05 AAS Troubleshooting

SAP/CSC/CAM/AAS-013 rev 3
Feb 2004
TROUBLESHOOTING FOR ATOMIC

ABSORPTION SPECTROPHOTOMETER (AAS),
AA-6200, AA-6300, AA-6601/AA-6701 & AA-6800
The AAS may not operate properly because of incorrect operation, the
consumable parts have deteriorated, maintenance and regular inspection not carried
out, etc. The following are some problems, which users may come across and ways
to solve them. If the problems persist or the cause of the problem is not clear,
contact us.
(1) The power supply indicator lamp does not light when the power switch of
AAS is switched on.
Ensure that the power cable is firmly connected to the AAS.
Ensure that the main power supply is switched on.
(2) No communication between AAS and computer.

Make sure that the communication cable between AAS and computer is connected
firmly.
Check the setting of communication port:
(a)
(b)
(c)
(d)
AA-6200 - section 5.9.1 in Instruction Manual.

AA-6601/6701 - section 3.6.7 in AA-6601/6701 Instruction Manual (Reference).
AA-6800 - section 5.8.3 in AA-6800 Instruction Manual.
AA-6300 - check [COM Port] under [Instrument]-[Configuration].
(3) The optional accessories (ASC-6000/6100, GFA-6500/EX7/EX7i) are not

recognised when initialisation is performed.
Ensure that the ASC-6000/6100 and/or GFA-6500/EX7/EX7i are switched on.
Ensure that the communication cable between AAS and ASC-6000/6100 and/or GFA-
6500/EX7/EX7i is properly (firmly) connected.
(4) Wavelength origin search error at initialisation.

Remove any obstacle in the optical light path.
(5) The D2 lamp is not turned on.

Ensure that the D2 lamp is properly inserted into the socket.
D2 lamp defective. Change D2 lamp in:
(a) AA-6200 - section 6.3 in AA-6200 Instruction Manual.

(b) AA-6601/6701 - section 4.4 in AA-6601/6701 Instruction Manual (Users
System Guide).
(c) AA-6800 - section 6.4.2 in AA-6800 Instruction Manual.
(d) AA-6300 - section 8.4.2 in AA-6300 Instruction Manual.
1
Shimadzu (Asia Pacific) Pte Ltd, Singapore
(6) The hollow cathode lamp does not light up.

Ensure that the current value is not set to 0 mA.
Ensure that the hollow cathode lamp is properly placed in the socket.
Hollow cathode lamp is defective - change the lamp.
(7) Line Search failure.

Ensure that the hollow cathode lamp is identical for the element measured.
Ensure that the turret position is correct for the hollow cathode lamp.
Ensure that the hollow cathode lamp is properly placed in the socket.
Ensure that the analysis wavelength is correct.
Conduct wavelength adjustment:
(a) AA-6200 - section 5.8.3.2 in AA-6200 Instruction Manual.

(b) AA-6601/6701 - section 3.6.6.1 in AA-6601/6701 Instruction Manual
(Reference).
(c) AA-6800 - section 5.9.5.2 in AA-6800 Instruction Manual.
(d) AA-6300 - go to [Instrument]-[Maintenance]-[Wavelength Adjustment].
In Emission mode, use a higher concentration of standard solution.

(8) Hollow cathode lamp energy insufficient for line search.

Hollow cathode lamp intensity is low - increase the lamp current slightly.
(9) Beam Balance failure.

D2 lamp energy too low. Adjust the position of D2 lamp in:

System Guide).
(d) AA-6300 - go to [Instrument]-[Maintenance]-[D2 Lamp Position].
D2 lamp defective. Change D2 lamp in:
(a) AA-6200 - section 6.3 in AA-6200 Instruction Manual.

System Guide).
2
(e) AA-6300 - section 8.4.2 in AA-6300 Instruction Manual.

Ensure that the analysis wavelength is less than 430 nm.
For elements with analysis wavelengths more than 430 nm, use either Non-BGC mode
(available in AA-6200/6601/6701/6800) or BGC-SR mode (available in AA6601/6701/6800).
In AA-6300, BGC-SR mode can only be used for analysis wavelength more than 600
nm if the AA-6300 is equipped with the optional photomultiplier.
BG signal too large to balance - the hollow cathode lamp intensity smaller than the
background light intensity. Increase the hollow cathode lamp current slightly or use a
smaller slit width (in case of BGC-D2 mode).
BG signal too small to balance - the hollow cathode lamp intensity is larger than the
background light intensity. Decrease the hollow cathode lamp current slightly or use
a bigger slit width (in case of BGC-D2 mode).
In BGC-SR mode, change the High Lamp Current value.
(10) Flame cannot be ignited.

The gas is not supplied to the AAS. Ensure that the main valves of gases are opened
and that the gas tubing are properly connected.
Check that the gas pressure supply is correct 0.09 MPa for acetylene and 0.35 MPa
for both air and nitrous oxide.
Check that the airflow rate is not too high, i.e. the flow rate should be around 8 L/min.
For nitrous oxide-acetylene flame, check that the high temperature burner head is used
and that the burner recognition plug (for AA-6200) or key (for AA6601/6701/6800/6300) is properly inserted.
For AA-6601/6701/6800, check that the gas leak check has completed:
.
(a) AA-6601/6701 - section 4.2.1.2.2.1 in AA-6601/6701 Instruction Manual

(Reference).
(b) AA-6800 - section 5.9.8 in AA-6800 Instruction Manual.
Ensure that the drain liquid level is sufficient:
(a) AA-6200 - ensure that the U-tube is filled with water.

(b) AA-6601/6701 - section 4.2.1.2.2.1 in AA-6601/6701 Instruction Manual
(Reference).
(d) AA-6300 - go to [Instrument]-[Gas Controller Status].
Ensure that the suction force of the ventilation system is appropriate (600 1200
m3/h). Too much suction force can cause the flow of gas from the burner head to be
sucked away before it can be ignited by the pilot flame.
(11) Air-acetylene flame cannot change to nitrous oxide-acetylene flame.

Ensure that the main valve of the nitrous oxide gas is opened and/or the gas tubing is
connected.
Ensure that the nitrous oxide-acetylene flame is correctly selected in the software:

(b) AA-6601/6701 - section 4.2.1.2.1 in AA-6601/6701 Instruction Manual
(Reference).
3
(d) AA-6300 - section 4.2.2.10 in AA-6300 Instruction Manual.

Ensure that the high temperature burner head is used and that the burner recognition
plug (for AA-6200) or key (for AA-6601/6701/6800/6300) is properly inserted.
(12) Abnormal photometric (e.g. lower or poor reproducibility absorbance,

emission readings, etc.) value.
Check if the accumulated lighting hours of light sources (hollow cathode lamp and D2
lamp) have exceeded the standard time and need to be replaced.

Ensure that the AUTOZERO key was not pressed during measurement.
Incorrect standards/samples. Prepare the standards/samples again.
Specific for flame analysis:

Ensure that the sampling nozzle is not clogged or/and leaking.
Recheck the analytical conditions such as the horizontal position and angle of
burner.
Unstable flame - the gas supply pressure is not consistent. Ensure that the gas
pressure does not fluctuate.
Unstable flame - the quality of gases is not good. Ensure that the gas supplies are
free from water, moisture and dust.
While aspirating water through the nebulizer, check that air-acetylene flame is
lean blue if not, the acetylene gas supply is finishing and organic solvent from
the cylinder tank is flowing to the burner head, causing the flame to turn orange.
The acetylene cylinder should be replaced if the pressure decreases to 5 kg/cm2.
For nitrous oxide-acetylene flame, the red portion height should be at least 1 cm.
Ensure that the water/solvent used in the analysis is clean. This can be checked
by aspirating water/solvent through the nebulizer and checking that air-acetylene
flame is lean blue, i.e. similar to when water/solvent is not aspirated.
Ensure that the drainage is good. Ensure that drain tube is hanging freely in the
air inside the drain container, i.e. the water level does not touch the end of the
tube.
m3/h). Too much suction force can cause the flame to flicker as well as create
excessive noise.
Ensure that the sample is sufficient for the sampling nozzle.

Ensure that the sample is not removed during measurement.
For AA-6200 and AA-6800, the impact bead in the nebulizer is loose. This can
be checked by dismounting the nebulizer:
(b) AA-6800 - section 6.2.2.1 in AA-6800 Instruction Manual.
Note: The user is advised to contact us if not familiar with dismounting the nebulizer
which can be hazardous if not carried out properly.

(a)
(b)
(c)
(d)
(a)
(b)
(c)
(d)
Unstable flame - check that the burner slot is not clogged by carbide (especially
for nitrous oxide-acetylene flame) or salts. Clean the slot with thick paper or
razor. Also, the interior of the burner head might be dirty. For details:
AA-6601/6701 - section 4.2.1 in AA-6601/6701 Instruction Manual (Users
System Guide).
The nebulizer might be clogged. Clean it with cleaning wire:
AA-6200 - section 6.1.2.1 in AA-6200 Instruction Manual.
AA-6601/6701 - section 4.2.2.1 in AA-6601/6701 Instruction Manual (Users
System Guide).
AA-6800 - section 6.2.2.1 in AA-6800 Instruction Manual.
AA-6300 - section 8.2.2.1 in AA-6300 Instruction Manual
The polyethylene tube covering the capillary of nebulizer might be broken and
cause leakage. Replace the polyethylene tube:
(b) AA-6601/6701 - section 4.2.2.2 in AA-6601/6701 Instruction Manual (Users
System Guide).
(d) AA-6300 - section 8.2.2.2 in AA-6300 Instruction Manual
The nebulizer chamber is dirty. Clean as:

(a) AA-6200 - section 6.1.3 in AA-6200 Instruction Manual.
(b) AA-6601/6701 section 4.2.3 in AA-6601/6701 Instruction Manual Users
System Guide).
Ensure that the drainage is good to prevent the collection of liquid in the
chamber. The drain tube should be hanging freely in the air inside the drain
container, i.e. the water level does not touch the end of the tube.
Specific for GFA:
Ensure that the water/solvent used in the analysis is clean. This can be checked
by injecting just water into the graphite tube. The absorbance reading obtained
should be very low.
Ensure that the sample is sufficient for the sampling nozzle; otherwise, the nozzle
cannot reach the sample and fails to suck the sample.
The graphite tube has deteriorated as sample may dissolve tube. Change the
graphite tube:
(a) AA-6601/6701 and GFA-6500 - section 4.5 in AA-6601/6701 Instruction Manual
(Users System Guide).
(b) AA-6800 and GFA-6500 - section 6.5 in AA-6800 Instruction Manual.
(c) AA-6800/6300 and GFA-EX7/EX7i section 5.1 in GFA-EX7 Instruction
Manual.
5
The graphite cap, graphite holder, window plate sockets and surfaces of window
plate sockets are contaminated. Clean these parts as:
(c) AA-6800/6300 and GFA-EX7/EX7i - section 5.2 and 5.3 in GFA-EX7
Instruction Manual.
The emission-detecting hole of the graphite holder or/and temperature sensor is

dirty. Hence, the amount of light reaching the temperature sensor is inaccurate,
causing the temperature of the tube to fluctuate. Clean the temperature sensor:
(c) AA-6800/6300 and GFA-EX7/EX7i - section 5.4 in GFA-EX7 Instruction
Manual.
The graphite cap is misaligned, so that the emission detection hole in the surface
of the cap is not properly facing the light inlet of the photosensor unit. Hence,
the amount of light reaching the temperature sensor is inaccurate, causing the
temperature of the tube to fluctuate. Ensure that the alignment is good.
The seal (Teflon ring) is contaminated. Clean by:

Manual.
The pyrolytic tube was not conditioned by heat cleaning before use. This may
cause low sensitivity and poor reproducibility during starting time. The method
for conditioning the pyrolytic tube is:
(a) AA-6601/6701 and GFA-6500 - section 2.5.4.2 in AA-6601/6701 Instruction
Manual (Users System Guide).
(b) AA-6800 and GFA-6500 - section 2.5.4.2 in AA-6800 Instruction Manual.
(c) AA-6800/6300 and GFA-EX7/EX7i - section 2.4.5.2 in GFA-EX7 Instruction
Manual.
The heating program is not suitable, e.g. if the drying temperature is set too high,
the sample boils and scatter. Set a lower drying temperature and longer time.
Some elements such as Cd and Pb atomise instantaneously as they have low
atomising temperature this causes signals to decrease. Higher sensitivity can
also be achieved if the sensitivity mode is set to HIGH.
Standards/samples with low concentrations may deteriorate if not analysed

immediately.
Ensure that the sample injection is good, i.e. the autosampler pipette tip or
sampling nozzle does not touch the external or internal wall of graphite cap,
graphite holder or the surface of the graphite tube as this might cause the water
break.
The autosampler pipette tip or sampling nozzle has worn out and the volume of
injection is inaccurate. Replace the pipette tip or the sampling nozzle:
(a) ASC-6000 section 4.14 in AA-6601/6701 Instruction Manual (Users System
Guide).
6
(b) ASC-6100 section 4.3 and 4.4 in ASC-6100 Instruction Manual.
The flow line system such as tubing, nozzle, peristaltic pump, syringe and valve
of the autosampler has deteriorated, the tubing especially, can burst after
analysing organic solvents. In order to prevent this, rinse all flow lines with
diluted water so that the organic solvent will not remain inside the peristaltic
pump.
(13) Poor S/N, i.e. noisy baseline.

Ensure that the hollow cathode lamp is switched on. This can be carried out by
placing a white piece of paper in the atomiser unit. If red or orange light can be seen,
then the hollow cathode lamp is lit. If purple light is viewed, then the D2 lamp is lit.
The hollow cathode lamp is not warmed up sufficiently.

Check if the accumulated lighting hours of light sources (hollow cathode lamp and D2
lamp) has exceeded the standard time and need to be replaced.
Ensure that the optical axis of the hollow cathode lamp is correct, especially in the
case of AA-6200.
Ensure that line search has been carried out.

If the hollow cathode lamp is old or analytical wavelength is at the UV range, a bigger
slit width can be used.
Check if the optical axis of the lamp is correct:
(a) For flame analysis, first, ensure that the burner head position is correct. Then,
place a white paper in the optical path of the atomiser. If the beam from the
hollow cathode lamp cannot be seen above the burner head, then adjust the
optical axis of the lamp.
(b) For GFA, first, ensure that the atomiser unit position is correct. The beam from
the hollow cathode lamp can be seen if a white piece of paper is placed in front
of the left window plate socket of the GFA unit. The light beam can also be seen
on the white paper when placed on the right window socket.
The surfaces of the light source quartz window plate and monochromator quartz
window plate are dirty (at short wavelength, even adherence of fingerprints will cause
a noise). Wipe off the stain on the surfaces with soft cloth or lint-free tissue paper. If
the stain is hard to be wiped off, the soft cloth or lint-free tissue paper can be soaked
with alcohol.
Specific for flame analysis:
The optical axis may be distorted at wavelength of 200 nm or less if the burner is
hot. Do not remove the burner head when it is hot as the sample may evaporate
from the chamber. After the burner head has cooled down, carry out the
measurement again.
The nebulizer chamber is dirty. Wash by:

(a) AA-6200 - section 6.1.3 in AA-6200 Instruction Manual.
(b) AA-6601/6701 - section 4.2.3 in AA-6601/6701 Instruction Manual (Users
System Guide).
7
For AA-6200 and AA-6800, the impact bead in the nebulizer is loose. This can
be checked by dismounting the nebulizer:
(b) AA-6800 - section 6.2.2.1 in AA-6800 Instruction Manual.
Unstable flame - the gas supply pressure is not consistent. Ensure that the gas
pressure does not fluctuate.
Unstable flame - the quality of gases is not good. Ensure that the gas supplies are
free from water, moisture and dust.
Unstable flame - check that the burner slot is not clogged by carbide (especially
for nitrous oxide-acetylene flame) or salts. Clean the slot with thick paper or
razor. Also, the interior of the burner head might be dirty. For details:
AA-6601/6701 - section 4.2.1 in AA-6601/6701 Instruction Manual (Users
System Guide).
AA-6300 - section 8.2.1 in AA-6300 Instruction Manual
(a)
(b)
(c)
(d)
While aspirating water through the nebulizer, check that air-acetylene flame is
lean blue if not, the acetylene gas supply is finishing and organic solvent from
the cylinder tank is flowing to the burner head, causing the flame to turn orange.
The acetylene cylinder should be replaced if the pressure decreases to 5 kg/cm2.

For nitrous oxide-acetylene flame, the red portion height should be at least 1 cm.
m3/h). Too much suction force can cause the flame to flicker as well as create
excessive noise.
Ensure that the drainage is good to prevent the collection of liquid in the
chamber. The drain tube should be hanging freely in the air inside the drain
container, i.e. the water level does not touch the end of the tube.
Specific for GFA:
The graphite cap, graphite holder, window plate sockets and surfaces of window
plate sockets are contaminated. Clean these parts as:
Instruction Manual.
The socket window plates of the atomiser might be dirty. Clean off the stain
with soft cloth or lint-free tissue paper. If the stain is hard to be wiped off, the
soft cloth or lint-free tissue paper can be soaked with alcohol.
(14) For GFA, the graphite tube breaks easily.

The graphite cap, graphite holder, window plate sockets and surfaces of window plate
sockets are contaminated. Clean these parts as:

8

Instruction Manual.
The emission-detecting hole of the graphite holder or/and temperature sensor is dirty.
Hence, the amount of light reaching the temperature sensor is inaccurate, causing the
temperature of the tube to fluctuate. Clean by:
Manual.
The graphite cap is misaligned, so that the emission detection hole in the surface of
the cap is not properly facing the light inlet of the photosensor unit. Hence, the
amount of light reaching the temperature sensor is inaccurate, causing the temperature
of the tube to fluctuate. Ensure that the alignment is good.
The seal (Teflon ring) is contaminated. Clean by:

Manual.
The guide rods for the right cooling block in the atomiser unit is dirty which prevents
the smooth sliding of the block. For details:

(a) AA-6601/AA-6701 and GFA-6500 - section 4.8 in AA-6601/6701 Instruction
Manual (Users System Guide).
Manual.
(15) For GFA, the heating temperature program is not transferred.

The line was disconnected during processing. Perform optional connection:
(a) AA-6601/6701 and GFA-6500 - section 3.6.5 in AA-6601/6701 Instruction

Manual (Reference).
(b) AA-6800 and GFA-6500/GFA-EX7 - section 5.9.2 in AA-6800 Instruction
Manual.
(c) AA-6300 and GFA-EX7i - go to [Instrument]-[Option Connect].
(16) For GFA, the temperature stops increasing during heating.

Ensure that the heat switch of the GFA is on.
Ensure that the voltage supply and power capacity is sufficient for the specified
values.
The graphite tube has deteriorated. Replace the graphite tube.
(17) For GFA, during heat atomisation, spark occurs between window plate holder
and cooling block.
Ensure that the window plate holder is securely fastened.
(18) For GFA, the atomiser unit is noisy during the heating process.
Ensure that the left and right cooling blocks are properly aligned.
Graphite tube fails to contact. Ensure that the right cooling block may slide without
difficulty.
10

05 AAS Troubleshooting

Uploaded by

Document Information

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

05 AAS Troubleshooting

Uploaded by

Copyright:

Available Formats

SAP/CSC/CAM/AAS-013 rev 3

TROUBLESHOOTING FOR ATOMIC

(2) No communication between AAS and computer.

Check the setting of communication port:

AA-6200 - section 5.9.1 in Instruction Manual.

(3) The optional accessories (ASC-6000/6100, GFA-6500/EX7/EX7i) are not

6500/EX7/EX7i is properly (firmly) connected.

(4) Wavelength origin search error at initialisation.

(5) The D2 lamp is not turned on.

(a) AA-6200 - section 6.3 in AA-6200 Instruction Manual.

Shimadzu (Asia Pacific) Pte Ltd, Singapore

(6) The hollow cathode lamp does not light up.

(7) Line Search failure.

(a) AA-6200 - section 5.8.3.2 in AA-6200 Instruction Manual.

In Emission mode, use a higher concentration of standard solution.

(8) Hollow cathode lamp energy insufficient for line search.

(9) Beam Balance failure.

(a) AA-6200 - section 5.8.3.1 in AA-6200 Instruction Manual.

D2 lamp defective. Change D2 lamp in:

(a) AA-6200 - section 6.3 in AA-6200 Instruction Manual.

Shimadzu (Asia Pacific) Pte Ltd, Singapore

(e) AA-6300 - section 8.4.2 in AA-6300 Instruction Manual.

In BGC-SR mode, change the High Lamp Current value.

(10) Flame cannot be ignited.

and that the gas tubing are properly connected.

for both air and nitrous oxide.

(a) AA-6601/6701 - section 4.2.1.2.2.1 in AA-6601/6701 Instruction Manual

Ensure that the drain liquid level is sufficient:

(a) AA-6200 - ensure that the U-tube is filled with water.

(11) Air-acetylene flame cannot change to nitrous oxide-acetylene flame.

(a) AA-6200 - section 5.6.1.7 in AA-6200 Instruction Manual.

Shimadzu (Asia Pacific) Pte Ltd, Singapore

(d) AA-6300 - section 4.2.2.10 in AA-6300 Instruction Manual.

plug (for AA-6200) or key (for AA-6601/6701/6800/6300) is properly inserted.

(12) Abnormal photometric (e.g. lower or poor reproducibility absorbance,

lamp) have exceeded the standard time and need to be replaced.

Ensure that the analysis wavelength is correct.

Ensure that the sampling nozzle is not clogged or/and leaking.

Ensure that the sample is sufficient for the sampling nozzle.

Shimadzu (Asia Pacific) Pte Ltd, Singapore

The nebulizer chamber is dirty. Clean as:

Specific for GFA:

Shimadzu (Asia Pacific) Pte Ltd, Singapore

The emission-detecting hole of the graphite holder or/and temperature sensor is

The seal (Teflon ring) is contaminated. Clean by:

Standards/samples with low concentrations may deteriorate if not analysed

Shimadzu (Asia Pacific) Pte Ltd, Singapore

(b) ASC-6100 section 4.3 and 4.4 in ASC-6100 Instruction Manual.

(13) Poor S/N, i.e. noisy baseline.

The hollow cathode lamp is not warmed up sufficiently.

lamp) has exceeded the standard time and need to be replaced.

Ensure that line search has been carried out.

slit width can be used.

Check if the optical axis of the lamp is correct:

Specific for flame analysis:

The nebulizer chamber is dirty. Wash by:

Shimadzu (Asia Pacific) Pte Ltd, Singapore

Specific for GFA:

(14) For GFA, the graphite tube breaks easily.

sockets are contaminated. Clean these parts as:

Shimadzu (Asia Pacific) Pte Ltd, Singapore

(b) AA-6800 and GFA-6500 - section 6.6 in AA-6800 Instruction Manual.

The seal (Teflon ring) is contaminated. Clean by:

(a) AA-6601/6701 and GFA-6500 - section 4.9 in AA-6601/6701 Instruction Manual