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Clinical Biochemistry Analyzer(CA)

 Clinical Biochemistry Analyzer  Your Health Condition Revealed by Your Blood
 Identifying the Substance and Quantity by Change of Color
 Clinical Biochemistry Analyzer Application Example

Studying pathology using blood, indispensable clinical test data for
modern medicine
The Clinical Biochemistry Analyzer is an instrument that uses the pale yellow supernatant
portion (serum) of centrifuged blood sample or a urine sample, and induces reactions
using reagents to measure various components, such as sugar, cholesterol, protein,
enzyme, etc. These tests are performed for routine health checks or at hospitals, and the
results provide objective data enabling early detection and diagnosis of disease, as well as
indicating the effects of treatment and patient prognosis.
In addition, due to the increasing costs of medical care, medical equipment is also
expected to be economically efficient.  BioMajesty™ is the most economical instrument on
the market, using micro volume of samples and reagents to deliver highly­accurate, high­
speed processing through the incorporation of a sample dilution tray, which is an
outstanding unique feature of BioMajesty™ analyzers.
Furthermore, we have developed the Laboratory Information Systems as well as the
Laboratory Automation Systems, offering a total support to our customers and
streamlining the everyday laboratory activities.disc which is not available from other
makers. Moreover, our company has developed products for test information systems as
well as a total sample automatic transfer system to support all activities from drawing
blood to reporting; , allowing remarkable improvements in the speed and efficiency of
clinical testing work.
Your Health Condition Revealed by Your Blood
For example, to check kidney function, we measure and evaluate the concentration of
substances such as urea nitrogen and creatinine in blood. If more than a certain
concentration level is found in the blood, the doctor will probably tell you that “I'm a little
worried about your kidney function”. Urea is a final product that remains after protein, one
of the major nutrients inside the body, is metabolized,
This urea is filtered by the kidney and excreted as urine under ordinary circumstances.
However, if the kidney fails to work properly, the unfiltered urea remains in the blood, so
the urea nitrogen level in blood becomes high. On the other hand, creatinine is a break­
down product (final metabolite) which is produced when muscles move, and this is also
absorbed and excreted by the kidney. Therefore, if significant quantities of these
substances exist in the blood, it can indicate the possibility that the function of the kidney
has declined. For a healthy adult the upper limit for creatinine is 1.2mg (1.2g/1,000) in
100ml (1dl) of blood serum. If more than this quantity is detected, the kidney function is
considered suspicious. This example is for the kidney. There are other indicators, such as
for hepatic function using transaminase (AST or GOT, ALT or GPT), cholesterol, and
bilirubin concentrations, and for diabetes using blood glucose (Glu) concentration and
diastatic hemoglobinA1C fraction percentage (indicated with %), and so on. The
concentrations of various substances in the blood can tell us a great deal about the clinical
state. Today’s medicine requires this kind of test data to make accurate diagnoses. This
area is called biochemical examination in clinical testing.

Identifying the Substance and Quantity by Change of Color
Colorimetric Analysis Method and the Measurement Principle
BioMajesty™ is an automatic analyzer for biochemical testing, and it can analyze more than
100 different components in blood. The measurement principle is as follows.
You may recall the iodine­starch reaction experiment from a school science class. When you
add iodine solution to a starch solution, the solution will turn blue instantly. The existence
of starch can be confirmed in this way. In addition, if saliva is added to the colored
solution, the color will disappear. This is because the starch is dissolved by the function of
an enzyme called amylase contained in saliva. An automatic biochemical analyzer utilizes
this kind of reaction, and converts the quantity of a specific substance in blood into an
amount of color change for measurement. The analysis method of measuring the amount of
color change is called the colorimetric analysis method. The origin of this method is quite
old, and the shading of colors was originally evaluated by the naked eye. It is a method
that has been used since the age of alchemy. The automatic biochemical analyzer has
automated the sequence of operation processes which used to be conducted by hand and
evaluated by eye (or using a spectrophotometer) in the past.

Techniques for the measurement process
Summary of equipment BioMajesty™
The figure above shows the outline of BioMajesty™
The samples for BioMajesty™ are the pale yellow liquid portion of blood called blood serum,
and urine. A certain precise volume of sample (normally 30 micro liters) is collected by
using a dilution pipette, and diluted by 5 times using a dilution disc. The measurable
sample is 150 micro liters (μl). From this dilution sample, a precisely­measured amount of
2 to 25 microliters per test item is transferred to a reaction cell (1 eye drop in the rotating
reactor is about 40 microliters). The reaction cell already contains reagent transferred from
the reagent bottle in reagent turntable 1.
Reactions are induced in the samples in the reaction cells at a temperature of 37μ. If a
color reaction does not occur with one kind of reagent, it is possible to add a second or
third kind of reagent (reagent turn table 2). After allowing the reaction to proceed for a
certain time (normally 10 minutes), the color density is measured by using a colorimeter
(in the figure, “multi­wavelength photometer”). The mechanism of the colorimeter is to
shine a light through the sample being measured, and then electrically detect the amount
of transmission. The measured data is indicated numerically using A/D converters
(analogue→digital converter), calculated by CPU, and the results are output.
BioMajesty™ offers high dispensing performance of sample and reagent, reduction of
residual water to the minimum, due to a cleaning mechanism for the outside of the
pipettes and measures to eliminate residual­water in the reaction cells, and acquisition of
good accuracy measurement data.

Clinical Biochemistry Analyzer Application Example
BioMajesty™is a clinical biochemical analyzer that contributes to clinical testing by
achieving ultra­high­speed processing with ultra small volumes of reaction fluid.
It has been used in small and medium­sized hospitals and test centers (non­governmental
agency dedicated to analysis of patient samples), as well as large hospitals, such as
university hospitals, etc. The ultra small volume measurement function is expected to
contribute to the development of test items, such as for immunity, tumor markers, drugs,
infection markers, etc. as well as to the development of pharmaceutical products.

Photograph: Courtesy of Clinical  Department, Kitasato University Hospital.

PRODUCTS 
Scientific/Metrology Instruments
Field Emission Cryo-Electron Microscope

JEM-Z200FSC
CRYO ARM 200
TM

CRYO ARM is an electron microscope for observing bio-


TM

molecules such as proteins at cryo temperature. The


microscope equips a cold field-emission electron gun, an
in-column Omega energy filter, a side-entry liquid nitrogen
cooling stage, and an automated specimen exchange system.
The specimen exchange system can store up to 12 specimens
in the specimen exchange chamber.
CRYO ARM 200
TM

Field Emission Cryo-Electron Microscope


JEM-Z200FSC

The CRYO ARMTM 200, equipped with a Cold field emission gun (Cold FEG), an in-column Omega
energy filter, a side-entry liquid-nitrogen cooling stage and an automated specimen exchange system,
is a cryo-electron microscope (cryo-EM) that enables observation of bio-macromolecules at cryo-
temperature. The automated specimen exchange system features the storing of up to 12 samples. In
addition, the system allows for the exchange of an arbitrary one or more samples, thus enabling flexible
scheduling. Furthermore, the combined use of a newly-designed in-column Omega energy filter and a
Hole-free phase plate dramatically enhances the contrast of TEM images of biological specimens.

Main Features
■ Automated specimen exchange system ■ In-column Omega energy filter
The system is composed of a specimen stage to cool Equipped with an in-column Omega energy filter, the CRYO
samples to liquid nitrogen temperature and a cryo-transfer ARMTM 200 acquires energy filtered images and energy loss
system to automatically transfer the cooled samples to the spectra. Zero-loss images acquired with the microscope
cryo-stage. Liquid nitrogen is automatically supplied to the provide high contrast with reduced chromatic aberration.
liquid nitrogen tank as required. This automated system
features the storing of up to 12 samples and the exchange ■ Automated image acquisition software for Single Particle Analysis
of an arbitrary one or more samples while the rest of the The CRYO ARM TM 200 incorporates automated software. The
samples are kept cooled between the specimen stage and software allows for automated detection of holes on the specimen
specimen exchange system. grid for efficient acquisition of Single Particle Analysis images.

■ Cold field emission gun (Cold FEG) ■ Hole-free phase plate *1


A Cold FEG produces a high-brightness electron beam with This unique phase plate is suitable for higher contrast in
very small energy spread, offering high coherency. Thus, the biological specimens that originally provide only low contrast.
CRYO ARM TM 200 achieves high resolution, high contrast
imaging.
■ Auto adjustment functions *2
Auto focus, auto coma-free alignment, auto parallel-beam
illumination and other automated adjustments are available,
enabling image acquisition under optimum conditions.

*1: Optional unit. *2: Images acquired with the bottom mount camera are used.
Specifications

Main instrument Installation Room Requirements


Electron gun Cold field emission gun (Cold FEG) Room temperature 15 °C to 25 °C (fluctuation 0.2 °C/h or less)
Accelerating voltage 200 kV Humidity 60% or less
Energy filter In-column Omega energy filter Microscope power supply Single phase, 200 V AC, 8 kVA
Maximum specimen tilt angle ± 70° Cooling water
* Schottky field emission gun can optionally be configured. Flow rate 10.75 L/min.
Temperature 15 °C to 20 °C (fluctuation 0.2 °C/h or less)
Footprint
Options
Microscope room 6,000 mm (W) × 5,000 mm (D) or more
Accelerating voltage 100 kV
Utility room 6,000 mm (W) × 3,500 mm (D) or more
Hole-free phase plate
Ceiling height
Bright-field transmission electron detector
Microscope room 3,500 mm or more
Utility room 2,000 mm or more
Entrance

Specimen stage / Automated specimen exchange system Microscope room 1,200 mm (W) × 2,000 mm (D) or more

Specimen stage Utility room 1,100 mm (W) × 1,900 mm (D) or more

Coolant Liquid nitrogen


Automated liquid-nitrogen filling system built-in
Installation Room Layout
Specimen cooling temperature 100 K or less
Figure below shows an example of the standard layout when the
Temperature measurement position Specimen, Cryo-shield, LN2 tank
microscope operations are performed in a room separate from the room
Specimen movements of the microscope main instrument.
X, Y Motor drive (movements: ± 1 mm)
Piezoelectric elements (movements: ± 0.5 μm) Microscope room Utility room

Z Motor drive (movements: ± 0.2 mm)


Tilt-X Motor drive (tilts: ± 70°) HV tank

Rotation within the specimen plane 0° or 90°


Specimen exchange system Air-lock
6,000 mm

Automated cryo-transfer system built-in


Cooling temperature 105 K or less
(specimen exchange chamber)
Specimen exchange cartridge Up to 4 specimens can be changed at one time. Main instrument
Specimen parking stage Up to 12 specimens can be held.

5,000 mm 3,500 mm

Cable length used for remote control: 17 m

* Improvements or changes to device appearance or specifications may be made without notice.

No.1202G787C(Bn)
Scientific / Metrology Instruments
CROSS SECTION POLISHER

IB-19530CP

CROSS SECTION
POLISHER
Multipurpose stage
CROSS SECTION POLISHER(CP)

IB-19530CP
Multipurpose stage

Auto milling program

Precise positioning adjustment system

Principle of cross-section preparation by CP

In the CP, a shielding plate is mounted on the upper portion of the specimen, and then the portion protruding from the
shielding plate is irradiated with a Broad argon (Ar) Ion Beam (BIB). This procedure enables a cross section to be
prepared along the edge of the shielding plate. Compared with general mechanical polishing, the CP easily creates a
highly uniform cross section with no strain caused by milling. Thus, cross-section preparation can be made for various
specimens, such as composite materials and laminated materials. Patent: No. EP 1517355 B1, US 7722818 B2, JP 4557130 Patent related to rocking function

Mount the shielding plate on the processing position of a specimen.


At this time, make the specimen protrude from the edge of the
plate so that the protrusion is confined within 100 μm.
When this protruded specimen is irradiated by BIB, the protruded
portion is etched and a cross section is created.

2 CROSS SECTION POLISHER


1 Multi-purpose stage
Cross-section milling
Long life shielding plate achieves 3 times higher durability (approx. 8 h)*
*In the case of 8 kV accelerating voltage and ion source with 500 μm/h milling speed

Planar surface milling Option

A larger specimen (40 mm diameter) can be milled. The specimen tilt angle is adjustable from 0°to 90°.
Cross-section rotated milling Option

The use of the dedicated shielding material (cylindrical sample stage) allows ion-beam irradiation onto the specimen
from any direction (360°). This feature reduces streak-like milling marks during cross-section preparation.
Ion beam sputter coating Option

High-quality carbon coating is enabled by ion beam sputtering.

2 Auto milling program


Auto milling start mode
Immediately after reaching the preset chamber pressure, milling starts automatically.
Intermittent milling mode
Setting the times for repeatedly turning the ion beam ON and OFF suppresses temperature rise of the
specimen. Thus, thermal damage to the specimen is reduced.
Fine milling mode
After milling at high accelerating voltage, the milling mode is automatically switched to milling at low
accelerating voltage for enabling high-quality cross-section preparation in a short time.
In particular, this mode is effective for specimen preparation to analyze crystal structures.

3 Precise positioning adjustment system


(1) The standard cross-section milling holder has the processing position adjustment capability,
thus making it possible to adjust the position from the outside of the CP. Combined use with
a dedicated precise positioning microscope (option) facilitates adjustment of the processing
position at a high magnification.
(2) T he use of an optional holder, compatible with a scanning electron microscope (SEM),
enables additional processing after the milled specimen is observed with the SEM.

Comparison of mechanical polishing and CP milling


Specimen : Copper

5 μm 5 μm
Cross section prepared by mechanical polishing Cross section prepared by CP

Skilled techniques are required to prepare a cross section of Preparing a cross section with an argon ion beam
soft metals (copper, gold, etc.) by mechanical polishing. The enables creation of a uniform cross section with no
above backscattered electron image shows copper plating crystalline strain. The channeling contrast, which is
prepared by mechanical polishing. In this image, many dependent on the difference of crystal orientation,
scratches due to mechanical polishing are seen. Also, the can clearly be observed.
channeling contrast is unclear due to strains resulting from
polishing. CROSS SECTION POLISHER 3
Multi-purpose stage
A new CP, IB-19530CP, adopts a multi-purpose stage, thus expanding its applications to
cross-section milling, planar surface milling, cross-section rotated milling, carbon coating, etc.

Cross-section milling Planar surface milling Option

Ion beam Ion beam

Shielding plate

Specimen

Specimen

Carbon coating Option Cross-section rotated milling Option

Ion beam Ion beam

Specimen
Specimen

Carbon target

Shielding plate

Specimen stage
The standard specimen stage allows for the
use of a wealth of functions, from cross-
section milling to planar surface milling, and
carbon coating.

Standard specimen stage


X-axis movement Specimen holder Shielding plate

・In addition to cross-section milling, planar surface


milling, cross-section rotated milling and carbon
coating can be made.
・The cross-section milling holder can be used with the
optional precise positioning microscope, thus
enabling highly precise adjustment of the processing Y-axis
movement
position at a high magnification.

4 CROSS SECTION POLISHER


Cross-section milling

Mount the edge of the shielding plate on the processing position, and then irradiate an Ar ion beam onto
the target position. The portion protruding from the specimen is etched by the Ar ion beam for enabling
the creation of a uniform cross section along the shielding plate edge. Long life shielding plate achieves 3 times higher
durability (approx. 8 h)*. This high-durability shielding plate is effective to process materials with low milling rate.
*In the case of 8 kV accelerating voltage and ion source with 500 μm/h milling speed

A specimen with low milling rate


Specimen : Zirconia

Milling depth:1.5 mm

Accelerating voltage:8 kV, Milling time : 8 h 200 μm 1 μm

Milling a deeper position

It is possible to mill and observe a specimen where structures of interest exist in a deeper position.
*Example of using an optional holder (IB-11610NMSHA) Specimen : IC chip

Milling depth:3 mm

Accelerating voltage:8 kV 1 mm
Milling time : 7 h

5 μm

CROSS SECTION POLISHER 5


Planar surface milling
Large Specimen Rotation Holder (IB-11550LSRH)  Option

The use of the optional Large Specimen Rotation Holder (IB-11550LSRH) enables planar surface milling over a large area for specimens subjected to mechanical
polishing (beam irradiation angle is 0°to 90°). Beam irradiation at a low angle, with respect to the specimen surface, makes effective removal of scars caused by mechanical polishing, or
of crystalline strains on the surface. This leads to enhancement of the channeling contrast. On the other hand, the irradiation at a high angle, with respect to the specimen surface,
enables acquisition of the topographic information resulting from the difference of milling rate caused by the existence of crystalline grain boundaries or their internal crystalline structures.
The following example shows three backscattered electron images of a mechanically-polished copper plate, which is subsequently subjected to planar surface milling by changing
the irradiation angle of the Ar ion beam. The top two images show the result of low-angle milling (specimen tilt: 85°,ion beam irradiation angle: 5°,accelerating voltage: 4 kV, milling
time: 10 min). The bottom right image shows the result of high-angle milling (specimen tilt: 60°,ion beam irradiation angle: 30°,accelerating voltage: 4 kV, milling time: 3 min).
Specimen : Copper plate

Mechanical polishing

Ion beam


Low-angle milling

Specimen
High-angle milling

Backscattered electron image of a mechanically- 3 μm Backscattered electron image of the 3 μm


polished copper plate. Many scars due to polishing copper plate milled at a low angle. Scars due to polishing
are seen to make grain boundaries unclear. disappear and the channeling contrast is enhanced.

SEM image common data


Backscattered electron images, Accelerating voltage: 5 kV

Ion beam

30°

Specimen

Large Specimen Rotation Holder (IB-11550LSRH)


Backscattered electron image of 3 μm
Maximum specimen size : 40 mm dia. × 15 mm thick
the copper plate milled at a high angle.
Specimen tilt : 0°to 90°
Applying additional high-angle planar surface milling provides
the topographic information dependent on crystal orientation
(many surface irregularities) indicated by blue arrows.
Cross-section rotated milling
Cross Section Preparation Kit (IB-12540CKIT) Option  *This kit is attached to the Large Specimen Rotation Holder (IB-11550LSRH).

The use of a cylindrical shielding material enables cross-section preparation by irradiating the specimen from any direction (360°).
Even for a specimen with many voids, this milling technique reduces milling marks for enabling creation of a uniform cross section.
Comparison of milling performance
using a specimen with many voids Milling marks Specimen : Mechanical pencil core

Cross Section Preparation Kit


(IB-12540CKIT)
5 μm 5 μm
Cross section prepared Cross section prepared with the kit
with the shielding plate

6 CROSS SECTION POLISHER


Carbon coating
Option  

The use of ion beam sputtering enables carbon coating. A carbon-coated film with this capability has
high density, granularity and uniformity. Thus, this carbon coating suppresses charging and is effective for elemental
analysis and EBSD mapping of insulating materials.
This capability allows the coating of all of the specimens, to which cross-section milling, planar surface milling or cross-
section rotated milling, were applied by CP. In addition, specimens prepared by other techniques can be carbon-coated.

Specimen : Cross section of a printed part on a paper

50 μm 50 μm
Without coating With coating

Carbon coating holder


(IB-12510CCH)

Specimen : Concrete

500 μm 500 μm
Without coating  Backscattered electron image With coating  Backscattered electron image

The left SEM image is taken without coating. Abnormal contrast, due to charging, is seen.
The right SEM image is taken with coating. Carbon coating eliminates the influence of charging.

Carbon coating adapter


(IB-12530CCA)
※ T his adapter is attached to the
Large Specimen Rotation Holder
(IB-11550LSRH).

Large specimens (max. 40 mm dia. ×


max. 15 mm thick) can be coated
while rotating it.

CROSS SECTION POLISHER 7


Auto milling program

Auto milling start mode

This mode automatically starts milling. Immediately after reaching the preset chamber pressure, milling (ion-beam
irradiation) starts automatically.

Intermittent milling mode

The intermittent milling mode can set the times for repeatedly turning the ion beam ON & OFF and control the beam dose per unit
of time for suppressing temperature rise of the specimen. Thus, this mode is effective for milling low-melting-point metals, rubbers
and polymers. In the following two images, a differently-milled rubber specimen is shown. The left image shows a specimen without
intermittent milling, exhibiting deformation of the rubber part resulting from heat due to continuous ion-beam irradiation. On the
other hand, the right image shows a specimen with intermittent milling, leading to a reduced deformation by thermal damage.
Specimen : Chloroprene rubber

5 μm 5 μm
Without intermittent milling With intermittent milling
(ion-beam irradiation ON : 8 s / OFF : 30 s)

Fine milling mode

This mode automatically switches the accelerating Process time(h)


0 1 2 3 4

voltage from high to low at the end of high-voltage


ion milling so that finishing can be made. Owing to Conventional way
3.5 kV, 4 h
this mode, a high-quality (uniform) cross section is
With fine milling mode
prepared in a short time, which is equivalent to the
8 kV, 30 min
An equivalent-quality cross section is prepared in a short time.
conventional milling at low accelerating voltage.
3.5 kV, 5 min

The figures below are EBSD patterns of a cross section of a milled silicon wafer.
In the milling only at high accelerating voltage, non-crystalline layers on the milled cross section become thick, thus
making the EBSD pattern unclear. But the use of the finishing mode enables thin non-crystalline layers to be prepared
in a short time, thus providing the clear EBSD pattern.
Specimen : Silicon wafer

Without finishing milling voltage : 8 kV With finishing milling voltage : 8 kV + 3.5 kV

8 CROSS SECTION POLISHER


Precise positioning adjustment system
A variety of holders and optional attachments are available for precise adjustment of the
processing position.

Mount base specimen holder (standard)


Standard specimen holder
IB-11560MBSH
A new standard mount base specimen holder can use not only
the standard Positioning CCD Camera, but also a dedicated
Precise positioning precise positioning microscope (option) by removing the holder
adjustment from the CP. This capability enables more precise adjustment
of the processing position at higher magnification.

Precise positioning microscope

・Cross-section
observation
Positioning
CCD Camera ・Processing
position
adjustment

Precise positioning
microscope
(P/N:783118511)
Max. magnification:×150,
Positioning accuracy : Approx. 10 µm
Option

Precise positioning microscope TYPE2


(P/N:783120664)
Max. magnification:×500,
Positioning accuracy : Approx. 3 µm
Option

You can adjust the processing


position even the use of only the
standard Positioning CCD Camera.

FE-SEM compatible holder  Option

By using a holder (option) compatible with a scanning


electron microscope (SEM), it is possible to observe
an SEM image and mill the specimen alternately.

SEM observation

FE-SEM compatible holder Option

    IB-11610NMSHA

The use of the precise positioning microscope enables more accurate adjustment
of the processing position. It is possible to mill a cross section for a very small
structure (10 μm or less), including fine foreign materials, pin-holes and via.

Specimen: FIB-milled silicon wafer

Milled
face

Surface 10 μm Cross section 10 μm

CROSS SECTION POLISHER 9


Standard work process

1
Cutting material
Cut a material with a diamond cutter or similar tool to make a piece that can fit onto the specimen stub.

Specimen

Wax

Specimen stub

Attach the specimen to the specimen stub using wax.

2
Mounting and processing position adjustment of the specimen

Set the shielding plate Processing position adjustment

Shielding plate

3
Cross-section milling by ion beam irradiation
Ions are irradiated while the specimen is rocked, providing a high-quality (uniform) cross section.
※ Patent: No. EP 1517355 B1, US 7722818 B2, JP 4557130 Patent related to rocking function

4
SEM observation
Cross-sectional SEM image of a printed board

Milled surface (viewing surface)

A large cross-section area is obtained. 500 μm

10 CROSS SECTION POLISHER


Handy Lap

After cutting the material with a


diamond cutter, the use of the handy
lap makes it smoothly trim the edge
as needed (mechanical polishing) for
adjusting the specimen size.

The position of the shielding


Positioning
CCD Camera plate can be adjusted from
the monitor screen of the
CCD camera.

Specimen edge

Shielding plate

Enlarged image of the specimen edge taken with the CCD camera

Set the ion source voltage


and etching time from the
touch panel screen.
Touching the Start icon
automatically starts the
etching after the completion
of vacuum evacuation.

Monitor screen for operation

When the optional


I B -14510M C A M M i l l i n g
Monitoring Camera is
installed, the milling process
can be monitored in real-
time.

Monitor screen for milling and observation

CROSS SECTION POLISHER 11


Applications (soft materials)
Soft materials (copper, aluminum, gold, solder, polymers, etc.) can also be easily processed.
In conventional mechanical polishing, it was difficult to prepare those soft materials.

Cross section of bonded gold wire

The channeling contrast, dependent on the difference in crystalline orientation of gold (Au), can clearly be observed in
the images below. The images thus demonstrate ideal milling with no strains. In addition, physical stress is not applied
during milling, thus visualizing the specimen-originated defects (voids) generated on the bonded interface.

Bonded Voids
gold wire

Backscattered electron images 10 μm 1 μm

Lead-free solder

The lower left figure is a cross-sectional SEM (backscattered electron) image of a bump (lead-free solder) prepared by CP. The lower middle
figure and lower right figure respectively show the backscattered electron image of the bonded interface and the EDS phase analysis
result (map) of the same area. These results demonstrate that alloy layers of copper and tin can clearly be observed and analyzed.
⑤ Ag

④ Sn

③ Cu6Sn5

② Cu3Sn

① Cu

Backscattered 100 μm 1 μm
electron images

Scales of butterfly Tablet (medicine)

Cross section of scales from the wing of a Morpho The following SEM image is a backscattered electron image of a
butterfly. Milling was performed without resin tablet subjected to planar surface milling using the optional Large
embedding so that the native state of Specimen Rotation Holder. Since milling can be made in a dry
the scale surface can be observed. condition, a water-soluble specimen like tablet can easily be milled.

1 μm

Secondary electron images 1 μm Backscattered electron image 10 μm

12 CROSS SECTION POLISHER


Applications (hard materials, composite materials, powders)
Hard materials (ceramics, glass, etc.), or composite materials containing the hard and soft
materials, can be processed.

Diamond blade

The following figures are a backscattered electron image of a diamond plate and the corresponding EDS maps of the
imaged area. A uniform cross section can be created for the diamond abrasive grains that are embedded in soft metal.

Elemental map:C Elemental map:O

Backscattered electron image 25 μm Elemental map:Cu Elemental map:Sn


(contrast adjusted by image processing software)

Fluorescent material

The following two images are an SEM (secondary electron) image of the surface of a powder-like fluorescent material
and an SEM (backscattered electron) image of the cross section of the same specimen milled by CP. The use of CP
allows preparation of a cross section from the powder specimen.

Surface morphology (secondary electron image) 10 μm Cross section (backscattered electron image) : 10 μm
Resin-embedded specimen

Dichroic mirror

The following figures are a cross-sectional SEM (backscattered electron) image of a dichroic mirror and the corresponding EDS maps of
the imaged area. Fine structures (multi layers), which selectively reflect the light with specific wavelength, can be observed and analyzed.

Backscattered 1 μm Elemental map:Si Elemental map:Ti Elemental map:O


electron image

CROSS SECTION POLISHER 13


Applications (hard materials,
composite materials, powders)

Crystal orientation analysis of a ceramic knife made of zirconia

CP easily allows cross-section preparation for a hard material like this knife.
The following figures show EBSD analysis results of the ceramic knife subjected to cross-sectional milling. A sharp
EBSD pattern (upper right figure) and a crystal orientation map (lower left figure) are acquired. An IQ map (upper left
figure) also provides high-quality crystalline information.

IQ map 5 μm An EBSD pattern acquired from zirconia

Phase : Zirconia
Size :X 18.4 μm, Y 12.2 μm
Step : 0.04 μm

Zirconia

FE-SEM : JSM-7200F, EBSD : EDAX/TSL,


CCD camera : DVC5, Software : OIM 7.2

IPF map surface orientation 5 μm

Hard disk

The following image shows a cross section prepared from magnetic recording layers on the top surface of a hard
disk. To protect the surface of this magnetic disk, metal coating is applied before the milling. Two magnetic recording
layers, with a very small thickness of approximately 10 nm, can be clearly observed.

Metal coating
(applied before the milling,
Magnetic recording layer to make protective layers)
(approx. 10 nm)

HDD disk

Backscattered electron image 100 nm

14 CROSS SECTION POLISHER


Specimen holders
The following table shows functions and features of the main specimen holders. A variety of
optional holders, are available for different purposes.

Function Model and Feature Max. specimen size


Model:IB-11560MBSH (Standard holder)
Cross-section IB-11560MBSH
Name:Mount base specimen holder
milling
W: 11 mm
・ Precise adjustment of the processing L: 10 mm
position is enabled using a precise T: 2 mm
positioning microscope. Shielding
plate
Positioning OM

Model:IB-11610NMSHA Option

(FE-SEM compatible holder)


Name:Specimen holder

・ The specimen can be observed without W: 11 mm


changing the holder. A nonmagnetic L: 8 mm
shielding plate is used. T: 3 mm
Shielding plate
・ Precise adjustment of the processing
SEM observation
position is enabled using a precise
IB-11610NMSHA
positioning microscope.

Model:IB-11550LSRH Option
Planar surface IB-11550LSRH(Common)
Name:Large specimen rotation holder
milling
・ Planar sur face milling can be made
while rotating the specimen. Changing Dia.:40 mm
the tilt angle provides sur face T: 15 mm
irregularities due to removal of polish Specimen
scars or preferential etching effects.

Irradiation angle : 0 to 90°

Model:IB-12540CKIT Option
Cross-section IB-12540CKIT
Name:Cross section preparation kit
rotated milling
① Dia.:1 mm
・ This kit is attached to IB-11550LSRH. The
  L: 1 mm
use of a cylindrical shielding material enables
cross-section preparation by irradiating the
② Dia.:0.5 mm
specimen from any direction (360°).
  L: 1 mm
・ Milling marks, generated in a specimen with many
voids or a composite material, can be reduced.

Model:IB-12530CCA Option
Carbon coating IB-12530CCA
(for planar surface- or cross-section rotated milling)
Name:Carbon coating adapter

・This adapter is attached to IB-11550LSRH.


Dia.:40 mm
A specimen, subjected to planar surface
T: 15 mm
milling or cross-section rotated milling, can
be coated while rotating it.

 (Specimens for planar surface milling or


cross-section rotated milling are coated) Carbon target

Model:IB-12510CCH Option
Carbon target
(for cross-section milling)
Name:Carbon coating holder

・ This holder accommodates a CP specimen stub


or IB-11610NMSHA for coating a specimen.

・ The holder also accommodates an SEM


specimen holder for coating the SEM specimen.

 (Specimens for cross-section milling are coated) IB-12510CCH

CROSS SECTION POLISHER 15


Specifications
Ion accelerating voltage 2 to 8 kV

Ion beam diameter 500 µm or more (full width at half maximum)

Milling speed 500 µm/h or more (Average over 2 h, Accelerating voltage 8 kV, Si equivalent, Edge distance 100 µm)

Specimen swing function Automatic swing of specimen during milling by ± 30°(patent No. 4557130)

Auto milling start mode When reaching the preset pressure, milling starts automatically.

Intermittent milling mode Ion beam irradiation time and stop time are settable (ON : 1 to 999 s, OFF : 1 to 999 s)

Maximum specimen size 11 mm (W) × 10 mm (L) × 2 mm (T) (with standard holder)

Specimen movements X-axis : ± 6 mm, Y-axis : ± 2.5 mm

Operation Touch panel, 6.5-inch display

Positioning for milling Monitor from above the specimen stage with a CCD camera. Milling position is also adjustable with OM.

Positioning camera Magnification : approx. × 70 (on 6.5-inch display)

Monitoring camera*1 Magnification : approx. × 20 to 100 (on 6.5-inch display) (with IB-14510MCAM attached)
Positioning camera and Monitoring camera can be switched for displaying one on the external
External monitor output*1
monitor (with IB-14510MCAM attached)
Preset function 4 sets of milling conditions (accelerating voltage, Ar gas flow, milling time, intermittent milling)

Gas for ion Argon gas

Gas flow control Mass flow controller

Pressure measurement Penning gauge

Evacuation equipment Turbo molecular pump, Rotary pump


Dimensions and weights
  Basic unit 545 mm(W)× 550 mm(D)× 420 mm(H), Approx. 66 kg (with IB-14510MCAM attached)
  Rotary pump 150 mm(W)× 427 mm(D)× 230 mm(H), Approx. 16 kg

Installation Requirements
Single phase 100 to 120 V AC, 50/60 Hz, Allowable input voltage fluctuation : less than 10%,
Power supply
Rating : 15 A or more
Maximum power
650 VA
consumption
Grounding 100 Ω or less
Dry argon, Purity : 99.9999% or more
Argon gas* 2

Pressure : 0.1 to 0.2 MPa (1.0 to 2.0 kgf/cm2), Hose joint : ISO 7/1 Rc 1/4   
Room temperature 15 to 25℃

Room humidity 60% or less (no condensation)

*1 With IB-14510MCAM attached, the specimen can be monitored in real time. The status of the specimen can be observed while milling is in progress.

The external monitor must be prepared by the customer.

*2 The argon gas, gas cylinders and regulator must be prepared by the customer.

To handle heat sensitive materials and materials that react to air

Cooling CROSS SECTION POLISHER IB-19520CCP


【With adjustment of cooling temperature and air-isolated system】

The IB-19520CCP is a CROSS SECTION POLISHER with the added functions of specimen
cooling (with adjustment of cooling temperature) and isolation from the atmosphere. This
is an ideal tool for preparing cross sections for SEM or low melting point materials, like
solder, which is susceptible to thermal deformation during milling; low glass transition
point materials like resins; and the materials that react to air, like battery materials.
IB-19520CCP

※ The screen images in the catalog include items that are still under development, and are subject to change without notice.

※ The specifications and appearance of the instrument are subject to change without notice.

No. 1201K767C Printed in Japan, Kp


TM

JEM-ARM300F
The JEM-ARM300F is a highly stable
microscope featured with the technology
cultivated through the development of
the JEM-ARM200F.

The spherical aberration corrector


can be mounted to STEM and/or
TEM lens systems.

The JEM-ARM300F is the


300kV-ultrahigh resolution electron
microscope of the unprecedented
performance.
300 kV STEM Imaging (GaN[211])
Dark-field image, Ga-Ga atomic column
63 pm
JEM-ARM300F
Atomic Resolution Electron Microscope

80 kV STEM Imaging (Si [110])


Dark-field image

300 kV STEM Imaging


Silicon nitride (β-Si3N4) crystal grain boundary
HAADF

63 pm 1 nm

1 nm
136 pm 1 nm

300 kV TEM Imaging (silicon nitride β-Si3N4) 80 kV TEM Imaging (graphene) ABF

1 nm
TM

Simultaneous STEM image acquisition


High-angle annular dark-field observation (HAADF) /
Annular bright-field observation (ABF)

1 nm 1 nm

Main specifications Installation room


Standard accelerating voltage 300 kV, 80 kV Floor 7,000 (width) × 8,000 (depth)
Ultra-high resolution High resolution space
Version configuration Double-corrector configuration
configuration
(STEM/TEM)
STEM resolution Ceiling
(300 kV) when height Crane hook position:
0.058 nm 0.063 nm 3,600 (height) or more
STEM corrector is
configurd * Depends on the specification.

Lattice resolution: Lattice resolution: 1,300 (width) × 2,000 (height)


TEM resolution 0.05 nm 0.06 nm Carry-in
* When the TEM corrector is configurd,
(300 kV) when Nonlinear information limit: Nonlinear information limit: entrance the height becomes 2,200 or more.
TEM corrector is 0.06 nm 0.07 nm
configurd Linear information limit: Linear information limit: (unit:mm)
0.09 nm 0.12 nm

External appearance and specifications are subject to change without notice.

No. 1305L783C Printed in Japan, Kp


Scientific / Metrology Instruments
Electron Spin Resonance Spectrometer

JES-X3 series
JES-X310 / JES-X320 / JES-X330
Electron Spin Resonance Spectrometer
ESR Spectrometer JES-
The ESR Spectrometer JES-X3 series has an improved low-noise Gunn oscillator
sensitivity compared to previous models.
ESR is the only instrument for directly detecting paramagnetic species.
This supports a variety of applications in research, development, inspection and

High sensitivity
The standard configuration includes a Gunn oscillator as the stable,
low-noise microwave oscillation source, and a cylindrical (TE011) cavity
with an internal modulation method providing modulation with good
uniformity and a high Q value, enabling high-sensitivity measurements.
The data is the ESR signals for 1 μM TEMPOL/benzene solution.

Signal : Power 1 mW

Noise : Power 200 mW

Magnetic field linearity


This figure shows the 6 ESR lines derived from Mn 2+ measured
by changing the center field by 20 mT for each spectrum. The
coincidence of each peak position, even under different field setting,
indicates the excellent field linearity of the magnet field.

1
X3 series ■ Improved sensitivity with the ultra-low noise
Gunn oscillator
■ Built-in microwave frequency counter
■ Intuitive user interface
providing a 30% improvement in ■ Various automatic measurement modes
■ 3 types of magnets to suit the application
■ Zero cross-field sweep function
■ Wide variety of attachments
evaluation.

High resolution
High-purity materials are used for the magnet pole pieces and
precisely engineered to provide a magnetic field with superior
uniformity. The addition of ring shims to the pole piece surface makes
it possible to obtain excellent uniformity over a wide range.
The separation of the t-butyl group (4.7 μT) showing the smallest
division of the galvinoxyl radical can be obtained.

Magnetic field stability


Data acquired near the center of the ESR signal for the perylene cation
radical. Even with a signal exhibiting fine splitting, there is no spreading,
demonstrating the exceptional stability of the magnetic field.

1 scan

50 scans

100 scans

2
Intuitive User Interface (ESR measurements)
All the functions needed for ESR measurements are presented in 1 window that can be operated intuitively.
Start the ESR system, adjust the microwaves from the Q-DIP window, set the acquisition conditions and

Q-DIP
Easily perform microwave adjustment.

Dynamic range
Switch between 5 settings.

Software for ESR analysis (P5)

(B) ■ Microwave adjustment functions


(A) Microwave adjustment can be performed automatically using AUTOTUNE, or
manually using various buttons.

(A) AUTOTUNE
Automatically optimizes the phase, coupling and detection of the resonance
frequency of the microwaves.
(B) MANUAL TUNE
Manually adjust the phase and coupling while observing the Q-DIP waveform.
(B)
(C) Show Q-value
Displays the approximate Q value.
(D) Mn Marker
(B)
(D) The insertion amount (0 to 1000) of the Mn marker can be adjusted.
(C)

3
start measurements.

ESR measurement

Sequential measurement
Automatic continuous measurement can be set.

Manual sweep
Check for presence of an ESR signal
before measurement and set start
position manually.

■ Sequential Measurement Mode


Various 2-dimensional measurements can be obtained by sequentially varying
the ESR measurement parameters automatically. Liquid Phase

Example of sequential measurement parameters


○ Temperature ○ Microwave power (saturation) ○ Modulation width
○ Detection phase ○ Crystal axis (anisotropic tensor) ○ Amplification

Parameter change increment


Solid Phase
Arithmatic sequence Geometric sequence User-defined sequence

E
R

Other functions
U
T
A
R
E
P
M
Interval time Repeat measurement Integration T
E

Data auto-save Save/Load parameter settings


ESR signal of the TEMPOL radical in glycerol
Temperature varied in 2 ℃ steps from – 35 ℃ to + 37 ℃

4
Data Processing for ESR Signal Analysis
The system is equipped with the tools required to obtain the information needed for ESR analysis
(g-factor, A value, spin, linewidth, etc.) from the acquired measurement data.

■ g-factor information
When a line is set on the ESR signal, the g-factor information can be extracted and a table of g-factors can be
generated. The g-factor table can be saved in text format and processed using spreadsheet software. Highly-precise
g-factors can be obtained by performing correction of the magnetic field using the Mn markers as a reference.

■ Spin calculation
The number of spins (radical concentration) can be calculated with the results presented in a list. The number of spins
is proportional to the doubly-integrated value (area) of the ESR signal. The number of spins for an unknown sample
can be determined by comparing the doubly-integrated value obtained for unknown samples with the value for a
standard sample, e.g. TEMPOL, with a known concentration. Sensitivity correction is applicable by doubly-integrating
Mn2+ signal as well.

5
■ Waveform Processing
Available processing includes arithmetic operations on the signal, conversion to exponential and logarithmic forms,
differentiation and integration, adjusting size and position for fitting signal, and baseline correction.

◦ Arithmetic operations ◦ Differentiation and integration


Arithmetic operations on waveforms. Differential and integral processing of waveforms.

◦ Spectrum separation
If the conditions are matched, spectrum separation may be possible using subtraction.

◦ Background elimination
When there are known substances mixed into the sample, or when paramagnetic impurities are found in the sample tube,
the arithmetic functions can be used to eliminate the background signal from the impurities.

① Sample including impurities

② Impurities

① - ② (Background elimination)

◦ AUTO SHIFT · AUTO GAIN ◦ X-Shift · Y-Shift


Signal position and intensity can be adjusted automatically. Data can be freely manipulated, including moving the signal
longitudinally or vertically, and varying the intensity.
◦ Smoothing
When power cannot be applied because the sample is easily saturated, or the concentration is low, a sufficient S/N
might not be obtained. In such cases, smoothing can be used to reduce the noise components.

◦ BASELINE correction
Baseline correction can be performed by approximating the baseline components using a regression curve.
· Linear approximation · Regression curve (2nd to 11th order curve)

Before baseline correction

After baseline correction

6
■ Various 2-Dimensional Displays
The display range can be set for signals and 2D data, and 2D data can be edited and created.

TEMPOL radical ESR signal


The microwave power range is varied in 1 mW steps from 1 to 20 mW

■ Peak information
By specifying an area on the ESR signal, it is possible to extract peak information (intensity, linewidth, intensity relative to
the Mn marker) and generate a peak table. The peak table can be saved in text format and processed using spreadsheet
software.

■ Other functions
◦ Partial signal zoom ◦ Batch conversion of multiple files into text format
The original spectrum data is a 64 K point binary format;
but, it is possible to compress the number of points and
convert the files into text format. All the data files contained
in a folder can be converted into text files at one time.

XY axis data in text format

7
Simulation Assisting ESR Signal Analysis

■ Simulation software
Simulation of Isotropic and Anisotropic ESR signals is included in the standard configuration. In the simulation for an ESR
signal for which the radical types can be estimated, the waveform is calculated from the signal-specific information, such
as the splitting width, g-factor, and linewidth, in addition to the actual measurement conditions like resonance frequency,
center magnetic field and sweep width.
For the anisotropic simulation, the anisotropic parameters (g-factor anisotropy, A-value anisotropy, linewidth anisotropy)
are used to calculate the waveform. Axial symmetry as well as rhombic anisotropy can be handled.

◦ Isotropic simulation ◦ Anisotropic simulation

Simulation of ESR signal of the Anthraquinone radical anion Simulation of ESR signal for copper

Sample Tubes
Sample tubes have an outer diameter of 2 to 5 mm, with the measurement section made from high-purity synthetic quartz.
For samples with a large dielectric losses and liquid samples, sample tubes with a smaller diameter, capillary tubes or aqueous
sample cells may be more suitable. Unit:mm

◦ Quartz For X-band 5 φ ◦ For X-band (Quartz tip) 3 φ ◦ Quartz For Q-band 2 φ
270  Part No.:780225392 Part No.:422000272 Part No.:620007125
100  Part No.:820374083
5φ 3φ 5φ 2φ

5φ 270 80 190 100

100

◦ For X-band (Quartz tip) 5 φ ◦ For X-band (Quartz tip) 2 φ ◦ For sample rotation device
Part No.:422000281 Part No.:422000990 A=5φ Part No.:800310641
3φ Part No.:800310659
5φ 2φ 5φ
A

100 170 80 190 300

* The caps for sample tubes are sold separately.

8
Attachments Enabling a Variety of ESR Measurements

■ Variable Temperature Controller (ES-13060DVT5)


◦ Features ◦ Composition
・Variable temperature range:103 to 473 K ・Temperature controller
・Temperature stability : ± 0.5 K ・Heating tube
・Dewar adapter Liquid Phase
・USB connection
・Metal Dewar
・Temperature control : Auto PID
・Variable temperature adapter
・Compressor flow : 17 L/min (air)
・Compressor
・Dewar volume : 10 L
(30 L Dewar also available as option
Variable temperature range : 113 to 473 K)

Solid Phase

ESR signal of the TEMPOL radical in glycerol


Temperature varied in 2℃ steps from -35 to +37 ℃

* Separate consultation required for 400 ℃ VT.


10 L Dewar 30 L Dewar

■ Liquid He Variable Temperature Controller (ES-CT470)


◦ Features ◦ Composition
・Variable temperature range : 2.5 to 470 K ・Cryostat
・Easy set-up : Assembly time : about 20 min ・Transfer line
・Rapid cooling : From room temperature to 4.2 K :15 min ・Dewar adapter and spacer
・Temperature stability : ± 0.5 K ・Flow meter
・Can use both UV radiation and Mn markers ・Temperature sensor
・Easy sample exchange ・Temperature controller
・Control using liquid nitrogen available ・Parts for assembly and spare parts
(Variable temperature range : 80 to 470 K)

* Additional rotary pump is needed for the experiments


conducted below 4.2 K.

ESR signal of silicon dangling bond

9
■ Aqueous Sample Cells (ES-LC12)
◦ Features ◦ Specifications
・Flat cell structure makes ・Volume:130 μL
it possible to minimize ・Sample tube outer shape (mm):12 × 1.5
reduction of sensitivity. ・Sample tube inner shape (mm):10 × 0.25
・Permitted temperature range:Room
temperature

50mm

ESR signal of DMPO spin adducts of superoxide


Holder Suction pump anion radical

■ Sample Angular Rotation Device (ES-12010)


◦ Features
・Angle setting resolution:0.06° (Rotation angle: 0 to 360° )
・Variable temperature controller (ES-13060DVT5) and the liquid
helium variable temperature controller (ES-CT470)can be used
concurrently.

◦ Compatible cavity
・ES-UCX2/ES-MCX3B

◦ Sample rod
・1 each of 5 φ, 3 φ are provided

Angular rotation spectrum (1.2° increments) of diamond


Ⅱ a monocrystal irradiated with an electron beam

■ Q-Band Microwave Unit (ES-SQ5)


◦ Features
・Temperature variation can be performed by attaching the Mn2+
(B) Q-band Cr3+
temperature control adapter (ES-UTQ3) to the variable temperature
unit (ES-13060DVT5) . ν = 34.85 GHz
・High filling factor H0 = 1248.8 mT
・Only small sample volumes needed (a few μL )
Mn2+( g =1.981)
(A) X-band
◦ Composition
・Compatible ESR systems : JES-X320/JES-X330 ν = 9.454 GHz
Cr3+
・Q-Band cavity H0 = 340.96 mT
・Q-Band microwave unit

◦ Sample tubes
ESR signal for Mn2+ containing Cr3+ as impurities is
・Q-Band dedicated sample tubes shown around the center field Ho.
(A) X-band, (B) Q-band

Q-Band microwave unit configuration


(Left) Q‐Band microwave unit
(Right) Q‐Band cavity

10
Attachments Generating Radicals by External Stimulation

■ Ultraviolet Irradiation Apparatus (ES-USH500 / USH500H / UXL500 / UXL500H)


◦ Features
・Variable temperature controller (ES-13060DVT5) and the liquid helium variable temperature controller (ES-CT470)can be used concurrently.
・Can choose a high-voltage mercury lamp or a xenon lamp.
・2 types of irradiation models for each light source.
・The ultraviolet irradiation accessory kit (ES-UVAT1) and condenser lens (ES-UVLL/UVLS) are required options.
・Selectable irradiation wavelength using colored glass filters.

Irradiation time

Variation in ESR signal intensity relative to the irradiation time of


polymethacrylic resin (optical fiber)

* A cart for moving the ultraviolet irradiation apparatus is not included.


* Please inquire about irradiation apparatus using optical fiber if needed.

■ Time-Resolved ESR System (ES-CIDEP)


◦ Features
・Time resolution of several hundred ns

◦ Composition
・Wide-band pre-amplifier (ES-WBPA4)
・Digital oscilloscope
・Time-resolved ESR software
・Cables

Sample:TMDPO / benzene solution


YAG laser: 355 nm (3rd harmonic)
* Laser light source and optical path not included.

11
■ Helix Electrode Electrolytic Cell (ES-EL30)
◦ Features
・ Can use with the Variable temperature controller
(ES-13060DVT5).
・ Measurement possible for highly-polar organic solvents
(DMSO, DMF, etc.) or with water as the solvent.

◦ Composition
・Electrolytic cell (glass vessel)
・Electrodes (Au),
Reference electrode (Ag)
・Sample tube (quartz)

Anthraquinone anion radical ESR signal

Helix working electrode Exhaust port Counter-electrode terminal

Working electrode terminal Reference electrode terminal

Please see the attachment brochure for other options, such as insertion type Dewar, ODMR, EDMR, ESRET, ENDOR, and so forth.

12
ESR Applications

Inspectio
n/ A
sse
ssm
Green tea
Pepper
Quartz Coral
en
t
Shell

Foods Fossils & Rocks


s
ion

Lipid
peroxide Antioxidant function assessment Tooth Dating Barite
act

Irradiated food detection Bone Dosimetry


OH O2
- -・ Disinfection / Sterilization Source location estimates Ruby
X re

Sugar Pearl
Active
Catalyst Adsorbed

ESR
Beer oxygen
Medicine Gemstones
Glass molecules
EDO

Living organisms
Active

Inorganic materials
is of biological R

nitrogen
Diamond
Biological Function analysis
membranes DNA Ceramics Coal
Metabolism / Activity Defect locations & structure Carbon
Capsules REDOX status etc. Bonding state
Lubricants
Conductivity etc. Petroleum

Pharmaceuticals Organic Basic research


/ Supplements and Resources
Surfactants Organic Superconductors
magnetic
materials conductors Semiconductors

technology
Crude drugs

Structural a
Saccharides
Organic materials Methane

Electrical materials
Analys

hydrate
Clathrate
compounds
Deterioration mechanisms Conductors
NO Reaction mechanisms Coating Conductive Performance / Durability Thin metal film
NO2 Results of radiation / exposure to light films polymers Recombination rate Flame

Gases etc. Withstand voltage characteristics etc. Gas

Polymer materials Combustion

n
Magnetic
Ferromagnet Photo/Thermal polymerization process

a
films Photocatalyst
Shear effect

l
Solar cells
Magnetic
Diamagnetic material

ysis
O2 Molecular motion etc. Methanol

Paramagnets materials Complexes Transition


Magnetic properties etc. Electron state etc. metals
Magnetic Synthetic
polymers resins
Rare earths Liquid crystals Enzymes

n t
me
CVD films IGZO

lo p
a l s d eve
M ate r i

Installation Example
Unit:mm

JES-X310 JES-X320 JES-X330


AC100V AC200V Cooling water AC100V AC200V Cooling water
AC100V AC200V Cooling water Single phase 500VA 3-phase 13kVA 22mm dia Single phase 500VA 3-phase 20kVA 22mm dia
Single phase 500VA 3-phase 2kVA 12mm dia
Dewar for VT Dewar for VT
Dewar for VT
800

800
800

Power
803

Power supply
613

600
600

supply Magnet Magnet


電磁石
600

Magnet
683
3800 or more

703
3600 or more

3800 or more

1400 1600
1180
1200

Spectrometer Spectrometer
1200

Data System Data System


1200

Spectrometer
Data System
800 800
800

3000 or more 3200 or more 3200 or more

13
Main Specifications

JES-X310 JES-X320 JES-X330


Electromagnet
Maximum magnetic field (T) ~0.65 ~1.3 ~1.4
Sub-polepiece magnetic field (T) - ~1.7 ~2.0
Sweep width (mT) ±0.01 to 250 ±0.01 to 500
Magnetic field setting accuracy ±5µT or ±0.1% or less (whichever is larger )
Long term stability 5×10-6
Pole diameter (root)/Effective gap(mm) 150 / 60 240 / 60 360 / 75
Microwave unit
Frequency range (GHz) 8.750 to 9.650
Frequency count display 7 digits (std)
Microwave output (mW) 0.0001 to 200
Microwave tuning Auto
Cavity
Resonance mode / Q value (no load) Cylindrical TE011 / 18000 or more
Mn marker Auto / Motor control
Data system
OS Windows® 10
Spectrum resolution (bit) 16
Analysis software/ Simulation Standard

Dimentions and Weight

External dimensions = Width × Depth × Height

JES-X310 JES-X320 JES-X330


Electromagnet (Including SHF table)
Dimensions(mm) 1,180×710×1,105 1,400×803×1,190 1,600×990×1,190
Weight kg 520 1,060 2,300
Spectrometer
Dimensions(mm) 300×602×602 / 35
Excitation power supply
Dimensions(mm) Included in magnetic chassis 683×613×895 703×803×1,114
Weight kg - 300 500
Power requirements
Spectrometer 1φ 100 V, 500 VA
Magnet(Breaker rating) 3 φ 200 V, 2 kV 3 φ 200 V, 13 kVA 3 φ 200 V, 20 kVA
30 A 60 A 100 A
Power supply fluctuation / grounding ± 5 % / Class D grounding
Cooling water
Water pressure (MPa) 0.05 to 0.2 0.15 to 0.3
Flow rate (L/min) / Temperature (℃) 6 / 15 to 25 8 /15 to 16/25 16 /15 to 25
Faucet outer diameter (mm) 12 22

* Appearance and specifications are subject to change without notice.


* The official name of Windows® is the “Microsoft Windows® Operating System”.
* Microsoft and Windows® are registered trademarks of Microsoft Corporation in the USA and other countries.

14
No.2101C829C(Bn)
Scientific/Metrology Instruments
Focused lon Beam System

JIB-4000
High-throughput FIB column with high operability
facilitates cross-section milling / observation,
STEM/TEM specimen preparation and fine processing.
JIB-4000 Focused
High Throughput FIB

High-throughput FIB column with high operability facilitates cross-section


milling/observation, SEM/TEM specimen preparation and fine processing.

Main features
l High-throughput processing achieved by a large-probe current FIB column
l User-friendly FIB system with new instrument design
l Compact size for flexible layout - Installation space reduced by 20%
(compared to JEOL conventional models)
l Twin stage* for easy specimen preparation for TEM
l Stage Navigation System* for fast determination of observation position
*Optional

Cross-sectional milling and Thin-film specimen Fine milling


observation preparation for TEM

1 JIB-4000 Focused Ion Beam System


Ion Beam System

JIB-4000 Focused Ion Beam System 2


FIB Processing

High Power FIB column


In the JIB-4000, the maximum probe current of the ion beam is increased to 60 nA. This achieves higher-speed processing,
shortening a processing time to 1/3 (compared to JEOL conventional models). High-speed processing with large probe current is
especially effective for facilitating cross-section milling for a wide area (100 µm or more).

Example: Cross-section milling of solder bump with 100 µm diameter

Before processing Deposition Rough milling Final milling

n Deposition n Rough milling n Final milling

Conventional models 300 min

80 min
0 100 200 300
Processing time [min]

Comparison of procesiing time with conventional models Milled cross section (SIM image)

Rapid and Mill modes Mill Rapid

Two milling modes, rapid mode for rough milling and mill
Rapid
mode for final milling, are preset in the JIB-4000. Optimum
milling is executed simply by selecting a desired mode.
Mill

2.7μm 7.3μm

1nA, Dose: 5 nC/μm2 SIM

Deposition
Ion-beam based deposition protects the specimen surface from damage due to FIB processing. The JIB-4000 comes with one
deposition unit and you can select a deposition material from carbon, tungsten and platinum. Up to two optional deposition units
can be installed. When changing a deposition material, the cartridge for a gas source is replaceable from the outside of a vacuum.

3 JIB-4000 Focused Ion Beam System


JIB-4000 Focused Ion Beam System

Low accelerating voltage processing


When a thin film for TEM is prepared by FIB,
Ga-doped layers are formed on both sides of the thin
film. However, the Ga-doped layers disturb TEM
(STEM) observation, depending on the specimen
category. In this case, by decreasing the accelerating
voltage during the final milling, you can make the 10nm 10nm
Ga-doped layers thinner. The JIB-4000 enables you to Ga-doped layers formed on Si single crystal.
vary the accelerating voltage of the Ga ion beam Left: Processed with 30 kV (thickness 23 nm) Right: Processed with 5 kV (thickness 6 nm)
between 1 kV and 30 kV.

Bitmap processing (optional)


The JIB-4000 can perform pattern-like processing
using binary pattern data in BMP format.
Simple drawing function enables you to create
simple figures on the monitor screen, such as line,
rectangle, circle, ring and polygon.

In addition, 3D-pattern processing is possible through


serial milling using multiple bitmap pattern-data file.

Automatic processing
The JIB-4000 enables you to set the processing procedure (recipe) for deposition, rough milling and final milling and also the
positions to be processed in advance, thus achieving continuous automatic processing of multiple positions. This function
increases the processing efficiency because all-night automatic processing is executed immediately before final processing, and
then, only the final processing is performed by the operator in the next morning.

Example: Thickness measurement of film prepared by automatic processing


Using automatic processing, five cross sections were prepared from a 10-mm square Si chip on which oxide film was formed.
The positions of the five cross sections in the Si chip are the center part and four edges (upper, lower, right, left). After the
completion of automatic processing, SIM images were acquired from the cross sections and the evaluation of the oxide-film
thickness was performed for each position.

Center part Upper edge Lower edge Left edge Right edge

The above images show the states of each position after automatic processing.
Automatic processing executes protective-film creation (carbon deposition), rough milling and final milling.

2.91um 2.93 um 2.92 um 2.93 um 2.91um

Center part Upper edge Lower edge Left edge Right edge

The above SIM images show cross sections prepared by automatic processing. (tilt angle: 60°)
SIM images reveal that the oxide-film thickness of each position is almost the same, verifying successful processing with uniform thickness.

JIB-4000 Focused Ion Beam System 4


TEM/SEM Specimen Preparation

The JIB-4000 is also used as a specimen preparation system for TEM thin-film specimens, SEM specimens and specimens to be
analyzed by an EPMA or Auger instrument. To help smooth specimen transfer to a TEM or SEM instrument, various optional
attachments are available.

Bulk-specimen motor stage Cross-section preparation for SEM


A cross section milled by FIB is subject to high-
& Airlock system
The bulk specimen stage affords observation of the resolution SEM observation and elemental analysis
entire surface of a specimen with 20 mm x 20 mm. The using an EDS.
airlock system enables rapid installation of a specimen
holder on the specimen stage.

Bulk-specimen motor stage Airlock system

Focused Ion Beam System Cross-section preparation for TEM


The JIB-4000 can prepare thin films from specific
micro areas with high accuracy.

Side entry goniometer stage (optional) Additional thinning for TEM specimens
This stage enables direct insertion of a tip-on holder, useful A sample is cut into a block by FIB, fixed on an
for additional processing of TEM thin-film specimens. FIB grid, and thinned by FIB.

5 JIB-4000 Focused Ion Beam System


JIB-4000 Focused Ion Beam System

Holder for SEM (SEM compatible specimen mount)


It is possible to use a JEOL SEM, EPMA or Auger SEM
instrument with a common specimen mount. An FIB- Thermal Field Emission SEM
processed specimen (placed on the specimen mount) is
transferred to an instrument with the specimen mount
attached, for observation and analysis. Since the same
specimen mount is used, the specimen is easily
positioned for an additional processing point.

Specimen mount

FIB bulk specimen FIB bulk specimen FE-SEM specimen


holder 2 holder 1 holder adapter

Atmosphere pick-up system (optional)


This system is for lifting out a prepared TEM specimen
SEM image [Specimen:512M-DRAM]]
in atmosphere and for transferring it onto a grid.

TEM
Atomic Resolution AEM

TEM compatible tip-on holder


The JIB-4000 employs a side-entry goniometer
stage commonly used with a JEOL TEM. Since a tip-
on holder and a shuttle retainer can be shared with
a JEOL TEM, you can easily repeat FIB processing
and TEM observation.

STEM image / EDS elemental maps [Specimen:256M-DRAM]

JIB-4000 Focused Ion Beam System 6


SIM Image Observation

High-resolution FIB column


The JIB-4000 is an effective tool for not only processing but also observation. Since the resolution of SIM (scanning ion microscope)
image is improved to 5 nm at 30 kV, clearer SIM images can be obtained.
In particular, SIM images offer better channeling contrast than SEM images. Because channeling contrast is produced by crystalline
orientations, SIM images are effective to evaluate metallographic structures and plated films. 

Example: Cross-section observation of Cu plating and NiP plating


Cross-section preparation and SIM observation were performed for a Fe substrate on which Cu and NiP plating was made. SIM
result was compared with that obtained with an LaB6 SEM. SIM image shows better channeling contrast than LaB6 SEM images,
clearly distinguishing crystal grains in the specimen.

NiP plating

Cu plating

Fe substrate

SIM image SEM SE image SEM BE image

Unlike the electron beam, the penetration depth of the ion beam into a solid is very small, thus SIM images reveal the top-surface
state of the specimen. In cross-section observation, SIM image does not contain information on an internal structural object,
precisely offering the cross-sectional state.

Example: Cross-section observation of magnetic recording layers on the backside of a ticket


SIM image clearly shows dispersion of
iron-oxide particles on a binder surface.
But in SEM image, the binder part is
transparent and this makes iron-oxide
particles appear inside the cross section,
disturbing image interpretation.

SIM image SEM image


Accelerating voltage: 30 kV Accelerating voltage: 15 kV

Wide view Measurement functions


The wide view mode facilitates the search of target processing positions Cursor measurement of an acquired image is possible on
with an ultra-low magnification (x 60). In particular, this capability is G U I . Tw o m e a s u r e m e n t m o d e s a r e a v a i l a b l e ;
useful when you want to find the target positions on large specimens measurement in the vertical and horizontal directions and
and for multi-position processing. depth measurement of cross sections. The result of depth
measurement is displayed with a value corrected by taking
account of a stage tilt angle versus a depth seen in the
monitor screen. Depth measurement is useful for
thickness measurement of layer structures.

7 JIB-4000 Focused Ion Beam System


Optional accessories that assist you in
specimen preparation

Atmosphere pick-up system


This system is for lifting out a prepared TEM specimen in atmosphere and for transferring it onto a grid.
This system consists of a micropipette preparation device, a glass probe preparation device and an
optical microscope with a manipulator.

Micropipette preparation device Glass probe preparation device Optical microscope with manipulator
(CCD camera is sold separately)

Specimen holders and adapter


The following specimen holders and adapter facilitate movement of the specimen prepared by FIB to another instrument for SEM or TEM
observation.

FIB Bulk-Specimen Holder 1 FIB Bulk-Specimen Holder 2 FE-SEM Specimen Holder Adapter Shuttle Retainer
& Specimen Mount

25.4 mm Specimen Holder Vice One Touch Holder One Touch Holder Shuttle Retainer Holder 1

Shuttle Retainer Holder 2 Pin & Specimen Mount Holder Pin & Specimen Mount Pin & Specimen Mount
10 mm dia. 5 mm dia.

JIB-4000 Focused Ion Beam System 8


Mouse-Based Easy Operations

Easy-to-understand user interface


The JIB-4000 user interface is displayed on a 24-inch wide monitor screen.
You can easily operate the JIB-4000 with the aid of appropriately-labeled large operation buttons and graphic icons.

1 2

1 Beam condition setting When you set relevant conditions, the conditions of accelerating voltage and beam current are
 automatically switched in a short time, supporting smooth operations.

2 Customized buttons You can allocate frequently used beam conditions to your customized buttons. Each user can
customize the buttons according to different purposes.

3 Various operation tabs Various operations, such as processing, stage movement and image saving, are integrated to the
corresponding tabs. You can easily access the buttons you want to use.

4 Displaying Since the specimen-holder status is graphically displayed on the monitor screen, you can precisely find the
specimen-holder status specimen status. In addition, the stage can be moved from the graphic display.

Simple setting of FIB processing


In the JIB-4000 user interface, three key processing modes (Depo, Rapid,
Mill) are preset for facilitating preparation of cross sections and TEM thin
films.
When you select a processing mode depending on your purpose, processing
is automatically executed with optimum beam scan conditions.
The processing conditions that you set can be saved in the process recipe.
When you want to repeat the processing for the same specimen, simply
calling the recipe proceeds to a desired processing. This feature improves
the processing efficiency and achieves proper processing not influenced by
skills of operators.

9 JIB-4000 Focused Ion Beam System


JIB-4000 Focused Ion Beam System

Stage Navigation System (SNS) (optional)


Before transferring the specimen to the instrument, by taking a color image of the specimen from a macro area using the stage
navigation system, this image is utilized for navigation of the field of view.
In addition, when you double-click a target position from a photo of the entire specimen holder, the specimen stage moves to the
corresponding position, eliminating difficulty in position search.

Smooth stage movement Image acquisition


Stage tilt and rotation are executed by a motor-driven Simply clicking the Photo and Save icons acquires an image. The
eucentric mechanism, achieving smooth movement with acquired images are displayed on a thumbnail view of the Image
little shift of the field. File tab. Since the photography conditions and position
In addition, you can preset the tilt angles frequently used for information are simultaneously saved during image acquisition,
processing or observation, making it easy to change the tilt you can go back to the position where the image was taken.
angles depending on your purpose. (Position Memory function)

Operation panel (optional)


All the operations can be performed using a mouse. You
can add optional operation knobs for the frequently
adjusted functions.

JIB-4000 Focused Ion Beam System 10


Focused lon Beam System

Principal specifications Installation requirements


FIB Power Single phase 100 V ± 10 %

Ion source Ga liquid metal ion source 50/60 Hz, 3 kVA

Accelerating voltages 1 to 30 kV (in 5 kV steps) Grounding terminal One, 100 q or less

Magnification ×60 (for searching for a field) Nitrogen gas* 0.4 ± 0.05 MPa
×200 to x300,000 Exhaust duct Exhaust pipe of 25 mm inside diameter
Image resolution 5 nm (at 30 kV) Room temperature 18 to 25 °C
Beam current Up to 60 nA (at 30 kV) Humidity 60 % or less
Movable aperture 12 steps (motor drive) External magnetic field 5 μT or less
Processing shapes by milling Rectangle, line, and spot Floor vibration Please consult your JEOL service office if any
adverse effect is anticipated due to floor
vibration and acoustic noise. JEOL service
Specimen stage personnel investigate the installation room
Bulk-specimen 5 axis goniometer stage before installing the instrument to judge the
maximum observable magnification.
Movement range X: ± 11 mm
Y: ± 15 mm
Z: 0.5 mm to -23 mm Example of Installation Layout
T: -5° to +60° 2650
R: 360°
Maximum specimen size 28 mm dia. (13 mm H) /
RP
50 mm dia (2 mm H) N2 Gas

Vacuum pump
RP/TMP/SIP Main Operation PC
1000
Console
2300

Console

Optional attachments
Gas injection system 2 IB-02100GIS2
Carbon Deposition Cartridge IB-52110CDC2
750 750
Tungsten Deposition Cartridge IB-52120WDC2

Platinum Deposition Cartridge IB-52130WDC2 850


Unit: mm
Side Entry Goniometer Stage IB-01040SEG

Probe Current Detector IB-04010PCD

Operation Panel IB-05010OP Special Specimen holders


Stage Navigation System IB-01200SNS 25.4 mm Specimen Holder SA0777
FIB Tip-on Holder EM-02210 Vice One Touch Holder SA0778
FIB Bulk-Specimen Holder EM-02220 One Touch Holder SA0779
FIB Bulk-Specimen Holder 1 EM-02560FBSH1 Pin & Specimen Mount Holder SA0780
FIB Bulk-Specimen Holder 2 EM-02570FBSH2 Shuttle Retainer Holder 1 SA0781
FE-SEM Specimen Holder Adapter EM-02580FSHA Shuttle Retainer Holder 2 SA0782
Shuttle Retainer EM-02280 Pin & Specimen Mount 10 mm dia. SA0789
Atmosphere Pick-up System EM-02230 Pin & Specimen Mount 5 mm dia. SA0790

*Nitrogen gas and the connection tube are customer-provided.


*Specifications subject to change without notice.

3-1-2 Musashino Akishima Tokyo 196-8558 Japan Sales Division Tel. +81-3-6262-3560 Fax. +81-3-6262-3577

• AUSTRALIA & NEW ZEALAND /JEOL(AUSTRALASIA) Pty.Ltd. Suite 1, L2 18 Aquatic Drive - Frenchs Forest NSW 2086 Australia • BELGIUM /JEOL (EUROPE) B.V. Planet II, Gebouw B Leuvensesteenweg 542, B-1930 Zaventem Belgium • BRAZIL
/JEOL Brazil Instrumentos Cientificos Ltda. Av. Jabaquara, 2958 5° andar conjunto 52 ; 04046-500 Sao Paulo, SP Brazil • CANADA /JEOL CANADA, INC. 3275 1ere Rue, Local #8 St-Hubert, QC J3Y-8Y6, Canada • CHINA /JEOL(BEIJING) CO., LTD.
Zhongkeziyuan Building South Tower 2F, Zhongguancun Nansanjie Street No. 6, Haidian District, Beijing, P.R.China • EGYPT /JEOL SERVICE BUREAU 3rd Fl. Nile Center Bldg., Nawal Street, Dokki, (Cairo), Egypt • FRANCE /JEOL (EUROPE) SAS Espace
Claude Monet, 1 Allee de Giverny 78290, Croissy-sur-Seine, France • GERMANY /JEOL (GERMANY) GmbH Gute Aenger 30 85356 Freising, Germany • GREAT BRITAIN & IRELAND /JEOL (U.K.) LTD. JEOL House, Silver Court, Watchmead, Welwyn
Garden City, Herts AL7 1LT, U.K. • ITALY /JEOL (ITALIA) S.p.A. Palazzo Pacinotti - Milano 3 City, Via Ludovico il Moro, 6/A 20080 Basiglio(MI) Italy • KOREA /JEOL KOREA LTD. Dongwoo Bldg. 7F, 1443, Yangjae Daero, Gangdong-Gu, Seoul, 134-814,
Korea • MALAYSIA /JEOL(MALAYSIA) SDN.BHD. 508, Block A, Level 5, Kelana Business Center, 97, Jalan SS 7/2, Kelana Jaya, 47301 Petaling Jaya, Selangor, Malaysia • MEXICO /JEOL DE MEXICO S.A. DE C.V. Arkansas 11 Piso 2 Colonia Napoles
Delegacion Benito Juarez, C.P. 03810 Mexico D.F., Mexico • RUSSIA /JEOL (RUS) LLC. Krasnoproletarskaya Street, 16, Bld. 2, 127473, Moscow, Russian Federation • SCANDINAVIA /SWEDEN JEOL (Skandinaviska)AB Hammarbacken 6A, Box 716,
191 27 Sollentuna Sweden • SINGAPORE /JEOL ASIA PTE.LTD. 2 Corporation Road #01-12 Corporation Place Singapore 618494 • TAIWAN /JIE DONG CO., LTD. 7F, 112, Chung Hsiao East Road, Section 1, Taipei, Taiwan 10023 Republic of China
• THE NETHERLANDS /JEOL (EUROPE) B.V. Lireweg 4, NL-2153 PH Nieuw-Vennep, The Netherlands • USA /JEOL USA, INC. 11 Dearborn Road, Peabody, MA 01960, U.S.A.
No. 1101K579C Printed in Japan, Kp
Scientific / Metrology Instruments
High Performance Gas Chromatograph – Time-of-Flight Mass Spectrometer

JMS-T200GC
AccuTOF GCx-plus
TM

GC-TOFMS & Direct TOFMS


with high speed, high resolving power,
and high mass accuracy.
High performance and all-round TOFMS

AccuTOF GCx-plus TM

AccuTOF GC
TM

The AccuTOF GCx-plus is the most advanced mass spectrometer system of the AccuTOF
TM TM

AccuTOF GCv
TM

GC series products. The AccuTOF GCx-plus provides solutions for a variety of applications.
TM

Solutions provided by AccuTOF GCx-plus TM

AccuTOF GCv 4G
TM

High performance p 3
TM
Basic performance of AccuTOF GCx-plus

p 5 Various ionization and sample introduction techniques


Reliable determination of elemental composition AccuTOF TM
GCx
The high-resolution and high mass accuracy AccuTOF GCx-plus TM
p 7 User friendly software
enables accurate elemental composition determination, which is a TM
p 9 AccuTOF GCx-plus technologies
powerful tool for the qualitative analysis of unknown compounds and
impurities. p11 A wide range of applications

p12
High-speed data acquisition Application 1
Chemistry
The AccuTOF GCx-plus performs high throughput analysis using
TM

Fast GC with its high-speed data acquisition capability (50 spectra/s).


It also supports GCxGC for ultrahigh separation analysis.

p13 Application 2
Material Science

A wide range of applications


All-round p15 Application 3
Polymers

A variety of ionization and sample introduction


techniques
p16 Application 4
While electron ionization (EI) is effective in acquiring structural
Environmental Science
information, detection of molecular ions is critical in qualitative
analysis of unknown compounds.

In addition to chemical ionization (CI), the AccuTOF GCx- TM

p17 Application 5
plus supports field ionization (FI), field desorption (FD), and Food Safety
photoionization (PI), which are powerful soft ionization techniques
for molecular ion detection.

The system also supports direct sample inlets for analysis of high p18 Application 6
boiling point compounds and rapid analysis. Metabolites

AccuTOF GCx-plus
TM

p19 Application 7
Fragrances

The AccuTOF GCx-plus is a superior gas chromatograph time-of-flight mass spectrometer


TM

p20 Application 8
(GCTOFMS) system that simultaneously accomplishes high-resolution analysis, Petroleum Products
high mass accuracy, and high-speed data acquisition.

p21 Specifications・Installation requirements

1 | AccuTOF GCx-plus | 2
TM
AccuTOF GCx-plus
TM
High performance
TM
Basic performance of AccuTOF GCx-plus

Solutions provided by AccuTOF GCx-plus TM

Basic performance of AccuTOF GCx-plus TM

Elemental composition determination by accurate mass analysis GCxGC analysis by ultrahigh speed data acquisition

Accurate mass measurements are easily accomplished 2-dimensional (2D) TICC of diesel fuel by GCxGC/TOFMS
Accurate results for reliable elemental composition determination in GCxGC analysis, which requires ultrahigh speed data

2nd column (polar) separation; Polarity


The AccuTOF GCx-plus consistently acquires high resolution, high mass accuracy, and high sensitivity data
TM acquisition.
for long periods of time. It also achieves high mass accuracy from low intensity peaks, facilitating reliable This is especially effective for nontargeted qualitative analysis
of trace components.
determination of elemental compositions. Furthermore, the AccuTOF GCx-plus, with its wide dynamic range, TM

can easily analyze compound mixtures at different concentrations.

High resolution High mass accuracy 1 ( at different concentrations, single ion )

Amount of injection Error


763.9546[M-F3 ] + [pg] [mDa]

1:    0.1 0.26
2:    0.5 0.54
R=11,424
3:    1 0.34
4:    5 -0.56 1st column (nonpolar) separation; Boiling point
5: 10 -0.04
6: 50 0.07
7: 100 0.21
8: 500 -0.02 Ultrahigh separation analysis GCxGC (comprehensive 2D GC)
9: 1000 0.08
GCxGC is an ultrahigh separation chromatography system designed to use 2
EI mass spectrum of perfluorotripentylamine EI mass spectrum of octafluoronaphthalene ( zoomed around m/z 272 ) and m/z columns having different polarities, trap the eluted components using a modulator
measurement errors of the molecular ion at various injection amounts
at the end of the 1st column at given intervals, and perform high-speed analysis

Intensity
High mass accuracy 2 ( single component, multiple ions ) Stable mass accuracy over time of the trapped components in the 2nd column. GCxGC is a powerful capillary GC
technique that features higher resolution chromatography than traditional capillary
5
Measured
accurate mass
Calculated
exact mass
Error
[mDa]
Inferred
formula
Unsaturation
GC and is capable of high-sensitivity analysis of components by group. This technique
Mass error ( mDa )

74.03625 74.03623 0.01 C3H6O2 1.0


3
87.04395
143.10639
87.04406
143.10666
- 0.10
- 0.27
C4H7O2
C8H15O2
1.5
1.5
requires a detector capable of high-speed data acquisition because the peak widths
Retention time[min]
199.16917 199.16926 - 0.08 C12H23O2 1.5 1 in the chromatograms are extremely sharp compared to traditional capillary GC.
213.18507 213.18491 0.16 C13H25O2 1.5
255.23156
267.26802
255.23186
267.26824
- 0.30
- 0.22
C16H31O2
C18H35O
1.5
1.5
-1 Peak width: 0.18 s
298.28640 298.28663 - 0.23 C19H38O2 1.0
Injector
1st column: Modulator:
-3
Ordinary capillary GC column Continuously repeats cold
Ex.: nonpolar to slightly polar Modulator trapping and thermal desorption :
-5
stationary phase in every 3 to 7 seconds
0 20 40 60 80 100 9 data points
Injections Detector: MS, etc. At a data acquisition speed of 50 spectra/s,
the AccuTOF GCx-plus is capable of ultrahigh
TM
1st column 2nd column:
EI mass spectrum of methyl stearate and accurate mass m/z measurement errors of the molecular ion of octafluoronaphthalene (OFN; m/z separation GCxGC analysis while maintaining
Narrow bore capillary GC
measurement results of the major ions 271.9867) when 100 fg of OFN was repeatedly measured for 100 times (GC column AccuTOFTM GCx -plus column ample data points across each chromatographic
GC oven 2nd column
bleeding at m/z 281.0511 was used as the internal mass reference) ・High-speed data acquisition Ex.: mid- to highly-polar peak.
・Always runs at high mass resolution stationary phase
・Accurate mass measurement
High sensitivity / Wide dynamic range

100fg CV=5.2%, IDL=16fg Linear response > 1x10 Wide mass range
4

Injection no.   Peak area


1 65745
Correlation coefficient: 0.999 FD mass spectrum of polystyrene 5200
2 67212 Oligomer analysis with direct MS
3 58394
The AccuTOF GCx-plus, with a wide mass range and
TM
4 70698
5 65897
6 65604
direct inlet system, can analyze samples with large
7 65994 molecular weights that are difficult to handle with GC.
8 65230
CV(%) 5.2
Intensity

IDL(fg) 16 Sample: OFN: 0.1, 1, 10, 100, 1000 pg (n=3, each)


EIC range: m/z 271.9867 ± 50 ppm
Data recording rate: 0.5 s
Calibration curve: logarithm
Correlation coefficient: 0.999
100 fg of octafluoronaphthalene (OFN) was measured continuously 8 times.
From the standard deviation of the EIC peak areas of OFN molecular ions, an
A 4 order linear response was verified by measuring 100 fg to 1,000 pg of OFN.
instrument detection limit (IDL) of 16 fg was calculated.
The wide dynamic range is critical for accurate qualitative/quantitative analysis.
CV: Coefficient of variation IDL: Instrument detection limit

m/z

3 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 4
TM
All-round
Various ionization and sample introduction techniques

Solutions provided by AccuTOF GCx-plus TM

A variety of ionization and sample introduction techniques

EI / FI / FD combination ion source (optional)


Why are multiple ionization techniques critical in GC/MS?
Features
EI, the most widely used ionization technique in GC/MS, is superior in sensitivity and reproducibility.
A single ion source supports EI (hard ionization) and FI/FD (soft ionization) techniques.
It is also supported by an immense database.
Switching between EI and FI/FD is simple and quick.
For any scientist using GC/MS in search
▶ No need to change the ion source
of further information, what is ultimately
▶ No need to change the GC-interface
Terpinen-4-ol (C10H18O) in tea tree oil important is molecular ion detection. EI,
HO ▶ No need to break vacuum
using a high ionization energy of 70 eV,
EI generates numerous fragment ions, from Effective use of EI/FI/FD:
which structural information is acquired. ▶ EI for qualitative analysis through library search

However, EI often fails to show strong ▶ FI for molecular weight determination

▶ GC/FI for type analysis of hydrocarbon samples


molecular ion signals. Consequently,
M+ . ▶ FD for polymer analysis
qualitative analysis results may be incorrect
▶ Accurate mass measurement
PI if they solely rely on database searches.

PI (Photoionization) ~ EI / PI combination ion source


Thus, it is critical in GC/MS analysis to
enhance the accuracy of qualitative analysis The PI Ion Source adds a vacuum ultraviolet light source to the standard EI Ion source, enabling photoionization.
by using various soft ionization techniques
M+ .
FI in addition to EI. On the AccuTOF GCx- TM
Aromatic hydrocarbons, which strongly absorb UV light, are preferentially
plus, FI, PI, and CI are optionally available as ionized with PI, making the technique useful for detecting aromatic
Filament hydrocarbons in a complex mixture.
soft ionization techniques. With the accurate
50 100 150 200 250 300 mass measurement capability for all MgF₂ window Average mass spectra of diesel fuel : n-Alkanes
m/z : Aromatic hydrocarbons
ionization techniques, elemental composition To mass analyzer
of the analyte can be reliably determined.
PI

FI and FD - Ideal soft ionization techniques for molecular weight determination


Deuterium lamp Ion repeller
FI
FI and FD are ionization techniques with a low level of internal energy in molecular ions compared to EI and CI.
Being soft ionization techniques with minimum fragmentation, FI and FD are ideal for molecular weight determination. Schematics of the ion source
50 100 150 200 250 300 350 400
m/z
FI ( Field Ionization ) FD ( Field Desorption )
▶ The sample is introduced to the ion source through GC or a ▶ The sample is applied onto the emitter and directly introduced CI
standard sample inlet system. to the system.
▶ Unlike CI, FI uses no reagent gas; no need to choose a reagent ▶ Suitable for analysis of thermally labile compounds.
Optional CI source comes with 3 different reagent gas lines, eliminating a lengthy process of reagent gas selection.
gas appropriate for the analyte. ▶ Ideal for samples soluble in nonpolar solvents.

▶ Analyzes powder samples dispersible in solvents.


Tip of the FD probe ▶ Analyzes low- to mid-polar metal complexes. Direct sample inlet system (optional)
▶ Analyzes high molecular weight samples not supported in

GC/MS, such as polymer. 2 types of direct sample inlet probes for different applications
▶ EI and CI supported

Schematics of FI Gas phase molecules Schematics of FD Condensed phase molecules


(neutrals) (neutrals)
DEP (Direct Exposure Probe)
GC column
M+[M+H]
.
, +,etc.
M+[M+H]
.
, +,etc. Ideal for high boiling point/thermally unstable compounds.
Anode
Anode
(Emitter)
(Emitter)
Platinum The sample, which is dissolved in a solvent, is applied to the
Cathode Cathode filament filament at the tip.
Electric current

Carbon emitter
e-
Carbon emitter
DIP (Direct Insertion Probe)
MS e- MS
Ideal for high boiling point compounds/samples insoluble
in solvent. A solid sample can be directly introduced to a
dedicated glass sample tube for analysis.
10kV
10kV

Glass sample tube


In FI and FD, ionization occurs by the removal of electrons from neutrals via the action of a high electric field.
Load-lock flange for DIP/DEP/FDP

5 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 6
TM
User friendly
User friendly software

Solutions provided by AccuTOF GCx-plus TM

User friendly software

AccuTOF GCx-plus main program “msAxel”


TM
Software for simultaneous quantitative analysis of multiple components - “Escrime”

1 Auto tuning by Tuning Assistant Escrime is designed to calculate EIC peak areas, plot calibration curves, and determine quantitative values. With further
▶ Accomplishes high performance tuning without a lengthy manual process. manipulation of the resulting data including separate or collective editing of area calculation ranges, this software significantly
▶ Facilitates easy acquisition of optimum sensitivity/resolution in all ionization modes (EI, CI, FI, FD, PI). speeds up the quantitation process.

Peaks of the components contained in multiple


2 Powerful automated functions
samples or peaks of multiple components in a
▶ Auto drift correction single sample can be presented on a single view.
Automatically performs drift correction on every The peak area calculation ranges can be
spectrum in acquired data. simultaneously changed, allowing for batch
▶ Auto data conversion analysis of more than 150 samples.
Automatically converts acquired data to netCDF
format. Blank
▶ Auto data transfer

Automatically transfers acquired data to any


location (PC for data analysis, etc.) 0.1 ppb

1 ppb

10 ppb

Sample

Pe a k a r e a r a n g e

Polymer analysis software “Polymerix”

FD mostly forms ions that reflect the molecular weights of analytes through the formation of M , [M+H] and [M+Na] , thus allowing for
+. + +

the calculation of the average molecular weight, degree of polymerization, and polydispersity from the m/z and the intensity of each
peak. Polymerix is designed to calculate the average molecular weight, degree of polymerization, and polydispersity of polymers,
3 Interactive views
and estimate the repeated structure and end groups from the data acquired in FD and FI.
  Chromatograms and mass spectra on a single view. Elemental composition determination using exact mass on the same view.
The example below is a visualization of the relative abundance (distribution) of each molecule in an ethylene oxide/propylene oxide
(EO/PO) block copolymer. Polymerix easily calculates the average molecular weight and polydispersity.
Other features, including isotopic
peak pattern simulation, elemental
Molecular distribution of EO/PO block copolymer
composition determination, and
calibration table editor, can be EO/PO block copolymer Repeat B, EO: (C2H4O)n
arranged as the user wishes.
CH3

H OCH2CH2 OCH2CH OCH2CH2 OH


x y z

PO: (C3H6O)n
Repeat A
FD mass spectrum of EO/PO block copolymer

Mn : Number average molecular weight


Mn Mw Mz PD
Mw : Weight average molecular weight

1053.2 1077.1 1100.9 1.0
Mz : Z average molecular weight
PD : Polydispersity index (Mw/Mn)

7 | AccuTOF GCx-plus | 8
TM
AccuTOF GCx-plus
TM
Standard EI ion source and
AccuTOF GCx-plus TM ion transfer system
Successfully eliminates 99.9% or more of He ions.
Stable high-transmission-rate (=high sensitivity) ion
transfer system maximizes detector lifetime.
( Patent JP3967694, US7034288, GB2404080 )

Automatic isolation valve rce m


agn
et

Sou
Allows for changing/cleaning of the ion source while
maintaining high vacuum in the mass analyzer Analyte ions
Helium ions
r lit
cto es
High response detector Sp
l it d
efle
m edia
t
li t le
ns
tic
len
s

Inter Sp o sta
High speed MCP detector unit with enhanced response ctr
Ele

Source magnet: Helps deflect low-mass carrier gas ions to maximize


detector lifetime.
Split lens: Guides helium ions to the intermediate slit where they
are rejected by optimizing the lens 2 voltage balance.
Mass analyzer Split deflector: Corrects the trajectory of the analyte ions.
Flight tube with enhanced thermal stability;
maintains high mass accuracy

Gas Chromatograph
(Agilent 7890B)
High vacuum system
Fully integrated in the spectrometer console
2 turbo molecular pumps
2 rotary pumps

Digitizer
Insures a 4 order dynamic range by the 4 GHz digitizer (ADC) and
high performance data acquisition system

Direct inlet flange


Supports analysis by GC and direct sample introduction (DIP, DEP, FDP)
techniques

New!

Auto-reservoir
Mass reference compounds and volatile samples can be introduced
automatically for easier accurate mass measurements.

9 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 10
TM
Application
A wide range of applications

Solutions provided by AccuTOF GCx-plus TM


Application 1

A wide range of applications


Chemistry

Rapid analysis within a minute with direct sample inlets


How does the AccuTOF GCx-plus support a wide range of applications?
TM

Direct sample introduction with FDP, DIP, or DEP, is optimum for confirming synthesized organic
The AccuTOF GCx-plus can be equipped with various direct sample inlet systems in addition to the compounds since the measurement is quick and accurate mass can be obtained. Direct sample inlets
TM

standard GC/MS interface, allowing analysis of both volatile and high-boiling point analytes. are also suitable for high boiling point analytes.
FI, FD, and PI, which are unique to AccuTOF GCx-plus, further expand applications.
TM

AccuTOF GCx-plus will provide solutions to your challenging problems.


TM

1. Analysis of organic electro-luminescence material


Mass spectra of organic electro-luminescence compound

An organic electro-luminescence compound was analyzed Desorption EI


with a combination of DEP and EI (a.k.a., Desorption EI, or
Application 1 Application 2 DEI) and with FD.
Chemistry p12 Material Science p13 Analysis time was within 1 minute for either method. M+.

Elemental composition was confirmed with measured


1. Analysis of organic electro- 1. Analysis of a photopolymerization initiator accurate mass with either method.
luminescence material 2. Analysis of antioxidant The FD mass spectrum was simpler and suitable for
2. Analysis of fullerenes 3. Analysis of pigments molecular weight confirmation.
4. Analysis of ionic liquid
5. Analysis of fluorinated compound
100 200 300 400 500

Application 8 Application 3

Petroleum Products p20 Polymers p15 FD


M
+.

C40H30
1. Ultrahigh separation analysis of 1. Pyrolysis GC/MS of acrylic resin
diesel fuel with GCxGC 2. Thermal extraction GC/MS of additives in a resin
2. Type analysis of microcrystalline 3. FD analysis of polystyrene
Measured accurate Calculated exact Error Inferred formulamass
wax with FD mass mass [mDa]
510.23380 510.23420 -0.40 C40H30

A wide range of


Application 7

Fragrances p19
applications
Application 4

1. GCxGC/TOFMS analysis of tea tree oil Environmental Science p16


2. GCxGC/TOFMS analysis of rose oil
1. Analysis of PCBs in oil 2. Analysis of fullerenes
Mass spectra of fullerenes
A mixture of fullerenes was analyzed with Desorption EI C60 M
+.

DEI and FD. With DEI, the mass spectrum


was more complex with fragment ions. With
FD, it was easy to conclude that the sample
C60 M 2+

was a mixture of C60 and C70. C70 M +.

Application 6 Application 5
C70 M 2+

Metabolites p18 Food Safety p17


1. Analysis of fatty acid methyl esters (FAMEs) 1. Analysis of agrochemical residues in food
2. Analysis of isomeric disaccharides
C60 M
+.

FD

C70 M +.

C60 M 2+

C70 M 2+

11 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 12
TM
A wide range of applications A wide range of applications

Application 2

Material Science Analysis of samples of various states


Pigments and an ionic liquid, which are insoluble or non-volatile and not amenable for GC, were analyzed in
1. Analysis of a photopolymerization initiator minutes and their molecular weights determined.

Mass spectra of Irgacure 907


Irgacure 907, a α-aminoalkylphenolic
photopolymerization initiator, does not show EI
FD mass spectra of pigments
molecular ion at all with EI. With FI, 3. Analysis of pigments
M +.

the molecular ion is easily observed. Copper phthalocyanine


575.08
Using FD ionization, the AccuTOF GCx-plus detected
TM

Intensity
molecular ions for the refractory and insoluble pigments.

Irgacure 907
C15H21NO2S Mw : 279.12930
FI m/z
M
+.

Pigment Green 7
M +.

1118.46

Intensity
C32H16CuN8 C32Cl16CuN8
Mw : 575.07939 Mw : 1118.45584

Copper phthalocyanine (top) Pigment Green 7 (bottom) m/z


Why is EI alone not sufficient?
EI mass spectra can be searched against mass spectral libraries and elemental compositions of the
observed ion can be inferred. However, a compound cannot be identified if the molecular ion is not FD mass spectrum of an ionic liquid
4. Analysis of an ionic liquid sample (MS Tips No. 113)
detected and there is no meaningful hit in the library search. It is absolutely important to detect molecular
C
ions with soft ionization methods such as FI and PI. Identification of unknowns is made quick and reliable 150.1
FD makes it easier to detect cations and cluster ions. Further
with the EI/FI/FD combination ion source or EI/PI combination ion source.
accurate-mass analysis allows for determination of the elemental
formula of each compound.

Intensity
Cationic compound (C) : Anionic compound (A) : C2A
Pyridinium compound Fluorinated compound (triflate) 580.2
2. Analysis of a high-boiling-point compound (antioxidant ) (MS Tips No. 123)

Since FI does not ionize column bleed, the TICC clearly shows the high-boiling-point compounds.
m/z
TICC (Sample: Irganox 1010)
GC/EI EI
Irganox 1010 Ionic species Measured accurate Calculated exact Error [mDa] Inferred formula
C73H108O12 Mw: 1176 mass mass
Mass spectra of a fluorinated compound
C 150.12887 150.12827 0.60 C10H16N
C2A 580.17664 580.17384 2.80 C22H32F6N3O4S2
EI
Intensity

5. Analysis of fluorinated compound [M-H2O] +.

GC/FI
FI Many fluorinated compounds show no molecular ions with EI. With CI,
Irganox 1010
some fluorinated compounds show a hydride-abstracted cation [M-H] , +

CI
which can be easily misinterpreted as a protonated molecule [M+H] . +
[M-H2O+H] +

With FI, the molecular ion M can be clearly observed.


+.

[M-H] +

Retention time [min]

FI
M
+.

High quality GC/MS interface with no cold spot


Irganox 1010 is one of the highest boiling point compounds amenable to GC/MS. Total ion current [M-H2O] +.

chromatogram of Irganox 1010 shows a sharp, symmetric chromatographic peak, thus supporting the 4-(Trifluoromethyl) cyclohexanemethanol
C8H13F3O
thermal homogeneity of the GC/MS interface. Mw : 182.09185

Irganox and Irgacure are trademarks of BASF.

13 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 14
TM
A wide range of applications A wide range of applications

Application 3

Polymers
1.Pyrolysis GC/MS of acrylic resin (MS Tips No. 101) 3. Calculating the average molecular
weight of polystyrene using FD FD mass spectrum of polystyrene 5200
Pyrolysis GC/MS is widely used as an analytical technique for high molecular weight polymers.
Instant thermal decomposition makes it a simple yet powerful technique with high reproducibility. The mass spectrum acquired from polystyrene
5200 using FD ionization shows ions at m/z 6500
TICC of acrylic resin Pyrolysis GC/EI/TOFMS or higher. The AccuTOF GCx-plus is effective for
TM

GC/TOFMS, which is capable of acquiring polymer analysis in the oligomer range in addition
exact-mass results in a single GC/MS analysis, to GC/MS analysis. For FD ionization, the system is
Methyl methacrylate
enhances the reliability of library search results. capable of speedy data acquisition within 1 minute.

Intensity
It is also effective for qualitative analysis of
peaks that cannot be identified through a library
Intensity

Mn Mw PD DPn DPw
Methyl acrylate search. The system also acquires an accurate
distribution of isotopes for molecular ions, which 4928.9 5309.4 1.1 46.8 50.5
is effective in molecular identification.
Mn : Number average molecular weight
Mw : Weight average molecular weight
PD : Polydispersity
Retention time [min]
DPn : Number average degree of polymerization
Simulation of isotope pattern DPw : Weight average degree of polymerization m/z
EI mass spectrum of Peak at 9.25 min ( ☆ on the TICC above)
56.05

Why is the AccuTOF GCx-plus highly useful for polymer analysis?


TM
70.08 Correct elemental composition
Pyrolysis/GC/MS is a widely used technique for polymer analysis. However, many of the pyrolysis products

Relative Intensity
Relative Intensity

83.09 Isotopic peak patterns Simulated isotopic peak pattern agrees


146.11 well with the measured mass spectrum. of even a common polymer are not in an EI mass spectral library. The AccuTOF GCx-plus helps with
TM

112.12 agree well. Accurate isotopic peak pattern helps with


narrowing down the possible elemental identifying pyrolysis products by determining molecular weights with various soft ionization techniques and
compositions.
elucidating elemental compositions with accurate mass measurements.
With FD, an oligomer, which is not amenable to GC/MS, can be directly analyzed. Its average molar
m/z
masses and polydispersity index can be obtained by processing the FD mass spectrum with polymer
m/z analysis software.
Elemental composition determination
Measured accurate Calculated exact Error [mDa] Inferred formula Unsaturation
mass mass
Wrong elemental composition
Relative Intensity

46.99437 46.99555 -1.18 CH3S 1.5 Application 4


Simulated isotopic peak pattern does

Environmental Science
55.05387 55.05478 -0.90 C4H7 1.5
not agree with the measured mass
69.06963 69.07043 -0.80 C5H9 1.5 spectrum.

83.08569 83.08608 -0.39 C6H11 1.5


112.12456 112.12520 -0.64 C8H16 1.0
146.11280 146.11292 -0.12 C8H18S 1.0
146.10955 3.25 C11H14 5.0 m/z
Analysis of PCBs in oil (FastGC) (MS Tips No. 130)

High selectivity at high resolution makes it possible to detect the PCBs contained in an oil sample.

EIC of pentachloro biphenyls in a transformer oil


2. Thermal extraction GC/MS of additives in a resin (MS Tips No. 138) The EICC acquired with the window width set to low
resolution (top, equal to QMS) was unable to eliminate the
Using thermal extraction GC/TOFMS, TICC of the thermal extraction GC/MS of a resin Low resolution EIC oil interference from the PCB impurities. The high-resolution
the system analyzed additives in a resin. m/z 325.88049 ±0.50 mass chromatogram (bottom) successfully detected
Intensity

Additives detected were squalene, decabromodiphenyl ethane the peaks of pentachlorinated PCBs by eliminating the
(bromine flame regardant), Irganox 1330 (antioxidant). interference.
Intensity

High resolution EIC


m/z 325.88049 ±0.05
Intensity

Retention time [min]


Retention time [min]

15 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 16
TM
A wide range of applications A wide range of applications

Application 5 Application 6

Food Safety Metabolites


Analysis of agrochemical residues in food Differentiation of structural isomers and co-eluting analytes with FI
Extracted Ion Current Chromatograms (EICC) of pesticides in carrot extract Co-eluting homologues, such as homologous fatty acid methyl esters, can be differentiated with FI as
GC/QMS equivalent GC/TOFMS
abundant molecular ions and minimal fragmentation.
High selectivity Structural isomers of disaccharides can be differentiated with FI as abundant molecular ions and structurally
informative fragment ions.

Intensity

Intensity
STD
High-resolution TOFMS can reduce the interference from matrix.
Peaks from the matrix that are detected at low resolution will be Retention time [min] Retention time [min]

eliminated at high resolution. This high selectivity reduces false


Interference 1. Analysis of fatty acid methyl esters (FAMEs)
Sample

Intensity

Intensity
positives and allows for more accurate quantitation. +
STD With EI, it was difficult to discern C18:3 FAME and C18:1 FAME as they have nearly identical retention times.
With FI, it was easy to recognize both as there were minimal fragment ions.
Retention time [min] Retention time [min]

Interference

N.D

Intensity

Intensity
Sample
No Interference
Retention time [min] Retention time [min]
EI mass spectra FI mass spectra

Simple analytical conditions Superior qualitative capability

GC/TOFMS detects all components that are ionized. Thus, the TOFMS performs high-resolution, high-mass-accuracy analysis over
operator is freed from the lengthy process of defining analytical a wide m/z range (m/z 35 to 600) without selecting a measurement
conditions such as SIM (Selected Ion Monitoring) and SRM (Selected mode such as SCAN and SIM. As a result, it allows for acquisition
Reaction Monitoring). Theoretically, there is no limit on the number of highly selective chromatograms for all ions observed,
of components that can be analyzed. The AccuTOF GCx-plus can demonstrating its superior qualitative capability. The acquired data
TM

perform simple simultaneous analysis of multiple components using can be used to analyze non target compounds as well.
its unique exact mass database for approximately 350 components
(1 quantitative ion and 4 qualitative ions per component, editable).

Superior sensitivity/reproducibility Limit of Quantitation (LOQ*) % RSD

The table on the right shows the limit of quantitation and the < 0.005ppm 161 < 5% 239

relative standard deviation of 353 components that were analyzed 0.005ppm - 0.01ppm 174 5~10% 109
simultaneously. The results demonstrate superior sensitivity and > 0.01ppm 18 >10% 5
reproducibility for simultaneous analysis of multiple components
*LOQ defined as 10 times the standard deviation of the quantitation values
obtained from 5 repeated injections of 40 pg (20 ppb x 2 μL) of each
compound.
2. Analysis of isomeric disaccharides*
High-throughput analysis - FastGC
Methyloxime-trimethylsilyl(TMS) derivatives of disaccharides are very easy to fragment, thus making it difficult to observe
Excellent separation Fast GC Measurement time: 8 minutes These chromatograms show the presence molecular ions with EI or protonated molecules with CI. FI produces abundant molecular ion as well as structurally informative
of 100 pesticide components. In the Fast fragment ions to differentiate isomers.
GC analysis (top), the system acquired data
while maintaining chromatographic separation
Intensity

FI mass spectrum of the methyloxime-TMS derivative of maltose


Maltose
in less than 1/4 of the time needed for the
Glu-Glu (1-4)
Measurement time: 38 minutes conventional analysis (bottom). The 50
Intensity

Conventional GC
spectra/second high-speed data acquisition
system enables high-throughput analysis.
Intensity

Retention time [min]


Retention time [min]

FI mass spectrum of the methyloxime-TMS derivative of laminaribiose


Laminaribiose
Glu-Glu (1-3)
Is a time-of-flight mass spectrometer suitable for quantitative analysis?
AccuTOF GCx-plus with a high performance digitizer achieves a wide dynamic range and high
reproducibility. AccuTOF GCx-plus with high sensitivity, high reproducibility, high qualitative analysis
TM

capability, and high throughput will be a major player for the analysis of agrochemical residues in foods.

* Furuhashi, T. & Okuda, K. Critical Rev. Anal. Chem., 1 - 16, doi:10.1080/10408347.2017.1320215 (2017).
FAME samples and TMS derivatives of disaccharides courtesy of Dr. Takeshi Furuhashi, Anicom Specialty Medical Institute Inc.
17 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 18
TM
A wide range of applications A wide range of applications

Application 7 Application 8

Fragrances Petroleum Products


1. Ultrahigh separation analysis of diesel fuel (GCxGC/TOFMS analysis)
Visualization, grouping, and non-target analysis
GCxGC can separate complex mixtures that cannot be separated by ordinary GC. Components that are at Exact mass measurements are easily 2-dimensional (2D) TICC of diesel fuel by GCxGC/TOFMS
trace levels but contribute significantly to sample properties can be found and identified. With mass spectral accomplished for GCxGC analysis. By
library searches and accurate mass measurements, separated components can be reliably identified. combining high resolution with GCxGC,
the system can qualitatively analyze trace
components.

2nd column (polar) separation; Polarity


* ZOEX GCxGC system used for measurement
GCxGC chromatogram created by ZOEX GC Image software
1. GCxGC/TOFMS analysis of tea tree oil

The compounds in an aroma oil were fully separated for grouping. The data offers a visual
representation of the complex aroma oil composition.

2D TICC of tea tree oil by GCxGC/TOFMS For compounds that do not produce molecular
ions by EI, FI can be used to detect molecular ions,
Cyclic monoterpene
diols and triols and determine the elemental composition, which
enhances the accuracy of qualitative analysis.
2nd column (polar) separation; Polarity

Acyclic monoterpene EI
alcohols

Cyclic sesquiterpene Molecular ion 1st column (non-polar) separation; Boiling point
Cyclic monoterpene alcohol not detected

Intensity
alcohols

m/z
2. Type analysis of microcrystalline wax (MS Tips No. 100)
FI

Type analysis makes it easy to obtain the FD mass spectrum of microcrystalline wax
Molecular ion detected average molecular weight, molecular weight
Intensity

Cyclic monoterpenes m/z error: -1.17 x 10-³


distribution, and the content of hydrocarbons
Cyclic sesquiterpenes
having different degrees of unsaturation.
m/z

1st column (non-polar) separation; Boiling point

Intensity
2. GCxGC/TOFMS analysis of rose oil
m/z
Components that cannot be separated by an ordinary 1D GC were separated, detected, and identified.
Group-type analysis of microcrystalline wax
3D TICC map of rose oil by GCxGC/TOFMS Mn : Number average molecular weight
Series Label Mn Mw Mz PD DPn DPw DPz Percent Series Percent Spectrum
1 (34.667, 1.506) easured accurate Inferred formula Calculated exact Error
M Mw : Weight average molecular weight
mass mass [mDa]
Total / Average 657.0 686.9 718.9 1.0 40.1 42.2 44.5 100.0 64.1 Mz : Z average molecular weight
204.1856 C15H24 204.1873 -1.7
PD : Polydispersity index
S1 CnH2n+2 571.1 617.3 665.3 1.1 33.6 36.9 40.3 17.3 11.1
DPn : Number average degree of plymerization
S2 CnH2n 529.7 655.0 680.8 1.0 37.9 39.7 41.6 24.2 15.5 DPw : Weight average degree of polymerization
δ -Cadinene S3 CnH2n-2 670.5 692.3 715.6 1.0 41.0 42.5 44.2 13.1 8.4 DPz : Z average degree of polymerization
C15H24
S4 CnH2n-4 715.6 739.0 764.7 1.0 44.3 46.0 47.8 8.4 5.4
S5 CnH2n-6 688.3 717.9 751.1 1.0 42.5 44.7 47.0 22.5 14.5
S6 CnH2n-8 710.0 739.6 772.8 1.0 44.2 46.3 48.7 14.5 9.3

2 (34.667, 2.384) easured accurate Inferred formula Calculated exact Error


M
mass mass [mDa]
168.0919 C13H12 168.0934 -1.5

FI and FD for the analysis of petroleum products


Petroleum products are highly complex mixtures of hydrocarbons. FI and FD are the only soft ionization
Biphenyl, 3-methyl
-C13H12 techniques universally applicable to various types of hydrocarbons, allowing the determination of molar
mass distributions and group-type analysis.
The AccuTOF GC series of instruments have been widely accepted in the petroleum industries worldwide.
TM

* ZOEX GCxGC system used for measurement GCxGC chromatogram created by ZOEX GC Image software

19 | AccuTOF GCx-plus
TM
AccuTOF GCx-plus | 20
TM
Specifications
Specifications . Installation requirements

AccuTOF GCx-plus TM

Specifications . Installation requirements

▶ Easy linkage to various optional software


▷ NIST mass spectral library


▷ Escrime for batch quantitative analysis of multiple components
Polymerix for analysis of polymers/ hydrocarbon types
1

GC Image for GCxGC analysis


2

* 1:Sierra Analytics. Inc. * 2 :GC Image. LLC

Installation requirements
AccuTOF GCx-plus AccuTOF GCx-plus AccuTOF GCx-plus
TM TM TM

Power supply Installation room


+ autosampler + autosampler
Main console Single phase Varying magnetic field 1×10 T or less
-6

+ direct probe
AC190- 210V or 220– 240V, 20A, 50-60Hz Static magnetic field 5×10 T or less -4

Gas chromatograph Single phase, Floor vibration Amplitude (p-p) 25μm or less,
AC 200V or 220V or 230V or 240V, 20 A acceleration 0.1m/s or less 2

Data system AC100-120V, 15A, 50-60Hz Room temperature 20 to 27 °C


AC200-240V, 7.5A, 50-60Hz Temperature fluctuation ±3 °C / h or less
Grounding 100 Ω or less Humidity 30 to 70% (no condensation)
Standard configuration Maximum heat generation 25,776 kJ/h (calculated from maximum
Gas power consumptions of mass spectrometer,
Nitrogen gas gas chromatograph, and data system)
Ion source Electron ionization Ventilation facility Ventilation facility for rotary pump exhaust
For purging ion source 0.5 to 0.6 MPa, 97% or better purity
Analyzer Reflectron time-of-flight mass analyzer is required
and analyzer For driving valves
Ion detector Dual microchannel plate
Helium gas
Data acquisition system Continuous averager
For gas chromatograph 0.5 to 0.68MPa, 99.999% or better purity,
Vacuum system 2 turbo molecular pumps, 2 rotary pumps
0.5ppm or less hydrocarbon content
Gas chromatograph Agilent 7890B
Data system Personal computer, LCD monitor, laser printer, rewritable DVD drive,
Windows®operating system, Power supply requirement depends on a specific configuration sold in each territory.
data system software (msAxel) Please inquire at a local sales office for details.

Example of an installation room


Optional attachments
Symbol Unit Width Depth Height Weight
・Direct insertion probe (mm) (mm) (mm) (kg)
・Direct exposure probe A Mass spectrometer 1,172 724 1,224 340
・EI/FI/FD combination ion source B Gas chromatograph 582 513 488 49
・FD/FI combination ion source FD sampling tool C Computer 168 450 456 15
・EI/PI combination ion source
C TFT LCD monitor 443 220 555 9.2
・CI ion source
D Laser printer 385 279 261 6
・FD sampling tool
Note
● From the rear of the basic unit of the gas chromatograph, high-temperature air is exhausted.

Never place anything behind the unit. 200mm space between rear panel of instrument and
wall is neces-sary at least.
● Exhaust line for rotary pump is required.

● A table for PC and printer is not included in the standard configuration of AccuTOF GCx-plus.
TM

Windows is either a registered trademark or a trademark of Microsoft Corporation in the United States and/or other countries.

21 | AccuTOF GCx-plus | 22
TM
AccuTOF GCx-plus
TM
*Specifications subject to change without prior notice.

No.2202D857C(Bn)

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