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think forward
Spectrometry Solutions
WDXRF
S8 TIGER(((
Bruker AXS
52
Instrument development begins with an analysis of users’ needs and analytical requirements.
What are their tasks and questions and what answers canwe provide? Which solutions will exceed their expectations?
In elemental analysis the analytical task is clear: which elements are in the sample and what are their respectiveconcentrations? The answers to these questions mustmeet the highest requirements with respect to accuracy,sensitivity and reliability.
However, users also expect the best solutions for morepractical problems: How can I reduce the time from sampling to result? What types of samples can I run andwhat is the easiest method I can use? How can I increasemy sample throughput and decrease my operating costs? Is there an instrument that is easy to use and meets my requirements?
The solution is surprisingly simple:
Elemental analysis with X-ray fluorescence allows you toreach your goals more rapidly, reliably and economically thanany other method. No other system combines flexibility,trouble-free operation and usability like the S8 TIGER.
Touch the
S8 TIGER(((
and
control its power
S8 TIGER with TouchControl™
3 54
Vacuum seal High intensity tube S8 TIGER status
TouchControl™ Automatic sample recognition Curved germanium crystal ( XS-Ge-C)
Range of detectors Automatic mask changer Automatic crystal changer
Collimators
Collimator masks
Filter wheel
EasyLoad™ with sample trays
Mobile on castors S8 TIGER with TouchControl™S8 TIGER – control its powerS8 TIGER with TouchControl™ S8 TIGER
76
The primary advantage of X-ray fluorescence (XRF) analysis is thatit is independent of the chemical bonding of the elements in the sample.
Other methods, such as ICP and AAS, require time-consuming,expensive and hazardous sample preparation techniques. XRF,however, can directly analyze each element without destroyingthe sample. With XRF, measuring any type of solid or liquid isas easy as 1-2-3.
Why is XRF so easy?
In XRF, the sample is excited with a primary X-ray beam, causing the sample to fluorescence. The primary X-rays ejectelectrons out of the inner atomic shells (K- and L-shell). The resulting “vacancy” is filled by an electron from an outeratomic shell.
This electron transition takes place only between the innershells of the atom, which are not involved in chemical bonding.Due to the independency of chemical bonding, the samplescan be analyzed directly without advanced sample preparation. This makes XRF the best method for elemental analysis.
How does XRF analyze elements?
During electron transition, an electron drops from a higher to a lower energy atomic shell to fill the vacancy. The difference in energy is released as X-ray fluorescence radiation. This radiation has a characteristic wavelength for each element.XRF uses these different characteristic wavelengths or ener-gies for elemental analysis.
What XRF techniques are available?
There are two different techniques. Energy dispersive X-rayfluorescence (EDXRF) analysis simultaneously acquires all X-ray energies emitted from the sample. The characteristic energies are separated using a single X-ray detector in a fixedposition. In contrast, wavelength dispersive X-ray fluorescence(WDXRF) analysis separates the characteristic wavelengthswith a very high degree of resolution. Optimized analyzer crystals and detectors are used to separate and count the emitted X-rays. WDXRF is unsurpassed in terms of analyticalaccuracy and precision.
How does X-ray fluorescence (XRF) work?
K
L
M
Ejected electron
X-ray
Bromine atom
X-ray fluorescence Kα
X-ray fluorescence Kβ
N
The sample is bombarded with X-rays. This excites the sample to generate X-rayfluorescence. The X-rays “shoot” individualelectrons out of the atoms of the elements,primarily out of the inner atomic shells K and L. The resulting vacancies are filledup again by electrons from higher energyshells. The excess energy of these elec-trons is then emitted in the form of X-rayfluorescence radiation. This radiation ischaracteristic for each element like a fingerprint and independent of the atom’s chemical bond. The intensity of the radiationis proportional to the concentration of theelement in the sample.
Wavelength dispersive X-ray fluorescence (WDXRF) with the S8 TIGER
X-ray source
Filter wheel
Vacuum seal
Heavy elements
setup
Light elements
setup
Collimator changer
Crystal
changer
Scintillation counter Proportional counter
Mask changerSample
XRF – source
of speed and power
Optimal analysis of all elementswith ultimate precision and accuracy
Independent of chemical bonding
Direct, non-destructive analysis ofsolid, powder and liquid samples
Easy sample preparation withinminutes
Safe method, no hazardous chemicals needed
The X-ray source and primary radiation filter guarantee that each element in the sample is optimally excited.
The masks cut out unwanted signals, e.g. from the sample cup.
The vacuum seal separates the sample chamber fromthe goniometer chamber. During loading the seal is closedand the goniometer chamber remains under vacuum. There-fore only the small volume of the sample chamber needs tobe evacuated for solids or flushed with helium for liquids. Dur-ing the measurement of liquids the vacuum seal stays closedto protect the components in case of spillage, safes heliumand enhances the stability.
In the case of wavelength dispersive X-ray fluorescence (WDXRF) each element is analyzed under optimal measurement conditions. For this purpose individual combinations of measurement parameters are set corresponding to the concentrationrange and to prevent line overlaps:
The collimators are used for improving resolution.
The analyzer crystals play a crucial role. They break down the multiple frequency fluorescence spectrum into the specific wavelengths for the elements. This signal separation is crucial for the outstanding resolution and sensitivity of WDXRF.
And finally, the detectors: For the detection of light ele-ments a proportional counter and for the heavier elementsa scintillation counter is used. Both detectors are perfectlysuited to the respective energy range.
9
The goal of any analysis is to producethe most accurate results in the shortest possible time. In elementalanalysis, speed leads to the shortesttime-to-result and the highest samplethroughput. Speed, accuracy and relia-bility demand outstanding technology.
S8 TIGER – Speed meets power.
Speed & Power
General Requirement
Advanced Requirement
Cement & Raw
Materials
Petro-chemistry
Minerals & Mining
Geology Metals & Slags
Ceramics,Refractories,
Glass
Plastics & Polymers
Chemistry & Catalysts
Research & New
Materials
Waste & Environ-
ment
1310
S8 TIGER
Performance
Ease of use
Lowest limit of detection
Best long term stability
Ultimate light element performance
Shortest time to results
Highest analytical flexibility
Material specific solutions
Universal standardless analysis
S8 TIGER(((
–
impressive technology
at your command
Lowest
Detection
Limit
Counts per
Second
(cps)
Min.
Time to
Result
Plug’n
Analyze
No
Detector
Gas
No
Cooling
Water
Industry proven elemental analyzer
Most flexible beam path
Unrivaled analytical performance
Lowest limit of detection
Highest analytical stability
12
Automatic collimator
changer:
4 position collimatorchanger
Optimized sensitivityand resolution for anyanalytical requirement
Huge selection of different openings from 0.12 – 2°
Automatic crystal
changer:
8 position crystal changer
Selection of more than15 crystals available
Application optimized analyzer crystals:
- Curved XS-Ge-C for lowest detection limitsof P, S, Cl
- High intensity XS-B for B
- Highest stability crystalfrom Al to S
Detectors:
Sealed proportionalcounter with high-transmission window
- Best light elementanalysis
- No counter gas required
High efficiency flowmeter for light element detection
High sensitivity scintillation counter for optimal heavy element detection
Vacuum seal:
Separation between sample and goniometerchamber
Unique protection of thegoniometer during themeasurement
Reduced helium consumption
Instant switch betweenliquid and solid samples
Automatic mask
changer:
Accommodates up tothree different masks
Ideal for the automatedanalysis of different sizedsamples
Optional contaminationshield to protect the goniometer
10 position filterwheel:
Optimized peak to background ratio for each element
Huge selection of filter materials and thick-nesses (Al, Cu, Brass)
X-ray tube window protection (DuraBerylliumshield – optional)
High precision masks:
Optimized beam path forsmallest samples
Lowest background, improved signal to noiseratio
Best possible detectionlimits for smallest sam-ples
S8 TIGER 3K:
High analytical perform-ance for industrial applica-tions
Full WDXRF, most flexiblebeam path
No compressed air
Dust sealed cabinet
Smallest footprint
Unique analytical performance, lowestcost of operation:
Impressive analytical performance, robust design:
Undisputed leader of the performanceclass:
S8 TIGER
Performance
Ease of use
Lowest limit of detection
Best long term stability
Ultimate light element performance
Shortest time to results
Highest analytical flexibility
Material specific solutions
Universal standardless analysis
S8 TIGER(((
–
impressive technology
at your command
Lowest
Detection
Limit
Counts per
Second
(cps)
Min.
Time to
Result
Plug’n
Analyze
No
Detector
Gas
No
Cooling
Water
Industry proven elemental analyzer
Most flexible beam path
Unrivaled analytical performance
Lowest limit of detection
Highest analytical stability
S8 TIGER 1K:
Highest intensity in class
No cooling water
No compressed air
No detector gas (option)
Economical, low electricalpower consumption
Smallest footprint
S8 TIGER 4K:
Superior analytical performance
170 mA at 4 kW for ultimate light element performance
Full 4 kW for lowest limitof detection
Most flexible beam path
No compressed air
Dust sealed cabinet
Smallest footprint
Light and heavy elements, solids and liquids,ppb to 100 % ... the demands made on XRF arechallenging and diverse. In order to provide theperfect solution to any analytical question, wehave integrated cutting-edge technology in theS8 TIGER.
Our technology starts at the source, the X-ray tube. The highintensity X-ray source provides the specific excitation energyfor every element; high-energy X-rays for the analysis ofheavy elements, and low-energy X-rays for light elements.You get distinctly improved detection limits for all elementsthroughout the periodic table.
To prevent air from absorbing the fluorescent X-rays, solidsare measured in a vacuum and liquids and loose powdersare measured in a helium atmosphere. With the S8 TIGER,the change between the different modes is very fast and reliable. In addition, both the X-ray tube and the beam pathare shielded against contamination. The high transmissionvacuum seal - unique to our spectrometers - protects thesensitive components in the spectrometer chamber evenduring actual measurements. In the event of sample break-age or leakage due to improper preparation, the samplechamber is easily accessible for cleaning.
Prior to measuring liquids and loose powders, the S8 TIGERonly needs to flush the sample chamber with helium. Whilethis is a matter of seconds with our system, the same procedure can easily take up to fifteen minutes with conven-tional systems that need to purge the entire goniometerchamber. The advantages of the S8 TIGER are easily apparent:switching between solid, powder and liquid samples asneeded without time-outs, extremely low helium consump-tion and absolute protection of the goniometer chamber.
In wavelength dispersive XRF, analyzer crystals are of vitalimportance. The S8 TIGER is equipped with up to eight high-performance crystals, each optimized for a specific elementrange and application. The benefits are outstanding resolu-tion of adjacent peaks from different elements and minimumdetection limits down to the ppb level. After diffraction bythe analyzer crystal, the X-ray signal is collected by the detec-tor. With the S8 TIGER, innovative proportional counters with,and without, the need to purge detector gas are available foranalyzing light elements. Sophisticated scintillation countersare available for the analysis of heavy elements.
To ensure maximum precision and accuracy, the spectrome-ter components interact seamlessly. All moving parts of thehigh precision mechanical goniometer on the S8 TIGER aresynchronized by electronic gearing. The S8 TIGER is a truepowerhouse instrument with the most compact dimensionspossible.
10
Sample loader:
EasyLoad:
Sample trays for convenient operation
Automatic liquid sampledetection
Selection of sample magazines:
Bare samples
Sample holders for flexibility
ONLINE interface for con-nection via belt or robot
X-ray tube:
1 kW: Unique excitation
Highest intensity in classwithout cooling water
Up to 50 kV or 50 mA
4 kW: Superior analyticalperformance
Highest excitation intensity
170 mA at 4 kW
Closest coupling anode to sample
15
S8 TIGER(((
– the fastest,
the strongest and the
fittest
Electronic gearing : The fastest, high-precision scanning – monitoring of samples in less than 2 minutes
High intensity X-ray source: The strongest – 170 mA and 24 kV at full 4 kW; best light element performance
XS-CEM analyzer crystal: The benefit is the most precise and accurate results with unrivaled stabiltity for Si and Al
0 2000 4000 6000
Running time [h]
Co
nce
ntr
atio
n [
%]
100,00
100,50 + 0,08 %
- 0,08 %
101,00
101,50
99,50
99,00
98,50
8000 10000 12000
XS-CEM
analyzer crystal
Unrivaled stability
Temperature independent
Benefit from the most precise and extremely accurate results
Electronic gearing
Accurate and precise positioning
High speed scans
Shortest time-to-results
Highest sample throughput
0 50 100
Current [mA]
Intensity
Ph
oto
n e
mis
sio
n [
%]
60
80
170
100 %100
120
40
20
0
150 200
High intensity
X-ray source
170 mA for best light element analysis
Full 4 kW for highest sensitivities
Most compact beam path, shortest sample to anode distance
Cool tube head for delicate samples
High intensity X-ray tube for bestexcitation
Best light element performancedue to 170 mA and most compactbeam path
Application optimized analyzercrystals
Unrivaled long-term stability dueto unique XS-CEM for Al and Si
strongest
fittest
Survival of the fittest! In XRF, fitness is determined by means of twodecisive factors - performance and speed; in order to survive, themost reliable and best possible results are needed.
Apart from its powerful, compact appearance, whatmakes our S8 TIGER the power pack for all elements?
Performance begins at the source of excitation. The new high intensity X-ray tube offers over 20% higher intensity compared to conventional X-ray tubes. Due to the great flexibility of the voltageand current, it permits target excitation of the element ranges. No sequential X-ray spectrometer offers greater performance.
Innovative, patented and award-winning: The analyzer crystals of our S8 TIGER.
Up to now, the analysis of boron in the ppm range was regarded as a trick that only experts were able to perform. Our new XS-B crystalat last permits analysis and detection limits in the lower ppm rangeto be performed as part of routine operation. XS-B provides: Twice the intensity and improved resolution at the same time. In addition to boron, for other light elements the multilayer crystals ofthe XS series also yield up to 30% more signal.
Unmatched stability for aluminum and silicon due to XS-CEM. The XS-CEM puts an end to thermal instabilities and long-term drifts.This is especially important when examining industrial minerals, cement, ceramics or glass. XS-CEM delivers what it promises.
Saving the best for last: The XS-Ge-C focusing analyzer crystal. This curved germanium crystal provides up to 50% more intensityfor the elements phosphorous, sulphur and chlorine.
Linear intensity range for major, minor and trace elements with 10 million cps – no compromises, no time loss and under optimal measurement conditions: DynaMatch™.
You are familiar with the problem of analyzing completely unknownsamples: either the peaks of the traces get lost in the backgroundnoise or the major elements overwhelm all others. Therefore, otherXRF systems have to make substantial compromises, optimizing the measurement either for the matrix elements or the traces. The S8 TIGER with DynaMatch adapts the power dynamically during the measurement and facilitates optimal conditions and results for all concentration ranges – without any compromises and fully automatic.
You can see that our S8 TIGER is faster, stronger and fitter – a true power pack.
14
fastest
Time < 2 min
Anyone can perform measurements;operation is simple and intuitive.These are not just dreams, but the reality of TouchControl with the S8 TIGER. Safe sample handling, automatic recognition, instant switching between solids and liquids,accommodating various sample sizes and a large sample magazine …in two words, EasyLoad and SampleCare.
S8 TIGER – the touch of your finger is all it takes!
TouchControl™, EasyLoad™ & SampleCare™
17
1918
Can anyone obtain high quality results without the need for extensive training or special skills? Yes, thanks to TouchControl™!
This is because with TouchControl we have consistentlyfavored easy, intuitive operation. The times of never-ending explanations, manuals that weigh a ton and operationwith adventures in body positioning belong to the past. With TouchControl, any user can perform measurementsjobs on the S8 TIGER. Using the touchscreen this is done asfollows: First, select the application and key in the sampleID. You can also add additional information, like preparationor sample weight. Then simply start the measurement andview the results on the monitor.
But it can be even easier: An operator places a sample in the loader and taps the touchscreen once; this starts apredefined automatic application – and that’s it.
With the touch of a few buttons the S8 TIGERmakes your worklife simple and easy.
The ultimate in
ease-of-use
– S8 TIGER(((
S8 TIGER with TouchControl™, EasyLoad™ & SampleCare™
TouchControl™:
Easiest operation due to intui-tive touchscreen interface:Three steps to accurate results!
No operator training required
Standalone operation in toughenvironments (no PC, mouseor keyboard)
Unmatched data integrity:Routine analysis is separatedfrom advanced tasks like cali-bration, evaluation, and exten-ded reporting
Online language switch withfree selection: English, German, French, Chinese,Russian, Spanish, Korean, Turkish, Portuguese, Italian,…
Tailored for industrial environ-ments, ”round-the-clock“ operation
Easiest operation with TouchControl™
1
The measurement of any sample is as simple as it couldbe: Just place the sample in themagazine and select the applica-tion! Perfect for industrial use:All routine applications are quickstart buttons!
2
Quick: Now you type in thesample ID. Direct on the touch-screen, no hassle with a PC,mouse or keyboard: Simplypress “MEASURE” to analyze!There is nothing to remember,it’s simply step-by-step.
3
Instant results: Each result is displayed on the touchscreen,sent to the printer and stored in the results database. Limit values are checked automati-cally and reported color coded.Different user access levels protect relevant data!
Start priority samples right away,pause running samples and continue
Ergonomic and quick sample loading
Reliable and fail-safe analysis –GLP compliant data protection
Designed for highest instrument uptime
2120
EasyLoad™:
75 positions, convenient handling
40 positions on two trays
35 positions on fixed positions
Ergonomic sample loadingwith trays
Fail-safe operation with auto-matic recognition of loosepowders and liquid samples
Industry proven tough hand-les and trays (no toys)
Direct handling of 51.5 mmrings from automated sample preparation
ONLINE version for con-nection via belt or robot
SampleCare™:
Low maintenance andhigh instrument uptimedue to unique protectionduring loading and unloading:
- Two integrated conta-mination shields fortube and goniometerprotection
- Dust reservoir
Unique protection duringmeasurements
- DuraBeryllium™ shieldfor tube window protection
- Unique vacuum sealwith high transmissionwindow for goniometerprotection
Easy, safe
and reliable
– S8 TIGER(((
–
work, as work
should be
SampleCare™ and EasyLoad™: the perfect combination for makingwork easier and fail-safe. In otherwords: industry proven.
Thanks to SampleCare you can rely on the S8 TIGER 100%. SampleCare constantly protectsall important system components from contamina-tion, which might lead to incorrect results or in theworst case to system stoppage. Our S8 TIGERwith SampleCare prevents this safely in 4 ways:The DuraBeryllium tube shield protect the head ofthe X-ray tube; the mask changer and the vacuumseal protect the goniometer chamber. If, by chanceanything should have gone wrong during prepara-tion, and the sample breaks or leaks out, it is not aproblem. System components are well protected,easy to access and can be cleaned with little effort.
EasyLoad makes work incredibly simple and gives you a sure hand: Either insert samples intoone of the fixed positions or fill a prepared sampletray as required, start the measurement or a wholemixed series of measurements and ... that's it!Thanks to EasyLoad that is all you have to do andyou need not worry that anything will go wrong.Owing to the automatic identification of the sampletype – solid or liquid – EasyLoad reliably preventsincorrect operation, such as measurement of liq-uids or loose powders under vacuum.
S8 TIGER with EasyLoad™ and SampleCare™ – sometimes you wonder:”Why didn’t someone else think upthese ideas before?“
Contamination
shields
Grabber with
automatic
sample
detection
Vacuum seal
Mask changer
Dust reservoir
DuraBeryllium
tube shield
Safe sample handling with SampleCare™
Dust
Liquids Sample Magazines – fit for every purpose
1
2
34
35
6
3
1
2
3
4
5
6
1
The right selection for alarge number of samples:108 positions, 40 mm diameter, flat
2
For highest sample flexibility: 60 positions forcup operation for auto-matic loading of all kinds ofsamples: large (51.5 mm),small, irregular shaped orheavy
3
Mixed operation: directhandling of bare, flat sam-ples (diameter 40 mm)and sample cups
Safe analysis of delicate sampleswith automatic sample recognition
Unique instrument protection dueto contamination shields
Lowest maintenance and bestsystem uptime
Most flexible sample handling –convenient sample loading withtrays
22
Flexibility is the ability to master a wide variety of challenges. Analytical flexibility means being able to characterize all elements, all concentrations and all types of samples.
With speed andperfection, flexibility becomes performance – the S8 TIGER.
Performance & Flexibility
Your standards
and SPECTRAplus
are all you need,
most of the time …
Seamless integrated standardlessevaluation for all kind of samples
Complete easy-to-use analyticalsoftware package for calibration,evaluation and reporting
Integrated Analytical Intelligence to achieve maximum analytical performance
Powerful state-of-the art fundamen-tal parameter matrix correction withunique variable alphas
User specific calibration (e.g.)
Elements available with WDXRF
Not availabe
27
SPECTRAplus brings additional performance to the powerful S8 TIGER – the XRF dream team!
We make it simple: SPECTRAplus analytical software package is all you need to start, run and win the most advanced analytical challenges!
But let’s proceed in the correct sequence:
1) The application
It is quite simple to create applications: SPECTRAplus
directly follows your workflow - from the definition of standard samples, through sample preparation, the calculation of the calibration and on to the final release ofthe application. SPECTRAplus supports you in all these steps:When creating your own measurement method, the integrated Analytical Intelligence assists you to achieve the best performance of the S8 TIGER. For matrix correction, you have the choice of theoretical and empiricalcoefficients as well as unique variable alphas.
2) The measurement
To start your measurements, you only enter the sample data and assign the measurement method. That’s all! With asimple click you can even launch a whole series of samples.
3) The evaluation
Whether it is qualitative or quantitative evaluation –SPECTRAplus leaves all options open: Scan measurementsare always evaluated fully automatically, the elements areidentified and the concentrations are calculated. If you like,you can check and refine the results interactively.
4) The reporting
You define your own printout format, summarize the resultsin tables, and export the data to other programs just as youwish and need. For GLP compliant documentation the results are also archived in SPECTRAplus.
You see – even complex analytical tasksbecome straightforward with SPECTRAplus!
CALIBRATION
Element with selected analytical line
Calculated deviation of the calibration
Calibration curve
Matrix correction model: FP, variable alphamodel, empirical, theoretical,…
Overlay correction 5
4
3
2
1
INTERACTIVE QUANTITATIVE EVALUATION
Sample ID, database search
Element with calculated result, analytical line
Display of selected element peak
Alternative analytical line
Data export to result database, export and print5
4
3
2
1
12
34 5
1
2
3
4
5
24
25 27
… if you need
more elements than
your calibration offers,
just combine it with
QUANT-EXPRESS™
User-specific calibration (e.g.)
Elements with QUANT-EXPRESS calibration
Not available
Added elements with QUANT-EXPRESS calibration
Conventional “either-or” analysis Unique “as-well-as” analysis: seamless integration with QUANT-EXPRESS™
Either standard-based or standardless. Standard-based as well as standardless that’s QUANT-EXPRESS™
Conventional analysis is: Either standard-based or standardless.
”Either-or“ means: Either you have calibrated your systemwith your standards for routine work and know exactlywhich elements and concentrations you are looking for, oryou have an entirely unknown sample and want to obtainboth qualitative and quantitative information. Conventional systems work according to this “either-or” principle.
Our S8 TIGER is significantly better and more flexible. This is because our S8 TIGER withQUANT-EXPRESS™ can do both – we name it“as-well-as” analysis – not just “either-or”!
“As-well-as” means: Thanks to QUANT-EXPRESS the divide between standardless evaluation and standard-basedcalibrations has been eliminated. You benefit both from theadvantages of customized calibrations with your own stan-dards (maximum accuracy and maximum precision), as wellas from the flexibility and versatility of QUANT-EXPRESS.QUANT-EXPRESS comprises a unique multipurpose calibration prepared by us using innumerable certified standards. All our skill and experience of decades in XRFhave been invested in these calibrations and measurementmethods. We call it: integrated Analytical Intelligence.
QUANT-EXPRESS not only enhances the potential of your routine system, it also assists you with other tasks.When setting up your own calibrations, QUANT-EXPRESSautomatically creates the optimal measurement method tomatch each element and concentration range – quickly, simply and reliably.
The real class of QUANT-EXPRESS comes fully into its own, when performing the fast, reliable and completeanalysis of unknown solid and liquid samples.
Less than two minutes for a qualitative andquantitative screening of unknown samples –only QUANT-EXPRESS™ can do that for you.
SPECTRAplus brings additional performance to the powerful S8 TIGER – the XRF dream team!
We make it simple: SPECTRAplus analytical software package is all you need to start, run and win the most advanced analytical challenges!
But let’s proceed in the correct sequence:
1) The application
It is quite simple to create applications: SPECTRAplus
directly follows your workflow - from the definition of standard samples, through sample preparation, the calculation of the calibration and on to the final release ofthe application. SPECTRAplus supports you in all these steps:When creating your own measurement method, the integrated Analytical Intelligence assists you to achieve the best performance of the S8 TIGER. For matrix correction, you have the choice of theoretical and empiricalcoefficients as well as unique variable alphas.
2) The measurement
To start your measurements, you only enter the sample data and assign the measurement method. That’s all! With asimple click you can even launch a whole series of samples.
3) The evaluation
Whether it is qualitative or quantitative evaluation –SPECTRAplus leaves all options open: Scan measurementsare always evaluated fully automatically, the elements areidentified and the concentrations are calculated. If you like,you can check and refine the results interactively.
4) The reporting
You define your own printout format, summarize the resultsin tables, and export the data to other programs just as youwish and need. For GLP compliant documentation the results are also archived in SPECTRAplus.
You see – even complex analytical tasksbecome straightforward with SPECTRAplus!
CALIBRATION
Element with selected analytical line
Calculated deviation of the calibration
Calibration curve
Matrix correction model: FP, variable alphamodel, empirical, theoretical,…
Overlay correction 5
4
3
2
1
INTERACTIVE QUANTITATIVE EVALUATION
Sample ID, database search
Element with calculated result, analytical line
Display of selected element peak
Alternative analytical line
Data export to result database, export and print5
4
3
2
1
12
34 5
1
2
3
4
5
QUANT-EXPRESS™ – Fit for every purpose
Fast Screening: Less than 2 minutes –a complete overview of your sample
Full Analysis: the full quantitative evaluation in 7 minutes
Best Detection: Powerful standardless evaluation down to the ppm level in 14 minutes
3
2
1
QUANT-EXPRESS™: Unique Line Library with Integrated Analytical Intelligence
Element line for a specific concentration range
Measurement conditions (peak position, excitationparameters, crystal, collimator, detector)
Calibration coefficients
Overlapping lines with correction factors4
3
2
1
312
1 2
3
4
28
As you already know, one main advantage of the XRF is thatalmost all elements of the periodic table can be measuredquickly and easily in all concentrations. However, one thingis clear:
Good quality samples are the basis of goodmeasurement results!
This sounds reasonable but other analytical methods keepsilent on this subject. Why is that so?
Quite simply, the way to good samples is significantly easier, more reliable and hence considerably cheaper using XRF analysis. The advantage of XRF over other methods isits ability to handle a wide variety of samples, including powders, liquids and solids. Unlike other methods, there is no need for elaborate dilution, digestion, or enrichment, nor must the instrument be recalibrated constantly.
Nevertheless, even for XRF samples must be selected and prepared correctly. This begins with representative sampling, goes through homogenization and ends with a smooth measuring surface.
So you can see that, unlike other methods, sample preparation for XRF is by no means sorcery. But if you stillneed a little help, we do not leave you out in the cold. Weare glad to advise you on selecting the correct equipmentand setting up sample preparation geared for your material.Ultimately, you obtain optimal procedures that your staff canfollow and perfect results, measurement after measurment.After all this is what counts!
So many samples,
so little time
Direct analysis of solids,powders and liquids
Safe method – no hazardousmaterials needed
Lowest cost of operation
Simple recipes for reliable results
Sample preparation
31
Pressing
5 min
Melting
10 min
Dripping
15 sec
Polishing
1 min
Direct
5 sec
Pressed pellets Database Query
Glass beads Automatic and interactive evaluation
Sample cups Print your results
Metal cuts
Direct Lines in SPECTRAplus
Prepared Samples Analytical Results
Copy and Export all relevant dataHTML, XML, TXT,…
Get pressed pelletPour powder intosample press
Finished powder material
Mill in grinding vesselAdd grinding tablets Use weighed amountof sample
Casting mold with finished glass bead
Heat crucible in melting furnace
Pour material into crucible
Pipette sampleamount to definedweight
Check for holesCover bottom of liquidcup with transparentfilm
Check surfaceMillCheck sample heightat molding cutter
Clamp metal cut
Mix sample and fluxAdd sample to fluxmaterial
Weigh sampleamount
Pour flux meltingagent into mortar
Pressing
5 min
Melting
10 min
Dripping
15 sec
Polishing
1 min
Fix the sample withthe clamp, ready
Mount the small sample in a cup using a small mask
Direct
5 sec
29 3130
Pressed pellets Database Query
Glass beads Automatic and interactive evaluation
Sample cups Print your results
Metal cuts
Direct Lines in SPECTRAplus
Prepared Samples Analytical Results
We are by no means telling you a secret if we point out thatthe most frequent form of sample preparation for XRF is thecreation of pressed pellets. The reason for this is clear, sincethe method is ingeniously simple and fast: Weigh out sam-ple material, grind and press it, and put the pressed pelletinto the S8 TIGER. To ensure that you obtain reliable and re-producible results, all you have to do is find the right recipeand then stick to it every time!
To obtain the most accurate results for major and minorcomponents you can melt the powder together with a fluxing agent. After it cools down, you have a glass disk ofhomogeneous composition.
Preparation of liquid samples is the easiest of all. For thispurpose, you use a cup covered with a transparent plasticfilm. Fill the cup with the predefined quantity of liquid andthen place the cup into the S8 TIGER. By the way, thismethod is also ideal for loose powder.
Finally, here is the preparation method for all solid samplessuch as metals or ceramics: cut, mill, grind or polish – anything that creates a smooth and clean sample surface isfine. If the sample already has an appropriate surface, youcan directly insert and measure it.
So you can see that sample preparation for XRF analysis is certainly not alchemy. Rather, it involves following simplerecipes. For your convenience and with a little “magic”,sample preparation can also be fully automated.
Sample preparation –
simple recipes, not
rocket science
Fast and easy with pressed pellets
Most accurate results with glass beads
Cup loading for loose powders and liquids
Solids with clean and smooth surfaces
Direct analysis of small samples
Copy and Export all relevant dataHTML, XML, TXT,…
Sample size Liquids, loose powders: up to 50 mlSolids: up to 51 mm (2”) Ø , 47 mm (1.8’’) in height
Collimator Automatic collimator changer (up to 4)
Masks Automatic mask changer (up to 3)Additional high precision masks available
Analyzer crystals Automatic crystal changer (up to 8)Included: XS-55, PET, LiF (200) Optional: XS-B, XS-C, XS-N, XS-PET-C, XS-CEM, XS-Ge-C, LiF (220), LiF (420), ADP, Ge, TlAP, InSb
DynaMatch™ Linear intensity range more than 10 million cps
Vacuum pump Integrated
Gas for analysis of liquids Helium or nitrogen, at reduced or normal atmospheric pressureand loose powders
Systems S8 TIGER 1K S8 TIGER 3K S8 TIGER 4K
1 kW 3 kW 4 kW50 kV max. 60 kV max. 60 kV max.50 mA max. 150 mA max. 170 mA max.
Power requirements 208 – 240 V (1P/3P) 208 V, 60 Hz (1P/3P)50/60 Hz 230 V, 50/60 Hz (3P)
Compressed air Not required
Detector gas No detector gas for PRO4 P10 gas (10% methane, 90% argon) sealed proportional counter for flow counter
External cooling water No cooling water Cooling water Water consumption automatically regulated and minimized, short term interruptions are compensated
Dimensions 135 cm x 84 cm x 90 cm; 135 cm x 84 cm x 104 cm; (height x width x depth) 53.1” x 33.1” x 35.4” 53.1” x 33.1” x 41”
Touchscreen: Allows additional width of 49 cm (19.3’’)446 kg 476 kg
TouchControl™ 1) Integrated touchscreen for easy and intuitive operation
SampleCare™ 1) X-ray tube and goniometer protected by contamination shieldsSample and spectrometer chamber separated by programmable vacuum seal
EasyLoad™ 1) Automatic sample recognitionPortable sample trays
Quality & safety DIN EN ISO 9001:2000 CE certified Fully radiation protected system; radiation < 1 µSv/h (BfS 09/07 V RöV)
Technical Data
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Bruker AXS Inc.
Madison, WI, USAPhone +1 (800) 234-XRAYPhone +1 (608) 276-3000Fax +1 (608) [email protected]
ww
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921
1) optional packages
Bruker AXS GmbH
Karlsruhe, GermanyPhone +49 (7 21) 5 95-28 88Fax +49 (7 21) 5 95-45 [email protected]
www.bruker-axs.com
TouchControl™, SampleCare™, EasyLoad™, DynaMatch™, QUANT-EXPRESS™ and SPECTRAplus™are trademarks of Bruker AXS Inc.
think forward
Diffraction Solutions
XRD
D2 PHASER
Bruker AXS
2
D2 PHASER – all-in-one desktop design
Compact all-in-one desktop design
Innovative high-end goniometer design
Integrated PC / monitor
DIFFRAC.SUITE software
Leading detector technology
3
Status display LEDs
1-dimensional LYNXEYE detector
USB and Ethernet connectors
D2 PHASER with openedfront cover
Transport handles
Internal chiller
Integrated drawer for keyboard and mouse
X-ray on status LEDs
What do you obtain when patented technologies, award-winning software, a fully functional PC with monitor and state-of-the-art detectors meet up with leadership in innovative X-ray diffraction?Perfect solutions for powder diffraction. And if it all fits onto a desktop, it is called D2 PHASER!
What enables this evolutionary leap to take place andhow can the amazing performance of this space savingsensation actually be explained?
First of all, you develop an ultra compact goniometer, file a patent, complete the system with all the other components for autonomous operation and package thewhole configuration together with a fully functional PC,monitor, keyboard and mouse, into a compact housing.
Second, you use the unique DIFFRAC.SUITE software for controlling the instrument and analyzing the data.Since its introduction the DIFFRAC software has devel-oped into a high performance tool for the characterizationof crystalline phases in research and industry.
Third, you use only the best components, for example the LYNXEYE detector. This state-of-the-art and extremely efficient 1-dimensional detector simultane-ously captures a large angular range and radically reducesthe measurement time: hours turn into minutes.
Combining all of these incredible innovations creates adesktop X-ray diffractometer which has the analytical performance and functions of a large instrument, butwhich is easy to transport and opens up the whole worldof powder diffraction without a lot of infrastructure.
D2 PHASER – never before was desktop X-ray diffraction better, smaller and morepowerful!
The whole world
of X-ray diffraction
on a desktop –
D2 PHASER
4
D2 PHASER – slide-up front cover for sample loading, monitor remains active
Phase identification and quantification
Degree of crystallinity determination
Phase properties (cell parameters, crystallite size, and lattice strain)
Crystal structure analysis
Wide variety of different sample holders of industrial standard dimension (Ø 51.5 mm)
Holders with various cavities
Holder for automatedsamplepreparation
Holder forclays
Low back-ground holders forsmall sampleamounts
Airtightholder for environment-sensitivesamples
Holder for filter samples
5
Wishes come true – comprehensive, unique and non-destructive characterizationof crystalline samples by means of X-ray diffraction (XRD) with the D2 PHASER.
Our D2 PHASER opens the door to modern XRD for you.This means qualitative and quantitative phase analysis,polymorphism investigation, the determination of crystallinity, all the way through to structure investigation– all of it fast, simple, efficient and with high quality.
It is not just its analytical performance that makes the D2 PHASER so revolutionary, but also its flexibility in handling very diverse samples. Different material properties require different sample preparations. Therefore, besides a series of standard sample holdersmade from PMMA or steel, the D2 PHASER also offersholders for small sample amounts, low-absorbing andweakly diffracting samples, for filters, for environment-sensitive samples and for examining materials that tendto show a preferred orientation.
LYNXEYE fast-lane edition
What makes the D2 PHASER absolutely unique is the integration of the world's leading 1-dimensional detectorfor X-ray powder diffraction: Our LYNXEYE.
With a performance enhancement in terms of intensityby a factor of more than 150, the D2 PHASER is actuallyplaying in the top class. Additionally the LYNXEYE allowssuppression of sample fluorescence providing an excel-lent peak-to-background ratio even for strongly fluores-cent samples, eliminating any need for secondarymonochromators.
D2 PHASER – X-ray diffraction in a new dimension!
D2 PHASER – the
desktop giant!
Cement & Raw Materials
Minerals & Mining
Geology & Exploration
Ceramics
Chemistry & Catalysts
Research& Education
Pharmaceuticals Environment
6
Plug’n
Analyze™
Hand Carry
Weight
On-Site
Ready
No
Water
Supply
No
PC &
Peripherals
No
High
Power
Can XRD – the best method for phase characterization – really produce high quality data without the need for a corresponding infrastructure?
Yes! With our D2 PHASER a new era begins. All that is required is a simple domestic wall socket andyou can start producing outstanding analytical results: Plug ‘n Analyze. Since it is a desktop system it requiresonly a minimum amount of space and is in no way inferior to a large system in terms of its analytical performance. Resolution, angular accuracy and data statistics set new standards in this class of analytical instruments; data quality which you can rely on and withwhich even complex questions can be answered.
Our D2 PHASER is a transportable all-in-one instrumentthat requires no additional cooling water or PC peripherals.This means that there is nothing to prevent it from beingused outdoors: simply switch-on a power generator, plugin the connector and start measuring!
D2 PHASER – X-ray diffraction tool for everyone – everywhere!
All-in-one is every-
thing you need –
D2 PHASER
Minimal electrical power consumption (650 W)
No cooling water supply
No significant tube ageing –practically endless tube lifetime
Minimal space required7
DIFFRAC.EVA
Qualitative phase identification - ICDD PDF2 and PDF4- User-defined databases
Semi-quantitative phase analysis - RIR method- Combined XRD-XRF analysis
Publication-ready reporting
DIFFRAC.TOPAS
Quantitative Analysis
Quantitative phase analysis- Crystalline phases- Amorphous phases
Degree of crystallinity determination
Spiking method
PONKCS method
DIFFRAC.TOPAS
Structure Analysis
Indexing (LSI and LP-Search methods)
Pawley and LeBail fitting
Rietveld structure refinement
Ab-initio structure determination- Simulated annealing- Charge Flipping- 3D Fourier analysis
Microstructure analysis
8
Our D2 PHASER delivers uncompromis-ingly good and reliable analyses. Thestrict quality standards of our entire product range are applied to the assem-bling, testing and certified safety of the D2 PHASER!
We give you our word: Good Diffraction Practice andBest Data Guarantee!
Safety assurance: Each instrument always complies with the world’shighest statutory requirements regarding X-ray safety,machine and electrical safety. This certainty is obtained after stringent scrutiny by independent institutions.
Two independent, fail-safe safety circuits and “X-rayOn” monitors guarantee that the most recent radia-tion and personal safety regulations are observed.
Alignment guarantee: The D2 PHASER is pre-aligned at delivery. Every single instrument must pass our strict test procedure,which is based on the internationally accepted refer-ence material corundum. The corundum reference issupplied with the instrument, so you can check yourinstrument at any time.
Detector guarantee: We guarantee that our 1-dimensional LYNXEYE is ab-solutely faultless! This is due to Bruker AXS’ uniquedetector design. By integrating the LYNXEYE detectorin the D2 PHASER it becomes the fastest and mostefficient desktop diffractometer in the world.
The best in its class: the D2 PHASER. Shake on it!
D2 PHASER – data-
quality, functionality
and safety without
any compromises
Unrivaled resolution
Instrument alignment – a sound base for accuracy!
Scintillation Counter
2Theta
Sample
X-Ray Source
Incident Beam
Diffracted Beams
Micro StripSensor
LYNXEYE
Common point detector setup
Advanced 1-D detector setup
XRD on polycrystalline material – more intensity with LYNXEYE detector
Co
un
ts
-0.040
0
1000
2000
3000
4000
5000
20.00
29.90 30.10 30.30 30.50 30.70 30.90
40.00 60.00 80.00 100.00 120.00 140.00
-0.030
-0.020
-0.010
0.000
0.010
0.020
0.030
0.040
+ 0.020°
SRM 660a
- 0.020°
LYNXEYE DetectorScintillation Counter
2Theta [°]
2Theta [°]
FWHM = 0.0421° 2Θ
Del
ta 2
Th
eta
[°]
9
Plug’n Analyze:
A simple domestic wallsocket is all you need
No installation
No alignment
No instrumentconfiguration
No infrastructure
No pre-installation requirements
All-in-one analytics:
Simple sample loading
Industrial standard sample holders
Theta/Theta geometry,horizontal samples
Fully-fledged integrated PC
On-site and remote operation
LYNXEYE detector:
Intensity increases by afactor of more than 150
100% working strips at delivery – guaranteed
Energy discrimination for sample fluorescencesuppression
1-D scanning and snap-shot mode; 0-D mode
Angular coverage > 5.5° 2Theta
X-ray source:
Common sealed X-ray tube design
Low power load –no tube ageing
Virtually infinite tube lifetime
Cr, Co, Cu radiation
Island-mode:
Internal cooling system
High speed ethernet connection
2 USB ports
In an XRD experiment performed on polycrystal-line material the incident X-ray beam is diffracted byinnumerous crystallites inspecific 2Theta directions.
To record the exact 2Theta positions a narrowslit in front of a point detector is required.
The LYNXEYE literally provides more than 150 integrated slits, allowingmore than 150 2Theta positions to be recorded simultaneously.
Very small peak width ofless than 0.05° 2Theta obtained by high-resolutionXRD measurement of LaB6 (NIST SRM 660a)with LYNXEYE detector;0.1° divergence and 1.5°Soller slit.
Why is this important?Good instrument resolutionis a prerequisite to resolveoverlapping diffractionpeaks in complex powderpatterns.
Angular accuracy≤ ± 0.02° 2Theta over thewhole angular range –guaranteed!
Why is this important? Accurate and verifiable instrument alignment is a basic requirement for accurate and reliable phaseidentification or structureanalysis.
Desktop design:
Minimum space requirements
Handles for convenienttransportation
Maximum X-ray safetywith radiation level significantly below 1µSv/h
Clearly visible warning and operating elements
Angular accuracy better than ±0.02°2Theta – guaranteed
10
Expert-mode
Full access to all settings:- User management- Database maintenance- Instrument configuration- Service tools
Full access to all instrument parameters:- Drives- Detector settings- Generator settings
4
3
Easy-mode
Real-time measurement display
Straightforward selection of scan parameters:- Angular range- Step size- Measurement time
2
1
1 1
3
4
22
Compatible with the entire Bruker AXS’ Diffraction Solutionsfamily
Fully network capable
Support of different user levels and modes
EVA – powerful phase identification
TOPAS – sophisticated quantitativephase and structure analysis
11
X-ray analysis has never been easier! Even inexperienced users produce perfectmeasurements from the very beginning thanksto the DIFFRAC.SUITE Easy-mode.
This is how X-ray analysis works in the Easy-mode:
Select COMMANDER plug-in, enter measurement time and angular range and start. That’s all!
If a method has already been defined, it goes even faster:
Select START JOBS, click on Method and off you go!
It goes without saying that the software solutions of ourDIFFRAC.SUITE go beyond this. In Expert-mode the fullscope of functions is available. Using the COMMANDER, CONFIGURATION and TOOLS plug-in the expert has controlover administration of experimental databases, user rightsand all the way through to the Audit Trail. Everything on the system works in a safe, simple and reliable way.
DIFFRAC.SUITE – performance made-to-measure:easy for anyone to operate, full functionalityand control for experts. Integrated within anetworked world.
Our D2 PHASER is fully network capable. This enables XRD experts in the central laboratory to access the data thathas been collected, no matter if they are next door or at theother end of the world. Use the D2 PHASER where it isneeded – on-site – and you will save time and money!
The D2 PHASER is a full-blown diffractometer: its measured data is fully compatible with all of our DIFFRAC.SUITE solutions. The familiar world ofsearch/match and structure databases, EVA, TOPAS,… all of this is available to the XRD specialist for identifying,quantifying and determining the characteristics of the crystalline phases.
D2 PHASER – Welcome to the world of Bruker AXS!
The ultimate in
ease of use –
D2 PHASER with
DIFFRAC.SUITE
All-in-one analysis
All
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Bruker AXS GmbH
Karlsruhe, GermanyTel. +49 (7 21) 5 95-28 88Fax +49 (7 21) 5 95-45 [email protected]
www.bruker-axs.com
D2 PHASER™, DIFFRAC®, LYNXEYE™, Plug’n Analyze™ are trademarks of Bruker AXS
Bruker AXS Inc.
Madison, WI, USAPhone +1 (800) 234-XRAYPhone +1 (608) 276-3000Fax +1 (608) [email protected]
Geometry Theta / Theta
Max. useable angular range -3 … 160 ° 2Theta(depending on detector)
Accuracy ± 0.02° throughout the entire measuring range
Achievable peak width < 0.05°
Alignment Not needed, factory aligned
X-ray wavelengths Cr / Co / Cu, standard ceramic sealed tube
X-ray generation 30 kV / 10 mA
Detectors Scintillation counter 1-dimensional LYNXEYE
Instrument type Portable, desktop
Exterior Dimension 61 x 60 x 70 cm (h x d x w)24.02” x 23.62” x 27.56”
Weight 95 kg
Power supply 90 – 250 V
External cooling water supply None
Computer Built-inOptional additional PC connected via LAN interface
Interfaces 2 x USB and 1 x LAN
Technical Data
Bruker AXS
think forwardXRD
Application Report XRD 8
D2 PHASER Desktop XRD:Silica Dust Analysis
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling cir-cuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market.
This report demonstrates its use for monitoring occu-pational exposure to respirable silica.
LYNXEYE
D2 PHASER
Filter Holder
D2 PHASER, LYNXEYE detector
Cu radiation (30 kV, 10 mA), Ni filter
Continuous scan from 26.1 to 27.1° 2ThetaStep width 0.01° Counting time:1) > 30 µg: 1 sec per step2) < 30 µg: 5 sec per step
1) Total scan time 5 min.2) Total scan time 25 min.
4° Soller collimators, 1.0 mm divergence slit, anti-scatter screen
LYNXEYE detector opening 5° 2Theta
Tab. 1: Experimental settings.
Lung cancer and other health issues are known to be associated with occupational exposure to crystalline silica, SiO2. This is a typical component of soil and rocks. Clear exposure/response relations were reported for e.g. miners, diatomaceous earth and construction workers, granite, pottery, refractory bricks, or foundry workers. Occupational exposure to respirable silica is a preventable health hazard and therefore, the concentrations are monitored.
X-ray powder diffraction is capable of distinguishing poly-morphs of crystalline silica (quartz, cristobalite, tridymite). Furthermore, XRD may account for the interference with other minerals that may additionally be present at the workplace. Sampling of the airborne particles on filters and their investigation is regulated by several national norms like NIOSH 7500, OSHA ID-142, MSHA P-2, and others. The concentration of an unknown silica phase is determined from a calibration, which needs to be established from refer-ence samples using e.g. the DIFFRAC.DQUANT software.
Filter papers with different amounts of quartz deposited were measured applying the D2 PHASER and a special sample holder for filters. Experimental details are summa-rized in Table 1. Figure 1 shows several diffraction scans of
Bruker AXS GmbHKarlsruhe, GermanyPhone +49 (7 21) 5 95-28 88 Fax +49 (7 21) 5 95-45 87 [email protected]
Bruker AXS Inc.Madison, WI, USAPhone +1 (800) 234-XRAYPhone +1 (608) 276-3000Fax +1 (608) [email protected]
All configurations and specifications are subject to change without notice. Order No. DOC-R88-EXS008. © 2009 Bruker AXS. Printed in Germany.
Fig. 1: Diffraction signals of a blank, 12, 30, 90, 150, and 210 µg quartz on filters at the position of the strongest quartz peak all measured with 1 sec per step. The inset shows the calibration curve of the net intensities determined using DIFFRAC.EVA vs. the known concentrations.
the 100% quartz peak. The different intensities are directly related to the concentration of the deposited quartz dust. The net intensities of the different specimens show a clear linear correlation with the concentrations (see inset).
The calibration fully complies with the NIOSH norm. The curve has zero offset of 2.7 µg (±5 µg permitted in NIOSH 7500). The limit of detection (LOD) in this example is about 8 µg. It can further be reduced by increasing the
measurement time. A counting time of 5 sec per step for example, increases the total scan time to about 25 min but reduces the LOD below 5 µg. The precision is better 1 % relative for concentrations exceeding 100 µg and better 10 % relative between 10 and 100 µg.
To conclude, our cost-effective desktop XRD system D2 PHASER allows for fast, precise and norm compliant analyses of airborne respirable silica particles on filters.
