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LAAN-E-MS-E030

GCMS
Gas Chromatograph Mass Spectrometer

Analysis of Chelate Compounds


Through Direct Sample Introduction
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Chelate compounds are generally refractory compounds composed of ligands and metal ions. Therefore, they are
difficult to measure with gas chromatographs. To obtain an electron ionization mass spectrum of refractory
compounds requires a pure sample that should be introduced by direct introduction (DI).
In this Application Datasheet, a chelate with ring-shaped phthalocynanine ligands, which are cross linked to four
phthalic imides by nitrogen atoms, is measured using the DI method.

Instrument

The direct introduction probe is shown in Figure 1 and a diagram of the principle is shown in Figure 2. The sample is
dissolved in a solvent and inserted into a glass sample cup placed on the end of the probe. After drying the solvent,
the probe is inserted into the mass spectrometer (MS) ion box. The sample is introduced to the ion source box by
heating the sample cup with a heater, and then ionized by electrons emitted from a filament.

Filament

Direct introduction probe Ion source box

O-ring
Heater
M+M-)

Sample cup

Fig. 1: Direct Introduction Probe (lower left) and Fig. 2: Principle Behind Direct Sample
Inserting the Probe into the MS Unit Introduction

Analysis Conditions
Table 1: Analysis Conditions

GC-MS GCMS-QP2010 Series


[DI] [MS]
Sample quantity: 1,000 ng Interface temperature : 250
Injection mode: Direct Sample Introduction Measurement mode : Scan
DI temperature: Room temperature -> (80 C/min) -> 500 C (10 min) Mass range : m/z 50-600
Event time : 0.5 sec
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Results
Figure 3 shows mass spectra obtained from measuring (A) phthalocyanine, (B) tin-chelated phthalocyanine, and (C)
copper-chelated phthalocyanine by direct sample introduction. The structural formula for phthalocyanine is shown
on the upper right.
In the mass spectrum for (A) phthalocyanine, the m/z molecular ion was detected as the base peak. For tin-chelated
phthalocyanine, molecular ions corresponding to tin isotopes 116Sn, 118Sn, and 120Sn were detected at 628, 630,
and 632 (B-2), and an isotope pattern characteristic of tin was indicated. Similarly for copper, molecular ions
corresponding to 63Cu and 65Cu isotopes were detected at m/z 575 and 577.

%
514
100 A
90
80
70 N N
N
60 H
50 N N
H
40 103 129 N
30 N N
20 257
10 76 156 193 230 288 383
0
100 150 200 250 300 350 400 450 500 550
%
%
100 632 150.0
90
B-1 B-2
125.0
80
70 632
100.0
60 630
50 75.0
40
316 50.0
30 124
20 25.0 636
10 624
64 101 146 188 248 575
0.0
0
100 200 300 400 500 600 625.0 650.0
%
100 575 %
C-1 200
90 C-2
80
70 150
60 575
50 100
40
287 577
30 50
20 128 191
63
10 81 0
154
0 550.0 575.0 600.0
50 100 150 200 250 300 350 400 450 500 550 600

Summary

The direct sample introduction method (DI) enables the mass spectra of chelate and other refractory compounds to be
obtained quickly and easily.

For Research Use Only. Not for use in diagnostic procedures.


Shimadzu Corporation (Shimadzu) reserves all rights including copyright in this
publication. Shimadzu does not assume any responsibility or liability for any damage,
whether direct or indirect, relating to, or arising out of the use of this publication. This
publication is based upon the information available to Shimadzu on or before the date of
publication, and subject to change without notice.
First Edition: October 2011

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