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Aim

To determine the concentration of Mn in unknown sample, using Microwave digestion for


sample preparation.

Introduction
Graphite furnace atomic absorption spectrometry (GFAAS) has increased sensitivity
that allows measurements of trace analyte, for this capability it has become a popular
analytical technique in recent years.
Because of high sensitivity, one practical problem that we mostly face is to control the
external contamination. Contaminants can be introduced to standards and samples
from a variety of sources, including reagents, solvents, the laboratory atmosphere and
contaminated glassware. These problems can give the impression that GFAAS is a
technique that requires many complex and poorly understood steps to be made before
an analytical method can be successfully developed and proved.

Graphite furnace instruments are basically made up of 5 parts as illustrated above. Light
source, atomization chamber, sample injection port, monochromator and detector. The
radiation source provide radiation that gives energy to the electrons of the sample. At
the atomization chamber it is where the analyte undergo drying, ashing and
atomization at different temperatures. There is also the sample injection port, this is
the point where the sample is introduced to the instrument for it to be analysed.
analyte meaning it can analyse both solid and liquid samples.
The basic principle of this instrument as follows
Drying: The solvents are evaporated from the sample and this normally happens in a
temperature range of 100-120 ⁰C. This step contributes to the precision and reproducibility
in optimizing the method if it’s new. It is also very advantageous as this technique uses
small volumes
Ashing: This step is commonly required for samples with organics and metal salts in
order to remove them and be left with analyte of interest, it is not required for nitrates and
clean samples but for accuracy reasons it is done. It is done is temperature range of 600-
800⁰C. It is advantageous as it removes matrix and minimize interferences.
Atomising: The actually analysis occurs here, the sample is atomized to obtain the signal
and concentration f it I sample. Sample is in gaseous atomic state and absorption of
radiation is measured. Occurs at the temperature range of 2000-3000⁰C.
Cleaning: Temperatures are ramped to above atomization in other to atomize and
remove anything that was not atomized in the atomization temperatures

Monochromator, the radiation is scattered as it is being released by the electrons and


also there is the presence of interferences that are producing their own radiation, so the
monochromator select radiation of the desired wavelength and point the radiation to the
detector. Lastly the detector, this is a device that convert the analytical signal the
readable data.

MICROWAVE DIGESTION
Many digestions are now carried out in a closed container using microwave radiation as
the source of energy. Vessels for microwave digestion are manufactured using Teflon (or
some other fluoropolymer) or fused silica. Both materials are thermally stable, chemically
resistant, transparent to microwave radiation, and capable of withstanding elevated
pressures. A typical microwave digestion vessel consists of an insulated vessel body and
a cap with a pressure relief valve. The vessels are placed in a microwave oven (typically
6–14 vessels can be accommodated) and microwave energy is controlled by monitoring
the temperature or pressure within one of the vessels. Microwave digestion has several
important advantages over an open-vessel digestion, including higher temperatures
(200–3000C) and pressures (40–100 bar). As a result, digestions requiring several hours
in an open-vessel may need no more than 30 minutes when using a microwave digestion.
In addition, a closed container prevents the loss of volatile gases. Disadvantages include
the inability to add reagents during the digestion, limitations on the sample’s size (typically
< 1 g), and safety concerns due to the high pressures and corrosive reagents.
GFAAS LABORATORY PRECAUTIONS:
1. Before turning on the instrument, ensure that the argon gas and cooling water are
turned on.
2. Before running any samples, ensure that the autosampler is properly aligned to
deliver sample to the furnace platform.
3. After placing sampling vials in the autosampler, make sure the lid is properly
aligned so that the robotic sampling tube can access the liquid in the sampling
vials.
4. The last user of the day should turn off the power to the main unit and the furnace
power supply, then turn off the argon gas and the cooling water. Do not exit the
software completely; exit to the Windows Desktop before quitting.
5. When finished, remove all sampling vials from the autosampler and dispose of the
solutions.

Parameters

1. Microwave digestion Parameters

Max 400W
Percent 100
Ramp 15:00
Temperature Control 180ºC
Hold 30:00
Method Name PVC
Sample Type Organic

Method:
Materials/Apparatus

1% Nitric acid preparation

 1x 20mL measuring cylinder


 1x 1000mL volumetric flask
 Plastic droppers
 200mL glass beakers
 Fume hood - extractor

Standard Preparation

 25mL volumetric flasks


 1000μL micropipette
 Micropipette tips
 100mL glass beakers
 Plastic droppers
 Vials
 1x weighing balance (micropipette calibration)

Sample Preparation
 Weighing balance
 Spatula
 10ml measuring cylinder
 Teflon digestion tubes
 Sample holder
 Microwave digestion unit
 50ml volumetric flasks
 Glass funnel
 Filter paper
 Plastic dropper
 Vials

Reagents

 Manganese Standard 1ppm (1000ppb)


 65% Concentrated Nitric Acid HNO3
 PVC beads (blue and red)
 Deionized water – AAS quality

Instrumentation

1. Microwave digestion Parameters

Max 400W
Percent 100
Ramp 15:00
Temperature Control 180ºC
Hold 30:00
Method Name PVC
Sample Type Organic

Experimental procedure
 0.5128g of Blue PVC was weighed into the MAD tube.
 The tube was topped with 10mL conc nitric acid and sealed properly.
 A blank was prepared by adding 10mL conc nitric acid into the tube and sealed
properly
 The tubes were placed into the MAD carousel and placed into the microwave
disgester.
 The above settings were chosen, the samples and blank were left to digest for
about 1 hour.
 1% nitric acid was prepared.
 Working standards for PVC analysis were prepared as below:
(Calculations for the standards are below)
 After digestion and cooling, the samples were transferred into a 50mL volumetric
flask and topped with nitric acid
 The sample was filtered, using filter paper and a funnel, until the solution was
clear
 The blank, standards and samples were transferred into vials
 The vials were placed in the auto-sampler
 GFAAS setup was followed using the work instruction.
 The work instruction was followed
 1 blank, 4 standards and 2 samples were analysed.
 Results were recorded and analysed.

 1% nitric ccid was prepared using the calculated below, 15mL was transferred
into a 1L volumetric flask, topped with distilled water and homogenised.
 25ppb Mn was prepared by quantitively transferring 625μL of 1000ppb Mn, into a
25mL volumetric flask. The flask was topped with 1% nitric acid and
homogenised.
 50ppb Mn was prepared by quantitively transferring 1250μL of 1000ppb Mn, into
a 25mL volumetric flask. The flask was topped with 1% nitric acid and
homogenised.
 75ppb Mn was prepared by quantitively transferring 1875μL of 1000ppb Mn, into
a 25mL volumetric flask. The flask was topped with 1% nitric acid and
homogenised.
 100ppb Mn was prepared by quantitively transferring 2500μL of 1000ppb Mn,
into a 25mL volumetric flask. The flask was topped with 1% nitric acid and
homogenised.

Pre-experimental data & calculations


Vol. HNO3 required to prepare 1L of 1% v/v HNO3:
C1V1 =C2V2
(65%)(V1) = (1%)(1000mL)
(1%)(1000𝑚𝐿)
V1 = (65%)
V1 = 15,40𝑚𝐿 ≈ 15mL
Volume of 1000ppb Mn required to prepare 25ppb in 25mL:
C1V1 = C2V2
(1000ppb)(V1) = (25ppb)(25mL)
25𝑝𝑝𝑏 𝑥 25𝑚𝑙
V1 = 1000𝑝𝑝𝑏
= 0.625mL
= 625μL

Volume of 1000ppb Mn required to prepare 50ppb in 25mL:


C1V1 = C2V2
(1000ppb)(V1) = (50ppb)(25mL)
50𝑝𝑝𝑏 𝑥 25𝑚𝑙
V1 = 1000𝑝𝑝𝑏
= 1.250mL
= 1250μL

Volume of 1000ppb Mn required to prepare 75ppb in 25mL:


C1V1 = C2V2
(1000ppb)(V1) = (75ppb)(25mL)
75𝑝𝑝𝑏 𝑥 25𝑚𝑙
V1 = 1000𝑝𝑝𝑏
= 1.875mL
= 1875μL

Volume of 1000ppb Mn required to prepare 100ppb in 25mL:


C1V1 = C2V2
(1000ppb)(V1) = (100ppb)(25mL)
100𝑝𝑝𝑏 𝑥 25𝑚𝑙
V1 = 1000𝑝𝑝𝑏
= 2.500mL
= 2500μL