Basic & Fundamental

Gas Chromatography
Mass Spectrometry (GCMS)

Juwita Ayu Lestari

Customer Support Engineer
Basic & Fundamental
Gas Chromatography

Mass Spectrometry Gas Chomatography

1. Basic
GC Industri
Teknik menguapkan campuran sampel • ilmu forensic
menjadi senyawa gas dan memisahkannya • Makanan
berdasarkan titik didih pada padatan atau • pengujian lingkungan
• Farmasi
cairan pendukung berpori.
• Petrokimia
• berat molekul rendah • Pestisida
• mudah menguap • Fragrance
GAS CHROMATOGRAPHY
1. Instrumentation – Carrier Gas

Kemurnian dan aliran gas pembawa sangat

penting untuk mencapai pemisahan yang baik
dan kromatogram yang dapat direproduksi.

• inert
• tidak mengganggu pemisahan dan pendeteksian
 2. Instrumentation – Injection Port

• Syringe
• Suhu Tinggi (150-250oC, maximum 450oC)
• Glass Insert

• Liquid samples: Approx. 1 to 2 µL

Note:
- GC use yellow septum
- GCMS use blue, red or green septum
 2. Instrumentation – Injection Port
Glass Insert
• Glass insert SPLIT bisa

menggunakan split & splitless

mode
• Glass insert SPLITLESS hanya

menggunakan splitless mode

Split : konsentrasi tinggi, muatan matriks tinggi, atau

situasi di mana analit dengan titik didih lebih rendah
ditargetkan.
Splitless : sangat ideal untuk trace analysis sampel
dengan konsentrasi analit yang sangat rendah.
Direct : Thermally Labil, volatilitas rendah dan/atau
reactive analysis
3. Instrumentation – Column Oven

1. Isothermal

2. Temperature program
4. Instrumentation - Column

• capillary column
fused silica glass tube
• dilapisi dengan fasa cair atau bahan
penyerap atau mempunyai lapisan
ikatan kimia.

Note:
• For GCMS use inner Diameter 0.25 mm,
Length 5 to 100 m (most commonly 30 m)
Basic of GC

GC Separation principle.
The compound in red have a stronger interaction with the stationary phases and
gets retained long separation of the mixture where the red compound
has a longer retention time than the blue compound (RT red > RT blue)
 Basic of GC

and the part where a component

is detected is called a peak

The part at
which nothing
is detected is The vertical axis shows
called the
the signal intensity
baseline

The horizontal axis shows the time until the component

reaches the detector, called retention time
Basic & Fundamental
Gas Chromatography
Mass Spectrometry (GCMS)
Introduction to GCMS
Detektor MS
• membantu mengidentifikasi jumlah
(kuantitatif) dan jenis senyawa (kualitatif)
dalam sampel
• Mengukur berat molekul atau atom analit

Hasil:
• Berat molekul
• Struktur molekul Identifikasi yang tidak diketahui
dalam sampel
Introduction to GCMS

Samples that can be analyzed by gcms

• Volatile compound
• Stable compound in high temperature
• Compound who having molecular weigh <1000
Mass Spectra
Instrumentation of GCMS
 1. Instrumentation of GCMS - Interface

conductivity tube
• Interface

High thermal
• Vacuum Pump

Heater
• Heater

suhu Interface dijaga tetap tinggi (misalnya From

GC
To ion source
50-350 C) untuk memastikan bahwa senyawa
yang dielusi dari GC tetap berada dalam fase
gas dan hanya senyawa volatil yang masuk ke
MS.

Nut column
To vacuum pump
1. Instrumentation of GCMS - Interface
Mengapa MS memerlukan vakum tinggi?

• Jika MS dalam vakum rendah (ada gas lain : He, udara, air)
• Ion target (yang dibuat di sumber ion) dapat bertabrakan dengan gas-gas ini dalam
perjalanan menuju detektor

Vacuum Pressure: 10-3 to 10-4 Pa

3. Instrumentation of GCMS – Turbomolecular pump
Two pump are generally used in a differential-pumped GCMS

1. The turbomolecular pump (TMP) 2. rotary-pump

pompa cadangan untuk mengeluarkan gas buang dari
pompa utama yang menghilangkan gas pembawa dari GC dan pompa utama.
mencegah hidrokarbon
4. Instrumentation of GCMS – Ion Source

In GCMS ion source Ion

(mengubah molekul gas) bermuatan

Melalui electron bombardment pada

collision/reaction
Instrumentation of GCMS – Ion Source
4. Instrumentation of GCMS – Ion Source
Electron Ionization

Ion source Filament 1

Emission Current Molecular Ion
70 eV

Thermal e-
e-
M M+
Electrons
Fragment Ions To
M Quadrupole
A+
Filament 2 M+*
(Electron trap)
B-

Fragmentation

Due to this reason, EI is commonly referred to as hard ionization

Molecular and Fragments Ion
Unknown Identification GC-FID
Unknown Identification GC-MS
Instrumentation of GCMS
Detector

Ions that exit the mass analyzer are detected and the
abundance or intensities are measured

Bench-top GC-MS usually use electron multiplier

detector
GC-MS Analysis Modes

SCAN
SCANMODE
MODE Qualitative and Quantitative Analysis

- For identification of compounds using mass spectrum

(qualitative analysis), usually by library search.
- Quantitative analysis
- For determination of SIM mode parameters

SIM
SIMMODE
MODE Quantitative Analysis

- Higher sensitivity, because SIM sensitivity is tens to hundred times

higher than that of SCAN mode
- MS set to measure only specified masses

31
3.1.1 Scan Mode

Advantages Scan Chromatogram

• Qualitative information from mass spectra
• Information about non-target components Qualitative analysis
Quantitative analysis
Disadvantage
• Lower sensitivity than SIM mode

Scan Mass Spectrum

Time
0.3 sec 0.3 sec
Event Time

32
Analysis in GCMS

Qualitative
Using Library
3.1.3 SIM Mode
Advantages
• Higher sensitivity than SCAN mode SIM Chromatogram
Disadvantages
• Complete mass spectra not obtained Quantitative analysis
• Only information about target components

SIM Mass Spectrum

0.3 sec 0.3 sec 0.3 sec

Event Time
0.3 sec Time
Library search not possible

34
Analysis in GCMS

m/z yang terdeteksi

Target Ion
Untuk Perhitungan

Reference Ion
Untuk Konfirmasi
Analysis in GCMS

Quantitative
Using Standard
Auto Tuning

Auto tuning should be performed at least 2 hours after:

- starting up the instrument
Auto Tuning
Inten.(x100)

10.0 69 F F
F F F F
F F
F F F F
F F
7.5 F N F
219 F F
F F
F F
5.0
F F
131
F F
2.5 F

100 264
414 502
31 169 246 376 466 614
0.0 314
100 200 300 400 500 600 m/z

PFTBA = Perfluorotributylamine (MW = 671)

Auto Tuning
Items to check:
- Intensity of m/z 28 relative to intensity of m/z 18
• Possibility of vacuum leak if intensity of m/z 28 is higher
than intensity of m/z 18
- Detector gain is 2 kV or less
• If the value is greater than 2 kV, detector replacement or
other maintenance is required
Thank you