01-0019-01 Flame Methods Manual For AA

AAS AAS
FLAME METHODS MANUAL

FOR ATOMIC ABSORPTION
Part No. 01-0019-01
Copyright GBC Scientific Equipment Pty Ltd © 2016
All rights reserved
Information in this document is subject to change without notice and does not represent a
commitment on the part of GBC Scientific Equipment Pty Ltd.
No part of this publication may be reproduced, distributed, transmitted, stored in a retrieval
system, or reduced to any electronic medium without the prior consent of GBC Scientific
Equipment Pty Ltd.
GBC Scientific Equipment Pty Ltd assumes no responsibility for any errors that may appear in this
document or any damages arising out of the use or inability of this document.
GBC Scientific Equipment Pty Ltd acknowledges the various trademarks and proprietary names of
companies and products mentioned in this document. GBC Scientific Equipment Pty Ltd is not
affiliated with any of these organisations. No approval or endorsement by the organisations
mentioned is intended or given either expressly or by implication.
GBC Scientific Equipment Pty Ltd reserves the right to change any in part or all specifications
without prior notice.
Each GBC instrument has a unique serial number.
Printed in Australia
GBC Part Number: 01-0019-01
Revision Number: 2
Issue Date: October 2016
GBC Scientific Equipment Pty Ltd
A.C.N. 005 472 686

4 Lakewood Boulevard
Braeside Victoria 3195
Australia
Telephone: 61 3 9588 6666

Facsimile: 61 3 9588 6677
URL: http://www.gbcsci.com
Email: [email protected]
Table of contents
GBC Flame Methods Manual for Atomic Absorption 3

Table of contents
TABLE OF CONTENTS................................................................................................................... 3
AN INTRODUCTION TO FLAME SPECTROSCOPY.............................................................................. 9
Flame emission spectroscopy.................................................................................................... 10
Atomic absorption spectroscopy ................................................................................................ 10
Atomic fluorescence spectroscopy ............................................................................................ 11
ATOMIC ABSORPTION – INSTRUMENTAL REQUIREMENTS ............................................................ 13
Hollow cathode lamps............................................................................................................... 14
Atomisation .............................................................................................................................. 16
Flame atomisation................................................................................................................16
Nebuliser .........................................................................................................................17
Bead adjustment..............................................................................................................18
Spray chamber ................................................................................................................18
Burners ...........................................................................................................................18
Air-acetylene flame ..........................................................................................................18
Acetylene cylinders ..........................................................................................................19
Nitrous oxide-acetylene flame...........................................................................................19
Flameless electro-thermal atomisation ..................................................................................20
Advantage of ramp rate over fixed heating ........................................................................20
Vapour generation method ...................................................................................................22
Monochromator ........................................................................................................................ 23
Resolution ...........................................................................................................................23
Detector read out...................................................................................................................... 24
INTERFERENCES ....................................................................................................................... 27
Spectral interferences .............................................................................................................. 28
Non-atomic absorption correction.........................................................................................30
Chemical interferences ............................................................................................................. 31
Matrix effects .......................................................................................................................31
Stable compound formation .................................................................................................32
Ionisation interference..........................................................................................................32
OPTIMISATION TECHNIQUES...................................................................................................... 35
Choice of wavelength................................................................................................................ 36
Lamp current optimisation......................................................................................................... 36
Bandpass optimisation .............................................................................................................. 36
Optimisation of sample introduction system ............................................................................... 36
ANALYTICAL PROCEDURES ........................................................................................................ 39
Calibration ............................................................................................................................... 40
4 GBC Flame Methods Manual for Atomic Absorption

Table of contents
Calibration curve..................................................................................................................40
Method of ultimate precision ................................................................................................41
Method of standard additions ...............................................................................................41
Single addition method.....................................................................................................41
Multiple addition method..................................................................................................42
Secondary calibration.......................................................................................................42
TERMS AND DEFINITIONS .......................................................................................................... 43
CONVERSION FACTORS AND SAMPLE CALCULATIONS.................................................................. 45
RECOMMENDED FURTHER READING ........................................................................................... 47
STANDARD ANALYTICAL DATA OF THE ELEMENTS ....................................................................... 49
Silver (Ag)...............................................................................................................................51
Arsenic (As)............................................................................................................................52
Aluminium (Al) ........................................................................................................................53
Gold (Au).................................................................................................................................54
Boron (B) ................................................................................................................................55
Barium (Ba).............................................................................................................................56
Beryllium (Be).........................................................................................................................57
Bismuth (Bi) ............................................................................................................................58
Calcium (Ca) ...........................................................................................................................59
Cadmium (Cd)..........................................................................................................................60
Cobalt (Co)..............................................................................................................................61
Chromium (Cr) .........................................................................................................................62
Caesium (Cs)...........................................................................................................................63
Copper (Cu).............................................................................................................................64
Dysprosium (Dy) ......................................................................................................................65
Erbium (Er)..............................................................................................................................66
Europium (Eu)..........................................................................................................................67
Iron (Fe)..................................................................................................................................68
Gallium (Ga) ............................................................................................................................69
Gadolinium (Gd).......................................................................................................................70
Germanium (Ge).......................................................................................................................71
Hafnium (Hf)............................................................................................................................72
Mercury (Hg)...........................................................................................................................73
Holmium (Ho) ..........................................................................................................................74
Indium (In) ..............................................................................................................................75
Iridium (Ir) ..............................................................................................................................76

Table of contents
Potassium (K)..........................................................................................................................77
Lanthanum (La)........................................................................................................................78
Lithium (Li)..............................................................................................................................79
Lutetium (Lu) ...........................................................................................................................80
Magnesium (Mg) .....................................................................................................................81
Manganese (Mn) .....................................................................................................................82
Molybdenum (Mo)....................................................................................................................83
Sodium (Na) ............................................................................................................................84
Niobium (Nb)...........................................................................................................................85
Neodymium (Nd)......................................................................................................................86
Nickel (Ni) ..............................................................................................................................87
Osmium (Os)............................................................................................................................88
Phosphorus (P)........................................................................................................................89
Lead (Pb) ................................................................................................................................90
Palladium (Pd) ........................................................................................................................91
Praseodymium (Pr) ..................................................................................................................92
Platinum (Pt) ...........................................................................................................................93
Rubidium (Rb) .........................................................................................................................94
Rhenium (Re) ..........................................................................................................................95
Rhodium (Rh) ..........................................................................................................................96
Ruthenium (Ru)........................................................................................................................97
Antimony (Sb)..........................................................................................................................98
Scandium (Sc).........................................................................................................................99
Selenium (Se) .......................................................................................................................100
Silicon (Si)............................................................................................................................101
Samarium (Sm)......................................................................................................................102
Tin (Sn).................................................................................................................................103
Strontium (Sr)........................................................................................................................104
Tantalum (Ta)........................................................................................................................105
Terbium (Tb) .........................................................................................................................106
Tellurium (Te) .......................................................................................................................107
Titanium (Ti) .........................................................................................................................108
Thallium (Tl) ..........................................................................................................................109
Thulium (Tm).........................................................................................................................110
Uranium (U) ..........................................................................................................................111
Vanadium (V) ........................................................................................................................112

Table of contents
Tungsten (W).........................................................................................................................113
Yttrium (Y) ............................................................................................................................114
Ytterbium (Yb) .......................................................................................................................115
Zinc (Zn) ...............................................................................................................................116
Zirconium (Zr) .......................................................................................................................117

Table of contents
This page is left blank intentionally

An introduction to flame spectroscopy

Flame spectroscopy is an analytical technique used for the qualitative and

quantitative determination of an element in a sample. In this method the
sample, in the form of a homogeneous liquid, is introduced into a flame
where thermal and chemical reactions create ‘free’ atoms capable of
absorbing, emitting or fluorescing at characteristic wavelengths. Flame
spectroscopy can be subdivided into the different processes occurring, to
give us Flame Emission Spectroscopy, Atomic Absorption Spectroscopy and
Atomic Fluorescence Spectroscopy.
Flame emission spectroscopy

In emission spectrometry thermal energy (in the form of a flame, spark or
plasma source) is used to excite free atoms to higher energy levels. The
atoms will subsequently emit characteristic radiation that can be isolated by
a monochromator. The emitted radiation is proportional to the concentration
of atoms present. For emission analysis the temperature of the excitation
source has to be high in order to excite large quantities of free atoms. When
using a flame, the stoichiometry and observation position have to be
optimised to observe the equilibrium position of the excited state population,
so as to obtain a stable reading.
Emission spectrometry suffers from a major disadvantage in that emission
spectra are complex due to emission by other species in the sample and by
the flame, causing considerable interferences. Flame emission spectrometry
is instrumentally the simplest of the flame spectrometric techniques and as
such is the oldest known method.
Atomic absorption spectroscopy

The technique of Atomic Absorption developed by Sir Alan Walsh of CSIRO
in the mid 1950's has become the preferred method of elemental analysis.
Walsh discovered that the majority of free atoms in the commonly used
flames were in the ground state, but that the flames did not also have
enough energy to excite these atoms (except for the Group I elements). A
light source emitting a narrow spectral line of the characteristic energy is
used to excite the free atoms formed in the flame. The decrease in energy
(absorption) is then measured.
The absorption is proportional to the concentration of free atoms in the
flame, given by the Lambert-Beer law.
ABSORBANCE = log10 Io
= K.C.L.
It
where Io = Intensity of incident radiation emitted by the light source.
It = Intensity of transmitted radiation (amount not absorbed).
C = Concentration of sample (free atoms).
K = Constant (can be determined experimentally).
L = Path length.

Atomic Absorption is similar to Ultra-Violet Spectroscopy in that similar

wavelengths and the same relationship (Lambert-Beer's law) are used, but
differs in the fact that a line source is used, and the sample compartment (a
flame or electrothermal atomiser) is positioned before the monochromator
and not after it.
In practical atomic absorption analysis the Lambert-Beer's law can be
reduced to:
αC
It
Since the instrument is calibrated by standards and the sample
concentrations interpolated from these. The method is not absolute but
comparative, as such the constant does not have to be determined as do
the extinction coefficients in UV spectroscopy.
As well as atomic absorption occurring, there is also emission from the
sample, the flame, and other species in the sample. To isolate the atomic
absorption from all the other effects, the energy from the light source is
‘coded’ by modulation (turning ON and OFF at regular intervals) and the
electronics are synchronised to ‘see’ only signals from this source. By this
method flame emission, which is basically steady-state is not seen by the
electronics, only the atomic absorption is observed.
Atomic fluorescence spectroscopy

The process of fluorescence is similar to atomic absorption in that the free
atoms are excited to higher energy by characteristic radiation, however the
detector is placed at right angles to the radiation source to observe
fluorescence (characteristic energy given off by the atoms as they fall from a
higher energy level to a lower level). There are two types of fluorescence
commonly observed:
1. Resonance Fluorescence. This is where the emitted radiation has the
same wavelength as the excitation radiation.
2. Stepwise Line Fluorescence. This is where the emitted radiation is at a
different wavelength to the excitation radiation (the loss of energy is
via two or more steps).
Atomic fluorescence has the potential of simultaneous multi-element
analysis, with similar freedom from interferences as atomic absorption
spectroscopy. The dynamic ranges of both emission and atomic
fluorescence are much greater than atomic absorption, by virtue of the fact
that it is much easier to measure a small signal relative to zero, rather than
a small reduction from a reference level (i.e. in atomic absorption we set a
point of nil absorption and measure the loss of light in relation to the full
light available). However at present there are several instrumental problems
to overcome to make atomic fluorescence a viable alternative to atomic
absorption.


.

Atomic absorption – instrumental
requirements

Atomic absorption – instrumental requirements
Hollow cathode lamps

A hollow cathode lamp is used as the radiation source to excite the free
atoms in the flame. The hollow cathode lamp produces a narrow spectral
line characteristic of the material of the cathode and the fill gas (neon or
argon). Figure 1 shows the construction of a hollow cathode lamp. The
hollow cathode (made of the element or its compound) and ring anode are
enclosed in a glass envelope, filled with either argon or neon at a reduced
pressure of 7.5 mBar (10 torr). The fill gas is chosen to reduce spectral
interference. For elements with resonance wavelengths in the UV, quartz is
used as the window material, and Pyrex for the others.
A potential of 150–400 volts is applied to the electrodes (anode positive and
cathode negative) which causes the fill gas to ionise. The gas ions are
accelerated by the applied potential, and collide with the cathode releasing
a cloud of atoms from the cathode (this process is termed ‘sputtering’).
These atoms are further excited by collisions with gas ions to a high energy
state.
Characteristic wavelength is then emitted by the atoms as they fall to the
ground state.
The cathode and anode are designed to produce a stable contained
discharge, which yields a very narrow line output (typically 0.001 nm).
Figure 1: Hollow cathode lamp construction

Since the light output of a hollow cathode lamp is proportional to the lamp
current, minor current variations will cause light output variations, for this
reason the lamp current is very accurately controlled. Increasing the lamp
current enables lower amplifier gain settings to be used, thus improving the
signal to noise (S/N) ratio. However there are two limiting factors:
1. Maximum current is specified by the manufacturer which should not
be exceeded or permanent damage may occur, such as bulk
sputtering of cathode material, reduction of life, thermal evaporation
or melting of the cathode.
2. Operating at an increased current with some elements causes severe
curvature of the calibration curve, and reduction of sensitivity due to
self absorption.
The manufacturer of the lamp specifies an optimum operating current and
a maximum current. The maximum current should not be exceeded. The
operating current however, in most cases is only a guide. Optimum lamp
current can be determined by analysing a solution at various lamp currents
(maintain flame conditions, burner position and uptake rate constant). A
plot of Absorbance vs Lamp Current (Figure 2) is then made and a point
chosen that does not show a major change in absorbance for a minor
change in lamp current for a gain setting that is not so excessive as to
create a noisy signal (i.e. minimise EHT).
Self absorption occurs where ground state atoms in the cathode atom cloud
absorb the emitted radiation (the process we want to happen in the flame).
This phenomenon increases with increasing lamp current.
A
b
s
o
r
b
a
n
c
e
Lamp Current (mA)
Figure 2: Absorbance versus lamp current

Atomisation
For atomic absorption to occur, the atoms have to be introduced into the
excitation beam as ‘free’ atoms. Analysis is normally conducted from a
solution in which the atoms are chemically bonded and solvated. To form
free atoms, the solvent has to be removed and the chemical bonds broken
to form free atoms. This is generally done in one of three ways: by a
chemical flame, by flameless heating or by hydride generation.
Flame atomisation
The flame atomiser consists of three major components, nebuliser,
spray chamber and a burner. A diagram of the system is shown in
Figure 3.
Figure 3: Flame atomisation system

The overall system has to convert the liquid into an aerosol, select the
correct droplet size (reject the oversized droplets) and transfer the
sample to the burner, where atom formation occurs. This is principally
the heart of an AA system. If too large a droplet is introduced into the
flame, the atoms may be lost before they are ‘freed’ to absorb.
Examination of the process will show that the particles have to be de-
solvated and converted to ‘free’ atoms, before the flow of gases ‘wash’
the particles out of the light beam. The operation of the basic
components are:

Nebuliser
The nebuliser used in atomic absorption is the pneumatic type (shown in
Figure 4) in which the flow of gases through the orifice creates a vacuum
drawing the sample up into the capillary. Adjustment of the position of the
capillary effects the uptake rate by varying the vacuum.
Figure 4: Nebuliser
As the solution passes through the venturi an aerosol is formed. The impact
bead at the end of the nebuliser is used to produce a greater proportion of
small particles, which are easier to atomise. All GBC atomic absorption
instruments have a variable, corrosion resistant nebuliser fitted as standard.
The advantages of variable nebulisers are:
• Sensitivity can be varied by adjustment of the uptake rate.
• When aspirating organic solvents the uptake rate can be adjusted for
minimum flame disturbance by the solvent acting as a fuel.
• Factors such as viscosity and surface tension effect the nebulisation
efficiency and can be compensated with a variable nebuliser.
• The uptake rate needed for optimum sensitivity in an air-acetylene
flame will not necessarily produce a maximum signal in the nitrous
oxide-acetylene flame, especially for refractory elements. In general,
for the nitrous oxide-acetylene flame a slower uptake rate is needed.
At higher uptake rates significant cooling of the flame is encountered
with a reduction in sensitivity.

Figure 5 shows a typical variation of absorbance vs uptake rate that is found

with a variable nebuliser. As can be seen, an uptake rate of 4–6 mL/min is
optimum for air-acetylene. However an uptake rate of 2–4 mL/min is
generally better for nitrous oxide-acetylene.
A
b
s
o
r
b
a
n
c
e
1 2 3 4 5 6 7 Sample Uptake Rate (mL/min)
Figure 5: Typical variation of absorbance versus uptake rate
Bead adjustment
The bead is factory set for optimum performance and minimum noise and
should not be changed. A method is described under instrument
optimisation in the unlikely event that the bead or nebuliser needs to be
changed.
Spray chamber
The spray chamber acts as a classifier to remove large particles and supply
a constant feed of fine particles to the burner. If the larger particles reach
the burner, considerable noise will be seen and the flame temperature
reduced. Because these large particles cannot be volatilised quickly, light
scattering occurs. For optimum sensitivity, particles of a consistent size (less
than 10 μm) should reach the burner.
Burners
A laminar flow premix burner with a long path length is used in atomic
absorption. Materials to minimise sample contamination are used in its
construction. The GBC burners are of all titanium construction for
robustness, stability and inertness. Two types of flame are commonly used,
the properties of these two flames are:
Air-acetylene flame
This is the most widely used flame in atomic absorption spectroscopy, with
most elements showing best sensitivity in the stoichiometric flame. Four
easily distinguishable flames are used:
1. Oxidising flame (lean) – a very stiff flame with small inner blue cone.

2. Stoichiometric flame – a stiff flame with bigger blue cone and an

almost luminous appearance.
3. Luminous flame as the name suggests the flame is luminous, however
the blue cone is still prominent.
4. Reducing flame (rich) – extremely luminous flame almost sooty at the
top.
The temperature of this flame is approximately 2300°C and is not hot
enough for elements forming refractory oxides.
Acetylene cylinders
The high solubility of acetylene in acetone (300:1 by volume at 1100 kPa)
enables it to be supplied dissolved in acetone. Acetylene cylinders are filled
with a porous material, which carries the acetone. Cylinders should always
be used in a vertical position to minimise liquid acetone entering the gas
line. As the cylinder pressure falls, the acetone entering the gas stream
increases, producing instability of the flame and erratic results for flame
stoichiometry sensitive elements, such as calcium, tin and others. To
overcome this, acetylene cylinders should not be run at a pressure lower
than 500 kPa (70 psi).
CAUTION:
Never pressurise the acetylene lines above 100 kPa (15 psi). At higher
pressures acetylene can spontaneously decompose or explode. Acetylene and
copper react to form an explosive compound. Copper tubing and fittings
should not be used for acetylene. Fittings supplied with the instrument are
safe. If in doubt about other fittings contact your gas supplier.
Nitrous oxide-acetylene flame

This is a much hotter (approximately 2900°C) and faster burning flame and
should only be used with a nitrous oxide-acetylene burner. A large range of
refractory elements can be analysed with this flame, due to the higher
temperature and strongly reducing nature. A nitrous oxide-acetylene flame
has three distinct zones: an initial combustion zone whitish-blue in colour, a
secondary interconal zone red-pink in colour (normally called a red feather)
and a blue diffusion zone. The four types of flame are distinguished by:
1. Oxidising flame (lean) – a very stiff clear flame in which the red
feather is 1 cm tall or less.
CAUTION:
Never run the flame without ‘red feather’.
2. Stoichiometric flame – a clear flame with evidence of slight yellow at

the junction of the red feather which is 1–2 cm tall.
3. Reducing flame (rich) – a yellow flame with the red feather just
visible.
4. Very reducing flame – a flame that is extremely luminous with almost
the formation of soot.
A flame shield should be fitted to the instrument and protective glasses
worn when using this flame to reduce the emitted UV radiation.

Care should be exercised with nitrous oxide on cold and humid days in that
the flow of gas through the regulator forms ice and under extreme
conditions can freeze up the regulator causing erratic results. Consult your
gas supplier if in doubt.
Flameless electro-thermal atomisation

In this method the nebuliser, spray chamber and burner are replaced by an
electrically heated carbon furnace.
The graphite furnace by virtue of its small size ensures a large population of
‘free’ atoms in the optical path (the efficiency of a nebuliser/burner system
is of the order of 10% whilst that of the graphite furnace is about 90%) and
requires extremely small volumes of samples, typically 2–50 μl. Due to the
greater efficiency of the furnace the sensitivity is greater by 10–200 times
(depending on the element).
The graphite furnace power supply applies power to the furnace in ten
steps. Each step can be programmed for three parameters:
1. Final temperature.
2. Ramp time.
3. Hold time.
Advantage of ramp rate over fixed heating

DRY – The ability to set an initial and final temperature, with an associated
ramping rate, means that a sample can be dried more reliably by starting at
a temperature well below the boiling point and ramping past it. A
compromise does not have to be made as to time and temperature.
ASH – The ramping facility is more important in this stage in that, generally,
the sample will contain volatile (acids, organic complexes) and non volatile
(inorganic compounds) components, that have to be removed prior to the
atomise stage. Using the ramp rate facility, a low starting temperature can
be set and the temperature ramped at a very slow rate (i.e. as low as
0.5°C/sec.). A slow rate enables the ashing of very volatile compounds, thus
avoiding the possibility of losing analyte by spitting if a faster rate is used. In
order that the ashing can be optimised for organic and inorganic
compounds ten stages are provided, eight of these stages can be used to
ash if required.

Control of the applied power is via a power feedback circuit that monitors
the voltage and current supplied to the furnace. A maximum of 300 Amps is
available for rapid heating, to ensure maximum efficiency of free atom
production in the atomise stage.
The sample is introduced into the furnace with the minimum of sample
preparation due to the ashing stages provided, however light scatter and
non-atomic absorption are higher in electrothermal atomisation.
The result is a transient peak, compared to a relatively stable reading
produced in flame atomisation. A diagrammatic display of output versus
time is shown in Figure 6.
T
e
Furnace Temperature Profile
m
p.
Final Hold Time

Temp.
Ramp
Time
Initial
Temp.
Time
Step 1 Step 2 Step 10
Figure 6: Furnace temperature profile

Vapour generation method

Antimony, arsenic, bismuth, germanium, lead, selenium, tellurium and tin
form volatile hydrides when treated with sodium borohydride. Mercury
forms elemental mercury vapour when reduced with either sodium
borohydride or stannous chloride. The GBC HG3000 is shown in Figure 7.
Figure 7: HG3000 hydride generator

The solution to be analysed is acidified and continuously pumped using a
peristaltic pump into a mixing manifold with 0.6% NaBH4 dissolved in 0.6%
NaOH and 20–30% HCI.
Argon or nitrogen gas is used to sweep the vapour produced into a quartz
cell.
The quartz absorption cell is placed on a burner to allow the light from the
hollow cathode lamp to pass through its centre. For Hg analysis the flame is
not lit during the analysis. Hence the reason it is referred to as ‘cold vapour’
technique.
For all the other vapour forming elements the cell needs to be heated using
an air-acetylene flame to ensure the decomposition of the hydride formed.
If even greater sensitivity is required for Hg analysis, a closed cell (part no.
40-0018-01) is required. This cell must not be heated.
For Hg determinations, stannous chloride can also be used as a reductant.
For Hg analyses to ppt levels, the MC3000 Mercury Concentrator can be
used. Stannous chloride is recommend for this application as this reductant
only reduces Hg and none of the other hydride elements which may also be
present. If borohydride is used in this application then any As or Se will be
also reduced and these ‘poison’ the gold trap and compromise the
sensitivity for Hg analyses.

Monochromator
In atomic absorption spectroscopy a monochromator of high resolution is
not essential. A medium resolution monochromator capable of 0.2 nm
resolution is quite adequate. A more important parameter is high light
throughput, since this determines the gain setting required (especially for
hollow cathode lamps having a weak output).
Resolution
The resolution of a monochromator (the minimum repeatable bandpass)
depends on a variety of factors such as focal length, number of lines per
millimetre on the grating and the width of the entrance and exit slits.
For atomic absorption spectroscopy the most common slit sizes used are
0.2, 0.5 and 1.0 nm. A narrow slit width is used when trying to isolate two
close lines such as for vanadium shown in Figure 8.
318.4
318.34
E
n 318.54
e
r Vanadium H.C. Lamp
g
y
Wavelength (nm)
Figure 8: V peak showing various absorption wavelengths which would

require 0.1 nm slit width to separate the various wavelengths

It is interesting to note that because the width of a spectral line is typically

less than 0.001 nm, reducing the slit width by half also reduces the light
throughput by half (i.e. a linear relationship exists) however for continuum
radiation the spectral bandwidth is governed by the slit width. So, reducing
the slit width by half has the effect of reducing the energy by a factor of 4.
Figure 9 shows the effect pictorially.
E E
n n
e e
r r
g g
y y
Slit Width Slit Width

Hollow Cathode Continuum Source
Spectral (Line) Output Output
Figure 9: Comparison of spectral output from hollow cathode lamp compared

to D2 source
This is very important where strong broadband emission is reaching the

photomultiplier (e.g. flame analysis of barium or incandescence from the
graphite furnace). Reducing the slit width reduces the emission by a factor
of four times but only halves the spectral energy.
Detector read out

A photomultiplier tube is almost exclusively used in atomic absorption as
the detector. This could be a narrow response type such as a Hamamatsu
R106 tube whose peak response is in the range of 185 to 500 nm, although
it can be used for wavelengths of up to 700 nm. More common however is
the use of wide range photomultiplier tubes with peak response of 185 to
850 nm, thereby eliminating the need to change PM tubes.
The detector ‘sees’, as well as the hollow cathode light, a component
caused by flame emission. As mentioned above, the output of the hollow
cathode lamp is coded by modulation. The electronics are synchronised to
this modulation rate so that only light of this frequency is detected. Figure
10 shows the output obtained from the photomultiplier with respect to time
for both single beam and double beam operation.

Reference Sample Beam
Lamp On -------------100%T--------------
Lamp Off
Dark Current and Flame Emission

Single Beam Double Beam
Figure 10: This diagram compares single beam and double beam
measurements. Note: With GBC asymmetric modulation, shown on right, twice
as long is spent measuring sample beam compared to reference beam
When the hollow cathode lamp is ON, the 100% transmittance level is set,
(0 ABS) and during the lamp OFF time, the 0% transmittance is set, despite
the fact that there is some output from the detector. This component of
output is caused by emission from the flame, stray light and dark current.
Correction for these factors is automatically performed during the lamp OFF
time. The display on the GBC spectrophotometers is a digital display of
absorbance or direct concentration. Transmission is used in the emission
mode.


Interferences

Interferences
Interference is classed as any process causing an erroneous result to be

obtained. Two categories are used for classification of interferences,
Spectral and Chemical.
Spectral interferences
Although atomic absorption spectra are very simple, there are a few cases
where line overlap is observed, some of these are given in Table 1.
Table 1
Element Wavelength Interferent Wavelength
Al 308.33 V 308.21*
Cu 324.75 Eu 324.76*
Fe 271.90 Pt 271.90*
Ga 403.30 Mn 403.31**
Hg 253.65 Co 253.65***
Mn 403.31 Ga 403.30**
Si 250.69 V 250.69*
* V.A. Fassel, J.A. Rasmuson and T.G. Cowley, Spectrochima Acta 23B,
579 (1968).
** J.E. Allen, Spectrochim Acta, 24B, 13, (1969).
*** D.C. Manning and F. Fernandez, Atomic Absorption Newsletter 7, 24
(1968).
The above type of interference is thankfully rare in atomic absorption
spectroscopy, however care should be taken in setting up a method to
identify possible interferences. Where they are found, alternate lines should
be used or the interferent removed chemically. Other forms of spectral
interference are:
1. A non-absorbing line or weakly absorbing line emitted by the hollow
cathode lamp is also passed by the monochromator.
2. Stray light.
3. Non-atomic absorbance (e.g. scattering of light or molecular
absorption).
The effect of an unresolved line or of stray light is to cause curvature of the
calibration curve. As stated previously the Lambert-Beer's law states:
It
Where I0 = Intensity of incident radiation emitted by the hollow cathode
lamp.
It = Intensity of transmitted radiation (amount not absorbed by the
sample).

Interferences
In the ideal case where there are enough free atoms to absorb all the
incident radiation, the resultant absorbance will be:
ABSORBANCE = log10 100 = ∞
0
This is not possible in typical systems, since there is always a part of the
radiation that cannot be absorbed, either because it is an unresolved non-
absorbing line adjacent to the absorbing line, or the light path does not
completely go through the flame, or due to stray or scattered light. In the
typical situation, the Lambert-Beer's law becomes:
I’t + K
where I’t = the absorbable radiation.
K = a non-absorbing component.
If we suppose the value of K is 1% (i.e. I’t = 99 max) we will have the
following results for the ideal and the typical system. At zero absorbance I’t
and It are maximum hence we have
IDEAL ABS = log10 100 = log10 1
100
=0
TYPICAL ABS = log10 100
= log10 1
99 + 1
=0
For a case of 50% transmittance we have

IDEAL ABS = log10 100 = 0.301
50
TYPICAL ABS = log10 100 = 0.292
50 + 1

IDEAL ABS = log10 100
= 1.000
10
TYPICAL ABS = log10 100
= 0.959
10 + 1
= 2.000
1
TYPICAL ABS = log10 100 = 1.699
1+1

=∞
0
ABS = log10 100 = 2.000
0+1

Interferences
As can be seen, the results differ more as the absorbance increases. The
maximum possible absorbance for the typical case above is 2.0 Abs. This
becomes even smaller with larger values of unabsorbable light (i.e. if K =
5% then we have
ABS = log10 100 = 1.301
0+5
so in this case an absorbance of 1.3 Abs is maximum).
If we graph the above results we obtain the trend as shown below in Figure
11.
Ideal Case
A
b Typical (1%)
s
o
r Typical (5%)
b
a
n
c
e
Concentration
Figure 11: Calibration curves shown with increasing absorbance
In spectroscopic analysis best precision is obtained at an absorption of
0.434 (36.8 %T). In atomic absorption the optimum working range is 0.2–
0.8 Abs. Where gross curvature and possible errors are minimised.
Non-atomic absorption correction

Non-atomic (continuum) absorption is the error caused by molecular
absorbance (either of the flame species or of the sample matrix) and light
scattered by solid particles in the optical path. Both effects are more
pronounced at the lower wavelengths (below 350 nm). The loss in light is
seen as an absorbance, because even the modulated light is thus affected,
and so erroneously high results are obtained, unless the error is corrected.
The method used in correcting for non-atomic absorption is to use a light
source that emits a continuum (broadband) output, as distinct to spectral
lamps emitting very narrow lines. There are two such light sources currently
used, a hydrogen continuum lamp in the same type of package as a hollow
cathode lamp and a deuterium arc lamp. Non-atomic absorption can be
corrected in two ways:
1. The samples are analysed with the hollow cathode lamp and then re-
analysed using a continuum source and the latter result subtracted
from the former. The limitation with this method is that the analysis
has to be performed twice, with the possibility of a varying non-atomic
absorption. This is particularly unacceptable in graphite furnace
analysis where the signal is not steady state.

Interferences
A modification of the above method is to use an adjacent non-

absorbing line not more than 2 nm away if the hydrogen lamp does
not have enough energy (i.e. Ba line 553.6 nm, Mo line 553.3 nm) or
a hydrogen lamp is not available.
2. Non-atomic absorbance measurement can be performed
simultaneously by using a continuum source during the OFF time of
the hollow cathode lamp. Since the output of the continuum lamp is
broad (limited by the slit width) compared to a spectral line (i.e. 0.001
nm or less compared to say 0.5 nm) the absorbance with the
continuum lamp is virtually only the background (in the case here a
difference of some 500 times). If the signal processing subtracts the
absorbance obtained with the continuum source from the absorbance
obtained with the hollow cathode lamp the resultant is the ‘true’
atomic absorption (neglecting the extremely small error above which
is insignificant compared with other errors encountered).
For accurate correction the optical paths of the hollow cathode lamp
and the continuum lamp must be accurately superimposed through
the sample compartment (either flame or graphite furnace), so that
the two beams are absorbed to a similar degree.
A hydrogen continuum lamp is commonly used to background correct
over the wavelength range 185–350 nm. This range is extended
slightly by the use of a deuterium arc lamp for the range 185–430
nm. The two continuum lamps have similar source diameters to
hollow cathode lamps and the light beams can be easily
superimposed for accurate correction.
NOTE:
Hydrogen continuum lamps have cathodes made of either nickel or
molybdenum. Care should be exercised when simultaneously background
correcting for these elements, since the spectrum of the cathode is
superimposed on the continuum.
Photron hydrogen continuum lamps are normally made of molybdenum
cathodes with a nickel cathode available on special request.
Chemical interferences
Matrix effects
Chemical interferences are those that influence the number of free atoms
reaching the optical path to be absorbed. Factors such as precipitation of
the sample prior to entry into the nebuliser are critical, as are the physical
characteristics of solutions, such as viscosity, surface tension, density, pH
and solvent vapour pressure, since all these parameters influence
nebulisation. For accurate results, the standards and samples should be
matched as closely as possible with respect to the above physical
parameters (better then 10%). Other forms of chemical interference are
stable compound formation and ionisation.

Interferences
Stable compound formation

Stable compound formation is responsible for many of the depressive
effects that are observed, both in atomic absorption and flame emission
spectrometry. It arises because the element forms a stable compound either
with a species in the matrix, (typical examples are the depression of
absorbances of alkaline earth metals in the presence of phosphate,
aluminate, silicate) or with a species in the flame such as aluminium,
vanadium, boron, etc. which form stable refractory oxides not broken down
in the cooler air-acetylene flame. Use of the high temperature nitrous oxide-
acetylene flame dissociates these refractory compounds. Alternatively a
releasing agent such as lanthanum or strontium will help to prevent the
formation of the refractory compounds.
Lanthanum works as a releasing agent by forming more stable compounds.
It is added in a sufficiently large quantity to complex the interferent. The use
of such releasing agents is given in the standard operating conditions for
each element.
Ionisation interference
The temperatures of the air-acetylene or nitrous oxide-acetylene flames may
cause appreciable ionisation of the analyte. To overcome the effect, an
easily ionisable element such as potassium, sodium or caesium is added at
levels of 1000 μg/mL – 4000 μg/mL to produce an excess of electrons in the
flame, thus inhibiting ionisation of the analyte. The calibration curve
obtained when ionisation occurs is shown in Figure 12. The upward
curvature is due to greater ionisation occurring at lower concentrations than
at higher concentrations. A list of ionisation potentials, and the degree of
ionisation of some of the elements are given in Table 2 below.
A
b
s s e
o
l Ca
r a
I de ca
l
b p i
a Ty
n
c
e
Concentration
Figure 12: Graph showing ideal Abs obtained in easily ionised solutions
compared to typical case

Interferences
TABLE 2
Element Ionisation Concentration DEGREE IONISATION (%)

Potential μg/mL
Air- Nitrous Oxide-
eV
Acetylene acetylene
Al 5.98 100 – 14
Ba 5.21 50 – 92
Be 9.32 2 – 0
Ca 6.11 2–5 – 4
Cs 3.89 27 73 –
K 4.34 4 38 –
La 5.61 1000 – 40
Mg 7.64 2 – 6
Na 5.14 2 12 –
Sr 5.69 5 13 84
Information on other elements can be found in the CRC Handbook of

Chemistry and Physics or CRC Handbook of Spectroscopy Volume 1.

Interferences

Optimisation techniques

Choice of wavelength
Most elements can be analysed at more than one wavelength, the choice of
which depends on a variety of factors:
1. Use of a line of sufficient intensity to give an acceptable signal-to-
noise ratio (for some elements the lamp spectrum is pure enough to
use a wider slit width, without introducing excessive curvature to the
calibration curve).
2. Use of a wavelength that does not require excessive dilution of the
sample.
3. Use of a line free from spectral interference and that also produces a
large linear range of the calibration curve.
Lamp current optimisation

Recommended currents given by the lamp manufacturer are generally the
best settings to use. The use of as low an operating current as possible is
advised in order to prolong the life of the lamp, and to minimise curvature
due to self absorption. However if the signal is noisy, a higher lamp current
will have to be used, taking care not to exceed the maximum current stated
by the manufacturer.
Bandpass optimisation
The bandpass is set to the maximum possible that does not cause excessive
curvature by the introduction of stray and unabsorbable radiation. A guide is
given in the optimum operating conditions for each element. In general, the
narrower the bandpass, the greater the absorbance and the more linear the
calibration curve.
The limiting factor is the loss of energy associated with very narrow
bandpasses, and the resultant need for high amplifier gains.
Optimisation of sample introduction system

The sample introduction system comprises: nebuliser, impact bead, spray
chamber, burner and flame. After optimising the wavelength and zeroing
the absorbance reading, the burner is adjusted by using the horizontal,
rotational, and vertical controls. The aim in adjusting the burner is to locate
the optimum position of the flame in the light beam.
NOTE:
The optimum position differs between absorbance and emission operation.
With emission, the burner is generally lower than for absorbance.

A quick and approximate optimisation of burner position is, without the

flame running, raise the burner until it starts to block the light path (seen by
an increase of absorbance on the digital display). Using a white card, trace
the light path along the burner, adjusting rotation and horizontal controls
until the burner slot is aligned with the beam. Lower the burner until it ‘just’
does not interfere. Final optimisation is performed for maximum absorbance
with the flame ignited and a standard aspirating. Optimisation of the vertical
control will be less critical than the horizontal, and rotational controls, since
these two effect the path length of the sample compartment. Only a few
degrees of rotation effects the absorbance signal dramatically.
Nebuliser adjustment varies the sample uptake rate, and therefore the
number of sample atoms reaching the light path. As stated previously, an
uptake of 3–6 mL/min is optimum for pneumatic nebulisers. Good practice
is to use an uptake of 2–4 mL/min for nitrous oxide-acetylene flames and 4–
6 mL/min for air-acetylene.
CAUTION:
Nebuliser adjustment on nitrous oxide-acetylene is not recommended, this is
best done on the air-acetylene flame.
Optimisation of the nebuliser is normally carried out with a 5 μg/mL Cu

solution (due to the minimal effect of flame conditions on the absorbance of
Cu). The most significant optimisation of the nebuliser with respect to good
absorbance and low noise, is the position of the impact bead. The optimum
position for the nebuliser is a gap of 0.4 mm (0.015 inch) between the bead
and the end of the venturi (the thickness of the burner cleaner).
Also of importance is the central location of the bead over the venturi
opening as shown in Figure 13. The bead position is factory set, and does
not normally have to be adjusted.
Correct Position Incorrect Position
Venturi
Bead
End View
Figure 13: Diagram showing correct position of glass bead compared to

venturi position

The function of the spray chamber is firstly to ensure thorough mixing of the
gases and aerosol, secondly to classify the aerosol droplets reaching the
burner. Oversized droplets are drained out ‘smoothly’ to minimise noise.
Periodically aspirating a detergent solution will maintain a clean surface for
efficient draining, and thus decrease noise. Use of a detergent in samples
and standards, to modify surface tension yielding improved nebulisation
efficiency is a helpful trick to remember. If using an organic solvent, the
spray chamber should be dried of water, and the solvent used in the drain-
trap in order to minimise noisy readings due to immiscibility problems.
Flame optimisation is performed by aspirating a standard and adjusting the
fuel control for optimum absorbance. Where interference is suspected, two
standards should be prepared, an aqueous standard and a standard in a
synthetic matrix and the flame conditions optimised so that both standards
absorb to the same extent. If this cannot be achieved the interference
should be investigated further (i.e. background correction, releasing agent
etc.) or the method of standard additions used.

Analytical procedures

As with other methods in analytical chemistry, the purest possible reagents

should be used to avoid contamination of the samples. The use of ‘AnalaR’,
or purer reagents is recommended. Solvents and chemicals used should be
aspirated as a blank to account for any possible contamination.
The most convenient method of obtaining standards for atomic absorption,
is the purchase of pre-prepared standards (usually a 1000 μg/mL
concentration). Preparation of standards from pure metals or oxides is
recommended when highly accurate analyses are required (pre-prepared
standards are generally accurate to ± 0.5%). Use pure metal wire, granules
or foil. Avoid using powders due to possible oxide formation on the powder
surface, which may be considerable and potentially cause huge errors.
Standards should be stored in concentrations of 500 μg/mL or higher in
plastic bottles made of polypropylene, polyethylene or Teflon. Glass should
be avoided, especially for low concentrations.
Calibration
Calibration curve
This is the most common method where interference effects are known to
be absent. Usually at least three standards and a blank are used to cover
the range 0.1 to 0.8 Abs. The calibration is performed by using the blank
solution to zero the instrument.
The standards are then analysed with the lowest concentration first, and the
blank run between standards, to ensure the baseline (zero point) has not
changed. Samples are then analysed and their absorbances recorded. A
graph of Absorbance versus Concentration is plotted and a typical curve is
shown in Figure 14.
A3
A
b
s
o A2
r
b AS
a
n
c A1
e Std1 Std2 Std3
C1 CS C2 C3
Concentration
Figure 14: Standard addition calibration curve

Where Al, A2, A3 = Absorbances of Standards 1, 2 and 3.

C1, C2, C3 = Concentration of Standards 1, 2 and 3.
As = Absorbance of sample.
Cs = Concentration of sample.
The above calibration can be performed in the concentration mode in which
case the concentration of the sample is read off directly.
Method of ultimate precision

Where ultimate precision is required, two standards are made giving
absorption very similar to the sample, in the range 0.4 to 0.6 Abs (one
slightly below and one slightly above the sample absorbance). Zero is set
using the low standard and 1.000 concentration with the high standard. If
the difference between the standards is small (say 0.10 Abs) a very
accurate reading can be made and a precision of 0.1% to 0.2% is possible.
The assumption is made of linearity of the calibration curve between the two
standards. If this is in doubt, intermediate standards should be made up as
well.
Method of standard additions

Where the matrix is difficult to match and extraction of the analyte or
interferent is impractical, or not possible, the method of standard additions
should be used. This method relies on the addition of a small known
amount of standard to an aliquot of sample. Two methods are commonly
used, a single addition with the result being calculated and a multiple
addition method where the results are plotted. In both cases it is important
to ensure:
1. The calibration curve is linear over the range of concentrations used.
2. Non-atomic absorbance is corrected for.
Single addition method

Two solutions, either a stock solution of the sample from which aliquots are
used, or individual amounts (volumes or weights) are needed (provided the
amounts taken are the same for both solutions). A known amount of
standard is added to one and an equivalent amount of blank to the other,
both solutions are made up to the same final volume. The result is given by
As x d
Cs =
As+d – As
Where Cs = Concentration of sample.
d = Concentration of added standard.
As = Absorbance of sample solution.
As+d = Absorbance of (sample plus standard) solution.
NOTE:
Cs has to be multiplied by the dilution factors to obtain the actual sample
concentration.

Multiple addition method

In this method four equal aliquots of the sample are taken and varying
amounts of standards are added to three of the aliquots, while blank is
added to the fourth. All aliquots are made up to the same final volume and
analysed. The additions are as follows:
Aliquot 1 2 3 4
Addition of Nil Approx 50% Approx 100% Approx 150%
Standard of expected of expected of expected
Results are plotted on an Absorbance versus Concentration curve that
extends the concentration axis to the left of zero as well as shown in Figure
15.
NOTE:
The concentration axis is labelled as added conc.
A4
A
b
s
o
r A3
b
a A2
n
c A1
e
Std1 Std2 Std3 Std4
CS C1 C2 C3 C4
Concentration
Figure 15: Standard additions plot showing relationship between additions

and Abs
Where S1 – S4 = Solutions 1–4.
A1 – A4 = Absorbances of solutions 1–4.
C1 – C4 = Added concentration (C1 = nil addition).
Cs = Extrapolated concentration of sample.
NOTE:
Cs has to be multiplied by the dilution factors to obtain the actual sample
concentration.
Secondary calibration
Where many similar samples have to be analysed by the method of
standard additions, one sample can be analysed fully by standard additions
and the resultant curve can be used as the calibration curve for the
remaining samples.

Terms and definitions

Terms and definitions
Sensitivity – The concentration of an element that will produce a

transmittance of 99% (absorbance of 0.0044), also known as reciprocal
sensitivity or characteristic concentration.
Detection limit – The minimum concentration of an element which can be
detected with 95% certainty. This is that quantity of the element which gives
a reading equal to twice the standard deviation of a series of at least 10
determinations at or near blank level.
Detection limit = 2 x Std. Dev. x Conc.

Mean Abs.
Optimum working range – The concentration range of an element that will
produce an absorbance range of 0.2 – 0.8 Abs.

Conversion factors and sample
calculations

Conversion factors and sample calculations
The traditional term used in atomic absorption spectroscopy to define the

concentration of a sample has been Parts Per Million, abbreviated to PPM
(atomic absorption spectroscopy was then considered a trace analysis
system). Current accepted terminology is μg/mL or mg/L although PPM is
still widely used (old habits die hard).
The following terms are all equivalent:
ppm, μg/mL, mg/L, ng/μl, μg/g, mg/kg.
To convert between the weight and volume terms:
μg/g = μg/mL ……………………………………1
D
Where D = specific gravity or relative density of solvent. To convert between
% of material and μg/g the relationship is:
μg/g = % Wt x 10000 …………………..………2
Example
A metal sample has to be determined for aluminium and the expected
content of aluminium is 80%. From the standard analytical data on
aluminium the optimum working range for the wavelength 396.2 nm is 25–
110 μg/mL. What sample weight and dilutions are required to be within the
concentration range?
Using equation 2
μg/g = 80 x 10000
= 800000
To bring this into the range, a dilution of 16000 is required for a 1 g sample
(i.e. assume the sample to absorb in the middle of the working range, so the
final concentration to aim for is 50 μg/mL). Hence:
800000 = 16000
50
A possible dilution sequence would entail dissolving an accurately weighed
0.5000 g sample to 1 litre, giving a dilution of 1000/0.5 = 2000 times. A 25
mL aliquot of this solution is further diluted to 200 mL, to give a final dilution
of
1000 x 200 = 16000
0.5 25

Recommended further reading

Recommended further reading
1. ATOMIC ABSORPTION SPECTROSCOPY 2nd edition

M. Slavin, Wiley – Interscience, New York.
2. FLAME EMISSION AND ATOMIC ABSORPTION SPECTROSCOPY
Vol 1. Theory.
Vol 2. Components and techniques.
Vol 3. Elements and matrices
J.A. Dean and T.C. Rains, Dekken, New York 1969, 1971, 1975.
3. ATOMIC ABSORPTION SPECTROPHOTOMETRY 2nd edition
W.T. Elwell and J.A.F. Gidley, Pergamon Press, Oxford 1966.
4. SPECTROCHEMICAL ANALYSIS BY ATOMIC ABSORPTION
W.J. Price, Heyden, London 1979.
5. ATOMIC ABSORPTION SPECTROSCOPY: APPLICATIONS IN
AGRICULTURE, BIOLOGY AND MEDICINE
G.D. Christian and J.J Feldman, Wiley – Interscience, New York 1970.
6. ATOMIC ABSORPTION SPECTROCHEMICAL ANALYSIS
B.V. L'vov, Adam Hilger, London 1970.
7. ATOMIC ABSORPTION SPECTROMETRY IN GEOLOGY
E.E. Angino and G.K. Billings, Elsevier, Amsterdam 1972.
8. ELECTROTHERMAL ATOMISATION FOR ATOMIC ABSORPTION
SPECTROMETRY
C.W. Fuller, Chemical Society, London 1972.
9. TOXIC METALS AND THEIR ANALYSIS
E. Berman, Heyden, London 1980.
10. APPLIED ATOMIC SPECTROSCOPY Volume 2
E.L. Grove, Plenum Press, New York 1972.

Standard analytical data of the
elements

Standard analytical data of the elements
The following pages provide analytical data. The sheets are arranged by
symbol in alphabetic order (e.g. potassium K precedes lanthanum La).
Index to Analytical Data

Element Symbol Page Element Symbol Page
Aluminium Al 53 Nickel Ni 87
Antimony Sb 98 Niobium Nb 85
Arsenic As 52 Osmium Os 88
Barium Ba 56 Palladium Pd 91
Beryllium Be 57 Phosphorus P 89
Bismuth Bi 58 Platinum Pt 93
Boron B 55 Potassium K 77
Cadmium Cd 60 Praseodymium Pr 92
Caesium Cs 63 Rhenium Re 95
Calcium Ca 59 Rhodium Rh 96
Chromium Cr 62 Rubidium Rb 94
Cobalt Co 61 Ruthenium Ru 97
Copper Cu 64 Samarium Sm 102
Dysprosium Dy 65 Scandium Sc 99
Erbium Er 66 Selenium Se 100
Europium Eu 67 Silicon Si 101
Gadolinium Gd 70 Silver Ag 51
Gallium Ga 69 Sodium Na 84
Germanium Ge 71 Strontium Sr 104
Gold Au 54 Tantalum Ta 105
Hafnium Hf 72 Tellurium Te 107
Holmium Ho 74 Terbium Tb 106
Indium In 75 Thallium Tl 109
Iridium Ir 76 Thulium Tm 110
Iron Fe 68 Tin Sn 103
Lanthanum La 78 Titanium Ti 108
Lead Pb 90 Tungsten W 113
Lithium Li 79 Uranium U 111
Lutetium Lu 80 Vanadium V 112
Magnesium Mg 81 Ytterbium Yb 115
Manganese Mn 82 Yttrium Y 114
Mercury Hg 73 Zinc Zn 116
Molybdenum Mo 83 Zirconium Zr 117
Neodymium Nd 85

SILVER (Ag) Atomic Wt. 107.868

Reagents for Standards Preparation
Aqueous: Silver metal wire 99.99%.
Silver nitrate AR.
Non-aqueous: Silver 4-cyclohexylbutyrate.
Silver 2-ethylhexanoate.
Preparation of 1000 μg/mL standard:
Dissolve 1.5748 g of AgNO3 in distilled water and dilute to 1 litre to obtain
1000 μg/mL Ag.
Atomic Absorption
Lamp current: 4.0 mA.
Flame type: Air-acetylene (oxidising).
Optimum
Wavelength Slit Width Working Range Sensitivity
nm nm μg/mL μg/mL
328.1 0.5 1.4 – 5.5 0.03

338.3 0.5 2.8 – 11 0.06
Interferences
Few interferences reported on air-acetylene flame.
Flame Emission
Wavelength: 328.1 nm.
Slit width: 0.2 nm.
Flame type: Nitrous oxide-acetylene.

ARSENIC (As) Atomic Wt. 74.922

Aqueous: Arsenious oxide (99.99%).
Dissolve 1.3203 g of dried As2O3 in the minimum volume of 20% NaOH
solution practicable and neutralise with nitric acid. Dilute to 1 litre to give
1000 μg/mL As.
Atomic Absorption
Flame type: Nitrous oxide-acetylene (Stoichiometric).
Optimum
nm nm μg/mL μg/mL
193.7 1.0 30 – 190 0.64

197.2 1.0 40 – 200 0.88
189.0 1.0 70 – 300 1.3
Interferences
Molecular absorption by the flame and solution species is considerable in the low ultraviolet
region. The background should be corrected by the use of a continuum lamp. Air-acetylene
has a higher sensitivity but is not as transparent as nitrous oxide-acetylene. Arsenic can
also be determined at the ultra trace levels using the hydride generation technique.
Emission
Arsenic is not normally determined by emission.

ALUMINIUM (Al) Atomic Wt 26.98

Aqueous: Aluminium metal foil or wire (99.99%).
Non-aqueous: Aluminium 4-cyclohexylbutyrate.
Aluminium 2-ethylhexanoate.
Dissolve 1.0000 g of Al in 25 mL of concentrated hydrochloric
acid and a few drops of concentrated nitric acid. Dilute to 1 litre to
give 1000 μg/mL Al.
Atomic Absorption
Flame type: Nitrous oxide-acetylene (slightly reducing).
Optimum
nm nm μg/mL μg/mL
396.2 0.5 25 – 110 0.55

309.3 0.5 25 – 135 0.55
308.2 0.5 35 – 160 0.70
237.3 0.5 140 – 580 2.8
236.7 0.5 180 – 725 3.8
Interferences
Aluminium is partially ionised in the nitrous oxide-acetylene flame. Add potassium nitrate or
chloride at a final concentration of 2000 μg/mL K to samples and standards to suppress
ionisation.
Flame Emission
Slit width: 0.2 nm.

GOLD (Au) Atomic Wt. 196.967

Aqueous: Gold metal foil (99.99%).
Dissolve 1.0000 g of gold in 20 mL of aqua regia (5 mL conc. nitric acid and
15 mL conc. hydrochloric acid) and dilute to 1 litre to obtain 1000 μg/mL Au.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
242.8 0.5 3.5 – 14 0.08

267.6 0.5 7.0 – 30 0.16
Interferences
Gold is readily ionised. Addition of potassium nitrate or chloride at a final concentration of
2000 μg/mL K will suppress ionisation. The method of standard additions is recommended
when the samples are of unknown matrix. Careful matrix matching is strongly recommended.
Flame Emission
Slit width: 0.2 nm.

BORON (B) Atomic Wt. 10.81

Aqueous: Boric Acid AR.
Di-sodium tetraborate AR.
Non-Aqueous: Methylborate.
Dissolve 8.8190 g of Na2B4O7.10H2O in distilled water and dilute to 1 litre to
give 1000 μg/mL B.
Atomic Absorption
Flame type: Nitrous oxide-acetylene (reducing).
Optimum
nm nm μg/mL μg/mL
249.8 0.2 340 – 1400 7.5

208.9 0.2 820 – 3300 18
Interferences
No major interferences reported. Flame stoichiometry and burner height should be carefully
adjusted.
Flame Emission
Slit width: 0.2 nm.

BARIUM (Ba) Atomic Wt. 137.34

Aqueous: Barium carbonate A.R.
Barium chloride A.R.
Non-aqueous: Barium 4-cyclohexylbutyrate.
Dissolve 1.4369 g of dry BaCO3 in 20 mL of 1N hydrochloric acid and dilute
to 1 litre to give 1000 μg/mL Ba.
Atomic Absorption
Flame type: Nitrous oxide-acetylene (oxidising).
Optimum
nm nm μg/mL μg/mL
553.6 0.5 8 – 30 0.18

350.1 0.2 4100 – 20000 90
Interferences
Barium is partially ionised in a nitrous oxide-acetylene flame. Add potassium nitrate or
chloride to give a final concentration of 2000 μg/mL K in samples and standards. Barium
emits strongly at the 553.6 nm line and causes ‘shot’ noise to be excessive at high
concentrations. Reducing the slit width to 0.2 nm and increasing the lamp current to 20 mA
will reduce this. Restricting the absorbance range to 0.2 – 0.6 Abs is also recommended.
Flame Emission
Slit width: 0.2 nm.

BERYLLIUM (Be) Atomic Wt. 9.012

Aqueous: Beryllium metal (99.99%).
Beryllium oxide (99.99%).
Beryllium sulphate (99.99%).
Dissolve 19.6555 g of BeSO4-4H2O in distilled water. Add 5 mL of conc.
Hydrochloric acid and dilute to 1 litre to give 1000 μg/mL Be.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
234.9 0.5 1–5 0.015
Interferences
Silicon, magnesium and sodium depress the absorbance. Aluminium interference is
reduced by the addition of hydrofluoric acid.
Flame Emission
Slit width: 0.2 nm.

BISMUTH (Bi) Atomic Wt. 208.981

Aqueous: Bismuth metal strip or wire (99.99%).
Dissolve 1.0000 g of bismuth in 50 mL of conc. nitric acid. Dilute to 1 litre to
give 1000 μg/mL Bi.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
223.1 0.2 9 – 36 0.2

222.8 0.2 36 – 150 0.7
306.8 0.2 36 – 150 0.8
227.7 0.2 270 – 1100 6.0
Interferences
No major interferences have been reported for bismuth. The Hydride generation technique
can be used to determine low levels.
Flame Emission
Slit width: 0.2 nm.

CALCIUM (Ca) Atomic Wt. 40.08

Aqueous: Calcium Carbonate AR.
Non-Aqueous: Calcium 2-ethylhexanoate.
Dissolve 2.497 g of dried CaCO3 in 25 mL of 1N hydrochloric acid and dilute to
1 litre to give 1000 μg/mL Ca.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
422.7 0.5 1–4 0.02

239.9 0.5 180 – 760 4.0
Interferences
Chemical interferences are common for air-acetylene. Addition of a releasing agent (2000–
5000 μg/mL strontium or lanthanum) helps to remove the interference, as does a lean
flame. In nitrous oxide-acetylene an ionisation buffer (2000 μg/mL potassium) is needed.
Flame Emission
Slit width: 0.2 nm.

CADMIUM (Cd) Atomic Wt. 112.40

Aqueous: Cadmium metal AR (99.99%).
Cadmium Oxide AR.
Cadmium Sulphate AR.
Non-aqueous: Cadmium 4-cyclohexylbutyrate.
Cadmium 2-ethylhexanoate.
Dissolve 1.0000 g of cadmium metal in 20 mL of 5N hydrochloric acid
containing 0.5 mL of conc. nitric acid and dilute to 1 litre to give 1000 μg/mL
Cd.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
228.8 0.5 0.2 – 1.8 0.009

326.1 0.5 180 – 800 4.0
Interferences
No major interferences reported for cadmium.
Flame Emission
Slit width: 0.2 nm.

COBALT (Co) Atomic Wt. 58.933

Aqueous: Cobalt metal (99.99%).
Non-aqueous: Cobalt 4-cyclohexylbutyrate.
Dissolve 1.0000 g of cobalt in minimum of 6N nitric acid and dilute to 1 litre to
give 1000 μg/mL Co.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
240.7 0.2 2.5 – 9 0.05

304.4 0.2 45 – 180 1.0
346.6 0.2 90 – 450 2.3
347.4 0.2 225 – 900 4.3
391.0 0.2 6300 – 27000 132
Interferences
Few interferences reported.
Flame Emission
Slit width: 0.2 nm.

CHROMIUM (Cr) Atomic Wt. 51.996

Aqueous: Chromium metal (99.99%).
Non-aqueous: Tris (1-phenyl-1,3-butanedione)chromium(III).
Dissolve 1.0000 g of chromium metal in 50 mL of conc. hydrochloric acid
and dilute to 1 litre to obtain 1000 μg/mL.
Atomic Absorption
Flame type: Air-acetylene (highly reducing).
Optimum
nm nm μg/mL μg/mL
357.9 0.2 2 – 15 0.05

359.3 0.2 4 – 20 0.09
360.5 0.2 5 – 30 0.10
425.4 0.2 7 – 40 0.17
428.9 0.2 15 – 60 0.35
Interferences
Iron, cobalt, nickel, barium, aluminium and sodium cause interference with chromium
absorbance. These effects are removed by the use of the nitrous oxide-acetylene flame.
Cr(iii) and Cr(vi) give different responses and it is best either to oxidise the species to Cr(vi) or
to reduce to Cr(iii).
Flame Emission
Slit width: 0.2 nm.

CAESIUM (Cs) Atomic Wt. 132.906

Aqueous: Caesium chloride AR.
Dissolve 1.2667 g of dried CsCl in distilled water and dilute to 1 litre to give
1000 μg/mL Cs.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
852.1 1.0 4 – 18 0.1

894.5 1.0 5 – 20 0.12
455.5 0.5 270 – 1000 5.3
459.3 0.2 900 – 3600 21.0
Interferences
Ionisation of caesium depresses the absorbance. Add potassium nitrate or chloride to give a
final concentration of 2000 μg/mL K to both samples and standards.
Flame Emission
Slit Width: 0 .2 nm.
Flame type: Air-acetylene.

COPPER (Cu) Atomic Wt. 63.54

Reagents For Standards Preparation
Aqueous: Copper metal foil or wire (99.99%).
Non-aqueous: Copper 4-cyclohexylbutyrate.
Dissolve 1.0000 g of copper in 50 mL of 6N nitric acid and dilute to 1 litre to
give 1000 μg/mL Cu.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
324.7 0.5 1–5 0.025

327.4 0.5 2.5 – 10 0.050
217.9 0.2 7.5 – 30 0.16
222.6 1.0 45 – 180 1.0
249.2 0.5 180 – 730 4.0
244.2 1.0 400 – 1700 9.0
Interferences
Few interferences have been reported for copper.
Flame Emission
Slit width: 0.2 nm.

DYSPROSIUM (Dy) Atomic Wt. 162.50

Aqueous: Dysprosium oxide AR.
Dissolve 1.1 476 g of Dy2O3 in 25 mL of 5N hydrochloric acid and dilute to 1
litre to give 1000 μg/mL Dy.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
421.2 0.2 25 – 90 0.5

419.5 0.2 45 – 180 1.0
419.2 0.2 550 – 2200 12.0
Interferences
Dysprosium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
nitrate or chloride to give a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

ERBIUM (Er) Atomic Wt. 167.26

Aqueous: Erbium metal (99.99%).
Erbium oxide AR.
Dissolve 1.1435 g of Er203 in 25 mL of 5N hydrochloric acid and dilute to 1 litre
to obtain 1000 μg/mL Er.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
400.8 0.2 30 – 125 0.7

389.3 0.2 130 – 510 2.8
408.8 0.2 220 – 880 4.8
Interferences
Erbium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate or
chloride to give a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

EUROPIUM (Eu) Atomic Wt. 151.96

Aqueous: Europium oxide AR.
Dissolve 1.1579 g of Eu2O3 in 10 mL of 6N nitric acid and dilute to 1 litre to
obtain 1000 μg/mL Eu.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
459.4 0.5 18 – 70 0.4

333.4 0.5 5400 – 22000 120
Interferences
Europium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate
or chloride to give a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

IRON (Fe) Atomic Wt. 55.847

Aqueous: Iron metal wire (99.99%).
Non-aqueous: Iron 4-cyclohexylbutyrate.
Dissolve 1.0000 g of iron in 20 mL of 5N hydrochloric acid and 5 mL of 6N
nitric acid and dilute to 1 litre to obtain 1000 μg/mL Fe.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
248.3 0.2 2–9 0.05

372.0 0.2 20 – 80 0.45
386.0 0.2 36 – 145 0.80
392.0 0.2 680 – 2700 15.0
Interferences
Slight depression caused by mineral acids, nickel and cobalt. Interference from citric acid
and other organic acids can be overcome with phosphoric acid.
Flame Emission
Slit width: 0.2 nm.

GALLIUM (Ga) Atomic Wt. 69.72

Aqueous: Gallium metal (99.99%).
Dissolve 1.0000 g of gallium in 50 mL of 6N nitric acid and dilute to 1 litre to
obtain 1000 μg/mL Ga.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
287.4 0.2 60 – 250 1.4

294.4 0.2 70 – 270 1.5
417.2 0.2 130 – 550 3.0
403.3 0.2 230 – 910 5.0
272.0 0.2 1300 – 5400 30.0
Interferences
No reported interferences except a drop of sensitivity if the acetylene cylinder pressure falls
below 700 kPa (100 psi).
Flame Emission
Slit width: 0.2 nm.

GADOLINIUM (Gd) Atomic Wt. 157.25

Aqueous: Gadolinium oxide AR.
Dissolve 1.1526 g of Gd2O3 in 20 mL of 5N hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Gd.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
407.9 0.2 700 – 2800 15.0

368.4 0.2 900 – 3700 20.0
405.8 0.2 1300 – 5000 28.0
Interferences
Gadolinium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
nitrate or chloride to give a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

GERMANIUM (Ge) Atomic Wt. 72.59

Aqueous: Germanium metal (99.99%).
Dissolve 1.0000 g in 20 mL of aqua regia (5 mL of conc. nitric acid and 15
mL of conc. hydrochloric acid) and dilute to 1 litre to obtain 1000 μg/mL Ge.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
265.2 0.5 70 – 280 1.5

271.0 0.5 145 – 580 3.2
275.5 0.5 145 – 580 3.2
269.1 0.5 300 – 1200 6.5
204.2 0.5 390 – 1600 8.5
303.9 0.5 1400 – 5400 30.0
Interferences
Flame Emission
Slit width: 0.2 nm.

HAFNIUM (Hf) Atomic Wt. 178.49

Aqueous: Hafnium metal (99.99%).
Dissolve 1.0000 g of hafnium in 5 mL of hydrofluoric acid and 5 mL of
distilled water. Add 10 mL of conc. nitric acid dropwise allowing time for the
reaction to subside between additions. Dilute to 1 litre to obtain 1000 μg/mL
Hf.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
307.3 0.2 450 – 1800 10

368.2 0.2 2600 – 10200 56
377.8 0.2 4500 – 18000 99
Interferences
Most metals interfere. Matrix matching of samples and standards even for minor
components is recommended or the method of standard additions should be used.
Presence of fluoride improves sensitivity.
Flame Emission
Slit width: 0.2 nm.

MERCURY (Hg) Atomic Wt. 200.59

Aqueous: Mercuric chloride AR.
Mercury metal (99.99%).
Dissolve 1.3535 g of mercuric chloride in water and dilute to 1 litre to obtain
1000 μg/mL Hg.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
253.7 0.5 73 – 290 1.6
Interferences
The presence of reducing agents such as stannous chloride and ascorbic acid may reduce
Hg(11) to Hg(1) or elemental mercury. Hg(1) and Hg(11) have different sensitivities. Addition
of stannous chloride to all standards and samples prior to analysis will overcome the
problem. The cold vapour technique can be used to determine Hg at trace levels.
Flame Emission
Slit width: 0.2 nm.

HOLMIUM (Ho) Atomic Wt. 164.930

Aqueous: Holmium oxide AR.
Dissolve 1.1455 g of Ho203 in 20 mL of 5N hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Ho.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
410.4 0.2 36 – 145 0.8

405.4 0.2 60 – 240 1.3
412.7 0.2 390 – 1550 8.5
425.4 0.2 3000 – 11800 64.0
Interferences
Holmium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate
or chloride to give a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

INDIUM (In) Atomic Wt. 1 14.82

Aqueous: Indium metal (99.99%).
Dissolve 1.0000 g of indium metal in 25 mL of 6N nitric acid and dilute to 1
litre to obtain 1000 μg/mL In.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
303.9 0.2 18 – 70 0.4

325.6 0.2 28 – 110 0.6
271.0 0.2 360 – 1450 8.0
Interferences
Indium is partially ionised in the air-acetylene flame. Addition of potassium nitrate or chloride
at a final concentration of 2000 μg/mL K will suppress ionisation. Sensitivity will drop if
acetylene cylinder pressure drops below 700 kPa (100 psi).
Flame Emission
Slit width: 0.2 nm.

IRIDIUM (Ir) Atomic Wt. 192.22

Aqueous: Iridium powder (99.99%).
Ammonium chloroiridate AR.
Dissolve 2.2943 g of (NH4)2lrCl6 in water and dilute to 1 litre to obtain 1000
μg/mL Ir.
Atomic Absorption
Flame type: Air-acetylene (reducing).
Optimum
nm nm μg/mL μg/mL
208.9 0.2 130 – 550 3.0

263.9 0.2 260 – 1100 6.0
264.0 0.2 260 – 1100 6.0
266.5 0.2 450 – 1800 10
254.4 0.2 680 – 2700 15
Interferences
Interferences with iridium are extremely diverse. Lanthanum at 1000 μg/mL and sodium and
copper at 1% levels are used to overcome interferences.
Flame Emission
Slit width: 0.2 nm.

POTASSIUM (K) Atomic Wt. 39.102

Aqueous: Potassium chloride AR.
Non-aqueous: Potassium 4-Cyclohexylbutyrate.
Dissolve 1.9067 g of dry KCl in distilled water and dilute to 1 litre to obtain
1000 μg/mL K.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
766.5 0.5 0.4 – 1.5 0.008

769.9 0.5 1.1 – 4.4 0.024
404.4 0.2 145 – 580 3.2
Interferences
Ionisation in the air-acetylene flame is reduced by addition of caesium, sodium or rubidium at
levels of 1000 to 2000 μg/mL.
Flame Emission
Slit width: 0.2 nm.

LANTHANUM (La) Atomic Wt. 138.906

Aqueous: Lanthanum oxide AR.
Preparation of 1000 μg/ mL standard:
Dissolve 1.1728 g of La203 in 20 mL of 5N hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL La.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
550.1 0.2 1800 – 7300 40

357.4 0.2 4550 – 18200 100
403.7 0.2 12000 – 47000 260
Interferences
Lanthanum is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
nitrate or chloride at a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

LITHIUM (Li) Atomic Wt. 6.939

Aqueous: Lithium sulphate AR.
Lithium carbonate AR.
Non-aqueous: Lithium 4-cyclohexylbutyrate.
Dissolve 9.2200 g of Li2SO4H2O in water and dilute to 1 litre to obtain 1000
μg/mL Li.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
670.8 0.5 1–4 0.02

323.3 0.2 365 – 1460 8.0
610.4 0.5 3100 – 13000 68
Interferences
Ionisation of lithium causes depression of absorbance. Addition of potassium nitrate or
chloride to give a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Wavelength: 670.8.
Slit width: 0.2 nm.

LUTETIUM (Lu) Atomic Wt. 174.97

Aqueous: Lutetium oxide (99.99%).
Dissolve 1.1372 g of Lu2O3 in 25 mL of 6N nitric acid and dilute to 1 litre to
obtain 1000 μg/mL Lu.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
336.0 0.5 320 – 1300 7.0

356.8 0.5 530 – 2100 11.5
331.2 0.5 730 – 2900 16.0
337.7 0.5 850 – 3400 18.6
Interferences
Lutetium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate
or chloride at a final concentration of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

MAGNESIUM (Mg) Atomic Wt. 24.312

Aqueous: Magnesium metal ribbon, or turnings (99.99%).
Dissolve 1.0000 g of magnesium metal in 50 mL of 5N hydrochloric acid
and dilute to 1 litre for 1000 μg/mL Mg.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
285.2 0.5 0.1 – 0.4 0.003

202.6 1.0 5 – 20 0.1
Interferences
Chemical interferences are common for the air-acetylene flame. Addition of a releasing agent
(2000 – 5000 μg/mL strontium or lanthanum) helps to remove the interference. In the nitrous
oxide-acetylene flame an ionisation buffer (2000 μg/mL K) is needed.
Flame Emission
Slit width: 0.2 nm.

MANGANESE (Mn) Atomic Wt. 54.938

Aqueous: Manganese metal wire or foil.
Non-aqueous: Manganese 4-Cyclohexylbutyrate.
Dissolve 1.0000 g of manganese in 50 mL of 6N nitric acid and dilute to 1
litre to obtain 1000 μg/mL Mn.
Atomic Absorption
Flame type: Air-acetylene (Stoichiometric).
Optimum
nm nm μg/mL μg/mL
279.5 0.2 1 – 3.6 0.02

279.8 0.2 1–4 0.022
280.1 0.2 1.4 – 5.5 0.03
403.1 0.2 7 – 27 0.15
Interferences
No reported interferences in an oxidising air-acetylene or a nitrous oxide-acetylene flame.
Flame Emission
Slit width: 0.2 nm.

MOLYBDENUM (Mo) Atomic Wt. 95.94

Aqueous: Ammonium molybdate AR.
Molybdenum trioxide AR.
Dissolve 1.5003 g of MoO3 in 10 mL of conc. hydrochloric acid and dilute to
1 litre to obtain 1000 μg/mL Mo.
Atomic Absorption
Flame type: Nitrous oxide-acetylene (reducing, slightly luminous).
Optimum
nm nm μg/mL μg/mL
313.3 0.2 5 – 20 0.11

317.0 0.2 8 – 30 0.17
319.4 0.2 10 – 42 0.23
320.9 0.2 90 – 360 2.0
Interferences
Addition of an excess of a refractory element such as aluminium at a level of 1000 μg/mL Al
acts as a releasing agent for Mo.
Flame Emission
Slit width: 0.2 nm.

SODIUM (Na) Atomic Wt. 22.99

Aqueous: Sodium chloride AR.
Sodium carbonate AR.
Non-aqueous: Sodium 4-cyclohexylbutyrate.
Dissolve 2.5420 g of dry NaCl in distilled water and dilute to 1 litre to obtain
1000 μg/mL Na.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
589.0 0.5 0.18 – 0.7 0.004

589.6 0.5 0.4 – 1.5 0.008
330.2
330.4 } 0.5 100 – 380 2.1
Interferences
Sodium is partially ionised in the air-acetylene flame. Addition of caesium or potassium
chloride at a final concentration of 2000 μg/mL K or Cs will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

NIOBIUM (Nb) Atomic Wt. 92.906

Reagrents for Standards Preparation
Aqueous: Niobium metal (99.99%).
Dissolve 1.0000 g in 5 mL of hydrofluoric acid (40%) and 5 mL of water. Add
dropwise 10 mL of conc. nitric acid. Dilute to 1 litre to obtain 1000 μg/mL Nb.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
334.9 0.2 910 – 3700 20

358.0 0.2 1000 – 4000 22
408.0 0.2 1090 – 4400 24
405.9 0.2 1090 – 4400 24
Interferences
Ionisation of niobium is suppressed by the addition of potassium nitrate or chloride at a level
of 2000 μg/mL K.
Flame Emission
Slit width: 0.2 nm.

NEODYMIUM (Nd) Atomic Wt. 144.24

Aqueous: Neodymium oxide AR.
Dissolve 1.1664 of Nd2O3 in 10 mL of conc. hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Nd.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
463.4 0.2 220 – 870 4.8

492.5 0.2 270 – 1100 6.0
471.9 0.2 450 – 1900 10.0
Interferences
Ionisation in the nitrous oxide-acetylene flame can be reduced by addition of potassium
nitrate or chloride at a final concentration of 2000 μg/mL K. Silicon, aluminium, iron and
fluoride depress the signal.
Flame Emission
Slit width: 0.2 nm.

NICKEL (Ni) Atomic Wt. 58.71

Aqueous: Nickel metal (99.99%).
Non-aqueous: Nickel 4-cyclohexylbutyrate.
Dissolve 1.0000 g of nickel metal in 50 mL of 6N nitric acid and dilute to 1
litre to obtain 1000 μg/mL Ni.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
232.0 0.2 1.8 – 8 0.04

341.5 0.2 6 – 25 0.12
352.4 0.5 6 – 28 0.14
351.5 0.5 20 – 80 0.4
Interferences
The two lines 341.5 nm and 352.4 nm are preferred for routine analysis over the 232.0 nm
line due to excessive curvature caused by an unresolved non-resonance line at 232.14 rim.
Non-atomic absorbance is not as great at 341.5 nm as it is at 232.0 nm.
Flame Emission
Slit width: 0.2 nm.

OSMIUM (Os) Atomic Wt. 190.2

Aqueous: Osmium tetroxide AR.
Dissolve 1.3365 g of OsO4 in 100 mL of 4N sodium hydroxide and dilute to 1
litre to obtain 1000 μg/mL Os.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
290.9 0.2 46 – 180 1.0

426.1 0.2 730 – 2900 16
Interferences
No major interferences reported.
Flame Emission
Slit width: 0.2 nm.

PHOSPHORUS (P) Atomic Wt. 30.974

Aqueous: Phosphoric acid.
Dissolve 3.1638 g of H3PO4 in 1 litre of distilled water to give 1000 μg/mL P.
Atomic Absorption
Flame type: Nitrous Oxide-acetylene (strongly reducing).
Optimum
nm nm μg/mL μg/mL
213.6 0.5 2000 – 20000 100
Interferences
Flame Emission
Phosphorus is not normally determined by emission.

LEAD (Pb) Atomic Wt. 207.19

Aqueous: Lead metal shot or sheet (99.99%).
Non-aqueous: Lead 4-cyclohexylbutyrate.
Dissolve 1.0000 g of lead in 20 mL of 6N nitric acid and dilute to 1 litre to
obtain 1000 μg/mL Pb.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
217.0 1.0 2.5 – 20 0.06

283.3 0.5 7.0 – 50 0.16
261.4 0.5 100 – 460 2.5
Interferences
Few interferences reported. Non-atomic absorbance correction may be required at the 217.0
nm wavelength. The 283.3 nm line is often preferred for routine analysis.
Flame Emission
Wavelength: 405.8 nm,
Slit width: 0.2 nm.

PALLADIUM (Pd) Atomic Wt. 106.4

Aqueous: Ammonium tetrachioropalladate (11) AR.
Dissolve 2.6719 g of (NH4)2PdCl4 in distilled water and dilute to 1 litre to obtain
1000 μg/mL Pd.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
244.8 0.2 3 – 11 0.06

247.6 0.2 4 – 15 0.08
340.5 1.0 20 – 80 0.44
Interferences
Use of lanthanum (5000 μg/mL) or EDTA (0.01 M) is used to eliminate interference from
aluminium, cobalt, nickel and the noble metals.
Flame Emission
Slit width: 0.2 nm.

PRASEODYMIUM (Pr) Atomic Wt. 140.908

Aqueous: Praseodymium oxide AR.
Dissolve 1.1703 g of Pr2O3 in 10 mL of conc. hydrochloric acid and dilute
to 1 litre to obtain 1000 μg/mL Pr.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
495.1 0.2 910 – 3650 20.0

513.3 0.2 1820 – 7300 40.0
473.7 0.2 2050 – 8200 45.0
Interferences
Ionisation in the nitrous oxide-acetylene flame is reduced by the addition of potassium nitrate
or chloride at a final concentration of 2000 μg/mL K.
Flame Emission
Slit width: 0.2 nm.

PLATINUM (Pt) Atomic Wt. 195.09

Aqueous: Ammonium hexachioroplatinate (IV) AR.
Dissolve 2.2753 g of (NH4)2PtCl6 in distilled water and dilute to 1 litre to obtain
1000 μg/mL Pt.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
266.0 0.2 46 – 185 1.0

306.5 0.2 95 – 211 2.1
283.0 0.2 155 – 620 3.4
293.0 0.2 170 – 680 3.7
299.8 0.2 280 – 1100 6.0
271.9 0.2 380 – 1500 8.2
Interferences
Most noble metals interfere with platinum absorbance. The addition of 1% copper and 1%
lanthanum eliminate the interference.
Flame Emission
Slit width: 0.2 nm.

RUBIDIUM (Rb) Atomic Wt. 85.468

Aqueous: Rubidium Chloride AR.
Dissolve 1.4154 g of dry RbCl in distilled water and dilute to 1 litre to obtain
1000 μg/mL Rb.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
780.0 0.2 2–9 0.05

794.8 0.2 5 – 20 0.11
420.2 0.2 220 – 890 4.88
421.6 0.2 640 – 2600 14.0
Interferences
Ionisation in the air-acetylene flame is reduced by addition of potassium nitrate or chloride at a
final concentration of 2000 μg/mL K.
Flame Emission
Slit width: 0.2 nm.

RHENIUM (Re) Atomic Wt. 186.2

Aqueous: Potassium perrhenate (VII) (99.99%).
Ammonium perrhenate (VII) (99.99%).
Dissolve 1.5537 g of KReO4 in distilled water and dilute to 1 litre to obtain
1000 μg/mL Re.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
346.1 0.2 450 – 1820 10.0

346.5 0.2 780 – 3100 17.0
345.2 0.2 1100 – 4400 24.0
Interferences
Standards should be matrix matched to samples or method of standard additions used to
overcome possible interference from aluminium, barium, calcium, iron and magnesium.
Flame Emission
Slit width: 0.2 nm.

RHODIUM (Rh) Atomic Wt. 102.906

Aqueous: Ammonium chlororhodite AR.
Dissolve 3.8570 g of (NH4)3RhCl6 1.½H2O) in 50 mL of 10% hydrochloric acid
and dilute to 1 litre to obtain 1000 μg/mL Rh.
Atomic Absorption
Lamp current: 5.OmA.
Optimum
nm nm μg/mL μg/mL
343.5 0.5 4.5 – 18 0.10

369.2 0.2 8.0 – 31 0.17
339.7 0.2 11 – 45 0.25
350.2 0.2 18 – 73 0.40
370.1 0.2 40 – 110 0.85
328.1 0.2 430 – 1800 9.50
Interferences
Other noble metals interfere slightly and most anions depress the absorbance. Addition of
3% sodium sulphate reduces interference from anions.
Flame Emission
Slit width: 0.2 nm.

RUTHENIUM (Ru) Atomic Wt. 101.07

Aqueous: Ruthenium chloride AR.
Dissolve 2.0523 g of dry RuCl3 in 20 mL of 5N hydrochloric acid and dilute to
1 litre to obtain 1000 μg/mL Ru.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
349.9 0.2 23 – 90 0.50

372.8 0.2 34 – 140 0.75
379.9 0.2 70 – 280 1.5
392.6 0.2 270 – 1100 5.9
Interferences
Platinum, rhodium, lanthanum and hydrochloric acid increase the ruthenium absorbance.
Uranyl nitrate (4% W/V uranium) can be used as a releasing agent as can a mixture of
0.5% copper sulphate and 0.5% cadmium sulphate.
Flame Emission
Slit width: 0.2 nm.

ANTIMONY (Sb) Atomic Wt. 121.75

Aqueous: Antimony metal granul (99.99%).
Potassium antimonyl tartrate (99.99%).
Dissolve 1.0000 g of antimony in 10 mL of conc. hydrochloric acid, 1 mL of
conc. nitric acid and 10 g of tartaric acid, and dilute to 1 litre to obtain 1000
μg/mL Sb. Further dilutions should be made in 1% tartaric acid or 10%
hydrochloric acid to prevent precipitation of antimony oxychlorides.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
217.6 0.2 11 – 50 0.26

206.8 0.2 13 – 54 0.3
231.2 0.5 22 – 90 0.61
212.7 1.0 90 – 360 1.8
Interferences
Copper and lead interfere at high levels due to line overlap (lead line is 217.0 nm and copper
line is 217.9 nm). Use of the 206.8 nm line is preferred. The hydride generation technique
can be used to determine antimony at trace levels.
Flame Emission
Slit width: 0.2nm.

SCANDIUM (Sc) Atomic Wt. 44.956

Aqueous: Scandium oxide AR.
Dissolve 1.5338 g of Sc2O3 in 10 mL of 5N hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Sc.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
391.2 0.2 14 – 55 0.30

390.8 0.2 17 – 65 0.36
402.4 0.2 19 – 80 0.42
402.0 0.2 25 – 100 0.54
327.0 0.2 55 – 220 1.2
408.2 0.2 110 – 440 2.4
327.4 0.2 200 – 820 4.5
Interferences
Scandium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
Flame Emission
Slit width: 0.2 nm.

SELENIUM (Se) Atomic Wt. 78.96

Aqueous: Selenium metal pellets 99.99%.
Dissolve 1.0000 g of selenium metal in 20 mL of aqua regia (15 mL conc.
hydrochloric acid and 5 mL of conc. nitric acid) and dilute to 1 litre to obtain
1000 μg/mL Se.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
196.0 1.0 45 – 185 1.0

204.0 0.5 140 – 550 3.0
206.3 0.5 590 – 2400 13.0
207.5 0.5 2100 – 8200 45.0
Interferences
Non-atomic absorption by molecular species in the flame and solutions have to be
corrected by use of a continuum lamp. Selenium can be analysed in trace levels by the
hydride generation method.
Flame Emission
Selenium is not normally determined by flame emission.

SILICON (Si) Atomic Wt. 28.086

Aqueous: Silicon dioxide AR.
Non-aqueous: Octaphenylcyclotetrasiloxane Preparation of 1000 μg/mL standard:
Fuse 2.139 g of silicon dioxide with 10 g of sodium carbonate in
a platinum crucible. Dissolve in distilled water and dilute to 500
mL to obtain 1000 μg/mL Si.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
251.6 0.2 68 – 275 1.5

250.7 0.2 190 – 750 4.1
251.4 0.2 190 – 770 4.2
252.4 0.2 190 – 770 4.2
288.2 0.2 1090 – 4400 24.0
Interferences
Ionisation of silicon in the nitrous oxide-acetylene flame can be suppressed by addition of
sodium chloride at a level of 2000 μg/mL Na.
Flame Emission
Slit width: 0.2 nm.

SAMARIUM (Sm) Atomic Wt. 150.4

Aqueous: Samarium oxide.
Dissolve 1.1596 g of Sm2O3 in 10 mL of 5N hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Sm.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
429.7 0.2 280 – 1100 6.0

476.0 0.2 380 – 1550 8.4
520.1 0.2 440 – 1800 9.6
Interferences
Samarium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
Flame Emission
Slit width: 0.2 nm.

TIN (Sn) Atomic Wt. 118.69

Aqueous: Tin metal (99.99%).
Dissolve 1.0000 g of tin in 150 mL of conc. hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Sn.
Atomic Absorption
Flame type: Nitrous oxide-acetylene (reducing slightly luminous).
Optimum
nm nm μg/mL μg/mL
235.5 0.5 35 – 135 0.72

286.3 0.5 45 – 170 0.93
224.6 0.2 70 – 100 1.45*
233.5 0.5 200 – 700 3.67
266.1 0.5 980 – 3900 21.60
* The calibration curve is curved at higher concentrations and is of little use.

Interferences
Interferences are minimised in the nitrous oxide-acetylene flame. Tin can also be determined
using the hydride generation method.
Flame Emission
Slit width: 0.2 nm.

STRONTIUM (Sr) Atomic Wt. 87.62

Aqueous: Strontium carbonate AR.
Non-aqueous: Strontium 4-cyclohexylbutyrate.
Dissolve 1.6848 g of SrCO3 in 10 mL of 6N nitric acid and dilute to 1 litre to
obtain 1000 μg/mL Sr.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
460.7 0.2 2–8 0.04
Interferences
Strontium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate
Flame Emission
Slit width: 0.2 nm.

TANTALUM (Ta) Atomic Wt. 180.948

Aqueous: Tantalum pentachloride AR.
Tantalum metal 99.99%.
Dissolve 1.0000 g of tantalum metal in 10 mL of hydrofluoric acid (40%),
add 5 mL of water and 10 mL of conc. nitric acid dropwise. Dilute to 1 litre
to obtain 1000 μg/mL Ta.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
271.5 0.2 450 – 1850 10.0

275.8 0.2 2400 – 9500 52.0
Interferences
Iron, ammonium and fluoride improve the response. Add 0.1N ammonium fluoride to both
samples and standards.
Flame Emission
Slit width: 0.2 nm.

TERBIUM (Tb) Atomic Wt. 158.925

Aqueous: Terbium oxide AR.
Terbium metal (99.99%).
Dissolve 1.1762 g of Tb4O7 in 10 mL of 5N hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Tb.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
432.7 0.2 360 – 1500 8.0

431.9 0.2 470 – 1900 10.2
433.9 0.2 850 – 3400 18.6
Interferences
Terbium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate
Flame Emission
Slit width: 0.2 nm.

TELLURIUM (Te) Atomic Wt. 127.60

Aqueous: Tellurium metal chips (99.99%).
Dissolve 1.0000 g of tellurium in 20 mL of aqua regia (15 mL of conc.
hydrochloric acid and 5 mL of conc. nitric acid) and dilute to 1 litre for 1000
μg/mL Te.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
214.3 0.5 11 – 46 0.25

225.9 0.5 170 – 700 3.75
238.6 0.2 570 – 2300 12.5
Interferences
No severe interferences reported for tellurium. Tellurium can be determined at trace levels
by use of the hydride generation technique.
Flame Emission
Slit width: 0.2 nm.

TITANIUM (Ti) Atomic Wt. 47.90

Aqueous: Titanium metal (99.99%).
Dissolve 1.0000 g of titanium metal in 10 mL of hydrofluoric acid (40%) and
add 10 mL of water. Dropwise add 10 mL of nitric acid and dilute to 1 litre to
obtain 1000 μg/mL Ti.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
364.3 0.2 50 – 200 1.1

365.4 0.2 55 – 220 1.2
320.0 0.2 65 – 260 1.4
399.0 0.2 150 – 600 3.2
Interferences
Titanium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate
or chloride at a level of 1000–2000 μg/mL K suppresses ionisation. Aluminium, iron and
fluoride enhance titanium absorbance. Solutions are made up in 0.1% Al and 0.1% K.
Flame Emission
Slit width: 0.2 nm.

THALLIUM (Tl) Atomic Wt. 204.37

Aqueous: Thallium Sulphate AR.
Dissolve 1.2350 g of Tl2S04 in distilled water and dilute to 1 litre to obtain
1000 μg/mL Tl.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
276.8 0.5 16 – 65 0.35

377.6 0.5 50 – 200 1.1
237.9 0.5 110 – 450 2.4
258.0 0.5 400 – 1600 8.8
Interferences
No major interferences reported. Thallium is partially ionised in the nitrous oxide-acetylene
flame. Addition of potassium nitrate or chloride at a final concentration of 2000 μg/mL K will
suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

THULIUM (Tm) Atomic Wt. 168.934

Aqueous: Thulium oxide AR.
Dissolve 1.1421 g of Tm203 in 20 mL of 5N hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Tm.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
371.8 0.5 14 – 55 0.3

410.6 0.5 23 – 95 0.5
420.4 0.5 40 – 165 0.9
436.0 0.5 140 – 550 3.0
341.0 0.5 200 – 850 4.5
Interferences
Thulium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate
Flame Emission
Slit width: 0.2 nm.

URANIUM (U) Atomic Wt. 238.092

Aqueous: Uranyl nitrate AR.
Dissolve 2.033 g of UO2(NO3)2.6H20 in distilled water and dilute to 1 litre to
obtain 1000 μg/mL U.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
358.5 0.2 4500 – 18500 100

356.7 0.2 7000 – 28000 150
351.5 0.2 9600 – 39000 210
348.9 0.2 14000 – 55000 300
Interferences
Uranium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
nitrate or chloride at a level of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

VANADIUM (V) Atomic Wt. 50.942

Aqueous: Vanadium metal 99.99%.
Vanadium pentoxide.
Non-aqueous: Vanadium oxobis (1-phenyl-1,3-butanedionate).
Dissolve 1.0000 g of vanadium metal in 50 mL of conc. nitric acid and
dilute to 1 litre to obtain 1000 μg/mL V.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
}
318.3
318.4 0.2 20 – 90 0.5
318.5
306.6 0.2 50 – 200 1.1
439.0 0.5 200 – 800 4.4
Interferences
Vanadium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
nitrate or chloride at a final concentration of 2.000 μg/mL K suppresses ionisation. Addition of
excess aluminium (2000 μg/mL Al) or titanium removes interferences.
Flame Emission
Slit width: 0.2 nm.

TUNGSTEN (W) Atomic Wt. 183.85

Aqueous: Tungsten metal (99.99%).
Sodium tungstate AR.
Dissolve 1.7940 g of Na2WO4.2H2O in distilled water and dilute to 1 litre with
1% sodium hydroxide to obtain 1000 μg/mL W.
Atomic Absorption
Flame type: Nitrous oxide-acetylene (reducing slightly luminous).
Optimum
nm nm μg/mL μg/mL
255.1 0.2 260 – 1100 5.8

268.1 0.2 500 – 1900 10.4
400.9 0.5 670 – 2700 14.7
Interferences
The use of the 400.9 nm line is recommended for routine analysis because of the better
signal to noise ratio obtained. Standards should be matrix matched to samples or the method
of standard additions used.
Flame Emission
Slit width: 0.2 nm.

YTTRIUM (Y) Atomic Wt. 88.906

Aqueous: Yttrium oxide 99.99%.
Dissolve 1.270 g Y203 in 20 mL of conc. hydrochloric acid and dilute to 1 litre
to obtain 1000 μg/mL Y.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
410.2 0.2 90 – 370 2.0

407.7 0.2 140 – 550 3.0
414.3 0.2 200 – 800 4.4
Interferences
Yttrium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium nitrate or
chloride at a final concentration of 2000 μg/mL K will suppress ionisation. Samples and
standards should be matrix matched or the method of standard additions used.
Flame Emission
Slit width: 0.2 nm.

YTTERBIUM (Yb) Atomic Wt. 173.04

Aqueous: Ytterbium oxide AR.
Dissolve 1.1387 g of Yb203 in 20 mL of conc. hydrochloric acid and dilute to 1
litre to obtain 1000 μg/mL Yb.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
398.8 0.5 4 – 15 0.08

246.5 0.2 30 – 110 0.6
267.2 0.2 200 – 750 4.0
Interferences
Ytterbium is partially ionised in the nitrous oxide-acetylene flame. Addition of potassium
nitrate or chloride at a final level of 2000 μg/mL K will suppress ionisation.
Flame Emission
Slit width: 0.2 nm.

ZINC (Zn) Atomic Wt. 65.37

Aqueous: Zinc metal (99.99%).
Non-aqueous: Zinc 4-cyclohexylbutyrate.
Dissolve 1.0000 g of zinc metal in 40 mL of 5N hydrochloric acid and dilute
to 1 litre to obtain 1000 μg/mL Zn.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
213.9 0.5 0.4 – 1.5 0.008

307.6 0.5 3000 – 12000 66
Interferences
Non-atomic absorption should be corrected at 213.9 by use of a continuum lamp.
Flame Emission
Slit width: 0.2 nm.

ZIRCONIUM (Zr) Atomic Wt. 91.22

Aqueous: Zirconium metal (99.99%).
Dissolve 1.0000 g of zirconium in 10 mL of hydrofluoric acid (40%) and 10
mL of water. Add dropwise 10 mL of conc. nitric acid and dilute to 1 litre to
obtain 1000 μg/mL Zr.
Atomic Absorption
Optimum
nm nm μg/mL μg/mL
360.1 0.2 410 – 1650 9.0

303.1 0.2 620 – 2500 13.5
354.8 0.2 660 – 2600 14.4
301.2 0.2 750 – 3000 16.2
298.5 0.2 820 – 3300 18.0
468.8 0.2 3400 – 14000 74
Interferences
Addition of 0.2% ammonium fluoride reduces interference from chloride, fluoride, iron and
ammonia.
Flame Emission
Wavelength: 360.1
Slit width: 0.2 nm.

01-0019-01 Flame Methods Manual For AA

Uploaded by

Copyright:

Available Formats

01-0019-01 Flame Methods Manual For AA

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

01-0019-01 Flame Methods Manual For AA

Uploaded by

Copyright:

Available Formats

AAS AAS

FLAME METHODS MANUAL

Each GBC instrument has a unique serial number.

GBC Scientific Equipment Pty Ltd

A.C.N. 005 472 686

Telephone: 61 3 9588 6666

GBC Flame Methods Manual for Atomic Absorption 3

4 GBC Flame Methods Manual for Atomic Absorption

GBC Flame Methods Manual for Atomic Absorption 5

6 GBC Flame Methods Manual for Atomic Absorption

GBC Flame Methods Manual for Atomic Absorption 7

This page is left blank intentionally

8 GBC Flame Methods Manual for Atomic Absorption

GBC Flame Methods Manual for Atomic Absorption 9

Flame spectroscopy is an analytical technique used for the qualitative and

Flame emission spectroscopy

Atomic absorption spectroscopy

10 GBC Flame Methods Manual for Atomic Absorption

Atomic Absorption is similar to Ultra-Violet Spectroscopy in that similar

Atomic fluorescence spectroscopy

GBC Flame Methods Manual for Atomic Absorption 11

This page is left blank intentionally

12 GBC Flame Methods Manual for Atomic Absorption

GBC Flame Methods Manual for Atomic Absorption 13

Hollow cathode lamps

Figure 1: Hollow cathode lamp construction

14 GBC Flame Methods Manual for Atomic Absorption

Lamp Current (mA)

Figure 2: Absorbance versus lamp current

GBC Flame Methods Manual for Atomic Absorption 15

Figure 3: Flame atomisation system

16 GBC Flame Methods Manual for Atomic Absorption

GBC Flame Methods Manual for Atomic Absorption 17

Figure 5 shows a typical variation of absorbance vs uptake rate that is found

1 2 3 4 5 6 7 Sample Uptake Rate (mL/min)

Figure 5: Typical variation of absorbance versus uptake rate

18 GBC Flame Methods Manual for Atomic Absorption

2. Stoichiometric flame – a stiff flame with bigger blue cone and an

Nitrous oxide-acetylene flame

2. Stoichiometric flame – a clear flame with evidence of slight yellow at

GBC Flame Methods Manual for Atomic Absorption 19

Flameless electro-thermal atomisation

Advantage of ramp rate over fixed heating

20 GBC Flame Methods Manual for Atomic Absorption

Final Hold Time

Step 1 Step 2 Step 10

Figure 6: Furnace temperature profile

GBC Flame Methods Manual for Atomic Absorption 21

Vapour generation method

Figure 7: HG3000 hydride generator

22 GBC Flame Methods Manual for Atomic Absorption

Figure 8: V peak showing various absorption wavelengths which would

GBC Flame Methods Manual for Atomic Absorption 23

It is interesting to note that because the width of a spectral line is typically

Slit Width Slit Width

Figure 9: Comparison of spectral output from hollow cathode lamp compared

This is very important where strong broadband emission is reaching the

Detector read out

24 GBC Flame Methods Manual for Atomic Absorption