Solutions for Plastic Evaluation   C10G-E035

Solutions for Plastic Evaluation   C10G-E035
C10G-E035
Solutions for Plastic Evaluation
Index
Product Information
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Evaluation of Plastic Materials
Analysis purpose
Application
Instrument
Page
Quality Control
Determination of Hydroxyl Value in Polypropylene Glycol by NIR-PLS Method
FTIR
4
Particle Size Control and
Particle Size Distribution
High-Sensitivity, High-Reproducibility Measurement of Single-Digit Nanoparticles
Dispersed in Liquid
Single Nano Particle Size
Analyzer
5
Evaluation of Raw Materials
Analysis purpose
Application
Instrument
Page
Molecular Weight Distribution
Example of Recycling Preparative Separation of Polystyrene
HPLC
6
Structure and Composition
FTIR Measurement of Plastic Pellets and Powder by Single Reflection ATR Method
FTIR
7
8
Structure and Isomers
FTIR Analysis of Polybutadiene Microstructure Using Single Reflection ATR
FTIR
Structure and Copolymers
Quantitation of Vinyl Acetate in EVA
FTIR
9
Additives
Analysis of Additives in Plastic
GC/MS
10
Additives
Analysis of Additives in Plastic Using LCMS-2020
LC/MS
11
Additives
Analysis of Additives in Polymer Extract Using LCMS-IT-TOF (Part 1)
LCMS-IT-TOF
12
Additives
Analysis of Additives in Polymer Extract Using LCMS-IT-TOF (Part 2)
– Predicting the Structure of Additives and Attributing MS3 Measurement Results –
LCMS-IT-TOF
13
Additives
Analysis of Additives in Acrylic Sheets
MALDI-TOFMS
14
Additives
Quantitation of Reinforcing Materials in Epoxy Resins
Thermal Analysis
15
Evaluation of Impurities
and Byproducts
Analysis of Trace Homopolymer Components in Copolymers
MALDI-TOFMS
16
Impurities and Residues
Analysis of Residual Organic Solvents in Flexible Packaging Materials
GC
17
Analysis purpose
Application
Instrument
Surface Structure
Observing the Lamellar Structure of Polymer Film Using a Scanning Probe Microscope
SPM
18
Surface Structure
Analysis of Film Surface by FTIR-ATR Method
FTIR
19
Local Structure
Measurement of Water Melting in a Polymer Electrolyte Fuel Cell Membrane Using a DSC
Thermal Analysis
20
Local Structure
Near-Infrared Mapping of Adhesives Using an Infrared Microscope
Infrared Microscope Systems (FTIR)
21
Optical Properties
Measurement of Diffuse Reflectance in Plastic Using an Integrating Sphere
UV
22
Product Evaluation
Page
Orientation
Measurement of Polarized Light of PET Film Using FTIR-ATR Method
FTIR
23
Crystallization
Measurement of Commercial PET Bottles
Thermal Analysis
24
Thermal Characteristics
Measurement of Thermal Expansion Process in Epoxy Resin Using a TMA
Thermal Analysis
25
Mechanical Characteristics
– Static Strength
Evaluation of Mechanical Characteristics of Various Plastic Products Using Autograph
Autograph
26
Mechanical Characteristics
Fatigue and Impact Strength
Evaluation of Endurance (Fatigue Strength) of Various Plastic Products Using Servopulser
Servopulser/Hydroshot
27
Non-Destructive Inspection
Defect Inspection and Internal
Structural Analysis
Example of Analyzing and Observing the Internal Structure of Various Plastic Products
Using Industrial X-Ray Inspection
Industrial X-Ray
Inspection System
28
Analysis of Foreign Substances
on Film Using an Infrared
Microscope
Analysis of Foreign Substances
FTIR
29
Product Evaluation
Instrument
Page
Hazardous Substances
Hazardous Metals
Analysis of Cadmium in Plastics Using an AA Spectrophotometer
AA
30
Hazardous Substances
Hazardous Metals
Analysis of Hazardous Metals in Plastics Using an ICP-AES System
ICP-AES
31
Hazardous Substances
Hazardous Metals
Analysis of Hexavalent Chromium in Plastic Using a UV-VIS Spectrophotometer
UV
32
Hazardous Substances
Organic Substances
Analysis of Phthalate Esters in Plastic
GC/MS
33
Analysis of Hazardous Elements
Analysis of Hazardous Elements in Plastic Using an EDX Spectrometer
EDX
34
Halogen-Free Analysis
Analysis of Halogen Elements (Chlorine) Using an EDX Spectrometer
EDX
35
Model
Page
Fourier Transform Infrared Spectrophotometer
IRAffinity-1, IRPrestige-21
36
Single Nano Particle Size Analyzer
IG-1000
37
High-Performance Liquid Chromatograph
Prominence
38
Gas Chromatograph Mass Spectrometer
GCMS-QP2010 Ultra
Liquid Chromatograph Mass Spectrometer
LCMS-2020, LCMS-IT-TOF
MALDI-TOFMS
AXIMA Performance
42
Thermal Analyzer
DSC-60, TMA-60, DTG-60
43
Gas Chromatograph
GC-2014, GC-2010 Plus
44
Scanning Probe Microscope
SPM-9700, WET-SPM Series
45
Infrared Microscope System
AIM-8800
46
UV-VIS Infrared Spectrophotometer
SolidSpec-3700 (DUV), UV-2600/2700, UVmini-1240
47
Autograph
Autograph AG-X Series
48
Servopulser / Hydroshot
Tabletop Servopulser, Hydroshot HITS-T10
49
Industrial X-Ray Inspection System
inspeXio SMX-90CT, inspeXio SMX-225CT
50
Atomic Absorption Spectrophotometer
AA-7000, AA-7000G
51
Multitype ICP Emission Spectrometer
ICPE-9000
52
Energy Dispersive X-Ray Fluorescence Spectrometer
EDX-720
53
39
40-41
Product Information
Product
Product Evaluation
Product Information
Evaluation of
Raw Materials
Application
Evaluation of
Plastic Materials
Analysis purpose
Evaluation of Plastic Materials
Quality Control
Determination of Hydroxyl Value in Polypropylene Glycol by NIR-PLS Method
Polypropylene glycol (PPG) is a liquid manufactured by polymerizing propylene glycol and is used as a raw ingredient of polyurethane.
The hydroxyl value is an index of the content of free hydroxyl groups in polyols, such as PPG. JIS K 1557 (Plastics Polyols for use in the
production of polyurethane) specifies using titration to measure the hydroxyl value. However, titration requires equipment and reagents,
and is also time-consuming. In contrast, the NIR-PLS (near infrared-partial least squares) method allows calculating the hydroxyl value easily
and quickly by simply measuring the near infrared spectrum of the sample, then using PLS to calculate quantities.
H(OCH2CH)
n - OH
-
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
FTIR
CH3
Structural Formula of Polypropylene Glycol
Product Evaluation
NIR spectra for four homologous types of PPG with different hydroxyl values and a calibration curve created using the PLS
method are shown below. The NIR spectra indicate a difference in their peak intensities near 6990 cm -1 and 4850 cm -1. The
peaks near 6990 cm -1 correspond to the first overtone of the O-H stretching vibration, whereas the peaks near 4850 cm -1
correspond to a combination of the O-H stretching and bending vibrations.
1.75
Abs
Product Information
1.5
1.25
1
Corr. Coef.: 0.99996
MSEP
: 0.00008
SEP : 0.00901
0.75
6000
5500
5000 4500
1/cm
NIR Spectra of Polypropylene Glycol
Actual Hydroxyl Value (known concentration) vs.
Predicted Hydroxyl Value (quantitative value)
NIR Heating Transmission Cell
This cell allows measuring transmittance while liquid samples placed in the provided
6-mm diameter test tube are heated or held at a constant temperature. This is
especially convenient for quantitative analysis of multiple components in liquid
samples or when monitoring reactions during heating processes.
Specifications
• Measurement range
: 12,500 to 3,800 cm -1
• Temperature range
: Room temp. to 120°C
• Accessory recognition function : Included
• Test tube
6 mm dia. × 50 mm
NIR Heating Transmission Cell
4
LAAN-D-XX001A
Particle Size Control and
Particle Size Distribution
Evaluation of Plastic Materials
Single Nano Particle Size Analyzer
Sample provided by Professor Kokubo of Osaka University
Evaluation of
Raw Materials
Even fullerene hydroxide particle sizes, which typify samples in
the single-digit nanometer region, can be measured with high
sensitivity and good reproducibility. This enables accurately
evaluating the dispersivity of particles in the single nanometer region.
Particle Size Distribution (volumetric basis)
Normalized Particle Amount
Example of Measuring Fullerene
Hydroxide
Evaluation of
Plastic Materials
High-Sensitivity, High-Reproducibility Measurement of Single-Digit Nanoparticles
Dispersed in Liquid
Particle Diameter (nm)
This example compares IG-1000 and TEM measurement
results (mean particle diameter).
These show a very consistent relationship between sizes.
IG-1000
TEM
○
1.63
1.98
●
2.39
2.22
Normalized Particle Amount
Particle Diameter (nm)
Particle Size Distribution (volumetric basis)
Normalized Particle Amount
Example of Measuring Zinc Sulfide (ZnS)
Particle Size Distribution (volumetric basis)
Product Information
○ A (only)
● B (only)
△ A + B (mixture)
Even mixed samples can be measured. The IG method utilizes
the diffusion of a diffraction grating formed by particles to
measure samples, so the signal level is not dependent on
particle size. Therefore, this allows evaluating mixed samples.
In contrast, evaluating mixtures is difficult with methods that
use scattered light, because the signal level is proportional to
the cube of the particle diameter, even if the volume is the same.
Product Evaluation
Example of Measuring Mixed Samples
(colloidal silica)
Particle Diameter (nm)
Samples provided by Professor Mori of the Doshisha University
LAAN-D-XX002A
5
Evaluation of Raw Materials
Molecular Weight Distribution
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
HPLC
Example of Recycling Preparative Separation of Polystyrene
HPLC is widely used as a means to purify samples by separation, but the large preparative columns become quite expensive. Any
cost limitations affect column length and quantity to achieve better separation. In such situations, separation can be improved
by recycling the eluent band containing the target components through the column several times to effectively extend the
column length. In this example, a Prominence semi-preparative recycling system was used to separate polystyrene by GPC.
Fig. 1 illustrates the flow line of the Prominence semipreparative recycling system. The sample is loaded by
autosampler or manual injector, then separated by the
preparative column and eluted to the detector. Here, the
system uses a recycle valve to divert the eluate either to the
flow line leading to a fraction collector, or to the flow line
leading back to the pump inlet. By switching the recycle
valve to divert the flow back to the pump inlet when target
peaks are eluted, the sample can be recycled through the
preparative column as many times as necessary to obtain
a separation equivalent to using a longer column. Since
recycling the eluate does not consume any new mobile phase,
it also helps reduce solvent consumption.
Injector
Solvent
delivery pump
(LC-6AD)
UV-VIS detector
(SPD-20A)
Recycle kit
Preparative column
Recycle valve
Fraction collector
(FRC-10A)
Degassing unit
(DGU-20A3)
Semi-Preparative
Recycling System
Fig. 1 Flow Line of Prominence
Product Information
Fig. 2 shows an example of a recycle separation of polystyrene molecular weight markers (molecular weight = 781 and
polydispersity* < 1.15). Portions indicated by arrows are recycled. This shows how even polystyrene, which has low
polydispersity, can be separated into many oligomer peaks. By switching the recycle valve to the flow line leading to the FRC,
target peaks are easily collected.
Fig. 2 Example of Recycling Separation of Polystyrene
Analysis Conditions
Instrument : Prominence semi-preparative recycling system
Analytical Column : Shim-pack GPC-20025C+2002C+2001C
(each 300 mmL × 20 mm I.D.)
Mobile Phase : Chloroform
Flowrate : 3.0 mL/min
Column Temperature : Ambient
Detection : UV 254 nm
* Polydispersity = Weight-Average Molecular Weight / Number-Average Molecular Weight
6
LAAN-D-XX004A
Structure and Composition
Evaluation of Raw Materials
FTIR
The figure on the left below shows results from measuring various types of plastic pellets and powders. The single reflection ATR method
allows measuring pellet and powder samples directly by simply placing them tightly against an approximately 2 mm diameter prism.
Furthermore, it allows even new users to easily obtain qualitative information about measured polymers by using the spectral search function.
Evaluation of
Plastic Materials
FTIR Measurement of Plastic Pellets and Powder by Single Reflection ATR Method
ABS
Evaluation of
Raw Materials
Polycarbonate
PET
Product Evaluation
Nylon 6
Polyphenylene sulfide
Example of Measuring Plastic Pellets and Powders
Spectral Search Window
Example of Measuring Plastic Pellets and Powders
Product Information
Single Reflectance ATR Method
Single reflection ATR measures the infrared spectrum of a sample pressed against the surface of a prism approximately 2 mm in diameter.
It allows measuring samples by simply placing them in close contact with the center of the prism. Therefore, it is not restricted to flat
samples and can measure curved or powdered samples as well. Liquid samples can be measured by simply dripping them onto the prism.
A photograph of the DuraSamplIR II single reflection ATR attachment and an illustration of its optics are shown below. It irradiates the
sample with infrared light through the prism and obtains information about the sample surface (to a depth of about 1 µm) based on the
light reflected from the boundary surface. Not only does this eliminate the need for dilution or other sample pretreatment, but also allows
obtaining information about the sample surface easily.
Photograph of DuraSamplIR II
Diagram of Optics
LAAN-D-XX005
7
Evaluation of Raw Materials
Structure and Isomers
FTIR Analysis of Polybutadiene Microstructure Using Single Reflection ATR
Polybutadiene is a polymer with characteristics of both plastic and rubber. It is a collective term for multiple polymer configurations of
1,3-butadiene monomers. These can polymerize into three types of structures, the cis structure (cis-1,4-polybutadiene), the trans structure
(trans-1,4-polybutadiene), and the vinyl structure (1,2-polybutadiene). Of these structures, polybutadienes containing larger amounts of
the plastic-like vinyl structure are used for applications such as wrapping films, whereas polybutadienes containing larger concentrations of
the rubber-like cis structure are used for rubber products, such as tires and belts.
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
FTIR
1,3-butadiene: CH2 =CH-CH=CH2
-CH2
CH2-
CH=CH
-(CH2 CHCHCH2 )n -
-CH2
-CH2-CH-
CH=CH
CH-=CH2
Product Evaluation
CH2Cis Structure
Trans Structure
Vinyl Structure
Product Information
The proportion of cis, trans, and vinyl structures in a polybutadiene can be determined using NMR spectra, infrared spectra, and
other methods. The Morero method using infrared spectra is considered useful if the polymer contains a high proportion of cis
structures. The Morero method involves dissolving the sample in carbon disulfide and measuring the transmittance using a fixed
cell with 1 mm optical path length. Then the proportion of each structure is determined from the absorbance of the cis, trans,
and vinyl group peaks. Since this method uses transmittance measured using a fixed cell, it provides good sensitivity and enables
using dispersive IR systems for quantitation. However, this method requires weighing and dissolving samples, cleaning cells, and
other processing. It also requires a significant amount of carbon disulfide. In contrast, the ATR method allows measuring samples
directly, without requiring any pretreatment, and the prism can be cleaned with a tiny amount of alcohol or other cleaner.
Shown below are spectra of polybutadiene with 90% or
higher cis content obtained using a DuraSamplIR II single
reflection ATR attachment. The peaks near 733 cm-1, 912 cm-1,
and 966 cm -1 correspond to cis, vinyl, and trans groups,
respectively. Calibration curves for each group are shown to
the right, all of which show good linearity.
5
Cis
3.0
%
Tr
r=
0.2
0.3
0.4
0
Trans Concentration contrast, Wavenumber range : 944.9-
ATR Spectra of Polybutadiene
8
LAAN-D-XX006
Calibration Curves for Cis, Trans, and Vinyl Groups
Structure and Copolymers
Evaluation of Raw Materials
FTIR
The copolymer ethylene-vinyl acetate (EVA) offers good clarity and is used for a wide variety of products, such as fertilizer bags, wrapping
film, bottles, and tubes. Increasing the content of vinyl acetate in EVA increases its elasticity and thermal plasticity. Though there are several
methods available for quantitating the content of vinyl acetate in EVA, infrared spectrophotometry is easier and faster because analysis can
be performed without pretreating samples.
Evaluation of
Plastic Materials
Quantitation of Vinyl Acetate in EVA
Evaluation of
Raw Materials
Product Evaluation
ATR Spectrum of EVA
Product Information
The EVA spectrum above was measured using the ATR method. The peaks near 1736 cm-1 and 1238 cm-1 correspond to C=O and C-O
bond stretching vibration of vinyl acetate. The peaks near 2916 cm-1, 2849 cm-1, and 1464 cm-1 are primarily due to -CH2 in ethylene.
The results shown below on the left (enlarged view) are from samples containing 0%, 5%, and 7% vinyl acetate, measured using a
horizontal ATR attachment. The show that the peak intensity near 1736 cm-1 increases with increasing concentrations of vinyl acetate.
The calibration curve below on the right was created using the intensity ratio of peaks near 1736 cm-1 and 1464 cm-1.
In this way, the concentration of vinyl acetate in EVA can be determined from the peak intensities in infrared spectra.
ATR Spectra of EVA
with Vinyl Acetate Concentrations of 0%, 5%, and 7%
Calibration Curve of Vinyl Acetate
LAAN-D-XX007
9
Evaluation of Raw Materials
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
GC/MS
Additives
Analysis of Additives in Plastic
Polymer materials are often formulated using different types of additives depending on the grade or manufacturer. Analyzing a
sample extract generally requires separating the additives from the polymers. Conventionally, they are separated by solvent extraction
or precipitation methods, but that requires time-consuming pretreatment, including thoroughly washing the equipment used for
pretreatment. The thermal desorption GC/MS method described below improves productivity by facilitating quick analysis and utilizing
disposable pretreatment equipment (ECO cup).
Instrument Configuration
Product Evaluation
GCMS-QP2010 Ultra
Pyrolysis System: EGA/PY-3030D
(from Frontier Laboratories, Ltd.)
Product Information
Thermal Extraction of PS Plastic Shavings
(1 mg) for 5 Minutes at 300°C
Analysis of Evolved Gas from PS Plastic
10
LAAN-D-XX008B
Additives
Evaluation of Raw Materials
LC/MS
Pretreatment Method
One polymer bead
THF/MeOH
(50/50)
1 mL
Ultrasonic processing
Supernatant
Polymer beads used
in the analysis
LC/MS measurement
sample
Evaluation of
Raw Materials
An organic solvent (in this case, THF/MeOH = 1/1) was added to
a known quantity of a plastic sample. It was then sonicated and
the supernatant was extracted and directly analyzed. The sample
was ionized by ESI and APCI, and was monitored simultaneously
in both positive and negative modes using high-speed polarity
switching. Of the six types of additives observed, components
D and E were detected with higher sensitivity in negative mode.
Simultaneous monitoring in both modes provides sensitive and
accurate data, because the optimal ionization parameters can be
applied to each compound.
Evaluation of
Plastic Materials
Analysis of Additives in Plastic Using LCMS-2020
Product Evaluation
Product Information
MS Chromatograms of Polymer Additives
LAAN-D-XX009A
11
Evaluation of Raw Materials
Additives
Analysis of Additives in Polymer Extract Using LCMS-IT-TOF (Part 1)
An organic solvent (in this case, THF/
MeOH = 1/1) was added to a known
quantity of polymer beads. The samples
were then sonicated and the supernatant
was extracted and directly analyzed by
an LCMS-IT-TOF system. Measurement
results are shown in the chromatograms
on the left.
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
LCMS-IT-TOF
Product Information
Product Evaluation
Of the six types of additive peaks
observed, the below structural prediction
was performed for peak B.
Example: Predicting the Structure for Peak B
Example: Analysis Using Formula Predictor
The smaller the m/z number, the fewer the number of candidates. Using MSn analysis allowed the structural predictions to be narrowed
down.
12
LAAN-D-XX010A
Additives
Evaluation of Raw Materials
LCMS-IT-TOF
Evaluation of
Raw Materials
An organic solvent (in this case, THF/MeOH = 1/1) was added to a
known quantity of polymer beads. Then they were processed in a
sonicator and the supernatant was taken as the measurement sample
and measured by an LCMS-IT-TOF system. The composition was
then predicted for one of the six types of additive peaks observed.
This resulted in obtaining a predicted formula (C 28 H 52 N 2 O 4 ). (For
more details regarding the composition prediction process, refer to
Evaluation of Plastic Materials – 7A. Additives in the Plastic Analysis
Catalog.) Searching for this formula on the Internet revealed that it is
likely to be decanedioic acid bis (2,2,6,6-tetramethyl-4-piperidyl) ester,
an additive generally used as a stabilizer.
Evaluation of
Plastic Materials
Analysis of Additives in Polymer Extract Using LCMS-IT-TOF (Part 2)
– Predicting the Structure of Additives and Attributing MS 3 Measurement Results –
Product Evaluation
Ions detected in the MS3 measurement were then attributed to the
predicted compound. This confirmed that the detected ions suggested
the predicted structure, with minimal error for each product ion.
Product Information
Prediction Results for Each Peak
(For more details regarding the composition prediction process, refer to Evaluation of
Plastic Materials – 7A. Additives in the Plastic Analysis Catalog.)
Retention
Time
(min)
Name of Predicted
Compound
Composition
Formula
(Molecular
Weight)
Calculated
Value
Measured
Value
A
1.95
Triphenyl phosphate
C18H15O4P
(326.0708)
327.0781
([M+H]+)
327.0791
([M+H]+)
1.0 mDa
3.1 ppm
B
2.10
Decanedoic acid bis
(2,2,6,6-tetramethyl4-piperidyl)ester
C28H52N2O4
(480.3927)
481.4000
([M+H]+)
481.4014
([M+H]+)
1.4 mDa
2.9 ppm
C
2.55
Tinuvin P
C13H11N3O
(225.0902)
226.0975
([M+H]+)
226.0972
([M+H]+)
0.3 mDa
1.3 ppm
D
3.47
Onchitriol II A
C34H50O8
(586.3506)
585.3433
([M-H]-)
585.3435
([M-H]-)
0.2 mDa
0.33 ppm
E
4.29
2,2-Bis(3-sec-butyl-4hydroxyphenyl)propane
C23H32O2
(340.2402)
339.2330
([M-H]-)
339.2325
([M-H]-)
0.5 mDa
1.4 ppm
F
8.94
Irganox 1076
C35H62O3
(530.4699)
548.5037
([M+NH4]+ )
548.5049
([M+NH4]+ )
1.2 mDa
2.2 ppm
m/z
Error
LAAN-D-XX011
13
Evaluation of Raw Materials
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
MALDI-TOFMS
Additives
Analysis of Additives in Acrylic Sheets
Polymer materials degrade due to a variety of factors, including light, heat, mechanical and electrical factors, radiation, chemicals, and
moisture. Many different additives, such as antioxidants, UV absorbers, hindered amine light stabilizers (HALS), and thermal stabilizers,
have been developed to prevent such degradation and maintain the desired characteristics of the polymer material. The quantity of each
additive used varies depending on the specific purpose of the polymer material, but generally is in ultra trace quantities of about 1%
(w/w) or less. Even for the same polymer material, the type of additive can vary depending on the grade or manufacturer. Consequently,
analyzing the additives in polymer materials is extremely important for investigating or improving the performance of various polymer
materials.
In this example, an SEC-AccuSpot-AXIMA system is used to
detect the additives in a commercial acrylic sheet product.The
measurement sample was prepared by cutting about 1 g from a
commercial acrylic sheet and sonicating it immersed in 1 mL of
tetrahydrofuran (THF) for about 1 minute. The supernatant was
then used as the measurement sample (Fig. 1). Fig. 2 shows SEC
chromatograms for the samples extracted from the acrylic sheet.
The AccuSpot system was used to collect fractions at six second
intervals, from the time the primary peaks started eluting until they
finished (7 minutes to 17 minutes 30 seconds), resulting in 105
sample spots on a MALDI sample plate.
About 1 g of
acrylic sheet
THF
1 mL
Ultrasonic processing
Supernatant
Sample solution
Commercial Acrylic Sheet
Product Information
Fig. 1 Sample Preparation
Analytical Conditions
∙ SEC Column : Shodex GF310A-1E (1.0 mmI.D. ×250 mm)
Flowrate: 10 µL/min; Eluent: THF
Detector: UV ( λ = 220 nm); Injection volume: 1 µL
Mass Spectra
SEC Chromatogram
0.0
5.0
∙ AccuSpot Spot interval: 6 sec; Loadage: 1µL/well
Loadage (mixture of matrix and cationizing
reagent): 0.2 µL/well
9 min 00 sec
10.0
11 min 47 sec
500
1000 1500 2000 2500 3000 3500
m/z
14
LAAN-D-XX012
17.5
End of fraction
collection
17 min 30 sec
Fig. 2 Mass Spectra of Respective Fractions
Each spot was measured using a Matrix Assisted Laser Desorption
Time of Flight Mass Spectrometer (MALDI-TOFMS) to obtain
mass spectra (Fig. 2) corresponding to elution times. The fraction
collected after 11 minutes 10 seconds shows a peak detected
for the additive [IRGANOX 1010 + Na]+ at m/z 1200, which was
not visible before separation in the mass spectrum, even after
magnifying by five times (Fig. 3). In addition to the additives, three
different types of molecular weight distributions were detected
(
), with a peak near m/z 2000.
Since in each case, the interval between neighboring peaks is 100,
these molecular weight distributions are presumably all due to
oligomers consisting of identical monomer units.
Start of fraction
collection
7 min 00 sec
11 min 10 sec
15.0
∙ MALDI-TOFMS Matrix: Dithranol-20 mg/mL- THF
Cationizing reagent: Na-TFA-10 mg/mL
-THF
RT (min)
7 min 00 sec
X5
Before separation
Fraction after 11
minutes 10 seconds
Oligomer components
in the acrylic sheet
[IRGANOX 1010 + Na] +
1199.77
:100
:100
:100
1400 1600 1800 2000 2200 2400 2600 2800 3000 3200 3400
m/z
1000
2000
3000
4000
5000
6000
m/z
7000
8000
9000
Fig. 3 Detection of Additives in an Acrylic Sheet
Additives
Evaluation of Raw Materials
Thermal Analysis
Quartz and other reinforcing materials in plastics are quantitated
based on the quantity remaining after heating the sample in air until
the resin components are completely combusted. In this example,
the quantity of quartz in epoxy resin is quantitatively analyzed.
When the sample was heated in air, the epoxy resin was completely
combusted by 600°C and the weight decreased by 33.83%.
On the DTA curve, the transition of quartz was measured at
580°C, along with the endothermic and exothermic peaks due to
decomposition and combustion of the epoxy resin between 300 and
600°C.
Evaluation of
Raw Materials
The concentration of quartz was calculated as 100 - 33.83 =
66.17%.
Evaluation of
Plastic Materials
Quantitation of Reinforcing Materials in Epoxy Resins
Product Evaluation
Quantitation of Carbon Black in SBR
Product Information
The quantity of carbon black in resin is measured by heating the
resin and switching from a nitrogen atmosphere to air. In the figure
to the left, the amount of carbon black contained in SBR was
quantitated. First the SBR was heated in a nitrogen atmosphere
to decompose all components of the rubber other than carbon
black. After completely decomposing the SBR by heating to about
600°C, the atmosphere was switched to air. When the carbon
black combusted in air, the total decrease in weight was observed
and the carbon content was quantitated from the percentage
decrease. In the figure to the left, this resulted in a quantitated
value of 28.2%. Note, however, that combusting carbon black
generates residual inorganic matter.
Configuration of DTG Gas Flow Lines
Due to its unique gas flow line configuration, the Shimadzu
DTG-60 thermal analyzer can be used for a wide variety of
measurement applications. For measurements in inert gas, the
vacuum pump exhaust is utilized to displace the gas quickly. The
gas inlet is located near the sample, so that it is also possible to
measure samples with active gas flowing only to the sample area,
while keeping the separate balance area protected with inert gas.
LAAN-D-XX013A
15
Evaluation of Raw Materials
Evaluation of Impurities and Byproducts
Analysis of Trace Homopolymer Components in Copolymers
The following is an example of using an SEC-AccuSpot-AXIMA system to analyze trace homopolymer components in samples, based
on a model sample consisting of the binary copolymer poly(methyl methacrylate-b-n-butylmethacrylate) (poly(MMA-b-n-BMA)). A
microscale separation column was used to load all components onto MALDI sample plates without any sample loss. Fig. 1 shows the
SEC chromatogram of poly(MMA-b-n-BMA). The AccuSpot system was used to collect fractions at six second intervals, from the time the
primary peaks started eluting until they finished (for 5 minutes, from 8 minutes 20 seconds to 13 minutes 20 seconds), and load 50 sample
spots onto a MALDI sample plate. Each spot was measured in a MALDI-TOFMS system to obtain mass spectra (Fig. 2) corresponding to
elution times. The mass spectrum obtained from each fraction indicates a different molecular weight distribution.
Analytical Conditions
∙ SEC Column: Shodex GF310A-1E (1.0 mm I.D. × 250 mm)
Flowrate: 10 µL/min; Eluent: THF
Detector: UV ( λ = 220 nm); Injection volume: 1 µL
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
MALDI-TOFMS
∙ AccuSpot Spot interval: 6 sec, 1 µL/well
Mixture of matrix and cationizing reagent:
0.2 µL/well
∙ MALDI-TOFMS Matrix: Dithranol-20 mg/mL- THF
Cationizing reagent: Na-TFA-10 mg/mL -THF
Product Information
Fig. 1 SEC Chromatogram of Poly(MMA-b-n-BMA)
The fraction collected after 11 minutes and 18 seconds shows a detected molecular weight distribution not observed before separation
(Fig. 3). The 142 interval between adjacent peaks indicates that the molecular weight distribution with a peak near m/z 1200 (marked
with ● ) corresponds to the PnBMA homopolymer. Similarly, the 100 interval between adjacent peaks indicates that the molecular weight
distribution with a peak near 1800 (marked with ■ ) corresponds to the PMMA homopolymer. These results indicate that the poly(MMAb-n-BMA) in this example, contains trace amounts of the homopolymer components PnBMA and PMMA.
Fig. 2 MS Spectra of SEC-Separated Fractions
Fig. 3 Detection of Homopolymer Components
16
LAAN-D-XX015
Impurities and Residues
Evaluation of Raw Materials
GC
With such a high interest in security, safety, and health in recent years, measuring residual organic solvents in plastic products is now more
important than ever. Residual solvents are commonly analyzed using headspace gas chromatography, which involves placing the sample
in a vial and heating it to a given temperature for a given time, and then injecting the resulting gas phase into a gas chromatograph.
This allows using simple pretreatment procedures to measure highly volatile components with relatively high sensitivity. Due to the simple
pretreatment, samples can be left in the vial for analysis.
In this example, flexible packaging material was analyzed using the residual solvent measurement method (manual HS method) specified in
the Control Devices Manual for Manufacturing Flexible Packaging Materials: Flexible Packaging Hygiene Association Edition.
Silicone
septum for GC
Heat
GC-FID
Fold the sample into a 500 mL conical flask (sealed with a silicone rubber
stopper modified to enable acquiring gas with a gas tight syringe).
Heat at 80°C for
30 min
∙ Able to analyze highly volatile components (substances with low boiling
points) with high sensitivity
∙ Maintenance is easy because non-volatile
components never enter the GC unit.
∙ Liquid samples containing components
with high boiling points can be analyzed
more quickly than by direct injection.
∙ Using a fully automatic headspace sampler improves productivity.
Product Information
0.2 m 2 sample
F e a t u re s o f H e a d s p a c e
Methods
Product Evaluation
Residual solvent measurement method (manual HS method) specified in the
Control Devices Manual for Manufacturing Flexible Packaging Materials:
Flexible Packaging Hygiene Association Edition
Evaluation of
Raw Materials
Quantitative values from analyzing solids by headspace GC are calculated from the quantity of volatilized components in the gas phase
at a given maintained temperature. Therefore, unvolatilized components that remain trapped in the solid sample are not included in
quantitative values. Consequently, the method is used to measure and compare the quantity of volatile components evolved from different
samples under certain conditions.
Evaluation of
Plastic Materials
Analysis of Residual Organic Solvents in Flexible Packaging Materials
This method is not suitable for difficult-tovolatilize components.
Use a 5 mL gas tight syringe to acquire 1 mL of
headspace gas from the conical flask and inject it
into the GC.
System Configuration
GC-2014 + GCsolution
Example of Fast Analysis of Residual Organic Solvents in Flexible Packaging Materials
GC-2014 + GCsolution
LAAN-D-XX017A
17
Product Evaluation
Surface Structure
O b s e r v i n g t h e L a m e l l a r S t r u c t u re o f P o l y m e r F i l m U s i n g a S c a n n i n g P ro b e
Microscope
The surface of polymer films have a characteristic form typified by a lamellar structure that is related to the material's transparency and
strength. In this example, the surface of polyethylene film is observed via a scanning probe microscope (SPM) to simultaneously obtain a
three-dimensional image (left) and phase image (right) of the surface. The three-dimensional image shows that there are tiny bumps on
the surface. The phase image clearly shows the lamellar structure and crystallization of the polymer. The areas where crystalli zation has
progressed and become harder appear brighter. The image is 1.8 µm on each side. In this way, using an SPM allows easily observing the
structure and physical properties of polymer films under atmospheric conditions, without any special sample preparation.
Product Information
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
SPM
Micro Phase Separation of Block Copolymers Using a Scanning Probe Microscope
A phase separation structure can be observed in plastics
that include a mixture of two or more materials. The image
to the right is the block copolymer surface observed using
a s c a n n i n g p ro b e m i c ro s c o p e ( S P M ) . D u e t o t h e S P M s
high resolution capability, it clearly shows micro phase
separation structures. Due to its ability to observe samples
in atmospheric conditions, it is being used for an increasing
range of applications, such as to observe the heating, cooling,
tension, or cross sections of samples.
18
LAAN-D-XX018B
n
Surface Structure
Product Evaluation
FTIR
The ATR (attenuated total reflection) method obtains information about a sample surface held closely against a prism. Therefore, it
can be used to obtain information about coating materials, adhesives, or precipitates from within a sample on the sample surfaces,
without requiring any sampling or other pretreatment processes. The figures below show the results (black) from measuring a
commercial film and ATR spectrum (red) of typical polyethylene sample. This shows that the commercial film product is made of
polyethylene, but it also shows peaks that are not observed in the standard polyethylene.
Evaluation of
Plastic Materials
Analysis of Film Surface by FTIR-ATR Method
Evaluation of
Raw Materials
Product Evaluation
Product Information
ATR Measurement Optics with Sample Held Tightly Against Prism
ATR Spectrum of Commercial Film Product (Black) and ATR
Spectrum of Polyethylene (Red)
The figure on the right was obtained by removing the commercial film from the prism and measuring only what remained on the
prism. Since the ATR method involves pressing the sample against the prism, substances from the sample surface, precipitates from
within, or other substances can be transferred to the prism. In such cases, information from only the transferred substance can be
obtained by removing the sample and measuring again.
In this case, it was determined that the transferred substance was
a fatty acid amide, such as stearic acid amide. Fatty acid amides
are commonly used as polyethylene smoothing agents, releasing
agents, printing ink additives, or pigment dispersing agents.
ATR Optics for Measuring Transferred Substances
ATR Spectrum of Transferred Substances (Black) and ATR Spectrum
of Stearic Acid Amide (Red)
LAAN-D-XX020
19
Product Evaluation
Local Structure
Measurement of Water Melting in a Polymer Electrolyte Fuel Cell Membrane Using a DSC
The figure below shows the results from measuring the melting process of water in a solid polymer membrane at various water content
levels. At a 6.7% water content, a melting peak for water was not observed. The -23.8°C peak for a water content of 8.5% is presumably
due to the melting of water clusters in the solid polymer membrane. The two-stage peak in water content levels at 12.6% and higher is
presumably due to peaks for melting free water and water clusters. It shows that as the water content increases, the temperature peak
increases. In other words, the amount of free water increases. The temperature and area of the peak for water from clusters melting is
probably related to the size of the clusters.
Product Information
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Thermal Analysis
Melting of Water in Polymer Electrolyte Fuel Cell Membrane
Measurement of Water Melting in Silica Gel Pores Using a DSC
The figure below shows the results from hydrating silica gels A, B, and C with water weighing roughly the same as their
respective dry gel weights and then using a differential scanning calorimeter to cool the gels to about -40°C before heating.
In each sample, two melting peaks were measured. These presumably correspond to the water in pores melting at a lower
temperature and water outside the pores (on the surface) melting at a higher temperature. The peak temperature of pore
water melting appears at successively higher temperatures for silica gels A, B, and C. That is probably due to the melting point
decreasing as the pore diameter decreases.
Melting of Water in Silica Gel Pores
20
LAAN-D-XX021A
n
Local Structure
Product Evaluation
Infrared Microscope Systems (FTIR)
Evaluation of
Plastic Materials
Near-Infrared Mapping of Adhesives Using an Infrared Microscope
This example uses near-infrared spectroscopy to map a twosolution mixed type epoxy. The epoxy was measured using nearinfrared transmission by sandwiching a mixture of appropriate
amounts of ingredient A (epoxy resin) and ingredient B (polyol)
between two glass slides, as shown below. The image obtained
using the mapping software is shown on the right.
Evaluation of
Raw Materials
Product Evaluation
Adhesive Sandwiched Between Two Glass Slides
Image After Preview Scanning
Product Information
Spectra for 4 arbitrary points are shown below, in the upper figure and an intensity map of peak heights at 6071 and 4528 cm -1
is shown in the lower figure. The peaks at 6071 cm -1 correspond to the first overtone of the C-H stretching vibration on the epoxy
group, whereas the peaks at 4528 cm -1 correspond to a combination of the C-H stretching and bending vibrations. In the lower
intensity map, the peaks at 4528 cm -1 are present across the entire A and B mixture area, whereas the peaks at 6071 cm -1 are only
present near the center of the A and B mixture area. In the area above the center where 6071 cm -1 peaks are not observed (side
with ingredient B), the epoxy group has presumably reacted with the polyol and changed its structure.
NIR Spectra of 4 Arbitrary Points
Intensity Map of Peaks at 6071 cm-1 and 4528 cm-1
LAAN-D-XX022
21
Product Evaluation
Optical Properties
Measurement of Diffuse Reflectance in Plastic Using an Integrating Sphere
In this example, an ISR-2600Plus integrating sphere attachment was installed in a UV-2600 UV-VIS spectrophotometer to measures the
diffuse reflectance of two plastic caps (red and blue). The reflectance spectra are shown to the left and a photograph of the sample placed
in the integrating sphere is shown to the right. Barium sulfate was used as the reference sample. Based on the left figure, the blue cap
mainly reflects blue light in the 400 to 500 nm range, whereas the red cap mainly reflects red light in the 600 to 700 nm range. This
system allows measuring the reflectance easily by simply placing the sample in the integrating sphere.
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
UV
Product Information
Diffuse Reflectance Spectra of Plastic Caps
ISR-2600Plus Integrating Sphere
Measuring Color
The color measurement software allows converting spectral data to color values. The figure on the left shows the results from
using the color measurement software to convert the above cap data to L*a*b* color system values.
A chromaticity diagram of the L*a*b* color values is shown on the right, where the L* graph shown on the left side indicates
the brightness. The higher the data point, the lighter (brighter) the color and the lower the data point, the darker the color.
The a*b* graph on the right indicates the color saturation and hue. The closer the data point is to the center of the circle, the
less saturated (less colorful) the color and the closer it is to the perimeter, the more saturated the color. Similarly, the radial
angle indicates the hue. For example, reds are located toward the upper right. In addition to the L*a*b* color system, the color
measurement software can also use various other color systems, such as the Lab, L*u*v*, and Munsell systems.
Main Window of Color Measurement Software
22
LAAN-D-XX024B
Chromaticity Diagram
n
Orientation
Product Evaluation
FTIR
When polymers are stretched, the molecules tend to orient longitudinally parallel to the direction they are being stretched. The degree to which
they are oriented in the same direction can be determined from polarized light measurements. Film samples are generally measured using the
transmission method and polarizers. However, if the film is too thick, the peaks can become saturated, which prevents measurement. In contrast,
the ATR method offers the advantage of being able to measure films regardless of their thickness and obtains information about the sample surface
as well.
Direction of
stretching
Evaluation of
Raw Materials
Results from measuring the polarized light of unstretched PET film and PET film stretched to 3 times its original length are shown below.
Measurements were performed based on perpendicular polarized light (S), which provides information about vibration perpendicular to the incident
plane (the plane formed by the incident and reflected light). Samples were placed in two orientations. One with the direction of stretching parallel
to the incident plane (lateral orientation) and the other rotated 90 degrees to a perpendicular position (longitudinal orientation).
Evaluation of
Plastic Materials
Measurement of Polarized Light of PET Film Using FTIR-ATR Method
Longitudinal orientation
Lateral orientation
Longitudinal orientation
Lateral orientation
Product Evaluation
Infrared
light
Direction of perpendicular
polarized light vibration
Lateral Orientation
Unstretched PET Film
Stretched PET Film
Product Information
Longitudinal Orientation
There was almost no difference between the unstretched film spectra and no molecular orientation was observable. However, for the
stretched film, there were clear differences in their spectra, such as in the intensity ratio near 1712 cm -1 (due to C=O stretching vibration)
and near 1248 cm -1 (due to C-O stretching vibration). C=O stretching vibration was presumably oriented perpendicular to the molecular
axis, whereas the C-O stretching vibration was presumably oriented parallel to the molecular axis. Therefore, these results indicate
that the C=O stretching vibration increased when the sample was placed in the lateral
orientation, so that the stretching direction was parallel to the incident plane. Similarly,
CH2 CH2
C-O stretching vibration increased when the sample was placed in the longitudinal
n
orientation, so that stretching was perpendicular to the incident plane. Consequently,
Structural Formula for Polyethylene Terephthalate
these results show that the molecules were oriented longitudinally in the stretched film.
(PET)
Measurement of Polarized Light of PET Film Using ATR Method
Parallel polarized light refers to linear polarized light with an electric field parallel to the incident plane. Conversely, perpendicular
polarized light refers to linear polarized light with an electric field in a plane perpendicular to parallel polarized light. For
perpendicular polarized light, the evanescent wave generated at the reflection point during ATR measurements has a vector
in the X-direction, as shown below. For parallel polarized light, it has vectors in the Y and Z-directions. Therefore, information
about molecular vibration in the X-direction can be obtained using measurements with perpendicular polarized light, whereas
measurements with parallel polarized light provides information about molecular vibrations in the Y and Z-directions.
E
Infrared light
Z
Y
Infrared light
E
Ey
X
Ez
Ex
Perpendicular polarized light (S)
Parallel polarized light (P)
Orientation of Polarized Light and Evanescent Waves
LAAN-D-XX025
23
Product Evaluation
Crystallization
Measurement of Commercial PET Bottles
A differential scanning calorimeter (DSC) was used to compare the crystallization in commercial PET bottles for hot and cold beverages. In
the first run, an exothermic peak where crystallization presumably occurred, was observed for the cold beverage bottle near 100°C, but was
not observed for the hot beverage bottle. In the second run, given the same thermal history, almost no differences were observed between
the samples. Based on these results, presumably the hot beverage PET bottle has higher crystallization due to a difference in thermal history
experienced during molding. Separate X-ray diffraction analysis results also confirm that the hot beverage bottle has higher crystallization.
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Thermal Analysis
Product Information
DSC Measurement Results of PET Bottles
Crystallization of PEEK
This example investigates the relationship between the thermal history of PEEK and its crystallization. The figure below shows that when PEEK
film was heated, the glass transition occurred at 145°C, crystallization at 181°C, and melting at 342°C, which indicates it was not crystallized
before heating. In contrast, only a melting point of 339°C was measured for the PEEK pellets, which indicates it was already crystallized
before heating. This difference in crystallization probably occurred due to the rapid cooling experienced by the film sample during molding,
whereas the pellet sample cooled more slowly. This is consistent with DSC measurement results of pellets that were rapidly cooled after the
DSC measurement above, which showed the same glass transition, crystallization, and melting temperatures as the film.
DSC Measurement Results of PEEK
24
LAAN-D-XX026
n
Thermal Characteristics
Product Evaluation
Thermal Analysis
Evaluation of
Raw Materials
Product Evaluation
In this example, the thermal expansion
process in epoxy resin was measured.
T h e re s u l t s s h o w a c h a n g e i n t h e
thermal expansion coefficient at about
90°C. This is due to the glass transition
of the epoxy resin. Therefore, because
material characteristics change at
that point, it is necessary to know
what that temperature is. Glass
transition can also be measured using
other methods, such as DSC, but
thermomechanical analyzers (TMA)
a l l o w m e a s u r i n g t h e p o i n t w h e re
mechanical characteristics of the
material change.
Evaluation of
Plastic Materials
Measurement of Thermal Expansion Process in Epoxy Resin Using a TMA
Measurement of Shrinkage Behavior in PE Film Using a TMA
Product Information
Two types of PE film were heated
u n d e r t e n s i o n . T h e m e a s u re m e n t
results indicate that the films began
shrinking above 100°C and then
began stretching above 150°C. The
figure shows that the two types of
film shrank at different temperatures.
In the tension mode, the strain during
shrinking can be measured as well.
Various TMA Measurement Modes
The Shimadzu TMA-60 includes three
m e a su re m e n t m o d e s – e xp an s i o n ,
tension, and penetration, which can
be freely changed depending on
the sample shape and objectives.
Changing modes is extremely easy,
too.
Expansion Mode
Tension Mode
Penetration Mode
LAAN-D-XX027
25
Product Evaluation
E v a l u a t i o n o f M e c h a n i c a l C h a r a c t e r i s t i c s o f Va r i o u s P l a s t i c P ro d u c t s U s i n g
Autograph
The four figures below are examples of results from using a Shimadzu AG-X Autograph precision universal testing machine to evaluate static
mechanical characteristics of some typical plastic products. This data allows determining the fundamental characteristic values that are the
most important for mechanical design, such as strength, elongation, elasticity, and energy absorption.
These tests were performed in accordance with JIS standards applicable to the given specimen (sample) shape and test methods.
Evaluation of
Raw Materials
Vertical axis: Stress
Product Evaluation
Stress (MPa)
Example of Evaluating Polyethylene
Stress (MPa)
Evaluation of
Plastic Materials
Autograph
Mechanical Characteristics –
Static Strength
Displacement (strain) (%)
Horizontal axis: Elongation
Displacement (strain) (%)
Example of Evaluating Polyethylene
Stress (MPa)
Stress (MPa)
Product Information
Example of Evaluating Polypropylene
Displacement (strain) (%)
Displacement (strain) (%)
Example of Evaluating Polyvinyl Chloride
Example of Evaluating Polycarbonate
Evaluation of Plastic Film Characteristics Using Autograph
Thin plastic film materials are increasingly being used for functionally engineered materials. Therefore, it is critically important to understand
their characteristics, not only for controlling their functionality and performance, but also for use in developing new applications.
As one example, a 38 µm thick polyester film was evaluated to determine any differences in mechanical characteristics in directions parallel
and perpendicular to the direction it was stretched (due to mechanical stretching processes during film manufacturing).
Example of Evaluating Polyester Film
26
LAAN-D-XX029A
n
Mechanical CharacteristicsFatigue and
Impact Strength
Product Evaluation
Servopulser/Hydroshot
In actual usage, plastic products are always exposed to some sort of repeated stresses.In particular, if the item is used for
transportation equipment or as a structural member, then the endurance must be determined to ensure safety, which involves
repeatedly applying a load at high speed to evaluate its service life. Servopulser and Micro-Servo testing machines efficiently and
accurately apply loads to evaluate the service life of specimens.
Evaluation of
Plastic Materials
Evaluation of Endurance (Fatigue Strength) of Various Plastic Products Using Servopulser
Example of testing endurance of GFRP
Evaluation of
Raw Materials
Stress-Endurance Curve
Change in Stress-Displacement Curve Over Time
Change in Displacement (Upper/Lower Limits) Over Time
Product Evaluation
Change in Stress-Displacement Amplitude Over Time
Example of fatigue test of fuel cell electrolyte
membrane
Product Information
Evaluation of Impact Strength of Various Plastic Products Using Hydroshot
Data for evaluating impact strength is an important parameter for determining the safety and impact (energy) absorbing
characteristics of plastic products, such as those used in automobiles.Hydroshot impact testing machines obtain test force and
displacement data at loading speeds of up to 20 m/sec (72 km/h), where loading can be applied in either tensile or puncture modes.
High-Speed Tensile Testing of CFRP
High-Speed Tensile Testing of Polyester Film
LAAN-D-XX030A
27
Product Evaluation
Example of Analyzing and Observing the Internal Structure of Various Plastic
Products Using Industrial X-Ray Inspection
• Analyzing the interior of glass fiber reinforced plastic
The following is an example of analyzing the interior of glass fiber reinforced plastic (GFRP).
Using a CT image to observe the fiber orientation inside the material showed that the fibers were oriented differently in the surface
and center layers. Fibers in the surface layer were oriented parallel to the flow direction (direction the plastic material flowed during
manufacturing), whereas fibers in the center layer were oriented perpendicular to the flow.This result is also consistent with computer
analysis. Consequently, information about fiber orientation that was previously obtained by making FRP specimens and inspecting them
visually (or with a microscope) can now be obtained non-destructively.
Product Information
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Industrial X-Ray Inspection System
Non-Destructive Inspection Defect
Inspection and Internal Structural Analysis
Example of Observing Internal Structure of GFRP (Fiber Orientation)
Example of Analyzing and Observing the Internal Structure of Various Plastic
Products Using Industrial X-Ray Inspection
• Observing water inside a fuel cell
The following is an example of observing water in the gas diffusion layer of a polymer electrolyte fuel cell. This shows that the presence
of water can clearly be determined and the formation, distribution, and movement of water can be observed non-destructively. Therefore,
this inspection is expected to make a significant contribution to the development of fuel cells.
Example of Observing Internal Structure of Fuel Cells (Distribution of Water)
28
LAAN-D-XX031A
n
Analysis of Foreign Substances
Product Evaluation
FTIR
Microscope Photograph of Foreign
Substance on Film
Red box: 50×100 µm
Evaluation of
Raw Materials
The following are results from using an infrared microscope and the attenuated total
reflection (ATR) method to analyze trace contaminants discovered on the surface of
film. The fibrous substance, which was about 5 µm wide, and the film surface were
both measured to obtain a differential spectrum. From the resulting spectrum it was
determined that the fibrous substance was cellulose fibers. In this way, an infrared
microscope and ATR method can be used to obtain information about sample
surfaces, such as difficult-to-sample substances adhered to sample surfaces, without
any pretreatment.
Evaluation of
Plastic Materials
Analysis of Foreign Substances on Film Using an Infrared Microscope
Product Evaluation
Product Information
Measurement Results from Foreign Substance (Black) and Normal Area
Differential Spectrum (Cellulose)
Infrared Microscope
Infrared microscopes focus condensed infrared light on a sample and detect the light passed through or reflected from the sample
with a highly sensitive MCT detector. This enables measuring very small samples and micro areas that cannot be analyzed using the
FTIR system alone. Transmission, specular reflectance, ATR or other methods can be selected depending on the measurement sample
and purpose of analysis, which is extremely helpful for analyzing defects, such as foreign substances or deterioration, identifying
the respective layers of multilayer films, or analyzing micro-areas. Samples can be measured (transmittance or specular reflectance
measurement) by viewing the sample in the same manner as operating an optical microscope, and then specifying the measurement
location using the auto aperture. Unlike other instruments that analyze micro-areas by irradiating samples with high-energy visible
near-infrared laser light, X-rays, or electrons, infrared microscopes cause almost no change or damage to samples.
Infrared Microscope System
Photographs from Infrared Microscope
LAAN-D-XX034A
29
Product Evaluation
Evaluation of
Plastic Materials
AA
Hazardous Substances Hazardous Metals
Analysis of Cadmium in Plastics Using an AA Spectrophotometer
Atomic absorption (AA) spectrophotometers are able to analyze elements in solution with high sensitivity. Analysis of solid samples, such as
plastics, requires preparing a sample solution using pretreatment methods such as dry incineration or Kjeldahl digestion (wet digestion). In
this case, standard polyethylene samples BCR680 and 681 were prepared by dry incineration and Kjeldahl digestion and results were also
compared to those obtained by ICP emission spectrometry.
Evaluation of
Raw Materials
(1) Dry Incineration Method
Weigh 0.2 g of sample into a quartz crucible. Add enough sulfuric acid to immerse the sample. Heat the crucible on a hotplate until the
white SO3 smoke starts dissipating and then place it in an electric furnace and incinerate the contents to ash at 450°C. After incineration,
add 5 mL of hydrochloric acid (1 + 2) to the residue and evaporate it to dryness on a water bath. Add 10 mL of 1 mol/L nitric acid and
apply heat to dissolve the sample. After letting it cool, measure 20 mL of the digest solution. (Reference: Food Sanitation Inspection
Guidelines – Physics and Chemistry, 2005, supervised by the Japanese Ministry of Health, Labour, and Welfare)
(2) Wet Digestion Method
Product Evaluation
Weigh 0.2 g of the sample in a Kjeldahl flask. Add sulfuric acid, nitric acid, and hydrogen peroxide to the flask and heat it on a heating
mantle (at about 300°C) to digest the sample. The contents will become black with carbon and white SO3 smoke is emitted. After the
solution turns black with carbon, add more nitric acid and hydrogen peroxide and continue heating (at about 350°C). Repeat this process
until the contents turn pale yellow. After letting the flask cool, measure 20 mL of the solution. (Reference: BS EN1122 Method A: 2001)
Analytical Conditions and Results
Measurement Results
Product Information
Measurement results were obtained using the flame atomization method. The cadmium (Cd)
calibration curve used for measurements is shown in Fig. 1. Table 1 shows a comparison of data
obtained using different pretreatment and measurement methods (ICP emission spectrometry).
These show that both methods gave results that were roughly consistent with certified values.
Given flame atomic absorption spectrophotometry is used and the sample is diluted by 100
times before measuring, the lower quantitation limit in plastic is 0.5 mg/kg.
Analytical Conditions
Analytical wavelength: 228.8 nm
Slit width:0.7 nm
Measurement mode: BGC-D2
Acetylene gas flowrate:1.8 L/min
Air flowrate:15 L /min
Fig. 1 Calibration Curve for Cd by Atomic Absorption Spectrophotometry
Table 1 Quantitation Results of Polyethylene
Dry incineration
BCR680
BCR681
30
LAAN-D-XX035A
AA
ICP
140
141
20.0 21.0
Wet digestion
AA
ICP
142
140
22.0 21.4
Certified value
(mg/kg)
140.8
21.7
n
Hazardous Substances Hazardous Metals
Product Evaluation
ICP-AES
ICP emission spectrometers are able to analyze elements in sample solutions with high sensitivity. Solid samples, such as plastics,
require using dry incineration, wet digestion, microwave digestion, or other methods to pretreat samples to prepare a solution.
However, that requires selecting the appropriate pretreatment method for the elements being analyzed. This example introduces
results from using respective pretreatment methods to prepare solutions of plastic samples (standard polyethylene samples
BCR680 and BCR681) and then analyze them for hazardous metals, such as lead (Pb) and cadmium (Cd), using a Shimadzu
multitype ICPE-9000 emission spectrometer.
(1) Dry Incineration Method
Product Evaluation
Weigh 0.2 g of sample into a quartz crucible. Add enough sulfuric acid to immerse the sample. Heat the crucible on a hotplate until the
white SO3 smoke starts dissipating and then place it in an electric furnace and incinerate the contents to ash at 450°C. After incineration,
add 5 mL of hydrochloric acid (1 + 2) to the residue and evaporate it to dryness on a water bath. Add 10 mL of 1 mol/L nitric acid and
apply heat to dissolve the sample. After letting it cool, measure 20 mL of the digest solution. (Reference: Food Sanitation Inspection
Guidelines – Physics and Chemistry, 2005, supervised by the Japanese Ministry of Health, Labour, and Welfare)
Evaluation of
Raw Materials
Sample Pretreatment Methods
Evaluation of
Plastic Materials
Analysis of Hazardous Metals in Plastics Using an ICP-AES System
(2) Wet Digestion Method
Weigh 0.2 g of the sample in a Kjeldahl flask. Add sulfuric acid, nitric acid, and hydrogen peroxide to the flask and heat it on a heating
mantle (at about 300°C) to digest the sample. The contents will become black with carbon and white SO3 smoke is emitted. After the
solution turns black with carbon, add more nitric acid and hydrogen peroxide and continue heating (at about 350°C). Repeat this process
until the contents turn pale yellow. After letting the flask cool, measure 20 mL of the solution. (Reference: BS EN1122 Method A:2001)
Product Information
(3) Microwave Digestion Method
Weigh 0.2 g of the sample in a digestion vessel. Add nitric acid and hydrogen peroxide and seal the vessel. Digest the sample in
microwave sample pretreatment unit. After letting the digestion vessel cool, measure 20 mL of the digest solution. Note: For samples
containing large amounts of coexisting components, such as additives, use a small amount of hydrofluoric acid.
(Reference: US EPA SW-846 Method 3052)
Analytical Conditions and Results
Analytical Results
Analytical results are shown in Table 1. Good results were obtained, with lead (Pb) and
cadmium (Cd) results from dry incineration, cadmium (Cd), total chromium (Cr), and
mercury (Hg) results from wet digestion, and results for all elements from microwave
digestion consistent with certified values.
Discussion
The ICP emission spectrometer enabled measuring trace components with good precision.
Nevertheless, Hg results were low for dry incineration, presumably due to scattering at high
temperature and Pb results were low for wet digestion, presumably due to precipitation of lead
sulfate formed from reaction with the sulfuric acid used for digestion. Therefore, an appropriate
sample pretreatment method must be selected based on the elements being measured.
Analytical Conditions
Instrument: ICPE-9000
High frequency output: 1.2 kW
Plasma gas flowrate: 10 L/min
Auxiliary gas flowrate: 0.6 L/min
Carrier gas flowrate: 0.7 L/min
Sample introduction: Coaxial nebulizer
Spray chamber: Cyclone chamber
Plasma torch: Mini torch
Observation method: Axial
Table 1 Quantitation Results of Polyethylene
sample
Pretreatment
Element
Cd
Unit:mg/kg
BCR680
Dry incineration
BCR681
Wet digestion
Microwave
digestion
Certified
value
Dry incineration
Wet digestion
Microwave
digestion
Certified
value
141
140
140
140.8
21.0
21.4
21.7
21.7
Pb
105
< 0.2
108
107.6
13.1
< 0.2
13.5
13.8
Cr
105
112
112
114.6
16.2
17.2
17.5
17.7
Hg
< 0.2
24.0
25.6
25.3
< 0.2
4.3
4.6
4.5
As
28
31
30
30.9
4
4
4
3.93
LAAN-D-XX036A
31
Product Evaluation
Hazardous Substances Hazardous Metals
Evaluation of
Plastic Materials
UV
Analysis of Hexavalent Chromium in Plastic Using a UV-VIS Spectrophotometer
The content of hexavalent chromium is regulated by the ELV, WEEE, and RoHS directives, which regulate hazardous substances in Europe
(EU). Hexavalent chromium in plastic is analyzed by pretreating the sample to extract the hexavalent chromium into solution and then
analyzing the solution by colorimetry using a UV-VIS spectrophotometer. A process flowchart for extracting the hexavalent chromium from
plastic is shown to the right.
Evaluation of
Raw Materials
[IEC 62321 Ed.1]
(1) Prepare sample
(2) Pulverize by freeze shattering
(3) Extract by alkali extraction, then filter
(to separate sample from extract)
Filter
Product Evaluation
Alkali extraction
Adjust the sample volume
Add coloring reagent
Perform UV measurement
(4) Add diphenylcarbazide colorizing
reagent to extract
(5) Measure color level after specified time
Purify
Product Information
Process Flow of Actual Analysis
Process Flowchart of Extracting Hexavalent Chromium from Plastic
Colorimetric Analysis Using a UV-VIS Spectrophotometer
UV-VIS spectrophotometers disperse light from a light source with a grating to irradiate samples with the light, and then measure how
much light the sample absorbed based on the difference in light energy level before and after irradiating the sample. Hexavalent chromium
is analyzed by extraction into a solution and then colorization using diphenylcarbazide reagent. After colorization of the hexavalent
chromium, the spectrophotometer measures the level of color.
UVmini-1240 Hexavalent Chrome Analysis
I0
I
Diphenylcarbazide
I
Beer-Lambert Law
-εcl
Transmittance T = I/I0 = 10
ε: Absorption coefficient
c: Solution concentration
l: Optical path length
Measurement
AbsorbanceA = log (1/ T)
Coloring
= εcl
The solution concentration is
proportional to the absorbance.
32
LAAN-D-XX037C
Absorption Curve of Cr(VI) Diphenylcarbazide
Complex
n
Hazardous SubstancesOrganic
Substances
Product Evaluation
GC/MS
Instrument Configuration
GCMS-QP2010 Ultra
AOC-20i/s autoinjector
Evaluation of
Raw Materials
Various countries have established regulations to restrict the use of phthalate esters, which are commonly added as plasticizers in
plastic toys and consumer goods. Some of the phthalate esters subject to regulation include DEHP (bis(2-ethylhexyl) phthalate),
DBP (dibutyl phthalate), BBP (butyl benzyl phthalate), DINP (di-isononyl phthalate), DIDP (di-isodecyl phthalate), and DNOP (din-octyl phthalate). The analytical method typically involves extracting the phthalate esters from the plastic using solvents and
analyzing the extract “as is” or diluted. If concentration levels are relatively high and there are few interfering substances, then
GC-FID can be used for analysis, but plastic samples containing large numbers of interfering substances or phthalate esters such
as DINP or DIDP, which have many isomers, are analyzed using GC/MS.
Evaluation of
Plastic Materials
Analysis of Phthalate Esters in Plastic
Analytical Conditions
0.9
Product Information
1 DBP
2 DEHP
3 DINP
2
1.0
Product Evaluation
The sample (about 1 g of plastic) is immersed in 50 mL of acetone/hexane (3:7) at 40°C and left over night. Then the extract solution is
diluted to a known volume and injected into the GC/MS system.
TOTM
0.8
0.7
0.6
0.5
TIC
0.4
149.00
0.3
0.2
0.1
307.00
0.0
5.0
17.0
Example of Analyzing Plastic Toys
TOTM: Trioctyl Trimellitate
LAAN-D-XX038A
33
Product Evaluation
Analysis of Hazardous Elements
Analysis of Hazardous Elements in Plastic Using an EDX Spectrometer
Due to its ability to quickly, easily, and non-destructively analyze solids, powders, and liquids, X-ray fluorescence spectrometers have been
widely used for screening the five elements (Cd, Pb, Hg, Cr, and Br) regulated under the RoHS and ELV directives. This example measures
hazardous elements in the insulating jacket material of a LAN cable. Specifically, it shows results from analyzing Pb and Cd.
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
EDX
Product Evaluation
LAN Cable
EDX-720 Spectra for Pb (Left) and Cd (Right)
Product Information
A calibration curve was created and quantitative analysis performed using standard samples
prepared by adding the five RoHS elements (Cd, Pb, Hg, Cr, and Br) to PE and PVC plastic.
Features of the EDX Series
EDX series models are equipped standard with a primary filter that is optimal for hazardous
elements, which allows measuring the five RoHS elements easily and with high sensitivity.
In addition, a background internal standard correction function is included to correct for
the thickness, shape, and size of samples. Background internal standard correction corrects
quantitation values based on the ratio between continuous X-rays from the X-ray tube or
characteristic X-rays from the target and scattered rays.
Quantitation Results
Using an EDX System
Pb: 7600 ppm
Cd: 52 ppm
Analytical Conditions
Instrument: EDX-720
Tube voltage: 50 kV
Tube current: Automatic
Measurement time: 100 sec
Optimal filter used
Automatic Calibration Curve Selection Function
Measured Intensity (cps/uA)
When analyzing X-ray fluorescence, different sample types (PE versus PVC, for example) cause the X-ray fluorescence intensity to vary. The
automatic calibration curve selection function allows using the software to determine the presence of Cl, automatically select the optimal
calibration curve for PE or PVC, and then quantitate the content.
Standard Value (ppm)
34
LAAN-D-XX039A
n
Halogen-Free Analysis
Product Evaluation
EDX
Due to its ability to analyze solids, powders, liquids, and other samples quickly, easily, and non-destructively, X-ray fluorescence
analysis has been widely used for screening elements regulated by RoHS and ELV directives. More recently, the electrical/
electronic industries have been promoting the elimination of halogen elements, such as BR and Cl, from their products, in
addition to the five elements subject to the RoHS directive. In this example, Cl was analyzed in plastic.
Evaluation of
Plastic Materials
Analysis of Halogen Elements (Chlorine) Using an EDX Spectrometer
Evaluation of
Raw Materials
Product Evaluation
Cl Spectra
Calibration Curve for Cl Kα
Features of the EDX Series
The primary filter included standard for Cl allows easily measuring Cl with high
sensitivity. Also, attaching a vacuum measurement unit (option) allows analyzing Cl
with even higher sensitivity.
Product Information
The calibration curve was created using a standard sample prepared by adding Cl to
polyethylene (PE) plastic.
Analytical Conditions
Instrument: EDX-720
Spectrum: Cl Kα
Tube voltage: 15 kV
Tube current: Automatic
Measurement time: 100 sec
Optimal filter used
Analysis
The Cl content in a plastic plate specimen and plastic parts was measured. In addition, shape correction based on the
background internal standard correction function was used to correct for the thickness, shape, and size of samples. Background
internal standard correction corrects quantitation values based on the ratio between continuous X-rays from the X-ray tube or
characteristic X-rays from the target and scattered rays.
LAAN-D-XX040B
35
Product Information
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Evaluation of Raw Materials
Fourier Transform Infrared
Spectrophotometer
Analysis of Plastic Samples by FTIR
Many different types of information can be obtained from plastic samples using FTIR systems, such as information for checking raw
materials, the composition of plastic pellets or powders, bonding modes, isotope ratios, copolymer composition ratios, molecular
orientation, and information for analyzing foreign matter or other defects. Since FTIR allows analyzing samples easily and quickly, and also
allows analyzing micro areas and surfaces, it is especially useful for analysis and testing in various plastic product manufacturing processes.
Features of the Shimadzu IRAffinity-1
Fourier Transform Infrared Spectrophotometer
• Higher sensitivity and performance than general purpose systems
• IRsolution software is easy to operate and offers sophisticated functionality
• Expanding range of applications
Product Evaluation
This attractive and compact Fourier transform infrared spectrophotometer features a
dynamic alignment mechanism that keeps the interferometer continuously optimized
and a built-in dehumidifier that ensures easy maintenance. It offers an S/N ratio of
30,000:1 (given 4 cm -1 resolution, 1 minute accumulation, near 2100 cm -1, and peakto-peak), maximum resolution of 0.5 cm -1, and a compact design. In addition, the
IRsolution high-functionality, high-operability software and analysis support programs
(Contaminant Analysis Program and Pharma Report Program) ensure data processing
and postrun analysis can be accomplished easily.
IRAffinity-1
Product Information
Features of the Shimadzu IRPrestige-21
Fourier Transform Infrared Spectrophotometer
•
•
•
•
High sensitivity and high functionality
High reliability
Measurement range from near infrared to far infrared
IRsolution high-functionality, high-operability software
IRsolution High-Functionality Software
High-throughput optics, with features such as a high-energy ceramic light source,
temperature-controllable high-sensitivity DLATGS detector, and gold-coated mirrors,
achieves high S/N ratios above 40,000:1 (given a 4 cm -1 resolution, 1 minute
accumulation, near 2100 cm -1, and peak-to-peak). In addition, an advanced dynamic
alignment (ADA) mechanism keeps the interferometer continuously optimized and
a built-in dehumidifier ensures easy maintenance. A wide measurement range,
from near infrared to far infrared, and a wide assortment of accessories expand the
possible range of applications. In addition, the IRsolution high-functionality, highoperability software and analysis support programs (Contaminant Analysis Program
and Pharma Report Program) ensure data processing and postrun analysis can be
accomplished easily.
IRPrestige-21
36
Near Infrared Spectrum of Octanoic Acid
(tracking changes in hydrogen bonds due to heat)
n
Product Information
Single Nano Particle Size Analyzer
Evaluation of Raw Materials
Biological macromolecules, nanoparticles, and macromolecular nanoparticles made by combining such components are actively being
developed in drug formulation and other fields. For such nano-sized particles, the particle size distribution is one of the most important
physical properties. The IG-1000 Single Nano Particle Analyzer utilizes the induced grating (IG) technology developed independently by
Shimadzu for measuring the distribution of single-digit nanoparticles dispersed in liquid with high sensitivity and good reproducibility.
Product Evaluation
• Measures the distribution of single-digit size nanoparticles dispersed in liquid with
high sensitivity and reproducibility.
• Accurately measures samples with broad size distributions.
• Free from the tendency to overstate presence of large particles and not be able to
measure small particles.
• Measurement results are unaffected by trace amounts of large particles outside the
measurement range (such as aggregates or contaminants).
• Samples can be measured in normal environments, even without any careful pretreatment (filtering) processes.
• Allows using raw data (time course variations in intensity of diffracted light) to verify the validity of measurement results.
Evaluation of
Raw Materials
Features of the IG-1000 Single Nano Particle Size Analyzer
Measurement Range: 0.5 nm to 200 nm
Evaluation of
Plastic Materials
Analysis of Plastic Samples by IG-1000 Single Nano Particle Size Analyzer
IG-1000 Single Nano Particle Size Analyzer
Particle diameters are determined by forming a diffraction
grating from the particles and then measuring diffusion speed.
a
Product Information
The particle diffraction grating is formed using dielectrophoresis.
Samples are placed in a batch cell, then a comb-shaped electrode substrate is inserted
into the cell. When an alternating current is applied to the comb-shaped electrodes,
dielectrophoresis concentrates the particles dispersed throughout the liquid into a
particle diffraction grating pattern. When the alternating current is switched OFF, the
dielectrophoresis stops and the particle diffraction grating pattern begins diffusing.
Quartz Glass
Platinum CombShaped Electrodes
Illustration of Electrode Substrates
Sample Suspension
Alternating Voltage
Batch Cell
2a
Diffusion speed is determined from the time course change in
primary diffracted light intensity.
In previous systems based on light scattering methods, which use light scattered
from particles as the detected signal, the signal level drops rapidly as the particle size
decreases. That makes it extremely difficult to measure single-digit nanoparticles. In
contrast, the IG method uses the primary diffracted light from the macro structure of
a particle diffraction grating as the detection signal. Therefore, the signal level is not
dependent on particle size, making it possible to obtain more than adequate signal
even from single-digit nanoparticles, which in turn makes it possible to measure
particle size distributions with high sensitivity and reproducibility.
Particle size is determined from the relationship between particle
size and diffusion speed.
Large particles diffuse slowly and small particles, particularly single-digit nanoparticles,
diffuse quickly. The IG method determines particle size from the relationship between
particle size and diffusion speed.
Diffraction Grating Formed from Particles
(pitch is twice the pitch of the
comb-shaped electrodes)
Diffusion of Particle Concentration Diffraction Grating
Laser Light
Primary Diffracted Light
Dielectrophoresis
Dielectrophoresis
OFF
Intensity of Diffracted Light
Primary diffracted light is detected by irradiating the particle diffraction grating with
laser light. The primary diffracted light intensity decreases correspondingly as the
particle diffraction grating diffuses. In this way, the diffusion speed of the particle
diffraction grating is monitored based on the change in primary diffracted light
intensity as a function of time.
(Diffused)
Time
37
Product Information
Evaluation of
Plastic Materials
High-Performance Liquid Chromatograph
Analysis and Fractionation of Additives and Impurities Using HPLC and Preparative
LC Systems
Evaluation of
Raw Materials
Evaluation of Plastic Materials
Features of Shimadzu Prominence Series HighPerformance Liquid Chromatographs
Additives to polymer materials and products have various important functions that can determine product performance, such
as heat resistance or structural integrity. Impurities can affect the quality of products, making them less stable or resilient. HPLC
systems are used to separate and quantitate many different additives and impurities, whereas preparative LC systems are used to
separate and fractionate large quantities of additives and impurities for purposes such as structural analysis.
The Prominence series was developed to improve the efficiency of analytical processes
and improve operating and data reliability. Prominence HPLC systems offer new features
and outstanding performance compared to previous models, such as Web-based
monitoring and control, high-speed sample injection, and high-sensitivity detection.
Product Evaluation
▪ Improved Analytical Productivity
•
•
•
•
•
Fastest sample injection (10 sec for 10 µL)
Fully automated startup and shutdown
Self-diagnostic and self-repairing functions (expert function)
Energy saving auto-validation function
Web-control (allows access to the instrument via an Ethernet connection)
Prominence Series
Product Information
▪ Improved Analytical Reliability
•
•
•
•
High sensitivity and extended linearity
Nearly zero cross-contamination
Improved detector stability with a thermostatic flow cell
Improved flowrate accuracy
Features of Shimadzu Prominence Semi-Preparative Recycling
High Performance Liquid Chromatographs
▪ The semi-preparative recycling system includes a kit that minimizes the internal volume, which results in highly efficient
separation by closed loop recycling.
▪ By combining this system with appropriate columns, it is possible to achieve more than several million theoretical plates.
Prominence Semi-Preparative Recycling System
38
n
Product Information
Gas Chromatograph/Mass Spectrometer
Evaluation of Plastic Materials
Pyrolysis gas chromatography mass spectrometry is an especially powerful analytical technique for researching new materials,
polymer characterization, and other applications. That is because pyrolysis gas chromatography enables analyzing polymer
compounds—such as in insoluble or composite materials, and in ultra trace quantities—without requiring any complicated
pretreatment. In addition, it provides unique information that is difficult to obtain using other methods.
GCMS-QP2010 Ultra
Product Evaluation
The GCMS-QP2010 Ultra features a high-efficiency ion source, detector with
overdrive lens, and high-capacity differential vacuum mechanism to provide a system
with high sensitivity and high stability. The highly sensitive and exceptionally stable
GC/MS system decreases the lower detection and quantitation limits, which increases
the hit rate for mass spectra similarity searches for even ultra trace components.
Furthermore, decreasing the absolute sample quantity injected allows simplifying
concentration pretreatment and reducing contamination in injection port inserts
and columns. The newly designed electronic control platform offers the fastest scan
speeds in class. That means it is also perfect for other applications that require fast
scan speeds, such as simultaneous scan/SIM measurements or GC × GC/MS and fastGC/MS analysis.
Evaluation of
Raw Materials
Features of the GCMS-QP2010 Ultra
Evaluation of
Plastic Materials
Analysis of Plastic Samples by PY-GC/MS
Features of the Pyrolysis System (for polymer compound analysis)
Product Information
Pyrolysis-GC/MS is commonly used to measure samples related to plastics. It performs
analysis on plastics, rubbers, and other polymer compounds by decomposing them
at temperatures above 500°C and using GC/MS to analyze the resulting thermal
decomposition products. Since the decomposition products reflect the structure
of the original polymer compound, they can be used to identify the polymer or
perform more sophisticated structural analysis. An F-Search feature (polymer and
additive search software) is also provided to help identification. In addition to the
features of a conventional pyrolysis system, the double-shot pyrolyzer also enables
selecting more sophisticated analytical methods, such as evolved gas analysis with
programmed heating or thermal desorption with flash pyrolysis.
GCMS-2010 Ultra
EGA/PY-3030D
System Contents
GCMS-QP2010 Ultra, EGA/PY-3030D, AS-1020 sampler, etc.
Applications
Plastics, rubbers, polymers, and other macromolecule compounds, and trace organic
impurities in inorganic materials
Features of GCMSsolution
The GC/MS workstation software, GCMSsolution, offers extensive functionality
combined with ease of use. Intuitive controls, assistant bar and data explorer features
for providing data management functions, Word-like report functions, and in-depth
GLP/GMP support functions all contribute to a software package that helps improve
analytical productivity.
GCMSsolution
39
Product Information
Liquid Chromatograph Mass Spectrometer
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Evaluation of Plastic Materials
Analysis of Polymer Additives Using LCMS
The various types of additives added to polymer materials and products serve an important function that can determine that
product's performance. For example, for the same type of polymer, the formulation of additives can vary depending on the
brand or grade. This means that the information obtained from analyzing additives can be very important for market research or
product development.
Features of Shimadzu LCMS-2020
Liquid Chromatograph Mass Spectrometers
▪ From HPLC to UFLC
In addition to speed and separation capabilities, ultra fast LC (UFLC) succeeds in
offering both higher precision and expandability than possible with conventional
high-performance LC (HPLC) systems.
▪ Ultra Fast Speed
Product Evaluation
To achieve overall faster processing speeds, the LCMS-2020 offers not only faster
analysis, but also faster sample injection speeds and fully automated analytical
functions.
LCMS-2020
▪ Exceptional Reproducibility
Product Information
Even though the LCMS-2020 is ultra fast LC, it provides very high injection
reproducibility. It also offers unrivaled carryover suppression, which is critical for
LC/MS analysis.
▪ Extensive Expandability
In addition to ultra-fast analysis, the system also offers the flexibility to be used
for many other applications as well, such as normal HPLC or semi-preparative LC.
Using these features allows easily confirming the elution of components based on the
m/z value of known additives, highly selectively quantitating components, predicting
the molecular weights of unknown compounds, and more.
LCMSsolution Ver. 5 for LCMS-2020
Ultra-fast
Ultra-fast
Ultra-fast
Rapid 15-millisecond positive/negative
ionization switching
S upe rior sensitivity from UFLC
1 5 , 0 0 0 u / s e c f a s t s c a n n i n g s p e ed
The newly developed Qarray ® Optics achieves superior
Controls the voltage applied to the Quadrupole
sensitivity, reproducibility, and linearity.
according to the scan speed and m/z.
U F s w it c h i n g
UFsensitivity
To detect both positive and negative ions, analysis is
performed while switching between the positive and
negative ionization modes.
The LCMS-2020 adopts a high-voltage power supply
U F sca n n i n g
This new technology (patent pending) maintains
resolution and achieves high ion transmittance even at
high scanning speeds.
featuring novel technology (patent pending) to achieve
an ultra-fast polarity switching time of just 15 ms.
Polarity switching time
15 msec
Positive-ion
measurement
SIM 2CH
Polarity switching time
15 msec
Negative-ion
measurement
SIM 2CH
Positive-ion
measurement
SIM 2CH
Sample:
m/z 321: Chloramphenicol
m/z 344: Dibucaine
m/z 329: Furosemide
m/z 231: Isopropylantipyline
40
m/z 414: L-α-Narcotine
m/z 256: Diphenhydramine
m/z 267: Desipramine
m/z 278: Amitriptyline
n
Liquid Chromatograph Mass Spectrometer
Product Information
Evaluation of Plastic Materials
Predicting the structure of unidentified components in structures or compounds is very important in the analysis of competitor
products, identifying the cause of defects, and other applications. NMR and other techniques are available for predicting the
structure of organic substances. LCMS-IT-TOF, which enables accurate mass measurement and MS n analysis, is especially useful
for applications such as predicting the structure of trace additives or impurities in polymers.
Evaluation of
Plastic Materials
Predicting the Structure of Polymer Additives
Features of LCMS-IT-TOF Liquid Chromatograph Mass Spectrometers
Evaluation of
Raw Materials
Product Evaluation
• This hybrid mass spectrometer is designed for structural analysis and offers the fastest mass spectra measurement performance
available with high speed positive-negative polarity switching. This combination dramatically increases the amount of
information that can be obtained from a single measurement. This provides structural analysis with higher throughput and
reliability.
• Dual-stage reflectron (DSR) and ballistic ion extraction (BIE) enable acquisition of high resolution and highly accurate MS n data,
which allows accurate structural prediction of impurities.
• Compressed ion injection (CII) efficiently delivers ions to the ion trap, enabling the structural analysis of even ultra trace impurities.
• MS 3 measurements provide a powerful tool for determining impurity structures. Neutral loss surveys, composition prediction
software, and MetID Solution software all aid in structural elucidation.
Product Information
LCMS-IT-TOF Structure
MetID Solution
LCMS-IT-TOF Liquid Chromatograph Mass Spectrometer
41
Product Information
Evaluation of
Plastic Materials
Evaluation of Plastic Materials
MALDI-TOFMS
Analysis of Trace Components in Synthetic Polymers Using an SEC-AccuSpot-AXIMA System
SEC-MALDI-TOFMS systems provide a useful method of analyzing trace components in synthetic polymer samples by first using
size exclusion chromatography (SEC) to fractionate samples by size and then using MALDI-TOFMS to measure molecular weight
information from each fraction. Combining the organic solvent resistant Accuspot system with the AXIMA MALDI TOFMS
integrates the entire process from separation by SEC to analysis by MALDI-TOFMS. Therefore, SEC-AccuSpot-AXIMA systems
provide a powerful tool for analyzing trace components.
Product Evaluation
Evaluation of
Raw Materials
SEC-AccuSpot-AXIMA System
MALDI-TOFMS is widely used as a method for characterizing synthetic polymers. However, if multiple kinds of components are
mixed together, the components can mutually inhibit ionization, which results in detection of only the primary components, leaving
trace components undetected. The SEC-MALDI-TOFMS method can provide a useful way to avoid that problem by first separating
multi-component samples into different fractions. In a typical SEC-MALDI-TOFMS workflow, mixing matrix and cationizing reagents
with a large number of fractions for MALDI measurement followed by spotting the fractions onto a MALDI sample plate, is timeconsuming and impractical. In contrast, using an SEC-AccuSpot system, which mixes matrix or other reagents with fractions from
SEC and successively loads them onto MALDI sample plates, provides a fully integrated process of SEC fractionation and sample
spotting for measurement by MALDI-TOFMS. Using the SEC-AccuSpot-AXIMA system reduces the total analysis time to 1/4 the
time required previously. Therefore, SEC-AccuSpot-AXIMA systems provide a powerful tool for analyzing trace components.
Prominence
AccuSpot
AXIMA Performance
Product Information
Online
SEC (microscale)
MALDI-TOFMS
MALDI plate
Plate sensor
MALD plate
Before spotting
Spotting
After spotting
SEC-AccuSpot-AXIMA System
Features of the Organic Solvent Resistant AccuSpot System
▪ The AccuSpot is an automatic spotting system that mixes matrix or other reagent
with effluent from the LC unit and then successively spots the mixture onto MALDI
sample plates.
▪ Installing an optional GPC compliance kit enables using organic solvents as a mobile phase. GPC Compliance Kit
• Flow line parts are changed from PEEK to stainless steel or PTFE-based materials.
• An exhaust fan draws any gases from residual organic solvents out of the instrument and into the fume hood.
▪ The plate changer function enables continuous spotting of up to 9 MALDI plates.
▪ Computer interface enables central control of spotting parameters.
▪ Spotting monitor functionality is included standard
• The standard-equipped CCD camera allows monitoring of the actual spotting
process via the control computer.
42
Before spotting
Spotting
AccuSpot
After spotting
n
Thermal Analyzer
Product Information
Evaluation of Plastic Materials
Plastics consist of crystallized and non-crystallized areas. In the case of thermoplastics, increasing the temperature causes glass
transition and crystallization reactions in the non-crystalline areas, whereas the crystalline areas become soft and flow from
melting. As the temperature is increased further, oxidation and decomposition occur. Thermal analysis enables analyzing each
of these phenomena easily and quickly. Because these phenomena reflect the various characteristics of plastic products, thermal
analysis is useful not only for research and development, but also for quality control.
Evaluation of
Raw Materials
Shimadzu Differential Scanning Calorimeter
DSC-60
Evaluation of
Plastic Materials
Analysis of Plastic Samples Using Thermal Analyzers
• Peak height is about twice as high as previous Shimadzu models.
• Noise level is 1 µW or less.
• Includes a cooling chamber as standard.
Product Evaluation
Differential scanning calorimeters provide a useful means of quickly and easily
determining the changes in enthalpy and specific heat associated with the first-order
transition or relaxation phenomena of substances. In addition to a maximum noise
level of 1 µW and high sensitivity analysis, this new DSC system offers many other
unique features as well.
DSC-60
Product Information
Shimadzu Thermomechanical Analyzer
TMA-60
• Multiple types of measurement methods are available to accommodate a diversity
of sample shapes.
• Utilizes a new type of displacement sensor with high precision and low drift.
• Accurate automatic length measurement
Thermomechanical analyzers are able to use various types of measurement methods
(expansion, tension, and penetration) to evaluate material characteristics of
samples with a wide variety of shapes. With features such as an automatic length
measurement function and safety mechanisms, this model offers a higher order of
high performance and high functionality, combined with ease of operation.
TMA-60
Shimadzu Simultaneous Thermogravimetric and
Differential Thermal Analyzer
DTG-60
• Utilizes highly sensitive and highly stable balance mechanism.
• Plug-in type DTA detector
• Flow line configuration accommodates a wide range of applications.
Simultaneous thermogravimetric and differential thermal analyzers not only provide
higher basic performance levels, they also offer the flexibility to accommodate a
wide variety of applications related to interactions between samples and various gas
environments. This allows conveniently performing simultaneous measurements for
applications ranging from data acquisition to analysis.
DTG-60
43
Product Information
Evaluation of
Plastic Materials
Evaluation of Plastic Materials
Gas Chromatograph
Analysis of Plastic Samples Using a Gas Chromatograph
GC systems are used to analyze volatile components in plastics, such as for testing raw materials, testing elution, analyzing
residual monomers, or analyzing residual solvents. Due to its high reliability and ease of analyzing samples, GC systems are well
suited to a wide variety of applications, from R&D to process and quality control.
Product Evaluation
Evaluation of
Raw Materials
Features of GC-2014
The GC-2014 is a space-efficient multipurpose gas chromatograph featuring the
latest state-of-the-art technology.
• Compatible with either capillary or packed columns (or a combination of both)
• Multiple sample injection units and detectors can be installed.
• Space-saving design (40 cm wide)
• A high-performance electronic flow controller (AFC) enables setting column flowrate
precisely and easily.
• Easy to operate via an English language interface displayed on a large LCD screen
• Smart self-diagnostics function
• Equipped with compact high-sensitivity and high-stability detector
GC-2014
Features of GC-2010Plus
Product Information
The GC-2010Plus is a capillary gas chromatograph featuring the latest state-of-theart technology.
• An electronic flow controller (AFC) offers excellent reproducibility by precisely controlling capillary gas flow at high pressures and flowrate levels required for fast
analysis.
• High-performance oven enables rapid heating and rapid cooling.
• Multiple sample injection units and detectors can be installed.
• Electronic flow controller allows setting column and detector flowrates easily.
• Equipped with compact high-sensitivity and high-stability detector
• Easy to operate via an English language interface displayed on a large LCD screen
• Smart self-diagnostics function
GC-2010Plus
Features of GCsolution
The GC workstation software “GCsolution” offers extensive functionality, yet is also
especially easy to operate. With intuitive operations, assistant bar and data explorer
features for providing data management functions, Word-like report functions,
and extensive GLP/GMP support functions, the software helps improve analytical
productivity. It allows controlling GC-2010 series models, such as the 2014.
GCsolution
44
n
Scanning Probe Microscope
Product Information
Product Evaluation
Scanning probe microscope (SPM) is a generic term for microscopes that scan sample surfaces with a microscopic probe to
observe their three-dimensional shape or surface properties at high magnifications. SPMs are used for applications such as to
observe the surface of plastic materials and products, or analyze their structure or inspect foreign matter. SPMs allow observing
three-dimensional surfaces with higher resolution and magnification than optical or electron microscopes. Even insulating
samples can be observed directly without modification. SPMs can be used to observe not only shape, but also to measure other
physical properties, such as electrical properties, viscoelasticity, and hardness.
Evaluation of
Raw Materials
Shimadzu Scanning Probe Microscope
Features of the SPM-9700
• High Stability and High Throughput
Product Evaluation
A head-slide mechanism allows sliding the entire optical lever system as an
integrated unit. This means samples can be replaced without removing the cantilever
and samples can be approached completely automatically, regardless of sample
thickness. It also contributes to high throughput by allowing access to samples even
during observation. Due to the laser light shining continuously even during sample
replacement, stability is higher, which provides clearer and higher quality images.
Evaluation of
Plastic Materials
Analysis of Plastic Samples Using an SPM
SPM-9700
• Functionality and Expandability Satisfies a Wide Range of Requirements
Standard functionality includes contact, dynamic, phase, lateral force, and force
modulation functions. In addition, functionality can be expanded to include
electrical current, magnetic force, surface potential, nano-indentation, or nanothermal analysis functions.
Product Information
• Ease of Operation Minimizes Distraction Throughout Steps from Observation
to Analysis
Easy-to-understand graphical user interfaces (GUI) are used for functions, such as
the guidance function and navigation function.
• Wide Variety of 3D Rendering Functions Using Mouse Operations
3D operations, such as rotating or smoothing, can be performed freely in real time.
It includes texture and 3D cross sectional profile analysis functions that can be
overlaid on height or physical property information.
Environment Controlled SPM
Features of the WET-SPM Series
By adding an environment controlled chamber, SPM-9700 series SPMs can be
upgraded to a WET-SPM series system. Since the chamber is a glove box system,
samples can be prepared (such as cleaving, rinsing, heating, and drying) or replaced
within controlled environmental conditions. Depending on the combination of
functions and sample operations, some of the environmental controls available
include the following.
•
•
•
•
•
•
WET-SPM Series
Specific gas environment control
Environmental temperature and humidity control
Sample heating and cooling
Blowing gas on samples
Shining light on samples
Application of stress on samples
45
Product Information
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Product Evaluation
Infrared Microscope System
Analysis of Plastic Samples Using an Infrared Microscope System
Many different types of information can be obtained from plastic samples using FTIR, such as information for checking raw
materials, the composition of plastic pellets or powders, bonding modes, isotope ratios, copolymer composition ratios, molecular
orientation, and information for analyzing foreign matter or other defects. Using an infrared microscope system, which
combines an FTIR spectrophotometer with an infrared microscope, allows obtaining qualitative information about micro areas
easily. The AIM View software enables performing all operations via the computer, such as setting the aperture and moving the
automatic X-Y stage, and successfully transforms the system into one that is capable of performing highly sensitive infrared
microscopic measurements with ease. Using the AIM-MAP mapping software allows capturing the material distribution status of
sample surfaces.
Features of the AIM-8800 Infrared Microscope System
• AIM View provides total control.
Microscope operations are completely automated using automatic aperture, X-Y stage, and focus functions. Therefore, sample
points, background points, and aperture size settings are remembered and can be reproduced whenever necessary. In addition,
an auto-centering function was added, which centers the window image at any arbitrary point that is double-clicked.
Product Evaluation
• Enables highly sensitive measurements.
Optics have been designed for samples with sides of 50 µm square or less. This is especially beneficial for measuring micro-sized
samples and provides higher sensitivity with an S/N ratio of 2600:1 (given a 50 µm square sample and type 1 MCT detector).
• Uses a high-sensitivity maintenance-free MCT detector.
A glass dewar type MCT detector is used, which does not require maintenance. Metal dewar type MCT detectors used by other
manufacturers must be re-evacuated every year or two.
Product Information
• A wide variety of optional products are available.
A variety of optional products, such as an ATR, objective mirrors, diamond cell, and micro manipulator, are available for accommodating a wide variety of applications.
• Use of the optional AIM-MAP mapping software allows capturing the material distribution status of sample surfaces.
Infrared Microscope System
IRPrestige-21 + AIM-8800
46
n
UV-VIS Infrared Spectrophotometer
Product Information
Product Evaluation
Ultraviolet-visible (near-infrared) spectrophotometers are very effective in evaluating plastics. They are especially useful for
evaluating the physical properties of plastic samples, such as when using an integrating sphere to measure transmittance,
reflectance, and haze, or by using color measurement software to measure color. They are also widely used to analyze
hexavalent chromium for compliance with RoHS or other regulatory requirements.
Evaluation of
Plastic Materials
Analysis of Plastic Samples Using UV Light
Features of SolidSpec-3700 (DUV) UV-VIS-NIR Spectrophotometers
Evaluation of
Raw Materials
• World's first UV-VIS-NIR spectrophotometer equipped with three detectors
• Measures deep-UV regions below 190 nm.
• Extra large sample compartment accommodates a wider variety of samples.
Product Evaluation
This is the world's first UV-VIS-NIR spectrophotometer to include three detectors. It is
ideal for measuring samples in the electrical and optical fields, such as anti-reflection
films, high-reflection mirrors, or functionally engineered films. By purging the system
with nitrogen gas, DUV models allow measurements in the deep-UV region.
A 3-dimensional optical system and extra large sample compartment allow measuring
large samples up to 700 × 560 mm and using an automatic X-Y stage (option) allows
automatically measuring multiple points on samples up to 300 × 300 mm.
SolidSpec-3700 (DUV)
Features of UV-2600/UV-2700 UV-VIS Spectrophotometers
The key feature of the UV-2600 is its wavelength measurement range. If an
ISR-2600Plus integrating sphere attachment is used, this system can measure
wavelengths from 220 nm to 1400 nm, which includes the near-infrared region,
extending its usefulness to an even wider range of applications. It can also be used
to measure solar cell materials and various types of glass samples. The UV-2700 can
achieve ultra-low stray light levels, with transmittance of 0.000001% (1/10 of a
billionth) and an absorbance range up to 8. Due to a dramatically higher precision
level, it is able to measure higher absorbance levels. This means highly concentrated
samples can be measured without pretreatment, which not only saves the time and
trouble of diluting samples, but also means it can be used to evaluate transmission
characteristics of polarizing films.
Product Information
• UV-2600: Single-monochromator model that offers a wide wavelength range and low noise
• UV-2700: Double-monochromator model that achieves ultra-low stray light levels
UV-2600/2700
Features of UVmini-1240 UV-VIS Spectrophotometers
• Compact design equivalent to size of A3 (297×420 mm) paper
• Easy to operate
• Measures wavelengths from 190 to 1100 nm.
The UVmini-1240 is capable of everything from simple colorimetric analysis to
sophisticated quantitative analysis and spectral measurements. All systems are
equipped standard with photometric, spectral, and quantitative measurement modes.
The compact A3 (297×420 mm) size saves space. Measurement results are displayed
on a 6-inch backlit LCD screen. Functionality for printing and output via an RS-232C
cable is included standard, which also allows printing a copy of screen contents to
a standard printer. Measurement results can be saved in internal memory or saved
in an optional data pack. Furthermore, UV Data Manager software (option) is also
available as a tool for loading data to the computer. Of course, with a wide selection
of available accessories, it can accommodate a diverse variety of applications.
UVmini-1240
47
Product Information
Evaluation of
Plastic Materials
Product Evaluation
Autograph
Evaluation of Mechanical Characteristics of Plastic Products Using Autograph
Due to their various mechanical characteristics, plastic products are used in an extraordinarily broad range of applications.
The most fundamental of mechanical characteristics is the strength necessary to ensure safety and reliability. The Autograph
series are also able to obtain information about many other aspects of products, such as elongation, displacement, and energy,
providing important information not only for controlling product quality, but also for developing new products.
Evaluation of
Raw Materials
Features of Autograph AG-X Series
▪ New design introduces a new era (loading frame and software)
The loading frame is designed with a sophisticated look to match laboratories
and an interface located on the front side for easier operability. The specialized
TRAPEZIUM X software features a new design that provides a perfect balance
between aesthetics and ease-of-operation.
▪ Stress and strain controls enable precision control
Product Evaluation
An autotuning function enables highly precise stress or strain control by simply
setting the testing speed, which eliminates the need to specify gain or other
parameter settings.Eight times more precise control resolution than previous
Shimadzu models ensures accurate control even at low speeds (perfect for
constant force control used to test films, rubbers, and fibers).
Autograph AG-X Series
▪ World's first to offer test force measurement precision to 1/1000
Product Information
The high-precision model offers measurement precision to within 0.5 % of the
indicated value over a wide range of applied loads, from 1/1 to 1/1000 of the
load cell capacity rating. This means load cells can be exchanged less often (details
depend on individual specifications).
▪ Ultra fast 0.2 msec sampling
During tests, measurement data can be acquired at sampling intervals as short
as 0.2 msec. This allows evaluating composite materials and performing highly
reliable measurements.
Specialized TRAPEZIUM X Software
▪ Self-check function keeps machine in optimal condition
The system status can be confirmed via the self-check function that runs automatically during startup or via the checking
functions that periodically run in a guidance format. The function that automatically notifies users of scheduled maintenance
is also able to keep track of validation dates and other information.
▪ Easily accommodates a variety of tests and improves test efficiency
A color touch panel display (option) allows specifying test parameter settings and running tests without a computer. It allows
displaying graphs during testing. Test parameter settings configured on the computer can be saved in USB memory, which
can then be used to perform tests. By saving test results automatically in USB memory and plugging that into the computer,
identical operations can be performed as when the computer is connected to the testing machine.
A Variety of Accessories Expand the Range of Applications
T h e A u t o g r a p h s e r i e s o ff e r s a n e x t e n s i v e s e l e c t i o n o f
accessories available for accommodating a wide range
of specimens and objectives. By selecting the optimal
accessories, such as loading jigs (grips and so on) that apply
the desired force to specimens, sensors that accurately
measure the displacement (such as elongation and deflection)
at specific locations, or atmosphere conditioning systems for
controlling the testing environment (such as temperature and
humidity), it is possible to configure systems optimized for
testing objectives.
Accessory examples
Thermostatic Chamber
48
Grips and Extensometer
n
Servopulser/Hydroshot
Product Information
Product Evaluation
To ensure reliability and safety under actual usage conditions, it is essential to understand and control not only basic static
strength, but also endurance (with respected to repeated stresses) and impact resistance characteristics. Servopulser fatigue
testing machines are able to efficiently apply precise repeated loads and reproduce various load waveforms experienced in actual
operation. Hydroshot high-speed impact testing machines can obtain failure characteristics data at speeds up to 20 m/sec.
Evaluation of
Raw Materials
Features of Servopulser
Evaluation of
Plastic Materials
Evaluation of Endurance and Impact Characteristics of Plastic Products Using
Servopulser/Hydroshot Testing Machines
• Loading capacity and loading mode selectable based on a test object
The hydraulic configuration is able to repeatedly apply large loads (up to 300 kN for
standard models) at high speed, which allows fatigue testing of almost any material
or mechanical part.
Product Evaluation
• Stress and strain controls enable precision control
Closed loop servo control enables reproducing loading waveforms accurately
and faithfully. With fundamental cycle waveforms as well as random and actual
operating load waveforms, simulation testing can be supported as well.
• Select from two available controllers
Select either the compact 4830 controller or the 4890 controller, which allows
using various data analysis modes. Connected to a computer, these allow seamlessly
performing all testing tasks via the computer, including configuring test parameter
settings, executing tests, and analyzing data.
Tabletop Servopulser (Hydraulic)
Product Information
• Extensive assortment of accessories
A wide assortment of accessories, such as test jigs (grips and so on), various external
sensors (to measure elongation and displacement), and environment control devices
(such as high/low temperature and high/low humidity), are available for configuring
an evaluation system that is optimized for given objectives.
• Electromagnetic and pneumatic systems are also available
For smaller loading capacity requirements, electromagnetic (Micro-Servo) and pneumatic
(Air-Servo) systems are also available as an alternative to hydraulic actuation. These models
offer lower environmental impact and are ideal for fields such as electronics.
• Also capable of multi-axis testing
Multiaxial systems (maximum 4 axes) can also be configured, which are ideal for
testing the endurance of actual parts, such as automobile components. Features
include an interaxial interference correction function based on transfer functions
and a resonant frequency tracking function.
4830 Controller and Operation Computer
Features of Hydroshot
• Hydraulic actuation enables accurate speed control
Hydroshot testing machines feature accurate flowrate control of pressurized hydraulic oil
and enable high capacities (maximum 10 kN) and high loading speeds (maximum 20 m/sec).
• Two types available – puncture or tension
The product line includes two types, the HITS-P10 model for puncture testing and
the HITS-T10 for tensile testing.
• Accurate measurements
A test force detector (load cell) designed to minimize reflection of vibration and stress
waveforms during high-speed loading and a crosshead displacement detector ensure
accurate data acquisition. A non-contact type chuck displacement gauge (for tensile testing)
is effective in measuring the amount of deformation in the area closest to the specimen.
• Extensive assortment of accessories
An extensive line of accessories are available to configure the optimal system, such as
various light-weight grips best-suited to the given specimen, approach jigs for tensile testing,
and thermostatic chambers to control the temperature of the testing atmosphere.
• Specialized operating software
All machines include software designed specifically for operating Hydroshot
machines. This ensures that all operations, from setting test parameters to organizing
data can be performed as simply and safely as possible.
Hydroshot HITS-T10 High-Speed Impact
(Tensile) Testing Machine
49
Product Information
Industrial X-Ray Inspection System
Observing the Interior of Plastic Products Using Industrial X-Ray Inspection
(Fluoroscopy/CT) Systems
Light and strong fiber reinforced plastics (FRP) are not only used in construction materials and sport equipment, but also used to
reduce energy consumption in automotive and aerospace industries. Functionally engineered polymer materials are used in nextgeneration batteries (such as fuel cells, solar cells, and Li-ion batteries), which have been attracting significant interest. In many
cases, these materials have increasingly complicated structures with characteristics that cannot be adequately evaluated using a
conventional singular approach of evaluating physical properties. Therefore, there has been a growing interest in 3-dimensional
data analysis methods. This example offers a method of analysis that uses a CT system to observe samples with X-rays.
Features of Industrial X-Ray Inspection (Fluoroscopy/CT) Systems
• Obtains ultra high-speed and high-resolution (micron level) CT images (cross sections).
• A line of three models - small, medium and large, allows selecting the best model for the intended application.
• The user interface allows even first-time users to operate the system easily. For example, the manipulator can be operated by simply
moving the mouse pointer on the fluoroscopy screen. In addition, a large opening allows loading even bulky samples with ease.
• Since no troublesome calibration operations are required, high-quality images can be obtained easily by anyone.
• Image acquisition can be started immediately while irradiating the sample, by simply deciding the magnification rate.
• System functionality can be expanded to include 3D dimensional measurement or various other optional (software) analytical functions.
• Systems can be used to measure a wide variety of samples, from composite materials, electrical/electronic devices/parts, mechanical parts, and plant and biological samples.
Product Information
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Product Evaluation
inspeXio SMX-90CT Benchtop Microfocus X-Ray CT System
inspeXio SMX-225CT Microfocus X-Ray CT System
Operating Principle of X-Ray CT Scanning
50
n
Atomic Absorption Spectrophotometer
Product Information
Product Evaluation
Atomic absorption spectrophotometers are used to analyze trace hazardous inorganic elements in plastic, in particular cadmium,
lead, and arsenic. If there are only a few target elements being measured, this allows measuring them efficiently at low cost.
Plastic samples are normally pretreated by adding acid to thermally decompose them before measuring. Some plastics can
be simply dissolved in an organic solvent before measurement. If target elements are present in higher concentrations, flame
atomization is used, which allows a shorter measurement time. However, when measuring trace quantities, selecting the furnace
measurement method allows analyzing the samples more efficiently.
Evaluation of
Raw Materials
Shimadzu Atomic Absorption Spectrophotometers
Features of AA-7000
Evaluation of
Plastic Materials
Analysis of Plastic Samples Using an AA Spectrophotometer
• System configurations advancing together with needs
Compact dedicated flame models can be converted to a dual atomizer system
that can automatically switch between flame/furnace modes. Dedicated furnace
models are also available.
• Advance safety technology
The system features many safety mechanisms, such as the world's first automatic
flame extinction via flame vibration sensor, multimode automatic gas leak check,
and use of flame resistant materials.
Product Evaluation
• Fully featured flame analysis
A newly developed 3-dimensional double-beam optical system and sturdy
hardware provide outstanding stability.
AA-7000 Dual Atomizer System
Product Information
• World-class high-sensitivity furnace
Lower limit of detection performance was improved by reducing noise with
state-of-the-art optics. Stability is also improved by digital temperature control
and digital gas control.
• Dual atomizer system
(automatic flame/furnace mode switching function)
Automatically switches the atomization unit by software operation. A newly
developed drive mechanism cuts the switchover time in half from the previous model.
• Multifunctional autosampler
A single autosampler supports both flame and furnace analysis.
Commercial pipette tips can be used for nozzles in the furnace mode.
A rinse port in the overflow mechanism ensures nozzles are rinsed properly.
WizAArd High Functionality Software
• Features easy to understand and use WizAArd software
Extensive display features and highly flexible settings
Supports system control and precision control and includes hardware validation
software.
AA-7000G Furnace Model
AA-7000 Flame Model
51
Product Information
Product Evaluation
Evaluation of
Raw Materials
Evaluation of
Plastic Materials
Product Evaluation
Multitype ICP Emission Spectrometer
Analysis of Plastic Samples Using an ICP Spectrometer
ICP emission spectrometers are used to analyze trace hazardous inorganic elements in plastic, in particular cadmium, lead,
and arsenic. Plastic samples are normally pretreated by adding acid and thermally decomposing before measuring. This system
enables simultaneously measuring multiple elements with high sensitivity and high precision. Furthermore, it also enables
qualitative analysis to confirm the presence of most inorganic elements in samples.
Shimadzu Multitype ICP Emission Spectrometers
Features of ICPE-9000
• High throughput
Uses an Echelle spectrometer capable of high-speed measurement and large highresolution CCD detector.
• Equipped with Mini Torch
The mini torch offers equivalent sensitivity to a standard torch, but consumes half
the argon gas. The vertical orientation minimizes contamination and clogging,
which is especially reassuring for concentrated samples.
• Vacuum spectrometer
This is the first ICP emission spectrometer with a semiconductor detector that
is equipped with a vacuum spectrometer. No high-purity gases are necessary
for purging. This not only reduces operating costs, but also provides superior
spectrometer stability.
ICPE-9000
Product Information
• Even the first sample is easy to analyze with ICPEsolution software
Includes qualitative database calibration functionality.
Method Development Assistant automatically prepares measurement parameters.
Includes Automatic Wavelength Selection System.
Method Diagnosis Assistant checks for causes of errors.
ICPEsolution High Functionality Software
Solution method
Example of Problem-Solving Using Method
Diagnosis Assistant
Example of Automatic Wavelength Selection System
52
n
Energy Dispersive X-Ray Fluorescence
Spectrometer
Product Information
Product Evaluation
When samples are irradiated with X-rays, they emit fluorescent X-rays that are characteristic of the elements contained in the
sample. EDX spectrometers enable measuring samples rapidly for controlling the content of various additives or for analyzing
sample impurities or defects. More recently, due to their convenience, they have become widely used for screening five elements
regulated by the RoHS directive and four elements regulated by the ELV directive.
Features of EDX-GP/LE Energy Dispersive X-Ray
Fluorescence Spectrometers
EDX-720
Product Evaluation
• Allows directly and non-destructively measuring various forms of metals, plastics, powders, liquids, and other materials. biological samples.
• Measurements require only specifying the target area by viewing the CCD camera
image (optional).
• Rapidly measures the five RoHS elements and four ELV elements. A specialized primary filter is also included standard.
• Also can be used for general material analysis, defect analysis, or coating thickness
analysis.
Evaluation of
Raw Materials
Features of EDX-720 Energy Dispersive X-Ray Fluorescence
Spectrometers
Evaluation of
Plastic Materials
Analysis of Plastic Samples Using an EDX Spectrometer
Sensitivity is higher than previous models!
Product Information
• Includes screening analysis software with simplified operations.
• Also can be used for halogen-free analysis by using a specialized filter to increase sensitivity.
• Features a large sample compartment.
• Equipped standard with sample observation function (CCD camera).
EDX-GP/LE
Create reports with a single click!
Screening Analysis Software
53
Solutions for Plastic Evaluation
Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its
affiliates, whether or not they are used with trademark symbol “TM” or “®”.
Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu
disclaims any proprietary interest in trademarks and trade names other than its own.
For Research Use Only. Not for use in diagnostic procedures.
The contents of this publication are provided to you “as is” without warranty of any kind, and are subject to change without notice. Shimadzu
does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication.
www.shimadzu.com/an/
© Shimadzu Corporation, 2013
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