LABORATORIES \ ATOMIC ABSORPTION SPECTROSCOPY

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ATOMIC ABSORPTION SPECTROSCOPY LABORATORY

ANALYSIS TECHNIQUES:
     


Short description of the laboratory. TOP

The laboratory was setup in Electrochemistry Department, in the year 2006 and its main purpose is the determination of heavy metals from various products/samples.

Analysis and characterization techniques used TOP

Atomic absorption spectrometry
The novAA 400 G atomic absorption spectrometer
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Manufacturer: ANALYTIK JENA - Germany

Year: 2005

Main characteristics:

The novAA 400 G atomic absorption spectrometer, with state of the art transverse heated graphite furnace, MPE 60 autosampler with 89 positions, 6 lamp turret; is connected to a PC via  WinAAS software for work method optimization, automated result saving, storing and printing. As a reference, for each element that can be analyzed, a Cookbook is available, to ensure that every measurement is done correctly and precisely.

Possibility of overnight measurement is available, thanks to the 89 position autosampler; the apparatus can make the necessary dilution if the measured value is out of range, once the required lamps are loaded, the calibration curve is selected and the samples are loaded into the autosampler.

The transverse heated graphite furnace offers the following advantages:

  • higher measurement sensitivity compared to the longitudinal heated furnaces\
  • interference from matrices and contaminants is minimized
  • extremely low- volatility elements such as vanadium and molybdenum can be analyzed without difficulty

Cooling of the tube is realized automatically, a separate attachment ensures that the cooling water is kept at about 36 °C and, during analysis the graphite tube is cooled down rapidly.  
At the moment the following lamps are available: Cu, Cr, Pb, Zn, Ni, Mn, As, Co, Se, Cd, Hg, Ca, Mg, Ga, Al, Fe, Au, Ag, Pt, Sn, Sr.
Detection limit of the apparatus: µg/L

Usage/Applications:
The apparatus can be used to determine the concentrations of heavy metals from various samples: potable water, residual and underground water, soils, foodstuff, plastic materials, drugs, cosmetics, tissues, blood, etc.

Work techniques. Short description:
Before analysis, the metals are transformed to nitrates. Dilution, to an established concentration, is done with 0,5 % HNO3 (Merck purity or free of impurities). For each metal, intended to be analyzed, a calibration curve is made using standard solutions. Using the Cookbook, the optimal working conditions are established.

Graphite tube:

1 -  lock screw
2 – radiation sensor
3 – right side alignment
4 – cooling inlet and outlets
5 – power transfer cable

 


Stages Temperature, °C Heating speed,
°C/s
Duration, s
Drying 1 90 5 32
Drying 2 105 3 25
Drying 3 120 2 17.5
Pyrolysis 700 250 12.3
Auto Zero 700 0 6
Atomization 2100 1500 10.9

Calibration curve and measurement conditions for Ni

Cleanup 2400 500 4.6

Contact:
Person responsible for device:

 

Atomic absorption spectrometry using the hydride generator
Hydride generator HS 55/1
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Manufacturer: ANALYTIK JENA - Germany

Year: 2007

Main characteristics:

The HS 55/1 hydride generator is attached to the novAA 400 G,  presented above and it allows the determination of metals, like As, Sn, Te, Bi, Hg, Se, Sb, at concentrations as low as 1 ppm; The metals are transformed to hydrides (by the HS55/1 unit) and then atomized by the novAA 400 G unit. The apparatus is fitted with a peristaltic pump, batch reaction chamber (discontinued flow) and the sodium boron-hydride recipient. The maximum atomization temperature, for the hydrides is 2100 °C.

Work techniques:
NaBH4 (Merck, Fluka) and NaOH solutions are prepared and mixed in 3:1 ratio with ultrapure water. The recommended concentration is 1% NaBH4 and 0,33% NaOH. 5 ml of sample and 5 ml of sodium hydroxide and sodium boron-hydride are introduced in the into the reaction chamber. To eliminate the air/oxygen argon gas is used. A calibration curve is made, using solutions of known concentration, using the WinAAS software of the novAA 400 G unit.

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Spectrometrie de absorbţie atomică cu utilizarea unui cuptor de digestie cu microunde MWS – 2 Berghof
Microwave digestion oven Speed Wave MWS – 2
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Manufacturer: BERGHOF - Germany

Year: 2005


0 piece support system; DAP-60K with teflon recipients

Main characteristics:

The MWS-2 microwave digestion oven, equipped with a 1000W generator, 6 types of programs with 3 stages each, specially designed for various samples or substances.
(T-temperature, t-time, p-power).

Programes T1 t1 p1 T2 t2 p2 T3 t3 p3
Waters, DIN EN 11
P1
160° 5 min 80% 200° 10min 80% scade 10min 0
Soils EPA 3051A
P2
175° 10 min 99% scade 10min 0% scade 10min 0
Foodstuff
P3
P4
145° 10 min 80% 160° 10min 80% 190° 20min 80%
160° 15 min 80% 210° 15min 90% scade 15min 0
Plastic materials
P5
160° 5 min 80% 220° 40min 90% scade 20min 0
Tissues, blood
P6
130° 8 min 80% 155° 5min 80% 170° 12min 80%

Work techniques:
The samples are weight using the analytical balance, precision of  ±0,0001g, are introduced into the teflon reaction chambers where also 67 % HNO3 is added or Aqua Regia. (HNO3+HCl mixture). After the optimal program is chosen, the samples are introduced into the oven. The digested samples are filtrated and diluted with ultrapure water, at a volume of 250 or 500 ml, used later for measurements, experiments, etc.

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Water purification system
Deionization System EASYpure Barnstead / Thermo Scientific D13321
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Manufacturer: BERGHOF - Germany

Year: 2005

Main characteristics:

The apparatus is connected directly to the tap water inlet; the treated water possesses a resistivity as low as 18,2 MΏ·cm or 0,056 mS conductivity. Water purification is achieved via reverse osmosis, adsorption on the surface of active carbon, ion-exchangers treatment. The micro organisms are eliminated by UV radiation. 

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Measurement of halogenated ions from organic compounds
The AOX  multi  X 2000 analyzer
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Manufacturer: ANALYTIK JENA AG - Germany

Year: 2008

Main characteristics

Using the AOX  multi  X 2000 analyzer, the halogenated ions can be analized from organic samples, such as waters, sludges, wastewaters. The measurements are made according to DIN 38409/14 and EN 1485, (European Quality Standards) or the SR EN 1485:2000 (Romanian Standards). As the standards specify, the direct measurement of chlorine, bromine, iodine (except fluorine), from organic compounds, that are adsorbed on the surface on activated carbon. The result of the analysis are mentioned as chlorine ions. A sensitivity as low as 10 μg/l halogenated ions is available    


multi X 2000 module AP2P module
           

Work techniques:

The apparatus has 2 units, the main module, the AOX multi X 2000 is also attached to a PC and the AP2P module ensures the adsorption of halogenated organic compounds on the surface of activated carbon. The AOX multi X 2000 consists of combustion chamber, gas washer or scrubber, coulometric cell, carrier gas transport system and other various electronic equipment, are part of the apparatus. Variable speed two stirrer system, two 3-way-valves and two syringes drive the sample through the columns

The halogenated content of samples needs to be adsorbed on the surface of activated carbon, (AOX) or via extracting medias (EOX) or purged from the sample using a certain type of gas (POX). The retained halogens, (in case of AOX), are burned at 950°C, in a stream of high purity oxygen, in a quartz tube, resulting CO2, H2O vapors and HX. The water vapors are retained by the sulphuric acid from the scrubber; the of halogen ions are detected by micro-coulombmetry, in presence of acetic acid and other specific substances. Silver ions, generated from the anode, retain the halogen ions, forming AgX. Ag+   +      X-  →   AgX. The quantity of silver necessary to retain all the halogens, is directly proportional with their quantity, and so, according to Faraday’s law, the quantity of halogens can be calculated from the quantity of current used to generate silver ion from the anode.

Detecţia se efectuează prin micro-culometrie, în prezenţa acidului acetic sau a altor substanţe specifice. Creşterea concentraţiei în ioni de argint semnalează finalul titrării şi este pusă în evidenţă cu o pereche de electrozi indicatori. Cantitatea de halogenuri se calculează conform legii lui Faraday din cantitatea de curent consumată pînă în momentul transformării totale a ionilor halogenură

Contact:
Person responsible for device:

Phone: 0741-014876

 

Services offered: TOP
Contact: TOP

Head of Laboratory:

Phone: 0757 017125