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ICP - MS

Wahyu Wulan W
ICP MS

SAMPLE PREPARATION

METHOD VALIDATION
ICP - MS

Inductively Coupled Plasma merupakan teknis analisis untuk


indentifikasi logam dengan cara mengionisasi sampel kemudian
konsentrasinya diketahui menggunakan sebuah mass analyzer.

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Sample Introduction System
Nebulization
1 Bersama dengan gas Ar mengubah
sampel liquid menjadi aerosol

Desolvation
2 Mengubah aerosol menjadi partikel

Vaporization
3 Mengubah partikel menajdi molekul

Atomization
4 Mengubah molekul menjadi atom

Ionization
5 Mengubah atom menjadi ion

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Interface Region

Setelah ion diproduksi dalam plasma, kemudian


diarahkan ke spektrometer massa melalui daerah interface
pada keadaan vakum. Daerah antar muka ini terdiri dari dua
kerucut logam (biasanya nikel) yang disebut sampler cone
(1mm) dan skimmer cone (0,4mm), dimana ion dapat
melewati ke optik, untuk ditransfer ke dalam perangkat
pemisahan massa.

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Mass Analyzer

Sebagian besar ICP-MS menggunakan filter quadropole. Prinsip kerja filter qudropole adalah
sebagai filter massa dan hanya meneruskan ion-ion dengan rasio massa/muatan (m/z) tertentu. Ion
yang bukan dari m / z yang benar bertabrakan dengan batang atau keluar dari jalur di antara batang
dan akan dipompa keluar sistem 7
Detector

Fundamental purpose of the detector is to translate the number of ion striking the detector
into an electrical signal that can be measured and related to the number of atoms of that
element in the sample via the use of calibration standards
Uses a high negative voltage to attract positively charged ions
Most commonly used are discrete dynode detector

Ion striking Electron Striking next Amplification


active release surface of of signal
surface of detector
detector

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Interferences
TYPES MINIMIZED BY

Polyatomic Interference Optimization of nebulizer gas flow (1.5


40Ar, 35Cl, 75As 1.8 ml/min)
RF Power adjustment (500 800watt)
Sampling position within plasma

Cold plasma technique


Isobaric Interference
Collision or reaction cell
Fe dan Ni
HR Mass analyzer as double focusing
magnetic field sector

Matrix Interference
Use Internal standart

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ICP MS can be coupled with various separation techniques:
Liquid Chromatography : HPLC ICP MS
Capilarry Electrophoresis : CE ICP MS
Laser Ablation : LA ICP MS for surface
analysis and for materials
that are difficult to digest

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1. Multi elements analysis 1. Difficult to determine negative species
2. Wide elemental coverage (except: H, (Br, Cl)
noble gases, and F) 2. Dissolved solids/matrix effects
3. High sensitivity 3. High capital cost
4. Good matrix tolerance (handle acids, 4. Required skilled
solvent, matrix up to 0.5%)

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Sample Preparation
Acceptable Sample Types
1.Whole Blood
2.Serum
3.Urine
4.Hair
5.Nails
6.Liver Tissue
7.Plasenta
90% of problems with ICP-MS relate to Sample Introduction System

1. carry over
2. poor precision
3. poor linearity
4. istd instability
5. plasma igniton problems
things to solve
Check :

1. gas fitting, tubing, and connectors in good condition


2. peri pump is in good condition
3. nebulizer is clean
4. limit the maximum concentration exposed to the system
5. keep instrument clean
Mercury Memory Effect
a significant and difficult problem to overcome when using ICP-MS for
mercury analysis is the severe memory effect that is obvious for
mercury in the instrument, which has been attributed to a combination
of sample introduction, spray chamber and nebulisation effects.

non-linear calibration graphs


long washout times
decreasing sensitivity and signals dependent on the matrix.

11/2/2017
Eliminates Hg memory effec
A number of different reagents such as
Gold
combination of triton X-100/ammonia/ethylenedian netetracetic
acid (EDTA)
nitric acid
hydrobromic acid
2-mercaptoethanol (2-ME)

11/2/2017
Procedure
1. Mercury standard solutions (10 ppb, 20 ppb, 50 ppb) were
introduced into ICP-MS for 5 minutes
2. Then the above cleaning reagents were introduced into the
system for the same time (3 min) to wash mercury out.
3. Every time before applying a new washing reagent, the
accumulated mercury was washed out using 2-ME (0.1 %), which
was found more faster in eliminating the accumulated mercury
than the commonly used nitric acid (2 %) to make sure the same
initial status of mercury load in the ICP-MS system.

11/2/2017
Result

mercury concentration (10 ppb), all above reagents could wash mercury out
within 3 minutes.
higher mercury concentration like 20 and 50 ppb:
- HNO3 (2 %) could only wash about 21 % mercury out
- The inorganic sulfide and sulfate showed higher efficiency as 30%.
- EDTA and its sodium salts (0.1 %), gold, and Hydrobromic acid (0.1 %)
were of much higher efficiency as 75%, 73%, 68% and 70%, relatively. This
may be attributed to the chelating effect of EDTA, Au and Br-
- The most efficient reagents were the mercaptol reagents like 2-ME
(0.05%), cysteine (0.1%) and DTT (0.1%), which all washed the mercury out
in 3 minutes owing to the high affinity of -SH to mercury.

11/2/2017
VALIDASI METODE

1. Uji Presisi
2. Uji Akurasi
3. Uji Spesifisitas
4. Uji Linearitas
5. LoD, LoQ
6. Uji Recovery

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Uji Presisi
Dinyatakan sebagai SD/RSD dengan kriteria <6%

Uji Spesifisitas
Suatu metode adalah kemampuan suatu metode yang hanya
mengukur zat tertentu saja secara cermat dan seksama dengan
adanya komponen lain yang mungkin ada dalam matriks sampel

11/2/2017
Conclusion

ICP MS is an ideal choice for the laboratory


that is seeking the lowest possible detection limits
and the highest level of productivity.

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THANKS
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