TUGAS KIMIA ANALITIK III
Oleh
KHAERUL HATTA
( 105 05 092 )
RIZKI ANSHARI
( 105 05 093 )
ASTUTI TRIJAYANTI
( 105 05 094 )
HUMAILA RIZQI
( 105 05 096 )
TRIWIDIANSYAH
( 105 05 097 )
WERDI ISNA RETNOWATI
( 105 05 098 )
PROGRAM STUDI KIMIA
FAKULTAS MATEMATIKA DAN ILMU PENGETAHUAN ALAM
INSTITUT TEKNOLOGI BANDUNG
2007
TUGAS KIMIA ANALITIK
AA-6300
Next Generation Double Beam Atomic Absorption
Spectrophotometer
(SHIMADZU)
Atomic Absorption for the New Century
Features
High-throughput Dynamic Beam Management System
 Ensures long-term stability with low noise level
 Provides the highest level of sensitivity for trace-level analysis (Direct determination  Flame: Pb, 0.1ppm; Furnace: Pb, 0.3ppb)
Dual-Detector System with Dual Background-Correction Function
 Ensures maximum sensitivity and accurate background correction at all wavelengths
 Easy selection process provides optimum method for meeting analysis objectives
Burner Height and Gas Flow Rates are Automatically Set for Each Element and Matrix
 Ensures maximum sensitivity and superior detection limits
 Enables continuous measurement
WizAArd Software - A Match for this Electronic Records Era
The newly developed "WizAArd" (Windows-based 32bit) software is much easier to understand and use, with a
parameter editing function that enables conditions to be changed rapidly and comprehensive data processing
functions. It provides a high level of electronic records security functions for compliance purposes:





Manage user login ID names and passwords
Manage authority restrictions according to user level
Electronic signatures and audit trail functions have been equipped as standard
QA/QC functionality as required by the U.S. Environmental Protection Agency (EPA) has been improved
Hardware validation software is also standard.
Switch Smoothly Between Flame and Furnace - Without Tools
Simply remove the burner head and put in place the furnace section.
A single autosampler can be used for both flame and furnace, which negates the need to prepare the
autosampler for each analysis method.
Comprehensive Flame Analysis
Highly Sensitive and Stable Flame Analysis
The High-Throughput Dynamic Beam Manager System developed uniquely for the AA-6300 automatically sets
the photometric system to optical double beam for flame measurement, and to electrical double beam for
furnace measurement. Furthermore, the optical system has been designed to produce its maximum
performance in each of the measurement methods through the optimal adjustment of the light beam, highspeed operation digital filter, and employment of optical components.
Flame Analysis under Optimal Conditions at All Times
The AA-6300 conducts measurements by automatically setting the optimal conditions for not just the gas flow
rates, but also for the burner height for each element at all times.
Detailed methods - including the burner height - can be saved in files as measurement conditions, making it
possible for anyone to conduct optimal measurements at any time.
Safe Flame Measurement
The following safety mechanisms have been incorporated.
 Safe ignition/extinction sequence
 Flashback prevention through the gas pressure monitor
 Prevention of raw gas release when the flame dies out
 Burner misuse prevention
 Automatic flame extinction in a power failure
 Safety inspection support provided by software, and a self-diagnostics function that determines whether the
system safety mechanisms are in working order
Comprehensive Furnace Analysis
Highly Sensitive and Stable Furnace Measurement
Unique control of the gas flow inside the graphite tube at atomization (Patent 2067563) ensures high sensitivity
measurement - among the best in the world. Combining a high-sensitivity optical sensor with a digital
temperature control system enables temperature control with a high degree of precision over the entire
temperature region from drying to atomization. By employing the electronic controller, the flow rate of the inner
gas can be controlled precisely in 0.01L/Min units.
Furnace Analysis under Optimal Conditions at All Times
With a sophisticated autosampler, a maximum of 4 reagents (such as the diluent, standard solution, sample,
matrix modifier) can at first be mixed and then injected (without mixing as well).
The system can be set to automatically dilute and repeat the measurement if the calibration curve
concentration is exceeded.
Safe Furnace Mechanisms




Cooling water flow rate monitor
(Ar) gas pressure monitor
Over-current prevention device (double checked with the breaker and the optical sensor)
Furnace block cooling check
Specifications
AA-6300
Wavelength range
185 to 900 nm
Automated wavelength selection
Mounting
Aberration-corrected Czerny-Turner mounting, Number of grating
groove:1800 lines/mm, Forcal length: 298mm
Bandwidth
0.2 0.7 0.7(Low) nm (4 step automatic switching)
Detector
Photomultiplier (short wavelengths), semiconductor (long wavelength)
No. of lamps mounted
6 lamps, 2 user-selected lamps can be illuminated at the same time
(1 for measurement, 1 warming up for next measurement)
Photometric Mode
Flame: Optical double beam. Furnace: Electrical double beam
Background Correction
High-speed self-reversal method (BGC-SR), high-speed deuterium lamp
method (BGC-D2)
Lamp Mode
Emission, Non-BGC, BGC-D2
Burner Type
Air-cooled premix type
Burner Head
Made of titanium, 10cm slot (the 5cm slot for high temperature flames is
optional)
Nebulizer
Pt-lr capillary with teflon orifice and ceramic impact bead (Hydrofluoric
acids can be used)
Chamber
Polypropylene
Positioning Control
Automatic search for the optimal burner height, automatic adjustment of
vertical position, manual adjustment of back and forth position
Gas Control - Flow Control
Unit
Fuel gas, support gas, automatic flow rate setting (0.1L/min step),
automatic search for the optimal gas flow rate
Safety Measures
Safe ignition/extinction sequence
Automatic extinction in a power failure
Flashback prevention through gas pressuring monitoring
Burner misuse prevention
Prevention of raw gas release when the flame dies out
Ignition
Push ignite button
Software
Software based on Microsoft WindowsTM
Dimensions & Weight
835 (W) x 460 (H) x 545 (D) mm, 70 kg (not including the flue, protruding
parts)
Power Requirements
AC100V±10% (no sudden voltage fluctuations)
230VA, 50/60HZ
Ambient Temperature and
humidity range
Temperature: 10 ~ 35°C
Humidity: 20% ~ 80% (less than 70% when temperature is greater than
30°C)
Part Number:
Description:
BUCK 205AAS
Atomic Absorption Spectrophotometer
Detailed Product Information
The 205 Advantage
The Buck Scientific 205 AAS uses a unique burner system to get more sample to the flame, which results in more signal
and better sensitivity. We use an impact bead nebulizer to get an efficient generation of a fine aerosol of sample solution.
The short path spray chamber permits difficult solutions containing organics or high dissolved solids to be aspirated with
superb precision and minimal instabilities. To take advantage of this enhanced signal, we designed an optical layout that
provides the highest throughput of any commercially available spectrophotometer. Our very simple straight line optical
path uses a monochromator with a single reflector mirror. This cuts down on the amount of light loss often associated with
models having 10 or more mirrors. Because of this the Buck 205 AAS can detect far-UV elements, such as arsenic and
selenium, with ten times greater sensitivity.
•
Internal microprocessor and software can identify samples,
perform statistical analysis and graphically display calibration
curves.
•
Dual lamp power, one for warm up
•
High throughput "Stable Beam" optical system
•
Modulated HCL power supply to cancel DC emission from flame
•
Digital readout for absorbance, emission, direct concentration,
lamp currents and PMT voltage
•
Autozero, curve correction, integration and high gain damping
features
•
Bandpass resolution from 0.2 - 0.7 - 2.0nm
•
Burner safety interlock system for nitrous oxide/acetylene flame
operation
•
High sensitivity detection using quartz PMT detector
•
Analog and digital output for chart recorders/PC data systems
•
Compact design saves bench space
Wavelength
Range:
190 to 900nm
Burner/
Nebulizer:
Accuracy:
±0.2nm
Integration: User selectable times from 0.5 to
10 seconds for Stabilized
readings.
Precision:
±0.1nm
Calibration: Automatic, weighted least squares
fit to 1st, 2nd, 3rd, or 4th order
functions, up to 8 points.
Monochromator /
Optics:
Power Supply:


250mm Ebert Mount

0.2, 0.7, 2.0nm bandpass to cover
analytical wavelengths for use on
atomic absorption and emission
measurements
Display:
16 line backlit liquid crystal
display for all text & graphics
Output
Modes:
LCD Display, IEEE Parallel port for
dot matrix printer, RS-232 Serial
Port
600 lines/mm high efficiency
grating
100-240V.A.C. operating range,
50/60HzAC,<100 watts
Polypropylene spray chamber with
premix burner and high efficiency
adjustable nebulizers (SS or
Pt/Ru), Titanium burner heads for
Air/Acetylene, Argon/Hydrogen
and nitrous Oxide/Acetylene
operation
Hollow Cathode
Lamp:
Dimensions: 39" x 11" x 12"
Dual HCL modulated power supply, 0 to
25mA peak
Weight:
50 lbs. (80 lbs. shipping)
WFX-110 /120/130 AAS Spectrometer
Atomic Absorption Spectrophotometer
(QUALITESTTM)
Features








High sensitivity, simple and safe operation, low analytical cost, ensured by the patented flame
analysis technique (patent No. ZL9210560.7) adopting oxygen-rich air-acetylene flame as the
substitution for nitrous oxide-acetylene flame for high temperature element analyses. The flame
temperature of the oxygen-rich flame is adjustable continuously between 2300~2950℃. (Only for
WFX-110)
Fully automated microcomputer controlled operation
1. Automatic wavelength peaking for quick and precise operation.
2. Automatic spectral bandwidth selection.
3. Automatic hollow cathode lamp changeover.
4. Automatic instrument parameter setting, including light source power supply, photomultiplier high
voltage supply and background correction energy balance.
5. Automatic signal measurement and data processing. Fast sampling, photo-electric conversion,
noise smoothing, integration, curve fitting, background correction and data display can all be done
automatically.
Easy and flexible WINDOWS operating system, with multi-windows processing technology to
observe the signal profile, the measured results and the calibration curve at the same time. Various
analytical programs, data, signals and graphics can all be stored for later use.
Fully sealed optical system, keeping the optical elements clean and dry and ensuring long-term
high-energy throughput.
Optimum vibration-absorbing mechanism, ensuring good mechanical stability of the optical
system, reducing vibration interference in graphite furnace operation.
Two background correction systems, deuterium arc background correction system (with high
performance deuterium arc lamp) and S-H background correction system (only for WFX-110/120) to
realize background correction at all wavelengths.
Perfect safety protection measures, alarm and automatic safety protection to fuel gas leakage, air
pressure deficiency and abnormal flame extinction; spray chamber made of explosion-proof
material, all-titanium burner and explosion-proof stopper for flame analyses; alarm and protection
function to argon pressure deficiency, insufficient cooling water supply, over-heating and overcurrent etc. in graphite furnace analyses.
Multi-analytical functions, providing flame AA, graphite furnace AA, and hydride AA analysis and
flame emission analysis.
Specifications
Wavelength range
Wavelength accuracy
Resolution
Baseline stability
Main Specification
Background correction
Lamp turret
Hollow Cathode Lamps
Lamp current adjustment
Lamp power supply mode
Optical System
Detection and Data Processing
System
Monochomator
Grating
Focal length
Blazed Wavelength
Spectral Bandwidth
Detector
Software
Analytical method
Repeatable measurement
190-900n
±0.5nm
better than 0.3nm
0.005A/30min
The D2 lamp background correction capability at 1A is better than 30
times.
The S-H background correction capability at 1.8A is better than 30
times. (for WFX-120/110)
6-lamp turret (WFX-110/120), 4-lamp turret (WFX-130)
Automatic adjustment and display. Wide pulse current: 0~25mA,
Narrow pulse current: 0~10mA. (WFX-110/120)
Powered by two pulses (wide and narrow) simultaneously in WFX110/120; square-wave pulse in WFX-130.
Single beam, Czerny-Turner design grating monochromator
1800 l/mm
277mm
250nm
0.1nm, 0.2nm, 0.4nm, 1.2nm
Photomultiplier with high sensitivity and wide spectral range.
Ms-WindowsTM operating system
Working Curve Method (1st order and 2nd order fitting), Standard
Addition Method.
Maximum 20 times of repeat measurement, automatic calculation of
Condition reading
Result printing
Burner
Flame Analysis
Spray chamber
Nebulizer
Position adjustment
Protection for gas system
mean value, standard deviation and relative standard deviation.
With model function
Measurement data and final analytical report printout.
10cm single slot all-titanium burner for Air-C2H2 flame(WFX110/120/130); 5cm single slot all-titanium burner for oxygen-rich flame
(WFX-110).
All-plastic spray chamber.
High efficiency glass nebulizer with metal sleeve.
Adjusting mechanism for vertical, horizontal positions and the rotation
angle of the burner.
Fuel gas leak protection, abnormal flame extinction alarm, air-pressure
deficiency protection and explosion-proof device.
Automatic
Cu: Characteristic concentration≤0.05mg/L, Detection limit≤0.006mg/L;
Flame ignition
Normal Air-C2H2 flame
Characteristic Concentration and Oxygen-rich Air-C2H2 flame (only
Ba: Characteristic concentration ≤ 0.22mg/L
Detection Limit
for WFX-110)
Hydride generation
Hg: detection limit≤0.5ug/L
Power Supply
220V, 200W
Dimensions
1020 (L) x 492 (W) x 537 (H) mm
Weight
Unpacked 80kg
PEMBAHASAN
Setiap perusahaan pembuat perangkat Atomic Absorption Spectrophotometer
memiliki kelebihan dan spesifikasi tertentu atas produknya. Dalam tugas ini
akan dibahas perbandingan 3 perangkat AAS yang dikeluarkan oleh 3
perusahaan yang berbeda. Untuk lebih jelasnya, dapat dilihat pada tabel
perbandingan di bawah ini :
No
Spesifikasi
Tipe Alat
AA 6300
BUCK 205 AAS
WFX-110
/120/130
1.
Rentang
Panjang
Gelombang
185-900 nm
190-900 nm
190-900 nm
Pengukuran
2.
Jumlah Lampu
6
2
6
3.
Monokromator
Double beam
250 mmEbert
Single beam
Mount
4.
Detektor
Photomultiplier
Photomultiplier
& semiconductor
5.
Nebulizer
Pipa Pt-Ir (Dapat
Pt-Ru
Terbuat dari
menganalisis
kaca dengan
HF)
lapis logam
diluarnya
6.
Burner
5 cm dan 10 cm
Titanium
titanium
7.
Ukuran
berat alat
dan
5 cm dan 10 cm
titanium
835 (W) x 460
975 (L) x 275 (W)
1020 (L) x 492
(H) x 545 (D)
x 300 (H) mm,
(W) x 537 (H), 80
mm, 70 kg
25 kg
kg
Dari ketiga jenis produk AAS ini, masing-masing memiliki kelebihan dan
kekurangan.
Berdasarkan spesifikasi diatas, dapat dijabarkan beberapa
kelebihan dan kekurangan alat-alat tersebut. AAS tipe AA-6300 ini memliki
rentang pengukuran 185-900nm yang berarti daerah pengukurannya menjadi
lebih luas lagi dibanding kedua alat yang lain , yang hanya memliki rentang
pengukuran panjang gelombang 190-900 nm. Dengan rentang pengukuran
yang lebih luas, maka semakin banyak jenis sampel yang dapat dianalisis.
Jadi dari spesifikasi ini, AAS tipe AA-6300 yang paling baik.
Untuk produk AAS tipe AA-6300 dan WFX-110/120/130, memilki 6 lampu
yang terpasang sekaligus, sehingga memudahkan analis dalam menganalisis
macam-macam logam dalam waktu yang singkat. AAS tipe Buck 205 hanya
memiliki 2 lampu sehingga tidak lebih hemat waktu dibandingkan alat yang
lain.
Monokromator yang digunakan pada AA-6300 adalah jenis double beam yang
dapat mengatasi intensitas lampu yang tidak stabil sehingga pengukurannya
menjadi lebih akurat.
Namun, harganya lebih mahal dibandingkan dengan
WFX-110/120/130 yang hanya menggunakan single beam. Harganya lebih
mahal karena alat yang menggunakan double beam memerlukan perangkat
tambahan dibandingkan dengan alat yang menggunakan single beam.
Pada AAS tipe AA-6300, detektor yang digunakan ada 2 macam, yakni
photomultiplier untuk pengukuran panjang gelombang pendek dan detektor
semikonduktor untuk panjang gelombang panjang. Sedangkan AAS tipe WFX110/120/130 hanya dilengkapi 1 jenis detektor saja, yakni photomultiplier
sehingga untuk panjang gelombang yang panjang tidak dapat dideteksi.
Sedangkan alat ketiga, AAS tipe Buck 205 tidak diketahui jenis detektor yang
digunakan sehingga tidak dapat dibandingkan. Dari data ini, dapat diketahui
AA-6300 memiliki kelengkapan detektor dibandingkan kedua alat lain.
Nebulizer yang digunakan pada tipe AA 6300 adalah pipa kepiler yang terbuat
dari Pt-Ir, komponen Teflon dan keramik sedikit dan beberapa menggunakan
HF.
Perbandingan lainnya adalah ukuran dan berat dari perangkat AAS, semakin
compact dan ringan perangkatnya, maka semakin mudah perangkat tersebut
untuk dirawat. Dari ketiga alat di atas dapat diketahui bahwa tipe Buck 205
AAS yang paling memenuhi kriteria tersebut.
Tipe AA-6300 juga dilengkapi dengan autosampler yang memudahkan dalam
hal pengukuran banyak larutan. Selain itu, tipe ini juga dilengkapai dengan
stabilitas alat yang baik sehingga dalam beroperasi tidak mengeluarkan bunyi
yang memekakan telinga. Masalah keamanan menjadi jaminan utama dalam
perangkat tipe ini, dengan adanya pengendali gas yang digunakan dan
pencegahan adanya penyalahgunaan pembakar.
Penilaian terhadap ketiga alat ini tidak dapat dilakukan dengan sangat
terperinci karena informasi yang diberikan dari setiap alat berbeda. Menurut
kami, semakin lengkap informasi alat tersebut maka akan semakin baik
karena konsumen akan mampu memilih alat sesuai keinginannya dengan
informasi yang jelas tersebut.
KHAERUL HATTA
( 105 05 092 ) : 90
RIZKI ANSHARI
( 105 05 093 ) : 90
ASTUTI TRIJAYANTI
( 105 05 094 ) : 90
HUMAILA RIZQI
( 105 05 096 ) : 90
TRIWIDIANSYAH
( 105 05 097 ) : 90
WERDI ISNA RETNOWATI
( 105 05 098 ) : 90
Range Nilai 0 - 100