbreviations

A3.1
A3.2
A3.3
A3.3.3

A4
A4.1
A4.2
A4.3
A4.4
A4.5

A5
A5.1

Page 1 of 8 TS01016

2
2
2

References............................................................................................................... 2
Personnel ................................................................................................................ 2
Equipment .............................................................................................................. 3
Measuring Error ..................................................................................................... 4

Procedure

Standards ................................................................................................................ 4
Scope Verification .................................................................................................. 4
Moment of execution ............................................................................................ 5
Marking and Actions ............................................................................................. 5
Customer Reports ................................................................................................... 6

Attachments

Attachment 1, drawing example.......................................................................... 7

Positive Material Identification, PMI

A1

Scope
This procedure explaines the method of verification, acceptance/rejection criteria, marking and reporting for
positive material identification (PMI) of alloyed materials.

A2

Purpose
The PMI-test is utilized to assure that the material grade is in compliance to its 3.1 material certificate and
the E+H Flowtec material specification. The analyser determines the quantity of alloy elements as a
percentage. Based on the analysis of the components the corresponding material grade is evaluated. Due to
the measuring error of device and the limited penetration depth of energy into the material surface, the
determined values of the various alloy elements are not intended to verify and/or to substitute the chemical
analysis of the certified mill test report.

A3

Terms and Abbreviations

PMI

A3.1

Positive Material Identification

References
The following documents have been taken as a basis during the preparation of this instruction and are
considered an integral part of the PMI procedure.
-

A3.2

ASTM E1916-11
Identification and/or Segregation of mixed Lots of Metals
API 578
Material Verification Program for New and Existing Alloy piping Systems
Internal directive for radiation safety No. PU030D
Safety instruction for the x-ray Fluorescence Spectrometer No. 0006
Test instruction No. 71105474 Chapter A4.2.2.3.
Internal procedure No. 71036384

Personnel
For the production location in Switzerland, the operator qualification program is based on Swiss Law and
other applicable rules in relation to radiation protection.
Radiation protection Representative:
- Qualified by SUVA (Swiss organisation for security) for radiation protection.
- Trained by the manufacturer of the PMI analyser for the use of device.
- Trained by the PMI Analyser manufacturer on how to operate the device correctly.
- Responsible for the execution of enhanced radiation protection trainings of the operators
Operators:
Trained by the Radiation protection Representative of the PMI device in three sections:
- Radiation protection knowledge
- Safety rules
- How to operate the PMI analyser
All successfully completed trainings are signed by the operators and approved by the representative.
The operators need to recertify every two years. The training certificates are filed.
For production locations outside of Switzerland local Law and rules apply for the qualification of the
employees.

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A3.3

Equipment
The following portable analyzers (or equivalent) are in use:

Manufacturer
Model
Serial no.
Method

Division Reinach (CH)

OLYMPUS
Delta professional DPRO2000AP-C
S/N 540216
XRF

Division Reinach (CH)

Niton
XLT 898
S/N 8610
XRF

Division Cernay (F)

OLYMPUS
Delta DS-2000
S/N 501881
XRF

A3.3.1 Function of Analyzer

Principles of the X-ray fluorescence spectrometric analyze (XRF) in a few words:

By using XRF Spectrometry technique alloy elements in a sample can be identified and quantified. Highenergy X-ray photons are emitted from a source (X-ray tube) and strike the sample. The photons from the Xray tube have enough energy to knock electrons out of the innermost orbital of atoms in the sample. When a
high energy photon hits an atom, it may knock electrons out of inner orbitals. When this occurs, the atoms
become ions, which are unstable.
Electrons seek stability and the lowest possible energy state. Therefore, a more energetic electron from an
outer orbital will move into the newly vacant space in the inner orbital. Electrons in outer shells have more
energy than electrons in more inner orbitals. They need to release this excess energy as they drop down to
fill the vacancy in the inner shell. This released energy is given off as a photon which can be detected by an
X-ray detector.
The energy of the emitted energy is equal to the difference in energies between the 2 orbitals and is
characteristic of the element fluorescing.
A3.3.2 Elements to be analyzed
Material
1.4401/316, 1.4404/316L,
CF3M, 1.4410, 1.4462,1.4301,
1.4306/304L 1.4435/316L,
1.4541/321, 1.4542,
1.4539,1.4547, 1.4571/316Ti
2.4602, Alloy C22
2.4668 Inco7
Zr 702
2.4375
Titanium Grade 2/5/9
Tantalum

Mn

Cr
x

Mo
x

Ni
x

x
x

x
x

x
x
x

Cu

Co

Hf

Zr

Ti

Nb

Ta

x
x
x
x
x

The PMI Analyzers in use are not able to measure the percentage of carbon. Therefore it is impossible to
differentiate between some close related alloys materials, like for example 316 and 316L or 1.4401 and
1.4404.

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Positive Material Identification, PMI

A3.3.3 Measuring Error

The measuring error is specific to each alloy element and measurement. Generally the error equals a 2 sigma
error. This value means that it is 95% certain that the measured value varies in the given range, for example
the analyzer measured Cr 16.18 +/- 0.52, this means that it is 95% certain that Cr is between 15.66 and
16.7: In this case, Cr theoretical tolerances are between 16.5% and 18%. The analyzer will accept the value
because the measured value is within the tolerances, considering also the measuring error.

Remarks:
An X-ray fluorescence spectrometric analyze (XRF) PMI test is a superficial test. Since the x-ray energy
required for the analysis penetrates the material only around 0.05-0.15mm this depending on the
material under test and its homogenity. Therefore the analysis result is significantly affected by the surface
conditions (cleanliness, deposit passivation, oxidation, coatings, ..) and of course by the surface
inhomogeneity of the material. Due to this the measuringresults might be different comparing one testpoint
with another one.
A3.3.4 Calibration
Baseline Calibration:
Every 5 years the PMI analyzer is sent to the manufacturer for verification of the accuracy and maintenance.
The verification results are documented.
Daily Calibration:
When the analyzer is switched on, a recalibration based on a build-in sample can be performed in
accordance to the manufacturers instructions. This functional test is done at least once per working day.
The test does not give an analysis of the build-in sample.
Additional a verification of the analysis is done by testing a certified reference samplematerial made of
316L.

A4

Procedure

A4.1

Standards
The following Standards apply for the verification method.
ASTM E1916-11
API 578

A4.2

Identification and/or Segregation of mixed Lots of Metals

Material Verification Program for New and Existing Alloy piping Systems

Scope Verification
Per pressure retaining part of the flow instrument (100%) one measurement is executed in accordance with
this procedure.
Measurements of the welding seams are NOT included in the scope of the test. Optionally a PMI test of the
bare welding wire can be executed, but only in case this option has been ordered by the customer.

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A4.3

Moment of execution
Depending on the accessibility of the pressure retaining parts of the instrument, the PMI test can be
executed at two different moments in production:
1. The individual components are separated from other identical components on stock, and assigned to a
specific instrument by marking all parts with the individual serial number before the welding process.
2. The components are verified after they have been welded together into an instrument.

A4.4

Execution

A4.5

It has to be verified that the surface of the components is relatively smooth and free of foreign
materials, such as grease, oil, dirt, scale, paint and other contaminates that could influence the
measurement results.
After the calibration procedure of the PMI analyzer, the measurement is performed according to the
instruction manual of the manufacturer.
A measurement should last approx. 8 sec, the same procedure is applied in all E+H Flowtec
Divisions in order to optain the same measuring precision.
When all measurements are finished, the data of the Analyzer is uploaded and electronically
transmitted to the production related database. A print out of the PMI test result is generated from
the production database.

Acceptance Criteria
The percentages of alloy elements and their tolerances for the different material grades are stored in the
electronic library of the analyzer. After the measurement has been executed, the analyzer compares the
determined percentages of alloy elements with the material compositions as stored in the device according
to the corresponding EN or ASTM Material Standards.
In case the analyzer identifies a material grade which is specified in the internal production document, the
operator considers the component as accepted.
As mentioned in chapter A3.3.3 the result of a PMI Test depends on the surface conditions and might
slightly differ from measuring point to measuring point. Therefore the operator is allowed to repeat a PMI
Test, if the first measurement result was slightly out of tolerance.
Before proceeding the repetition of the test, the surface of the measuring point has to be polished (to avoid
the influence of any contamination on the surface).
If the second test on the polished surface is within tolerances, the PMI test result will be accepted.
In case of doubt, the radiation protection representative has to be informed. He decides about the further
actions and in case of nonconformity he starts the procedure to reject components.

A4.6

Marking and Actions

A waterproof felt pen used for marking contains a low halogenated ink, consisting of a chloride/fluoride
concentration < 200 ppm and a sulphur concentration < 400 ppm. In any case the ink of felt pen does not
affect the tested metal surface.
1

Accepted Components

a) Test of components before the welding process:

The unique device number and the markings acc. to the example in attachment 1 of this procedure are
applied on the accepted parts. Additionally the successful completion of PMI Test is registered in the
internal production documents of the respective device. Afterwards the tested parts are conveyed to the next
production steps. The marking stays on the components until they are welded into the device.
b) Test of components after the welding process:
The markings acc. to the sample in attachment 1 of this procedure are applied on the accepted parts of the
welded unit.

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Positive Material Identification, PMI

A4.7

Customer Reports
This chapter is not applicable for flowmeter ordered in compliance with AD2000. In case of AD2000
compliance a material identification without specific measuring results and designated measuring points is
sufficient.
For each flowmeter (serial number), a PMI test report is issued. The elements identified in the measurement
results are noted in point A3.3.2.
The PMI test report looks like the following example:

Rev.

date

approved

14.06.2011

FRU

23.06.2011

MSA

28.10.2011

MSA

26.08.2013

MSA/FRU

18.11.2013

MSA/FRU

Page 6 of 8 TS01016

Rev.

date

approved

Document no.: TS01016

Previous document: no.: 123005
Date: 31.10.2013
Author: DRL/MSA

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A5

Attachments

A5.1

Attachment 1, drawing example

For every device a schematic drawing indicates which parts should be PMI tested.
The drawing is attached to the test report (this does not apply for instruments delivered with the option
AD2000):

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Positive Material Identification, PMI

Appendix 1

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