G8 GALILEO G4 PHOENIX Brochure DOC-B78-EXS013 Lowres

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02719_Combustion_Analysis_MON58.qxp_210x279 16.03.

18 13:37 Seite 1

Oxygen Nitrogen Hydrogen Diffusible Argon


&
Trapped
Hydrogen

G8 GALILEO
G4 PHOENIX
Solutions for Inert Gas Fusion Analysis of Inorganics

Elemental Analysis
Innovation with Integrity
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*) Best H2 detection limit in an ONH system using a thermal conductivity detector with a dedicated
reference channel. Uniquely coupled infrared furnace for diffusible hydrogen applications. Uniquely
coupled mass spectrometer for ultra-low concentrations of hydrogen and argon with highest selectivity.

2 G8 GALILEO G8 GALILEO MS G4 PHOENIX G4 PHOENIX MS


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Control the World of Metals


with Just a Few Elements
Ores, metals, alloys and ceramics
shape our time.
For thousands of years, metals and alloys have played
a prominent role in the evolutionary history of humanity
and give names to entire epochs.
The three non-metals Oxygen (O), Nitrogen (N) and
Hydrogen (H) determine the quality, service life and
mechanical properties of all metallic materials. Unlike
metallic alloy components, the amount of O, N and H
sometimes changes considerably along the entire
process chain, from the production of raw materials
to the completion of the finished product.

Light elements make heavy work.


Even when present in trace amounts, O, N and H
have a very critical effect on the material properties.
However, low concentrations are difficult to analyze
with spectroscopic methods due to the atomic
properties of O, N and H. So what can be done?
Use the best method: Inert Gas Fusion Analysis.
No other method provides better detection limits,
reliability or stability.

Match the best ONH method, with the


ideal ONH systems: G8 GALILEO and
G8 GALILEO MS.
With the G8 GALILEO analyzers, Bruker is the only
company to offer fully integrated ONH solutions
combining the benefits of multiple dedicated systems
without any analytical compromise or technical
limitations!*)

G4 PHOENIX and G4 PHOENIX MS –


experts for the first element: hydrogen.
The accurate analysis of mobile hydrogen is
extremely important in many areas. Bruker offers
extremely powerful systems for the analysis of
diffusible and trapped hydrogen: G4 PHOENIX
and G4 PHOENIX MS.

@ inorganics

Oxygen Nitrogen Hydrogen Diffusible Argon


&
Trapped
Hydrogen 3
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The G8 GALILEO with Smart Mole-


cule Sequence™ guarantees proven
science and trustworthy results.
G8 GALILEO with
Why is the G8 GALILEO superior
to other ONH systems?
Smart Molecule
The G8 GALILEO performs direct and
unadulterated measurements of all gases
Sequence™ for Direct
emitted by the sample, in a 1:1 ratio – without
chemical transformation, repetitive measure-
ments, mathematical corrections or
Measurement and
unpublished algorithms.
The G8 GALILEO offers all possibilities of a
state-of-the-art solution for O, N and H in one
Real 1:1 Information
system, without analytical compromise.
The G8 GALILEO can measure even lowest
hydrogen concentrations in the ng/g (ppb) range
directly and reliably, without compromises.
The G8 GALILEO detects the exact tempera-
ture of the sample directly with FusionControl
and thus ensures that only the measured gases
(CO, N2 and H2) are formed – no CH4,
no other hydrocarbons.

What are the advantages of


Smart Molecule Sequence™?
Each of the three elements O, N and H is
analyzed 1:1, where the concentration of FusionControl for real-time sample temperature
CO ≙ O, N2 ≙ N and H2 ≙ H. detection, Bruker only

Nitrogen or argon can be used as an alternative


carrier gas, instead of the standard, but expen-
sive and rare carrier gas helium.
Not only nitrogen, but hydrogen as well is
measured using a highly sensitive DualChannel
Thermal Conductivity Detector (TCD) with a
separate reference channel. Comparison of
the measurement channel with the reference
channel ensures scientifically proven analyses.
The unique combination with a heat exchanger
guarantees exactly the same temperature of
reference and analysis gases. DualChannelTCD with integrated heat exchanger for
identical temperature of reference and analysis gases
Smart test setup and exact temperature control
result in less dust, offer system stability and
higher uptime.

G8 GALILEO –
ONH Analysis @ its best!

Unique gas calibration unit for standardless


hydrogen calibration with 10 independent volumes
4
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G8 GALILEO

O, N, H
@ its best
@ its best

G8 GALILEO – for direct measurement of emitted gasses – 1:1 Oxygen, 1:1 Nitrogen and 1:1 Hydrogen

5
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Highly flexible sample changer


and integrated crucible changer.
Sample changer with 20 or 40 positions.
Optional independent aggregate feed, with
20 samples plus 20 flux additives, important
for the measurement of hydrogen in titanium
alloys with nitrogen carrier gas.
Removable sample plates with robust,
failure proof sample containers.
Sample containers can even be easily
filled with chips.
Integrated crucible waste container
monitoring.

Fully automatic furnace cleaning. 20 position sample tray with failsafe sample chutes

Cleans upper and lower furnace electrodes


at freely programmable intervals.
Cleaning unit is safely placed behind
a glass pane.
Advantage: no intervention, no adjustment,
maximum safety and cleanliness.

Advanced electrode furnace


with sample port.
Maintenance-free and reliable sample Simultaneous cleaning of both electrodes
port without consumable parts.
No jamming due to O-ring sealed slider.
The sample port integrated into the
water-cooled furnace protects the sample
from undesirable heating during crucible
outgassing.
Different sample port inserts available for
different sample types and crucibles.
Upper and lower furnace electrodes can
be replaced easily and separately.
Fully automated crucible handling
Time savings and more stable results
through sequential analysis of up to five
samples (depending on material) in the
same crucible without prior outgassing
or opening the furnace.
Ongoing, contact-free temperature
measurement of the sample via
FusionControl, Bruker only.

Monitored waste bin for crucibles

6
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G8 GALILEO
Autosampler

AS

O, N, H
@ high throughput

@ high throughput

G8 GALILEO with 40 position autosampler for ONH analysis @ high throughput

7
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G8 GALILEO with Smart Conventional Systems


Molecule Sequence™ for
Direct 1:1 Measurement vs. with Simultaneous
Setup and Indirect
Measurement

Electrode furnace °C!


°C Electrode furnace, ? °C ?
with FusionControl no temperature
control
Emitted gases CO N2 H2 Emitted gases CO N2 H2 & CO2 CH4 … CxHy

Measured gas CO Measured gases CO CO2

Nondispersive low IR CO≙O Nondispersive IR CO


Infrared range CO Infrared CO O(a)
Detectors Detectors CO2
(NDIR) + REF (NDIR)
Drift free, high IR IR 1st detector CO
high range
due to reference range CO CO2 2nd detector CO2
channel low range

N2 Path H2 Path CO, N2 H2, CO2, CH4 … CxHy Path

Real Derivative
Oxidation Oxidizing Oxidation
CO –> CO2 CO –> CO2 CxHy –> CO2 (a)
H2 –> H2O –> H2O(a)
CO –> CO2 (b)
Trapping Trapping H2 –> H2O(b)
- CO2 Real - CO2 Derivatives
- H2O

Measured gases N2 H2 Measured gases N2 CO2 + CO2 H2O

Thermal Nondispersive
Conductivity
N2≙N Infrared IR H2O(ox)≙Hidm
Detector Detectors H2O
TC
(TCD) H2≙H (NDIR) CO2
N2 /H2 + REF O(b)
3rd detector H2O(ox) IR CO2 (ox)
high range
4th detector CO2 (com) CO2
low range O(a)
Oidm
O(b)
Trapping
Emitted = Measured - CO2
- H2O
1:1 Oxygen Measured gas N2

1:1 Nitrogen
Thermal TC
1:1 Hydrogen Conductivity
N2≙N
N2
Detector (TCD) Only N2 with TCD
8
+
(REF)
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We keep it simple and


measure real sample gases!
The aim is to determine the sample con-
tent of the three light elements O, N and H
in the trace range with absolute accuracy.
That's why our G8 GALILEO measures
CO, N2 and H2 directly, absolutely un-
changed, 1:1, and with ideal detection
techniques. Thanks to direct temperature
1:1
control of the sample, no hydrocarbons
and interfering CO2 are produced at all.
To us, ONH analysis must be simple or
it’s simply not accurate. CO≙O 2 x NDIR

N2≙N TCD

H2≙H TCD

1st NDIR: CO
vs.
2nd NDIR: CO2
4th NDIR: CO2 (com)

Others make it complicated


CO and measure derivatives.
O(a)
CO2 If the gases emitted by the sample must
≙ Oidm be chemically transformed into derivatives
CO2 to analyze them, this is called indirect
CO CO2(b) O(b)
CO2 (com) measurement (idm). Measurement errors
CO2 (ox) add up and standard deviations increase,
CO2(a) in particular in the case of multiple transfor-
CxHy mations, when different measurements
H2O(ox)≙Hidm H2O(a) are combined and when the measuring
molecules are generated from different
H2O(ox) ≙ Hidm origins. Conclusion: indirect measurement
O(b) H2 H2O(b) is more complicated.
Determining the hydrogen content via
3rd NDIR: H2O(ox)
water vapor has several disadvantages:
Oidm N2 ≙ N TCD
Water must be kept permanently in the
gas phase.
Water can only be measured with
insufficient sensitivity by IR detection.
In the IR spectrum, water interferes with
CO2, which needs to be mathematically
corrected.
N2≙N
9
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G8 GALILEO with Smart Conventional Systems


Molecule Sequence™ for
Direct 1:1 Measurement vs. with Simultaneous
Setup and Indirect
Measurement

Yes Temperature Control No

Electrode furnace °C! Electrode furnace, ?


with FusionControl °C! no sample
temperature control
°C ?
Emitted gases CO N2 H2 Emitted gases CO N2 H2 & CO2 CH4 … CxHy

Yes no CO2, no CH4, no CXHY No


CO N2 H2 no CO2 CH4 … CxHy CO N2 H2 & CO2 CH4 … CxHy

Nondispersive IR Nondispersive IR
Infrared Detectors
(NDIR)
CO CO
matched to
Infrared Detectors
(NDIR)
CO CO
all range
CO is measured with + REF low range
two detector ranges. IR The first oxygen value IR
(O(a)) is calculated from
The molecules from
the sample remain
untouched
CO
CO
matched to
the measurement of CO
and CO2, one detector
CO2
CO2
low range
for each molecule
1:1 Oxygen high range

CO
CO≙O Yes All Oxygen at Once No CO2
O(a)

Oxygen? Done!
O Oxygen? Not yet!
O(a) …
CO N2 H2 CO N2 H2 & CO2 CH4 … CxHy

10
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Oxygen performance @ its best

Oxygen: Average Value / Laboratory, Round-Robin Test “Oxygen in Copper”*)

40

+ 2σ
35
Oxygen [ng/g]

30 + 1σ

25 Round-Robin
Test Result

20 - 1σ

15
- 2σ

10
Lab. Lab. Lab. Lab. Lab. Lab. Lab. Bruker Lab. Lab. Lab. Lab.
7 12 9 4 6 8 10 3 5 11 2 1

The whole round-robin test certificate


is of course available on request.

Accuracy doesn’t Come by Chance –


Round-Robin Test “Oxygen in Copper”*)

Basic Questions: Why did the G8 GALILEO


perform so well?
Should the sample temperature
be monitored? FusionControl in the G8 GALILEO prevents
the formation of hydrocarbons and other
Does the direct measurement
undesirable byproducts that result from
all range of CO provide better results?
excessively high sample temperatures.
Does every chemical conversion Thanks to FusionControl’s exact sample
lead to greater uncertainties? temperature control, the traditional
approach of heating up the sample as
Should the formation of
low range
high as possible is no longer necessary.
hydrocarbons be prevented?
With the G8 GALILEO the carbon monoxide
The answer to these questions emitted by the sample is measured directly
is yes, four times over. The system and in a 1:1 ratio.
combining all of these advan-
Unlike the G8 GALILEO, conventional
tages is the G8 GALILEO.
systems increase the measurement error
The result of the “Analytical Determination by additional oxidation steps and multiple
of Oxygen in Copper” round-robin test measurements of different molecules.
supervised by the German Federal Institute
… for Materials Research and Testing shows
that Bruker's system delivers excellent
Conclusion: The smarter and
simpler the setup, the more
results, both in terms of accuracy and reliable the results, especially at
in terms of reproducibility. low concentration ranges and
tight tolerances.

*) “Analytical Determination of Oxygen in Copper” round-robin test by the


“Special Materials” working committee in the Chemists Committee of the Society 11
for Mining, Metallurgy, Raw Materials and Environmental Technology (GDMB)
under supervision of the German Federal Institute for Materials Research and Testing.
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G8 GALILEO with Smart Conventional Systems


Molecule Sequence™ for
Direct 1:1 Measurement vs. with Simultaneous
Setup and Indirect
Measurement

Yes Use Emitted Gases Only No


Emitted gases CO N2 H2 Emitted gases CO N2 H2 & CO2 CH4 … CxHy

Smart Molecule Sequence™ Simultaneous Setup

N2 Path H2 Path CO, N2 H2, CO2, CH4 … CxHy Path


He or Ar Carrier Gas N2 or Ar Carrier Gas He Carrier Gas

Yes No Derivatives No
remove remove change

CO H2 N2 H2 CO CO H2 CH4 … CxHy CO2 N2

Oxidation Oxidation Oxidation


from oxidation
from sample

from sample

from sample

CO –> CO2 CO –> CO2 CxHy –> CO2 (a)


H2 –> H2O –> H2O(a)
CO –> CO2 (b)
Trapping Trapping H2 –> H2O(b)
- CO2 - CO2
- H2O
N2 H2 H2O(ox) CO2 (ox) CO2 N2
measure measure measure measure

All molecules
N2 H2
Origin of CO Origin of CO2 N2 CO2 + CO2 H2O
are measured un-
changed as emitted 1. Sample 1. Oxidizing CO
from the sample – 2.Oxidizing CH4 … CxHy
Origin of N2 3.Sample Derivatives
real 1:1 measure-
ment 1. Sample Origin of N2
Origin of H2 H2O(a)
1. Sample H2O(ox)
1. Sample Origin of H2O
H2O(b)
1. Oxidizing H2 CO2(a)
2.Oxidizing CH4 … CxHy CO2(ox)
12 CO2(b)
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:39 Seite 13

Melting Points and Emitted Gases [°C]

1,000 °C 1,650 °C ~ 3,100 °C

CO2 CO H2 CxHy N2

0 250 500 750 1,000 1,250 1,500 1,750 2,000 2,250 2,500 2,750 3,000 3,250 3,500

Pb Al Mn Co Ti Cr Ta
Metals
Sn Zn Mg Cu Ni Fe Zr V Mo W

PbO FeO Fe2O3 CoO ZnO Al2O3 ZrO2


Oxides
Pb3O4 CuO Fe3O4 TiO2 V2O3 NiO Cr2O3 MgO

Cu3N CrN VN TiN HfN


Nitrides
Fe2N Mg3N2 Si3N4 AlN ZrN TaN

MgH2 LiH
Hydrides
AlH3 TiH2

0 250 500 750 1,000 1,250 1,500 1,750 2,000 2,250 2,500 2,750 3,000 3,250 3,500

There is no temperature equally suited for measuring O, N and H. As a matter of principle and also with respect
to sample preparation, simultaneous systems cannot work optimally for each of the elements at the same time.

To get Real Information, you Have to Measure


Real Gases – Directly, Unchanged – 1:1

At first glance, a simultaneous ONH measure- Thanks to the Smart Molecule Sequence™, the
ment seems to be a fast and cost-effective G8 GALILEO measures each element directly,
solution. Rather, in fact, existing simultaneous unchanged and under ideal conditions.
systems have to deal with a number of
CO is measured with two infrared detectors:
fundamental problems.
one for the ng/g range, one for the % range.
Instead of directly measuring the molecules emitted H2 is determined down to the ng/g range with a highly
by the sample, the sample gases must be elaborately sensitive thermal conductivity detector (TCD) with
processed and so derivatives are generated. Ultimately, reference channel, a scientifically proven method.
CO2 and H2O are measured from multiple sources.
N2 is analyzed with a highly sensitive TCD plus
The oxygen content is calculated using proprietary reference channel.
mathematical processing of different measured values.
In addition to helium, the G8 GALILEO can use different
Water vapor measurements are particularly difficult with carrier gases, for example argon and nitrogen, right out
simultaneous systems: of the box.
The gas tubing system must be permanently heated Optimized gas flow in the ambient pressure system
to prevent water vapor condensation. G8 GALILEO eliminates the need for complex and error-
Water vapor is measured using an infrared detector. prone flow compensation. In overpressure systems
This analysis method is by principle not ideal for the flow compensation is necessary, so that high oxygen
trace analysis of water. concentrations do not lead to incorrect nitrogen results.
Spectroscopic interferences during the IR measure-
ment of CO2 and H2O must be compensated using
complex mathematics, which are usually hidden.
13
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G8 GALILEO with Smart Conventional Systems


Molecule Sequence™ for
Direct 1:1 Measurement vs. with Simultaneous
Setup and Indirect
Measurement

Yes Hydrogen but Water Vapor No


Derivatives
Yes H2 @ TCD, Real Referencing No
N2 H2 N2 CO2 + CO2 H 2O

Thermal Nondispersive
Conductivity N2 / H2 Infrared Detector
Detector (TCD)
+ reference channel
(NDIR)
H2O
IR H2O(ox)
All molecules remain
untouched and are TC For the second oxygen
H2O measured with
low sensitive NDIR
analyzed as emitted N2 /H2 + REF value (Ob), CO2 from the
from the sample – IR
one by one
1:1 Nitrogen
sample plus CO2 (ox) from
oxidized CO and CxHy is
measured as CO2(com)
CO2
CO2 (com)
combined gas volume
1:1 Hydrogen oxidation & sample
both @ TCD sensitivity

N2≙N CO2 (com)≙O(b)


H2≙H Yes Real 1:1 Information No H2O(ox)≙Hidm

O(a)
Nitrogen?
Directly! N Hydrogen?
Directly! H Oxygen? Only mathe-
matically generated. O(b) Oidm ~
Bruker’s Sequential
Hydrogen? Via water vapor
and low sensitive NDIR. Hidm ~
Smart Molecule Sequence™ Trapping
Allows a Direct 1:1 Measure- - CO2
- H2O
ment of Unchanged
Emitted Gases! N2 N2≙N

Thermal TC Only the nitrogen


Conductivity N2 molecule remains
Detector (TCD) untouched

+
(REF)
Only nitrogen is
14
measured with a TCD. N
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:39 Seite 15

The G8 GALILEO analyzes the hydrogen


content directly as H2, using a highly
sensitive TCD plus reference channel.
This is necessary because the TCD
Hydrogen performance @ its best measurement is a comparative method
that needs to be permanently referenced
to an independent channel. This reference
H2 measurement with channel ensures reproducible and accurate
highly sensitive TCD. results, especially in the ng/g range.
Scientifically proven com- The G8 GALILEO guarantees real
parative measurement measurement results for hydrogen,
against reference channel. without unpublished algorithms.
Heat exchanger for exact
temperature matching of
reference and analysis gas.
Electronically adjustable
measuring range of the
TCD.
Real H2 Measurement with
TCD Quality, Proven Science
H2O measured with
low sensitive NDIR with Reference Channel

combined gas volume


oxidation & sample

Comparison Nitrogen in Steel Nitrogen Deviation Deviation Nitrogen @ ease


Carrier Gas Helium or Argon Content Helium Argon

[ng/g] [ng/g] [ng/g] The same analytical quality


without limitation for N2
Sample A 19.7 ± 0.33 ± 0.34 measurement with argon
carrier gas.
Sample B 28.1 ± 0.80 ± 0.67
Measurement with argon
Sample C 95.4 ± 1.19 ± 1.21 carrier gas is significantly
cheaper compared to
Sample D 199.1 ± 0.70 ± 0.82
helium.
Sample E 11.8 ± 0.46 ± 0.46 High supply reliability
thanks to argon.
Sample F 218.0 ± 2.24 ± 2.32

Only the nitrogen


molecule remains
untouched

15
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G8 GALILEO MS –
Infrared Furnace for
Diffusible Hydrogen &
Mass Spectrometer
for Utmost Sensitivity

Bruker’s infrared furnace offers perfect temperature


control with extremely slow or fast heating rates
and cooling within minutes.
A furnace with precise temperature control directly at the sample
is essential for the analysis of diffusible or trapped hydrogen.
Conclusions about the nature of the hydrogen deposition in the
metal structure can only be drawn by the exact correlation of the
outgassing temperature to the hydrogen concentration.
Bruker’s exclusive infrared furnace allows for extremely slow
or fast heating rates. The water cooling system of the furnace en-
sures that it cools down within minutes. The system is calibrated
using high-precision gas dosing.
The quartz furnace tube with its inner diameter of 30 mm is specif-
ically sized for large samples, such as the 1-inch weld samples.

Highest sensitivity – down to a few parts per billion


(ng/g) – is only offered by a mass spectrometer.
Mass spectrometry is widely recognized as an extremely sensi-
tive method that can analyze particle densities down to a few
molecules. However, in the traditional laboratory environment,
mass spectrometers are mainly used to analyze heavy molecules
and less for light elements or permanent gases.
With the G8 GALILEO MS, we offer the first industrial-grade
mass spectrometer coupled to an inert gas fusion analyzer, tailor-
made for the first element – hydrogen – and the determination of
argon. Previously unknown small concentrations of hydrogen and
argon can be routinely and easily analyzed thanks to the optimal
combination of extremely efficient gas inlet system, performance-
optimized ion source and highly sensitive detector.
As a matter of fact, it is built to last! The unique mass spectrometer
is robust, maintenance-free and functionally reliable to suit the
application environment.

Bruker is the only company worldwide offering the


smooth integration of an infrared furnace and/or
mass spectrometer into an excellent ONH system.
16
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G8 GALILEO G8 GALILEO MS G8 GALILEO MS

IR

MS MS
IR

O, N, H O, N, H O, N, H
dH Ar @ low ng/g dH & Ar @ low ng/g
TDS TDMS
@ low ng/g (ppb)

G8 GALILEO MS with infrared furnace


and mass spectrometer

Easily accessible particle filter, water-cooled


electrode furnace with FusionControl

Infrared furnace with thermocouple for an accurate


measurement of the actual sample temperature

G8 GALILEO MS for diffusible hydrogen


and highest sensitivity

Large diameter (Ø 30 mm) for 1-inch samples


like used in AWS A4.3

17
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:39 Seite 18

G4 PHOENIX MS G8 GALILEO MS

IR RF IR
High strength and low weight requirements
MS MS make the analysis of diffusible and trapped
hydrogen indispensable.
Applications of metallic materials in industry often
O, N, H require the properties of high strength and low weight.
dH @ low ng/g dH & Ar @ low ng/g
TDMS TDMS High-strength steels are increasingly used for modern
≥ 1,100 °C ≥ 3,000 °C assemblies, and highly complex stamped-bent designs
are made from rolled sheets and strips. The original
materials are rolled several times, thermally treated,
galvanized, bent, stamped, welded or coated during
the production process. The risk of penetration and
inclusion of reactive, atomic hydrogen occurring in all
environments increases with every production step.
Even the smallest amount of hydrogen can lead to
hydrogen embrittlement during recombination and
finally to component failure.

Using long-term measurements and tem-


perature profiles, Thermal Desorption
Mass Spectroscopy (TDMS) gives you
information about the type of hydrogen
inclusions within a metal structure.
@ low ng/g & TDMS The type of hydrogen inclusion – diffusible, weakly
or strongly trapped, or chemically bound – can be
directly correlated with the supplied activation energy
and leads to different peaks during the hydrogen
measurement using temperature profiles.
Don’t Miss a Molecule To ensure that long-term measurements of a few

–Thermal Desorption molecules are reliable, perfect temperature control


using an infrared or resistance furnace (depending on
the material) and a highly sensitive detector is required.
Mass Spectroscopy – Unique to Bruker’s G8 GALILEO MS, however, is the
use of a mass spectrometer for the trace analysis of
Only from Bruker hydrogen at concentrations of a few ng/g.

Highly sensitive hydrogen analysis using


TDMS is only available from Bruker.

Hydrogen Detection with Constant Temperature Hydrogen Detection with Temperature Ramp

Temperature

Hydrogen

0 10 20 30 40 50 60 70 0 10 20 30 40 50 60 70
Integration Time [min] Integration Time [min]
680 ng/g Hydrogen 620 ng/g Hydrogen

18
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:39 Seite 19

G8 GALILEO MS

MS

O, N, H
Ar @ low ng/g
300 μm
Metal structure without heat treatment,
argon content: 16,177 ng/g

Argon is the Element to


Analyze when it comes
to HIP and Additive
Manufacturing 300 μm

Metal structure after heat treatment, leading to


pore expansion due to argon gas expansion,
argon content: 16,177 ng/g

@ low ng/g State-of-the-art production processes,


such as Hot Isostatic Pressing (HIP), and
additive manufacturing require high-
precision argon analysis.
Compared to classical casting, forging, and machin-
ing processes, HIP and 3D printing offer many tech-
nical and commercial advantages. The objective of
modern processes is to produce a metal structure
that is as homogeneous and pore-free as possible,
even for complex component geometries. The
use of the inert gas argon is characteristic of these
production processes. However, argon is not only
used during component production, but also in the
atomization process during metal powder production.
As argon inclusions in the trace range can lead to
material failure of the component, the argon content
of process gases, metal powders, and final products
must be continuously monitored.

Hydrogen Detection with Temperature Steps Argon analysis? Only possible with the
G8 GALILEO MS for concentrations of
a few ng/g!
With the G8 GALILEO MS, Bruker is the only manu-
facturer worldwide offering a system for the reliable
and high-precision analysis of argon concentrations
of a few ng/g. Only the G8 GALILEO MS can deter-
mine whether the residual pores of a component
contain argon or other process gases. Other meas-
uring methods, such as optical microscopy or com-
0 10 20 30 40 50 60 70
puter tomography, fall short. The G8 GALILEO MS,
Integration Time [min] of course, can also be used as an ONH analyzer.
640 ng/g Hydrogen

19
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:39 Seite 20

Process Infrared & Mass


Gases Electrode Spectro-
Furnace meter

Carrier Gas:
Nitrogen, Helium, Argon

Calibration Gas:
Helium, Hydrogen, Argon
and Gas Mixtures
FusionControl low ng/g to %

Sample Mass MS
low ng/g
Spectro- H2/Ar to %
N2, He, Ar meter*)

Carrier Infrared °C!


Gas Furnace*) dH
IF
H2 IR
°C!
N2
Calibration Electrode
Gas Furnace EF CO
Ar
H2, He, Ar and
Gas Mixtures
Sample

Water-cooled electrode
furnace, optionally
with 20- or 40-position
autosampler, automatic
Easy switching between electrode cleaning and Industrial-grade mass
different carrier and calibra- automatic crucible changer. spectrometer tailor-made
tion gases. Precise temperature for hydrogen and argon.
N2 measurement with control of the sample with Detection limits in the lower
argon carrier gas: same FusionControl – exclusively ng/g range, particle density
analytical quality, without from Bruker. of a few molecules.
restriction, more affordable Additional infrared furnace*) State-of-the-art combination
and greater supply reliability. for diffusible hydrogen up to of extremely efficient gas
Unique gas calibration unit 900 °C – exclusively from inlet system, performance-
for standardless hydrogen Bruker. optimized ion source and
calibration with 10 inde- Easy accessibility and high-sensitivity detector.
pendent volumes. innovative design for high
reliability, maximum uptime
and low service costs.

20
*) Option
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:39 Seite 21

Nondisper- Smart Thermal


sive Infrared Molecule Conductivity
Detectors Sequence™ Detector
(NDIR) (TCD)

Emitted = Measured
1:1 Oxygen
1:1 Nitrogen
ng/g to % 1:1 Hydrogen ng/g to %

NDIR TCD
Detectors +
+ Reference
MS
Reference Channel
Channel Reference
H2 Path
Gas
Remove
CO
REF REF

+ H2 +
IR IR TC
CO CO N 2 H2

N2
low high ng/g to %
range range

N2 Path
Remove
CO and H2

Two powerful NDIR 1:1 analysis of emitted Scientifically proven


detectors*), one each for sample gases, unchanged. comparative measurement
low (ng/g) and high oxygen against reference channel.
Measurement for each
content (%).
element with optimal Heat exchanger for exactly
Powerful NDIR detector temperature and optimized the same temperature of
with electronic range sample preparation. reference and analysis gas.
selection.
No disruptive CO2, no Electronically optimizable
Drift free, due to reference unwanted hydrocarbons. measuring range of the
channel. TCD.
No multiple measurements,
Reliable, no moving parts, no oxidation, no conversion. N2 measurement with
and mature detector argon without restrictions.
No mathematical correc-
technology.
tions, no unpublished H2 measurement also with
algorithms. highly sensitive TCD.

21
*) Option
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:40 Seite 22

G4 PHOENIX G4 PHOENIX G4 PHOENIX MS

IR IR RF IR RF

MS

dH dH dH @ low ng/g
TDS TDS TDMS
≥ 900 °C ≥ 1,100 °C ≥ 1,100 °C

cm 6 5 4 3 2 1 0 1

G4 PHOENIX with infrared furnace (≥ 900 °C)


and resistance furnace (≥ 1,100 °C)

Metal Lattice

Ionic Covalent Molecule


Radius Radius Radius
[pm] [pm] [pm]
lattice distance
d = 287 pm
H+ · 0.00087 H 37 H2 202

Fe 63 Fe 125 – – –
· 3+

H +

H Li + 73 Li 134 – – –
Fe 3+

22
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:40 Seite 23

G4 PHOENIX MS –
The One and Only
Solution for Only
@ low ng/g & TD(M)S
One Task: Diffusible
Hydrogen @ its Best!

Hydrogen: its properties and The G4 PHOENIX offers one perfect


mechanisms of action are very solution for all three of these requirements:
remarkable and the subject of The G4 PHOENIX comes equipped with
G4 PHOENIX MS with
mass spectrometer many current research studies a highly sensitive thermal conductivity
worldwide – keyword: detector, for the analysis of hydrogen down
hydrogen embrittlement. to the ng/g range, and an infrared furnace
Hydrogen is the most common element in for accurate temperature control, very fast
nature, the lightest element in the periodic or very slow heating rates, rapid cooling,
table, and has the smallest atomic diame- and for temperatures up to 900 °C.
ter. Because of its small size, hydrogen dif-
The system is optionally equipped with
fuses effortlessly through any metal lattice.
an additional resistance furnace for higher
The challenging aspect about diffusible
temperatures, up to 1,100 °C.
0 1 2 3 4 5 6 cm hydrogen is that it collects within the de-
fects in the metal lattice and recombines at The G4 PHOENIX MS with mass
Typical steel welding samples,, that location to form much larger hydrogen spectrometer offers the ultimate solution
sample preparation acc. to ISO 3690 in terms of detection limits. It allows for
molecules. This results in an internal pres-
sure increase within the material, which hydrogen measurements with detection
ultimately leads to weak points, cracks limits in the lower ng/g range down to a
and material failure. particle density of a few molecules.

High-strength steels and oxygenated copper


Thermal Desorption Mass
grades are particularly susceptible to
Spectroscopy (TDMS) also
hydrogen embrittlement. There is a risk of
detects the type of hydrogen
introducing hydrogen in every mechanical,
deposition.
thermal and galvanic manufacturing step,
especially during welding and soldering. Temperature ramps and long-term
experiments in relation to the amount of
Large diameter (Ø 30 mm) for
typically 1-inch samples There is no better commercially hydrogen released enable conclusions
like used in AWS A4.3
available method for the analysis about the type of deposition and ultimately
of diffusible hydrogen other than about the type of material defects. The find-
carrier gas warm extraction, and ings from these experiments provide
no better system than Bruker's important information for process and
G4 PHOENIX MS. material optimization.

For the analysis of diffusible hydrogen, an


analyzer needs highest accuracy, extremely
low detection limits, and very precise
temperature control.
23
02719_Combustion_Analysis_MON58.qxp_210x279 16.03.18 13:40 Seite 24

aim 02719
Overview of Features and Benefits

Specification Benefit

Detectors Nondispersive IR absorption of CO, no moving parts, Reliable, maintenance-free performance


Oxygen dual-range detectors with reference beam and on-board without drift
linearization
Nitrogen and Hydrogen Thermal conductivity detector with reference channel Reliable, adjustable ranges, drift free
and adjustable gain amplifier
Argon and Hydrogen Mass spectrometer 1-100 amu, single quadrupole, Unique mass spectrometry performance,
optimized EI source and channeltron detector sensitivity: a few molecules
Carrier Gases He (O, N), Ar (O, N), N2 (H) each 99.995 % purity Flexible carrier gas choice without
(99.9990 % for trace analysis) compromises
Calibration Gas Pure gases or certified mixtures (99.999 % for each Easy, precise gas calibration without
compound), 10 individual volumes in the gas dose standards, directly tracable to fundamental
device to cover a huge range parameters (pressure, temperature, volume)
Sample Dimensions Electrode Furnace: 8 x 8 mm cross section (pieces,
chips, pins, granules), sample ports available for
special applications
Cooling Water Electrode Furnace: 4 l/min at 3 bar supply pressure Fits on every usual tap water line, tap
IR Furnace: 1 l/min at 3 bar supply pressure, water-saving design with solenoid valve,
15 – 20 °C inlet temperature, 100 – 240 V / 50 – 60 Hz chiller also possible

Bruker AXS is continually improving its products and reserves the right to change specifications without notice.
Power Supply 400 – 480 VAC (± 10 %), 50 – 60 Hz, 32 A, 7 kVA,
G8 GALILEO 1 Phase plus N or 2 Phase, grounding wire
Mass Spectrometer (MS) 230 VAC, 50 – 60 Hz, 250 VA Flexible, worldwide power and
current configurations
External Infrared Furnace 230 VAC, 50 – 60 Hz, 1,500 VA

G4 PHOENIX 230 VAC, 50 – 60 Hz, 2,200 VA

G8 GALILEO MS G4 PHOENIX MS

80 cm 63 cm 48 cm 63 cm 63 cm

83 cm
DOC-B78-EXS013 © 2018 Bruker AXS.
67 cm

48 cm 48 cm
30 cm

Depth 60 cm Depth 64 cm Depth 66 cm Depth 70 cm Depth 64 cm

~ 130 kg*) ~ 60 kg ~ 15 kg ~ 50 kg*) ~ 60 kg

*) Depending on configuration

Bruker AXS Worldwide offices Online information


info.baxs@bruker.com bruker.com/baxs-offices bruker.com/csonh-analysis

www.bruker.com

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