µEDX SeriesµEDX-1200/1300/1400

ShimadzuEnergy Dispersive Micro X-rayFluorescence Spectrometer

C142-E026C

X - r a y - c o n v e r g e n t O p t i c s

A c h i e v e H i g h l y

S e n s i t i v e M i c r o a n a l y s i s

Shimadzu Energy Dispersive Micro X-ray Fluorescence Spectrometer

µEDX Series

Easy plat ing th ickness measurements for electronic mater ia ls and components, detect ion of foreign matter, defect analysis, and mapping analysis

The microanalysis of electronic components, circuit boards, and foreign matter in foods was difficult

with conventional fluorescence X-ray spectrometers because of the poor sensitivity due to the small

sample size and the insufficient resolution even at sufficient X-ray intensity.

However, the Shimadzu µEDX Series of energy-dispersive micro X-ray fluorescence spectrometers

achieves high-sensitivity and high-resolution analysis of such samples, down to a minimum measured

diameter of 50 µm.Conventional high-speed, non-dispersive micro X-ray fluorescence spectrometers

lacked the resolution to handle complex samples and struggled to analyze light elements.

Similarly, the collimator-type energy-dispersive instruments lacked excitation intensity, resulting in

problems of low throughput and the necessity for tedious measurements in vacuum.

The Shimadzu µEDX Series are models for the 21st century, combining the resolution and flexibility

of energy-dispersive instruments with the speed and convenience of non-dispersive instruments.

Electronic materials and componentsComposition and thickness of thin films, plating, solder, etc.

Chemical engineering and chemicalsCatalysts, scale and sediments in plants, cosmetics, pigments, dyes, plastics

Oil and coalPetroleum, heavy oil, lubricating oil, polymers, coal, coke, etc.

CeramicsCement, blended cement materials, ceramics, clinker, limestone, clay, glass, bricks, rock, etc.

Machines and metalsComposition and plating thickness of machinery parts and metal materials

Non-ferrous metalsPrecious metals and alloys of copper, aluminum, lead, zinc, magnesium, titanium, etc.

EnvironmentFactory effluent, seawater, river water, atmospheric suspended particles, industrial waste, etc.

Pharmaceuticals, food, agricultureForeign bodies, soil, fertilizer, plants, foods, drinks, animal feed, etc.

Paper and pulpCoated paper, talc, toner, inks, etc.

OthersPrecious stones, cultural materials, excavated items

Quick and accurate surface component analysis in many fields

µEDX Series Product Line-up

for measurements of elementsAl to U

WD=6.5 mm (standard model)

for measurements of elementsNa to U

WD=1.5 mm (light element)

for measurements of elementsAl to U

WD=6.5 mm(high-throughput, no liquid nitrogen model)

1 Patented polycapil laries irradiate X-rays over a minute 50µm sample range to achieve highly sensit ive and accurate analyses.

2 Analyzes l ight to heavy elements in atmospheric air. (Patent pending)

3 Dual-CCD camera (high-magnif ication and low-magnif ication) al lows easy sample posit ioning and analysis while observing an image of the sample.

4 Standardless FP quantitation, thin-f i lm FP method of f i lm composit ion and f i lm thickness determination, and BG-FP method of polymer f i lm thickness determination are included as standard.

5 Automatic changeover of f ive primary f i l ters supplied as standard to eliminate undesirable characteristic X-rays from the X-ray tube and improve the S/N ratio.

6 Automatically maps multiple elements simultaneously. Optional transmission image unit al lows the simultaneous measurement of transmission X-ray images.

7 Thermoelectric cooling detector requires no l iquid nitrogen. (for µEDX-1400 only)

Optical System for Vertical X-ray Irradiation and Accurate Measurement Posit ion Sett ing

Sample stage

Filter

Zr

Ni

Ti

Al

OUT

Effective elements

Rh ~ Cd

Zn ~ As, Pb, Bi

Cr ~ Fe

Cl

Optical System Construction and Arrangement

Positioning laser

Transmission image observation unit (optional)

X-Y stage drive range100x100x40mm

Sample stage

Transmission imageobservation stage

X-ray tube

Primary X-ray filter

CCD camera

Detector

Dewar

Polycapillaries

300

without Zr filter

with Zr filter

200

100

22.00 24.00 [KeV]

Cadmium in Vinyl chloride

4

Optical System Construction and ArrangementThe µEDX Series conducts analysis by irradiating the sample surface with X-rays vertically from above. The arrangement of the capillaries and detector minimizes attenuation of the primary X-rays that irradiate the sample and the fluorescence X-rays generated from the sample (patent pending). This optical system permits analysis of elements from light elements to heavy elements in atmospheric air. The sample stage is PC-controlled in the X, Y, and Z directions to permit accurate height adjustment, with no influence from differences in sample thickness or measurement position. Drive in the X-Y directions permits quick and accurate determination of the measurement position.

Automatic changeover of f ive primary f i l tersThe automatic changeover mechanism for five types of primary filter is installed as standard to eliminate undesirable characteristic X-rays from the X-ray tube and improve the S/N ratio.

Posit ioning mechanismThe maximum stroke of the X-Y stage is 100 mm x 100 mm. The Z axis can move up to 40 mm to permit the measurement of thick samples.

µEDX Series

Polycapil lary X-ray Lens offers High-sensit ivity Micro Analysis

Polycapillary Lens

Collimator type

Analysis with conventional method Analysis with a fine beam High-sensitivity analysis with a fine beam

Monocapillary type Polycapillary type

Excitation X-ray intensity 1 Excitation X-ray intensity 10 to 50 Excitation X-ray intensity 100 to 1000

(1)

(2)

(3)

Unlike light, X-rays cannot be focused by a lens. However, if X- rays are introduced into glass or some other medium at an angle close to parallel, total reflection allows the direction of the X-rays to be changed.

If the medium is formed into a tapered cylinder, repeated total reflections result in the X-rays being focused onto a small diameter at the tip of the cylinder.

A bundle of fine capillaries, known as "polycapillaries," is an efficient means of providing X-ray irradiation with X-rays generated by an X-ray tube.

X-ray tube

Stage

X-ray beam

SampleObject

Stage

X-ray tube

Monocapillarylens

SampleObject

X-ray beam

Stage

X-ray tube

X-ray beam Polycapillarylens

SampleObject

5

Polycapil lary LensPatented polycapillaries irradiate X-rays over a minute 50 µm sample range to achieve highly sensitive and accurate analyses.

Polycapillaries are an X-ray focusing system that exploits the phenomenon of total internal reflection in glass fibers. X-rays generated by the X-ray tube pass through the polycapillaries to converge at a single point on the sample surface. Consequently, the polycapillary lens increases the X-ray intensity irradiating the sample. Irradiating the sample with X-rays at the target position only enhances the S/N ratio by reducing fluorescenceX-rays generated from adjacent areas.

All X-rays generated by the X-ray tubeconverge onto the sample

X-rays generated by the X-ray tube convergeonto the sample.

Only some X-rays generated by the X-raytube irradiate the sample

Easy Posit ioning of Large or Small Samples whileObserving the Sample Image

6

Determining Analysis Posit ion by Viewing Dual-CCD ImagePosition samples while observing the image from the low-magnification CCD camera. Very small samples can be positioned by switching to the image from the high-magnification camera.

AutofocusThe distances from the X-ray tube and detector to the sample must be held constant to achieve accurate quantitative analysis. The autofocus function makes vertical positioning easy.

Low-magnification image (approx. 20 x) High-magnification image (approx. 100 x)

1

1

5

5

2

2

3

3

4

4

Designating the Analysis Posit ionClick the mouse at the required position on the screen to move to that position Dragging the mouse moves the stage, similar to joystick operation. Fine adjustment is possible by pressing the arrow buttons on the screen or keyboard. After the measurement position is determined, register the center of the visual field as the analysis position.

µEDX Series

Image is refreshed in realtimeas the stage moves

7

Realt ime Scaling Stage Viewer (RSSV) FunctionThis function displays the entire stage when searching for the measurement position on a large sample. Click the target position on this image to move the stage to this position while displaying in realtime where the current position is on the stage. (Patent)This screen synthesizes the sample image to provide an overall view of the sample.

Multipoint analysisMultipoint analysis is also possible. The analysis positions are displayed superimposed on the sample image.

Synthesized image (50 mm x 50 mm)

1

2

3

Analysis of Specif ic ElementsMapping of Mult iple Elements

8

Element MappingDesignated elements can be mapped simultaneously. Display X-ray intensity distribution or film-thickness/composition distribution (all µEDX instruments). High-speed stage scanning rapidly acquires images (µEDX-1200 and µEDX-1300 only).

Film-thickness Distribution

Number of measurement points: 400 x 300

Measurement time per point:0.2 s

Number of measurement points: 200 x 150Measurement time per point: 0.1 s

Sample: power transistor radiation finThe film-thickness distribution can be displayed by calculating intensity data from the quantitative values.

Intensity Mapping Example

Sample: ivy leafHigh P distribution in white areas. High Mn concentration at tip.

Easily analyze living samples, without evacuating the sample chamber.

µEDX Series

9

Transmission Image Display (Option)Adding the optional transmission image unit allows the simultaneous measurement of transmission X-ray images.These images show inside electronic components, for example, which is not visible with fluorescence X-rays alone.

Qualitative MappingIf elements cannot be specified, spectra are measured at all points across the designated range and a composite spectrum is calculated. Qualitative analysis identifies the elements across the range from the composite spectrum. Mapping images can then be created for the target elements.

Sample: mobile phone componentAn Ni-plated cover is attached over the piezoelectric speaker (top of diagrams). The transmission image shows the structure below the cover.

Number of measurement points: 200 x 150Measurement time per point: 0.05 s

Sample: picture on ceramicQualitative analysis of the composite spectrum across the mapping range

Superimposed display of Fe, Cr and CoQualitative analysis of the composite spectrum identified the elements contained in the designated sample range.Intensity mapping images were created for the detected Fe, Cr, and Co and the images superimposed.

It was determined that: red areas contain significant Fe; green areas contain significant Cr; blue areas contain significant Co.

Transmission X-ray Image CCD Image Fluorescence X-ray Image

Fluorescence X-ray /Transmission X-ray Images

Number of measurement points :80 x 60Measurement time per point : 0.1 s

10

Multipoint Schedule Analysis

Sett ing Quantitation Condit ions

1

5

2

3

4

1

2

3

4

5

The sample image is displayed during measurements to allow confirmation of the measured positions.Previously registered position information can be recalled for routine analyses. Icons indicate measurement progress for confirmation at a glance.

Profile displayed during measurement. During qualitative / quantitative analysis, qualitative results are updated in realtime. Analysis results are displayed when measurements are complete. Previous analysis results can be confirmed.

The operation tree, element list and all other operation screens are displayed simultaneously to show all information immediately.Set multi-layer films up to 10 layers and 100 components. Sample form and film composition are clearly displayed.Thickness calculation simulations determine whether calculation as a film sample is possible.Using the FP method for film measurements permits quantitative analysis using a standard sample in a different form from the unknown sample.

Incorporates Shimadzu X-ray Expertise for Easy and Convenient OperationSimple, Mult i function Software

µEDX Series

11

Linking Images and DataThe list of measured points and sample image directory are displayed simultaneously. The measurement points are displayed superimposed on the sample image. Sample images and multipoint analysis results can be displayed in tabular form.

Creating ReportsReports incorporating the sample image, spectrum, and analysis results are easy to create. Search qualitative/quantitative data and quantitative data and display the analysis results in tabular form.Export tables of results in CSV format to a spreadsheet such as Excel(*). Display control charts and histograms for analysis results.

Spectrum MatchingMatching of both content and intensity. Designate one of four search modes: material evaluation, type classification, type evaluation and matching.

Network FunctionPermits data sharing within a network for smooth information exchange between production line and laboratory and notification of analysis results. Share date over a LAN. E-mail notification function automatically notifiles that analysis is complete, transmits analysis results, and reports errors to designated addresses.

Sample: modular cable terminals

Display of sample imageand analysis results table

Sample: glass beads

Summary display of lists and sample image

*Excel is registened trademark of Microsoft inc.

Determination of different kindCompares reference sample values to evaluate whether an unknown sample matches the reference sample

Classification of samle kind Evaluates the type of an unknown sample by registering element references and tolerances of multiple types

Determination of sample kind Evaluates the type of an unknown sample by registering the element content ranges of multiple types

Search best match Finds the type with the smallest discrepancy with an unknown sample by registering reference values for multiple types

12

Micro X-ray Fluorescence Spectromertry is Applicable across a Range of Fields from ElectronicHandles a Wide Range of Fields

Electronic materials : lead-free solder

Sample

Machinery parts: flexible cable

1.0mmCCD image (low magnification)

CCD image (low magnification)

1.0mm

Foreign matter in food: metal

Mean

Max.

Min.

R value

Sn

95.82%

96.01%

95.57%

0.44%

0.126

0.13%

Ag

3.38%

3.64%

3.20%

0.44%

0.128

3.79%

Cu

0.80%

0.83%

0.75%

0.08%

0.229

2.86%

(Measurement time: 40 s, number of repeated measurements: 10)

Qualitativeanalysis

Mapping

MappingTransmission analysis

Trans Image

Sample image

2.0mm

10.0 x 7.5mm FeKa

2.0mm

10.0 x 7.5mm

QuantitativeAnalysis

QuantitativeResult

FeCrNiMoCu

70.06%19.18%9.77%0.51%0.48%

StandarddevisionCoefficientof variation

Qualitative analysis

1.0mm

[ ]

µEDX Series

13

c Materials to Machinery Parts, Biological Samples, and Food

Sample

1.0mm

Jewelry : platinum ring

1.0mm

Biosamples : foods

5mm

1 : flour2 : vitamins3 : tealeaf4 : coffee

Qualitativeanalysis

Qualitativeanalysis

Qualitativeanalysis

Mapping

Superimposeddisplay

CCD image(low magnification)

CCD image(low magnification)

CCD image(Synthesized)

Machinery parts : CD retainer spring in CD-ROM drive

Thermoelectric Cooling Detector Requires No Liqid Nitrogen

Options For al l Models

14

No l iquid nitrogenWorld-first micro EDX with an thermoelectric cooling detector requiring no liquid nitrogen.

Rapid, Accurate AnalysisThe µEDX-1400 detector achieves highly accurate analysis in a short time. By measuring at higher counting rates than a liquid-nitrogen-cooled detector, it obtains the same count in approximately 1/5 the time.

µEDX-1400

Repeatability of quantitative values for Ni plating thickness (measurement time : 20 s)

Thermoelectric cooling detectorNumber of measurements

Mean

Standard deviation

Coefficient of variation

µEDX-1200

5

2.068 um

0.0364

1.76 %

µEDX-1400

5

2.072 um

0.0191

0.92 %

Consult your Shimadzu representative about sample holders.

Part name

Transmission image observation unit

X-ray pilot lamp

Cat. No.

212-23340

212-23395

Description

Detects transmission X-rays to obtain transmission images

Pilot lamp to indicate X-ray generation

µEDX-1400 Element range Al to U

EnvironmentAmbient temperature 18 to 28˚C Relative humidity 40 to 70%Power supply 100-120VAC, 6A, 50/60Hz 200-240VAC, 3A, 50/60Hz Grounded socketExternal dimensionsUnit 486(W)×649 (D)×704 (H) mmController 215 (W)×490 (D)×464 (H) mmWeightMain unit approx. 85 kgController approx. 15 kg

15

Specif ications

Instal lat ion Requirements

Major Specif ications

Measuring principle X-ray fluorescence spectrometry

Measuring method Energy-dispersive X-ray analysis

Sample types Solid, liquid, powder

Element range Na to U (µEDX-1300)

Al to U (µEDX-1200, µEDX-1400)

Max. sample size 200(W)×300(D)×40(H)mm

Measuring atmosphere Atmospheric air

X-ray generatorX-ray tube Rh target

Voltage 5 to 50 kV

Current 1 to 1000 µA

Cooling Air (fan forced)

X-ray convergence method Polycapillaries

Irradiated diameter Approx.50 µm

Primary filter Automatic changeover of five primary filters

(Al, Ti, Ni, Zr, OUT)

Detector (µEDX-1200, µEDX-1300)Type Si (Li) semiconductor detector

Liquid nitrogen supply During measurement only

Dewar capacity 3L

Liquid nitrogen consumption Approx.1 L/day.

Detection area 30mm2

Detector (µEDX-1400)Type Si drift semiconductor detector

Cooling method Thermoelectric

Liquid nitrogen supply Not required

Detection area 5mm2

Transmission image observation unit (option)Detector type Scintillation counter

Sample stageMax. stroke 100(W)×100(D)×40 (H)mm

Max. load 2 kg

Working distance 6.5 mm (µEDX-1200, µEDX-1400)

1.5 mm (µEDX-1300)

Sample observation unitCCD Dual CCD

Magnification Switchable low-magnification/high-magnification

Focussing Autofocus

Data processing hardwarePC IBM/PC compatible

OS Windows XP

Printer Color printer

SoftwareSample observations Controllable illumination light quantity

Perspective conversion

Realtime Scaling Stage Viewer (RSSV)

Qualitative analysis Smoothing

Peak catching

Automatic identification, manual identification

Peak fitting

Quantitative analysis Calibration curve method, FP method, BG-FP method

Film FP method

Correction functions including matrix

correction and internal standard correction

Thickness calculation simulation

Mapping analysis Step mapping, line analysis

High-speed mapping (µEDX-1200, µEDX-1300)

Full-profile (qualitative) mapping

Simultaneous transmission image measurement

(* with transmission image observation unit installed))

Element superimposition

Select pseudo color, concentration, bird’s eye or mesh display

Filter calculation processing

Report generation Simple report (displays images and analysis results)

Summary report (displays images and multipoint analysis results)

Tables (displays statistical results)

Generate control charts and histograms

Matching Four types of maching mode

Mapping of content and intensity

Network functions Email notification of analysis completion and errors,

transmission of analysis results

Maintenance functions Unit monitor : Continuous monitoring of X-ray output, count rate, etc.

Automatic control : X-ray ON/OFF schedule operation

Unit calibration :

Automatic calibration of energy and peak width at half height

*option

1800

649

800

464 70

070

4

486

215

Data processing

Control unit

µEDX unit

Installation Example(unit:mm)

• Necessary matters for safety are displayed by warning labels.

The contents of this brochure are subject to change without notice.

Printed in Japan 4795-12701-20AIT