Novaa 800
Novaa 800
Novaa 800
novAA 800
Atomic Absorption Spectrometer
Manufacturer Analytik Jena AG
Konrad-Zuse-Str.1
07745 Jena Germany
Phone + 49 3641 77 70
Fax + 49 3641 77 92 79
Email [email protected]
Edition 04.19
Contents
3
Contents novAA 800
4
novAA 800 Contents
5.6.3 Replacing the cannulas and guide on the autosampler arm of the AS-FD .............. 112
5.6.4 Replacing the cannula on the autosampler arm of the AS-F ................................... 113
5.6.5 Replacing the intake tube ....................................................................................... 113
5.6.6 Replacing the tube set on the AS-FD ...................................................................... 113
5.6.7 Cleaning up after cup overflow ............................................................................... 114
5.7 Cooling unit KM 5 ................................................................................................... 114
5.8 Piston compressor PLANET L-S50-15..................................................................... 115
8 Disposal......................................................................................................................... 124
Figures
5
Contents novAA 800
6
novAA 800 Basic information
1 Basic information
The user manual describes the following models of the novAA product family:
novAA 800 D – Combined device for flame and graphite furnace techniques
novAA 800 F for flame technique
novAA 800 G for graphite furnace technique
In this manual all these devices are collectively called novAA 800. Any differences be-
tween the models are explained in the relevant section. Unless otherwise stated, the
device shown on the illustrations is the combined device novAA 800 D.
The novAA 800 is intended for operation by qualified specialist personnel observing
this user manual.
This user manual is addressed to personnel familiar with analysis and provides infor-
mation about the design and function of the novAA 800 and the necessary know-how
for the safe handling of the device and its components. Furthermore, the user manual
includes information on the maintenance and servicing of the device as well as hints
on potential causes for malfunctions and their correction.
Conventions Instructions for actions which occur in chronological order are numbered and com-
bined in action units.
Warnings are marked by a warning triangle and a signal word. The type, source and
consequences of the danger are stated together with notes on preventing the danger.
The elements of the control and analysis program are indicated as follows:
Terms used in the program are identified with SMALL CAPS (e.g., Menu FILE).
Buttons are identified by square brackets (e.g., [OK] button)
Menu items are separated by arrows (e.g. FILE OPEN)
Symbols and signal words The user manual uses the following symbols and signal words to indicate hazards or
instructions. The safety instructions are always placed before an action.
WARNING
Indicates a potentially hazardous situation which might cause fatal or very serious
injuries (deformations).
CAUTION
Indicates a potentially hazardous situation which might cause minor or moderate inju-
ries.
NOTICE
Indicates potential damage to equipment or the environment.
7
Basic information novAA 800
The warranty duration and liability comply with the legal requirements and the provi-
sions in the general terms and conditions of Analytik Jena.
Deviations from the intended use described in this user manual result in limitations of
warranty and liability during a damage event. Damage to wearing parts is not included
in the warranty.
Warranty and liability claims are excluded for personal injury and property damage if
they can be attributed to the following causes:
use of the device other than intended
improper commissioning, operation and maintenance of the device
modifications of the equipment without prior consultation with Analytik Jena
operation of the device with faulty safety equipment or improperly fitted safety and
protection equipment
inadequate monitoring of the equipment components subject to wear
use of other than original spare parts, wearing parts or consumables
improper repairs
faults due to the non-observance of this user manual
8
novAA 800 Safety instructions
2 Safety instructions
For your own safety and to ensure error-free and safe operation of the novAA800,
please read this chapter carefully before using the appliance.
Observe all safety notes listed in this user manual and all messages and notes dis-
played by the control and analysis program ASpect LS on the monitor.
Besides the safety instructions in this user manual and the local safety regulations that
apply to the operation of the device, the general applicable regulations regarding acci-
dent prevention, occupational health and safety and environmental protection have to
be observed and complied with.
References to potential dangers do not replace the work protection regulations which
must be observed.
Warnings and information symbols have been attached to the novAA 800 which must
always be observed.
Damaged or missing warnings and information symbols can cause incorrect actions
leading to personal injury or material damage! Labels containing symbols must not be
removed or moistened with methanol! Damaged symbol labels must be replaced with-
out delay!
9
Safety instructions novAA 800
Fig. 2 Safety markings on the front and side panels of the device
10
novAA 800 Safety instructions
3 Caution! Hot surface! Hot surfaces! Risk of burns at the hot graphite
Caution! Emission of UV radiation! furnace and burner!
Dangerous UV radiation!
Do not look into the lamp beam, into the flame or
the graphite furnace without UV protection
goggles.
Danger of short circuit! Short circuit warning only for novAA 800 D + G
Handling with jewels not allowed! Do not wear any metallic jewelry (especially
around the neck). Not observing this instruction
may cause a short circuit in the electrically heated
furnace. The jewelry may become very hot and
cause burns.
4 Warning! Switch off lamps when door is opened! The ultraviolet light emitted by the (deuterium)
hollow cathode lamps can cause eye and skin
damage. Turn off the lamp current via ASpect LS
software before opening the lamp chamber.
The novAA 800 must only be operated by qualified specialist personnel instructed in
the use of the device. The instruction must also include conveying the content of this
user manual and the user manuals of other system components.
In addition to the safety at work instructions in this user manual the generally applica-
ble safety and accident prevention regulations of the respective country of operation
must be observed and adhered to. The operator must ascertain the latest version of
these regulations.
The user manual must be accessible to the operating and service personnel at any
time!
11
Safety instructions novAA 800
The various different models of the novAA 800 product family weigh between 95
and 130 kg. Use a lift truck to transport the device.
Four people are required to move the device in the laboratory by holding the device
on four firmly screwed-in carrying handles.
Perform a professional and documented decontamination of the device before
returning it to Analytik Jena. The decontamination protocol is provided by the ser-
vice when the return is registered. Analytik Jena must refuse acceptance of contam-
inated devices. The sender may be liable for any damage caused by inadequate de-
contamination of the device.
Protection against explo- The novAA 800 must not be operated in an explosive environment.
sion and fire
Smoking and open flames in the operating room of the novAA 800 are prohibited!
The operator is responsible for establishing a control method to ensure that the
NO2 and acetylene connectors are leak-tight.
Prior to starting up the device, the operator of the novAA 800 must verify the
proper condition of the device including the condition of its safety equipment. This
applies in particular after each modification or extension of the device or its repair.
The device must only be operated if all protective equipment (e.g. covers and
doors) are in place, properly installed and fully operational. The sound condition of
the protection and safety equipment must be checked regularly. Any defects must
be corrected as soon as they occur. Protective and safety equipment must never be
removed, modified or switched off during operation.
During operation, the operator must have free access to all connections and the
power switch on the right side of the device as well as to the power strip.
The ventilation equipment on the device must be in good working condition. Cov-
ered ventilation grilles or slits etc. may cause the device to break down or damage
the device. When placing the device and system components observe a minimum
clearance of 150 mm to walls and neighboring installations.
Prevent any liquids from entering the inside of the instrument. The liquids might
get into contact with electronic components and cause a short circuit.
Work on the electrical components of the novAA 800 may only be performed by a
qualified electrical technician according to applicable electro-technical regulations.
Lethal voltages may occur in the device! Contact with live components may cause
death, serious injury or painful electrical shock.
Observe the following notes:
The mains plug must be connected to a proper CEE power socket to ensure that the
device meets protection class I (ground connector). The device may only be con-
nected to power sources whose nominal voltage is the same as that on the type
12
novAA 800 Safety instructions
plate of the equipment. The protective effect must not be invalidated by the use of
an extension line which does not have a protective conductor.
The novAA 800 and its system components must always be switched off before
being connected with one another.
The auxiliary components that are to communicate with each other, for example
PC, monitor, printer, hydride system and cooling unit, have to be connected to the
power strip that is supplied with the device. The compressor needs a separate pow-
er supply. When connecting own components to the power strip, observe the max-
imum allowable drain current (see section "Energy supply" on page 40).
Before opening the device it must be switched off on the device switch and the
mains connector must be disconnected from the mains outlet!
The novAA 800 must be switched off before carrying out any electrical work and
the mains plug must be pulled out. Safe disconnection from the mains can only be
achieved by pulling out the mains plug. The power strip is still energized, even
when the novAA 800 is switched off at the mains switch on the right side wall. The
power strip socket to which the novAA 800 is connected is protected by a fuse in
both wires, one in the L conductor (line) and one in the N conductor (neutral). This
can mean in the case of a fault that connected components are supplied with volt-
age via the L-line, but no current can flow through the N-line, i.e., without a more
thorough check, the connected devices appear to be voltage-free, which is not true.
Any work on the electronics (behind the device enclosure) may only be carried out
by the customer service of Analytik Jena and specially authorized technicians.
2.5.2 Hazards associated with the operation of the flame and the graphite furnace
HCL, D2-HCL, the heated graphite tube (T > 1000 °C) and the flame of the burner
transmit optical radiation (in the UV range and the visible range). Do not look into
the rays emitted by the lamp, the graphite tube or the flame without UV protection
goggles. Protect the skin against UV radiation.
Switch off the lamp by means of the control and analysis software ASpect LS before
opening the lamp door: Set the lamp current in [mA] to zero in the OPTICAL
PARAMETERS section of the SPECTROMETER / CONTROL window. Open the drop-down
list BACKGROUND CORRECTION and select the option NO BACKGROUND. Click [CONFIGURE].
Negate the error message.
To observe the placement of the samples or the drying of liquid samples, the dental
mirror may only be inserted into the beam path from the left side of the graphite
furnace. When observing on the right side of the furnace, UV radiation may be re-
flected.
The sample chamber door (safety glass pane) must be closed and the flame super-
vised when it is burning. Ensure that the flame detector is working correctly.
For devices with hydride technique, only work with the sample chamber door (safe-
ty glass pane) closed.
The fuel gas pressure must not fall below 70 kPa to prevent the flame from firing
back. The integrated pressure sensor will automatically switch off the novAA 800 if
this condition is not met. In addition to that, monitor the pressure on the pressure
gage of the gas supply.
13
Safety instructions novAA 800
When using graphite furnace technique, do not look into the graphite furnace
opening without wearing protective goggles. Sputtering sample substances and hot
graphite particles may cause eye and face injuries.
High temperatures occur during flame and graphite furnace operation. Do not
touch hot parts such as the burner head or the graphite furnace during or immedi-
ately after a measurement. Observe the required cooling times.
Do not wear any metallic jewelry (especially around the neck) when working with
the novAA 800 D and G. Not observing this instruction may cause a short circuit in
the electrically heated furnace. In case of a short circuit, the jewelry may become
very hot and cause burns.
Electromagnetic dispersion fields with flux densities ≤ 100 µT occur in the vicinity
of the sample chamber due to the heating of the graphite tube.
When using graphite furnace technique, the sound level may rise up to 55 dBA. If
the nitrous-oxide-acetylene flame blows back into the mixing chamber, the mo-
mentary sound level lies below 130 dBA.
2.5.3 Safety instructions relating to the formation of ozone and toxic vapors
The UV radiation of the hollow cathode lamps (HCL, D2-HCL) and the N2O/acetylene
flame causes an interaction with the surrounding air to form toxic concentrations of
ozone exceeding the permissible limit. Furthermore, toxic byproducts may escape from
the samples or while the samples are processed.
Observe the following note:
The novAA 800 may only be operated when the exhaust unit is activated.
Always keep the sample chamber closed when the flame is lit.
14
novAA 800 Safety instructions
Operate the acetylene cylinder only in an upright position and secured against fall-
ing over. When the cylinder pressure is lower than 100 kPa, the acetylene cylinder
must be replaced to avoid acetone entering the automatic gas control.
The operator must carry out weekly safety checks regarding the status and for leaks
on all gas supplies and connectors including the ones on the device itself. Possible
pressure losses from closed systems and lines under pressure are to be determined.
Leaks and damaged must be repaired without delay.
The gas supply must be closed prior to inspections, service and repairs!
After successful repair and service of the components of the compressed air cylin-
ders or system the device must be checked for sound operation prior to recommis-
sioning!
Unauthorized assembly and installation are not permitted!
After changing the gas cylinder, thoroughly ventilate the cylinder location.
The operator is responsible for the selection of substances used in the process as well
as for their safe handling. This is particularly important for radioactive, infectious,
poisonous, corrosive, combustible, explosive and otherwise dangerous substances.
When handling dangerous substances local safety codes and guidelines must be
observed.
Warnings on the labels must always be observed. Only use labeled tubes. Use suit-
able body protection (laboratory coat, safety goggles and rubber gloves) when
handling samples.
The novAA 800 must only be operated under an activated laboratory exhaust hood
(hazards arising from the formation of ozone, combustion gases produced by the
samples, poisonous and combustible by-products from sample preparation pro-
cesses).
Keep flammable and explosive substances away from the flame.
Cleaning with hydrofluoric acid must be carried out in an exhaust chamber. The
operator must wear a rubber apron, gloves and a face mask when handling hy-
drofluoric acid.
Sodium borohydride (NaBH4) is highly corrosive, hygroscopic and, in solution,
extremely aggressive. Avoid dripping and spilling of reduction agent.
Biological samples must be handled according to local guidelines regarding the
handling of infectious material.
When measuring material containing cyanide you have to make sure that prussic
acid cannot be generated in the waste bottle, i.e. the waste solution must not be
acidic.
Ensure that all residue liquid from the nebulizer and the automatic sampler is di-
rected into the waste bottle supplied.
The operator is responsible for ensuring that waste materials such as drained
coolant and residue liquid from the waste bottle are disposed of in an environmen-
tally responsible manner and according to local regulations.
15
Safety instructions novAA 800
Examples of organic Methyl isobutyl ketone (MIBK) Flammable, highly volatile, noxious-smelling
solvents
Toluene Flammable, hazardous to health
Kerosene Flammable, hazardous to the aquatic environment,
hazardous to health
Methanol, ethanol, propanol Flammable, partly acutely toxic
Tetrahydrofuran (THF) flammable, hazardous to health, extremely volatile,
dissolves polyethylene and polystyrene
This list is not exhaustive. Other solvents could be considered when using the no-
vAA 800. If in doubt about the potential hazards ask the manufacturer to provide more
detailed information.
16
novAA 800 Safety instructions
17
Function and setup novAA 800
The following atomization techniques are available for the devices of the novAA 800
product family:
Burner-nebulizer system -
(flame technique)
Transversely heated -
graphite tube
(graphite furnace tech-
nique)
Cell unit
(hydride and mercury cold
vapor technique)
Transversely heated -
graphite tube with
Ir/Au coating
(HydrEA technique)
In the combined device novAA 800 D the flame atomizer and the graphite furnace are
both attached to a bracket on the height adjustment that can be tilted by 60°. Tilting
the bracket forwards into locking position puts the graphite furnace into the optical
axis. Tilting the bracket backwards up to an adjustable stop puts the flame unit into
the optical axis. Since both atomizers are aligned with the axis, changing from one
atomization techniques to the next can be done in a few minutes. The control and
analysis software ASpect LS uses the height adjustment to move the atomizer into the
correct operating position automatically. The depth of the atomizer within the sample
18
novAA 800 Function and setup
chamber is factory preset and may be adjusted manually for the flame atomizer using
an adjustment screw.
The novAA 800 F (flame) and the novAA 800 G (graphite) are both equipped with one
atomizer.
The core element of the graphite furnace mode is a closed, transversely heated graph-
ite furnace into which the samples are loaded from the top.
For flame operation, the novAA 800 is designed as a double-beam instrument, which
can also be used in single-beam operation. Core piece of the flame mode is the mix-
ing-chamber-nebulizer system with direction-independent stable nebulizer.
The time-controlled infection module SFS 6 is available for the flame injection tech-
nique. It switches the valves in a constant stream of carrier solution to couple the sam-
ple segments.
The hydride technique with latest-generation hydride systems (HS 50, HS 55 modular,
HS 60 modular) is the preferred process for the detection-sensitive determination of
the hydride-forming elements As, Bi, Sb, Se, Sn, Te and Hg. The cell unit of the hydride
system is placed on the mixing chamber instead of the burner in the novAA 800 D
and F and on the clamped connector in the novAA 800 G.
Alternatively, the combined device novAA 800 D and the novAA 800 G allow coupling
hydride technique with graphite furnace technique. The HydrEA technique ("Hydride
technique with electro-thermal atomization") consists in accumulating metal hydrides
or mercury vapor on the iridium-coated or gold-coated graphite tube and atomizing
them at temperatures of 2100 °C (metal hydrides) or 800 °C (mercury). This allows
attaining a very high sensitivity.
The novAA 800 is a double-beam instrument, which can be used in single or double
beam mode, depending on the selected technique. On the left side the 8-lamp turret
(item 8 in Fig. 5) is vertically arranged. The lamp turret can be equipped with
19
Function and setup novAA 800
1.5" hollow cathode lamps (HCL) as the primary radiation source. In front of the lamp
turret there also is a deuterium hollow cathode lamp (D2-HCL) (item 7 in Fig. 5) in
vertical arrangement for the classical background compensation.
An optical beam splitter (item 9 in Fig. 5) with reflection and transmission fields in
chess-board pattern unites the radiation of the active primary HCL with the continuum
radiation of the D2-HCL and splits it simultaneously into the sample and reference
beams. Identical beam paths with the same beam distribution and density in the spa-
tial angle used for both radiation sources ensure the optimal background compensa-
tion with the D2-HCL.
The reference beam is routed behind the sample chamber. A rotating sector mirror
(item 5 in Fig. 5) with 90° reflection sector and transmission sector brings the sample
and reference beams together.
For the graphite furnace technique with D2 background correction, the novAA 800 is
operated as a single-beam instrument.
The sample beam or combined sample/reference beam is projected onto the entrance
slit of a mesh monochromator (items 1 and 2 in Fig. 5). The mesh monochromator is
equipped with fixed slits of 0.2 nm / 0.3 nm / 0.5 nm / 0.8 nm / 1.2 nm bandwidth. It
20
novAA 800 Function and setup
selects the resonance wavelengths assigned to the element. The wavelength of the
monochromator is set according to the theoretical number of iterations, based on the
zero order as an initialization point and corrected by an amount which is calculated
from the device-specific wavelength interpolated function which is available as a poly-
gon curve. 9 interpolation points are distributed equally over the wavelength range
from the zero-th order up to 900 nm.
A peak-pick program is used to find the maximum of the particular line. The wave-
length is set via a step-motor-driven wavelength drive with a resolution of 0.005 nm
per step.
The optional accessory Air Purge Kit (APK) can be used to purge the spectrometer with
purified compressed air. The use of this equipment is advisable when the novAA 800 is
used in an operating environment with large quantities of dust, such as a mine.
The novAA 800 has an 8-lamp turret with a write/read unit for coded lamps. The cod-
ed lamps are equipped with transponders. The following information is saved: lamp
type, element(s), serial number, maximum/recommended lamp current and operating
hours. The use of uncoded lamps is possible. The lamp turret is designed for hollow
cathode lamps with a standard bulb diameter of 37.1 mm. The individual lamps are
rotated (PC-controlled) into the beam path, switched on and adjusted according to the
pitch circle in steps of 0.1 mm.
21
Function and setup novAA 800
A second heat circuit ensures that a second HCL can be preheated at the same time.
The continuum radiator, a deuterium hollow cathode lamp (D2-HCL), is installed in a
separate bracket (item 2 in Fig. 31 on page 54).
The electrothermal atomizer (EA) is an integral part of the novAA variants no-
vAA 800 D and G and a core element for working in EA mode and with the HydrEA
technique.
The furnace system is equipped with a graphite tube that is heated by contact ele-
ments positioned transversely to the coat of the tube. The transversely heated graph-
ite tube serves as an atomizer for the liquid sample injected with the AS-GF au-
tosampler. The required temperature of the graphite tube in the furnace is regulated
by means of a microprocessor controlled Ohmic heating.
Characteristics of the Constant temperature ratios along the entire tube length
graphite furnace
Realization of linear temperature-time runs according to a sensorless control model
on the basis of saved thermoelectrical parameters and an adaptive control
Protective gas flows, independent of each other and symmetrical to the furnace
center, which ensure effective graphite tube and furnace window cleaning, and
22
novAA 800 Function and setup
which also ensure fast and safe transport of the thermally disintegrated products of
the sample for disposal
Low consumption of protective gas while ensuring effective protection against the
interference with atmospheric oxygen.
When combined with the deuterium background compensation, the graphite furnace
technique achieves high levels of selectivity and sensitivity allowing the determination
of traces and ultra-traces even in samples with a complex matrix.
During analysis, each sample has to pass one furnace program (temperature-time
program). The furnace program consists of four basic steps:
Drying the sample
Thermal pretreatment, separation (ashing or pyrolysis) of distorting incidental
sample substances (matrix)
Atomizing the sample
Cleaning the graphite tube by baking out and preparing for the next measurement
The operator has the option to optimize these basic steps for each analysis problem
with the ASpect LS control software.
A safety circuit prevents the graphite furnace in the novAA 800 from continued and
uncontrolled heating in case of a communication failure between the control (PC) and
the AAS. The temperature sensor is attached to the rear of the stationary furnace
23
Function and setup novAA 800
(item 5 in Fig. 7). The safety circuit disconnects the main power supply of the device if
the cooling water temperature reaches ≥100 °C.
This prevents damage to the device resulting from continued heating of the furnace.
Once the cooling water temperature has fallen below the shutdown temperature, the
novAA 800 can be switched back on and re-initialized.
The transversely heated graphite tube is pneumatically pushed against circular elec-
trodes and held in this position. The electrodes are installed in two water-cooled metal
bodies, the stationary and the movable part of the furnace. There is another graphite
component located between the metal bodies that support the electrodes, the furnace
shroud. Together with the electrodes it forms an enclosure around the graphite tube,
which stabilizes the thermal radiation conditions of the graphite tube and also guaran-
tees chemically inert conditions. The graphite tube is pre-adjusted by means of defined
support points in the furnace while the atomizer is open. When the movable part of
the furnace is closed, the tube is lifted to its final position in a reproducible movement
and pressed into the contacts, without coming into contact with the furnace shroud.
When changing from the wall-type tube to the platform tube, bear in mind that these
special graphite tubes cover the free opening for the beam passage on one side. When
selecting the respective technique, the motor-driven height adjustment moves to the
optimum height position in a software-controlled movement.
24
novAA 800 Function and setup
The furnace shroud houses the gas channels for the separate supply of the primary gas
flow (purge gas) and the outer gas flow (protective gas). It is possible to add oxidizing
and reducing gases to the mixture of the inner gas flow to support the pyrolysis. Avoid
temperatures > 500 °C when using air to prevent the graphite tube from corroding.
The purpose of the inner gas flow is to remove all gases that are produced during the
drying process and the pyrolysis from the graphite tube.
Furthermore, the inner gas flow prevents analytes from condensing on the furnace
window and has an influence on the dwell time of the analyte atoms within the beam
path. The atomization usually interrupts the inner gas flow to allow the atoms to dwell
as long as possible within the beam path of the graphite tube. The desired result is a
high sensitivity.
The outer gas flow sweeps the graphite tube and is directed through the funnel insert
to the outside. The outer gas flow permanently surrounds the graphite tube with inert
gas to protect it from oxidizing with the atmospheric oxygen.
A cylindrical joint to the stationary part of the furnace is used to distribute the heat in
the furnace shroud and for dissipating the heat. This allows heating up the interior
walls of the atomizer to such high temperatures that prevent the analyte (the sample)
from condensing.
The cone attachment on the opposite side of the furnace shroud forms a precisely
defined gap in the rotatable part of the furnace together with the insulating ring en-
suring that the cell interior is sealed against the ingress of ambient air. In the event of
a tube rupture in the furnace shroud, the insulating ring in the movable furnace part
prevents a short circuit between the furnace parts.
The furnace shroud is drilled through in the direction of the optical axis, the outer
cylinders support the furnace windows (quartz cell windows). For cleaning, the win-
dows can be pulled off with a twisting motion.
25
Function and setup novAA 800
There are two graphite tube models: the standard graphite tube (wall-type tube) and
the graphite tube with PIN platform.
26
novAA 800 Function and setup
The radiation sensor is located on the right side of the graphite tube furnace and is
inclined in relation to the direction of radiation. It recalibrates the tube temperatures
by receiving radiation from the interior of the graphite tube on a sandwich receiver.
Using two wavelengths for detection, an independent quotient signal is derived for
temperature measurement which is independent of the degree of radiation of the
graphite tube. Recalibration takes place when formatting the graphite tube.
The furnace camera is an optional accessory that can be switched on via the software
control. The image recorded by the furnace camera would then be displayed in a sepa-
rate window on the ASpect LS user interface. The furnace camera monitors the pro-
cess, beginning with the injection of the sample into the graphite tube through to
completion of the drying process. This allows the operator to control and, if necessary,
correct the immersion of the dosing tube into the graphite tube, the dispensing of the
sample and other components as well as the drying procedure. The furnace camera
automatically shuts down before a pyrolysis process. The camera allows looking into
the graphite tube from the left. The interior is illuminated by a LED from the right.
27
Function and setup novAA 800
autosampler AS-GF accepts defined volumes of different solutions and places them
into the graphite tube. It enables the
Addition of up to five modifiers to the sample solution
Transport of the sample solution to the thermal pretreatment in the tube
Enrichment of samples
Placement of components in the preheated tube
Separate transport of components with intermediate purging
Automatic preparation of standards by dilution or by different volumes
Fixed, preselected or intelligent sample dilution
Fully automatic multi-element mode (night mode possible)
The sample tray of the AS-GF provides enough space for 100 sample cups (with
V = 1.5 mL) and 8 central cups for diluent, special samples, standards, modifiers etc.
(with V = 5 mL).
1 Autosampler arm with
cannula locking system
2 Tube guide with dosing tube
3 Sample tray with
sample tray cover
4 Metering syringe (500 µL)
5 Waste bottle
6 Storage bottle for purge solution
(or diluent)
The AS-GF is attached to the respective receptacles provided in the sample chamber
and electrically connected to the novAA 800. The device parameters of the AS-GF can
be set with the ASpect LS control software.
The graphite tube furnace of the novAA 800 is cooled by the mobile cooling unit KM 5
via a circulating cooling system. The working principle is an air-cooled heat exchanger
with fan. The cooling water temperature is preset to 35 °C. The cooling unit can only
28
novAA 800 Function and setup
cool effectively, if the preset value is at least 7 °C above room temperature. The maxi-
mum set point value is 50 °C.
The KM 5 has to be filled with 5 L of softened water (not distilled water). For installa-
tion and initial start-up of the device, please observe the information provided in the
separate operating instructions of the mobile cooling unit KM 5.
Flame atomic absorption spectroscopy is used for determining trace elements in the
concentration range from mg/L to µg/L and for determining the basic composition of
the major components. It requires a flame with constant properties. Furthermore, the
flame composition must be compatible with the element to be analyzed.
Motorized vertical adjustment of the nebulizer-mixing-chamber-burner system by
14 mm makes it possible to move the flame zone with the maximum absorption into
the direction of the beam.
The sample solution is aspirated by a pneumatic nebulizer and sprayed into the mixing
chamber. In the mixing chamber the sample aerosol is mixed with acetylene and oxi-
dant before it emerges from the burner slot. The flame is either 5 or 10 cm long and a
few millimeters wide, depending on the burner used. It is irradiated over its full length.
For the measurement of main components, the burner can be rotated by max. 90° on
the mixing chamber tube (transverse position). This reduces the absorption path. Cor-
respondingly, the sensitivity is lower. It is possible to set the rotation of the burner
using the scale on the burner.
The automatic gas control ensures that the flame is fed with a defined flow of acety-
lene and oxidant at a constant non-fluctuating pressure level. This guarantees the safe
and hazard-free ignition and quenching of the flame. The automatic gas control has
three gas inlets for acetylene, air and nitrous oxide.
A proportional control valve sets the fuel gas flow in steps of 5 L in a range between
40 and 315 NL/h of acetylene. The airstream first fills a reservoir with a capacity of
500 cm³ before the air flows to the nebulizer. The air in the reservoir is used to quench
the flame in regular operation and in the event of an accident. The oxidant flow to the
nebulizer is calculated from the set configuration and the inlet pressure. The oxidant
flow is measured and monitored. If auxiliary oxidant is used, the auxiliary oxidant flow
(air/nitrous oxide) is regulated in three stages.
A filament ignites the flame. The filament is swung from the rear panel of the sample
chamber to the center of the burner. It is possible to switch from the acetylene-air
flame to the acetylene-nitrous-oxide flame by blocking the air supply and adding ni-
trous oxide. The acetylene flow is increased at the same time. The acetylene-nitrous-
oxide flame is quenched in reverse order. The switching of the flames is executed in a
fully automated process controlled by the ASpect LS software.
29
Function and setup novAA 800
The nebulizer uses the sample solution to generate the aerosol required for the atomi-
zation in the flame. The oxidant passes the lateral connection to enter the nebulizer
and flows through the ring-shaped slit formed by the corrosion-proof platinum-
rhodium alloy cannula and the PEEK nozzle. The resulting negative pressure pulls the
sample solution out of the cannula and aspirates more sample solution. The aspiration
rate and the fineness of the aerosol are determined by the relative position of the
cannula to the nozzle. It can be set manually with an adjustment screw and a lock nut.
The resulting sample aerosol strikes the baffle ball. Larger droplets condense on the
baffle ball and run off via the siphon. The fuel flow strikes the surface of the baffle ball
at a right angle. The aerosol that is produced passes the mixing chamber to flow to the
burner. On the way through the mixing chamber, an equilibrium is reached. Other
large droplets are separated by gravity and run off via the siphon. The aerosol is dried
in the flame. During this process, the size of the droplets must be small. Fast evapora-
tion of drops when entering the flame is a precondition for atomizing the sample in
the hot zone of the flame. An incomplete vaporization of the extracting agent has a
negative effect on the accuracy of the analysis result. At the same time, the unvapor-
ized droplets disperse the radiation which results in an increased background absorp-
tion.
The mixing-chamber-nebulizer system is designed to allow the formation of a very
fine aerosol from the aspirated samples. The system requires little maintenance be-
cause the siphon is located directly next to the nebulizer. Large drops drain off imme-
diately and do not enter the mixing chamber. The impeller retains droplets and stabi-
lizes the aerosol cloud. Any liquid residues left in the system can run off into the si-
phon through the continuously rising mixing chamber tube. Furthermore, the baffle
ball must be permanently attached in a central position relative to the nebulizer. It
does not require any readjustment after the mixing chamber nebulizer system is
cleaned.
30
novAA 800 Function and setup
Fig. 14 Nebulizer-mixing-chamber-burner-system
1 Burner 9 Siphon sensor connection
2 Fixing screw for burner 10 Siphon
3 Fuel gas supply 11 Siphon sensor
4 Screw joints of mixing chamber parts 12 Mixing chamber head
5 Locking ring for nebulizer 13 Auxiliary oxidant supply
6 Nebulizer (sample liquid supply) 14 Safety plug
7 Oxidant supply 15 Mixing chamber tube
8 Siphon outlet
31
Function and setup novAA 800
The novAA 800 can be operated with the following types of flames and their corre-
sponding burners:
Acetylene-air flame with 50-mm-single-slit burner (universal burner) or
100-mm-single-slit burner for higher sensitivity
Acetylene-nitrous-oxide flame with a 50-mm-single-slit burner
For laboratory applications that require the determination of elements that are easy to
atomize and such that are difficult to atomize, it is advisable to use the 50-mm-single-
slit burner (universal burner) because it is not necessary to change this burner be-
tween the different measurements.
Uses of the different flame types:
Acetylene-air flame can be used for most elements
Acetylene-nitrous-oxide flame is required for difficult-to-atomize elements such as
boron, aluminum and silicon.
32
novAA 800 Function and setup
1 50-mm-single-slit burner
(universal burner)
2 100-mm-single-slit-burner
The burners made of titanium are inert with respect to the influences of aggressive
sample solutions. The burners can be exchanged easily and can be continuously rotat-
ed up to 90° in-between 2 stops. One stop is positioned in such a way that the burners
are aligned to the optical axis. The 90° stop sets the nonsensitive diagonal position of
the burners for determining main components.
3.7.4 Sensors
Manual or automatic sample supply can be employed for the flame technique and for
the mercury-hydride technique. Automatic operation and multi-element analysis re-
quires the use of an autosampler. The control software of the novAA 800 sets the
parameters and controls the functioning.
The novAA 800 can be operated with the following autosamplers:
The autosampler AS-F is an automatic autosampler.
The autosampler AS-FD also has a dilution function.
33
Function and setup novAA 800
The autosamplers use sample trays with the same diameter. The following sample tray
types are available:
139 positions Sample tray with 129 sample positions for 15-mL tubes on the
outer track and 10 sample positions for 50-mL tubes on the
inner track
54 positions Sample tray with 54 positions for 50-mL tubes
The sample trays should be selected according to the requirements of the analysis:
Available sample volume
Type of signal evaluation
The software-controlled autosampler arm reaches all the positions intended for sam-
ple-taking. The dipping depth into the sample and the special cups is preset, however,
it can be adjusted via the control software.
The novAA 800 supplies the autosamplers with operational voltage. Tray and au-
tosampler arm are driven by stepper motors. The tray is rotated. The autosampler arm
can be rotated and lowered by 120 mm.
At the top of the autosampler AS-F next to the sample tray there is a purge cup with
an overflow. In the autosampler AS-FD the purge cup is located in a plastic block to-
gether with a mixing cup. A diaphragm pump delivers the washing liquid from the
supply bottle into the purge cup – this action cleans the dipped cannula by washing it
inside and out. During the purging process a second diaphragm pump pumps any ex-
cess washing liquid to the waste receptacle located underneath the table.
The autosampler AS-FD features a separate Fluidics module with a metering syringe
(5000 µL). The Fluidics module is electrically connected to the autosampler and is
supplied with operating voltage via the novAA 800. Standards or samples are diluted
in the mixing cup by first placing the concentrate into the mixing cup. Then the diluent
is added at a high dosing speed (max. volume: V = 25 mL). A fixed waiting time en-
sures complete mixing. A diaphragm pump extracts the residual liquid that has not
been drawn in by the nebulizer.
34
novAA 800 Function and setup
The autosampler AS-FD with dilution function provides the following advantages:
Preparation of standards for calibration by diluting one or several stock standards
in the mixing cup
Dilution of the sample if its concentration is too high, i.e., its element content is
higher than 110 % of the calibration standard with the highest concentration
Dilution of all samples at freely selectable dilution ratios up to a ratio of 1:500
The injection module SFS 6 (Segmented Flow Star) is available as an optional accesso-
ry. It may be used in combination with an autosampler or in manual mode.
The SFS 6 ensures reproducible conditions in the flame. It permanently draws in purg-
ing and carrier solution which allows to keep the burner at a constant temperature.
Small sample volumes can be measured in a reproducible manner and gaged against a
carrier solution.
The operating principle of the injection module SFS 6 is based on a magnetic valve
with two inlets and one outlet to the nebulizer. The sample aspiration tube is located
at the energized inlet. It is dipped directly into the sample or is connected to the au-
tosampler cannula. The non-energized inlet is connected to the aspiration tube for the
washing or carrier solution.
There are two switching states:
Basic state: Sample path is blocked, washing solution path is free
Active state: Sample path is free, washing solution path is blocked
The injection module SFS 6 is controlled by the ASpect LS software.
35
Function and setup novAA 800
It is recommended to use the automatic cleaner of the burner head (scraper) for con-
tinuous and fully automated operation with a nitrous oxide flame. When working with
the nitrous oxide flame and particularly when working with a flame with very high fuel
gas content, as used for determining the elements silicon, tungsten, molybdenum and
tin, a carbon deposit will gradually build up on the slit of the burner. If these deposits
are not constantly removed, the burner slit will get clogged. This would lead to a low
reproducibility of the measurement results.
Once activated in the software and stored as a method parameter, the scraper guaran-
tees a continuous and reproducible measuring process without any disturbances and
interruptions. The automatic cleaning of the burner head varies with the composition
of the flame and the analysis task. On the other hand, the scraper can also be used for
the automation of the burn-in process of the nitrous oxide flame. When activated in
the FLAME / CONTROL window, a cleaning step is executed every 30 s.
The scraper is fixed to the burner head with two knurled head screws. It can be de-
tached if it is not needed. The scraper can be retrofitted to a 50-mm burner.
36
novAA 800 Function and setup
The Air Purge Kit (APK) is used in combination with the atomic absorption spectrome-
ters of the novAA series (novAA 800, novAA 400 P Flame) to purge the spectrometer.
The purging process with purified and dried air prevents the ingress of dust and cor-
roding vapors into the optical area of the spectrometer. This significantly improves the
quality of the chemical analysis and the service life of the spectrometer even under
difficult ambient conditions.
For a description of the Air Purge Kit, please refer to the corresponding manual of the
accessory.
The hydride systems available range from simple batch systems for users with small
sample volumes through to fully automated continuous devices with flow injection.
For a more detailed description of the hydride systems, please refer to the respective
accessory manuals.
37
Installation and initial start-up novAA 800
CAUTION
Prevent any unauthorized interference!
The device may only be assembled, installed and repaired by service engineers from
Analytik Jena or by technical personnel authorized by Analytik Jena.
CAUTION
Observe the safety instructions!
When installing and starting up the device, please observe the instructions provided in
the section "Safety instructions" on page 9. Compliance with these safety instructions is
a requirement for the error-free installation and the proper functioning of your AAS
measuring environment. Always observe all warnings and instructions which are dis-
played on the device itself or which are displayed by the control and analysis software
ASpect LS.
The novAA 800 will be delivered directly to the final instrument location by a transport
company. The delivery by this company requires the presence of a person responsible
for the instrument installation.
All persons designated for operating the device are obliged to attend the briefing of
the Analytik Jena service department.
The customer must ensure that the installation conditions at the place of installation
comply with the specifications stipulated by Analytik Jena (→ section "Installation con-
ditions" on page 38).
NOTICE
The device may only be assembled, installed and repaired by service engineers from
Analytik Jena or by technical personnel authorized by Analytik Jena. Any unauthorized
interference limits warranty entitlements.
The assistance of one person is required during some stages of the installation process.
The service engineer will test the device and document the test in the test report of the
novAA 800.
The operator must provide everything that is not included in the original delivery, but
required for operating the novAA 800. Operation of the novAA 800 demands certain
local and system-specific requirements:
Suitable place for assembly
Space requirement
Environmental conditions
Supply of inert gas, fuel gas and oxidant
38
novAA 800 Installation and initial start-up
Exhaust unit
Mains connection
CAUTION
Pay attention to the safety instructions in the chapter "Safety instructions" on page 9.
Observe work protection regulations. Warnings regarding potential dangers do not
replace valid work protection regulations!
The novAA 800 may only be operated within closed rooms. The location must be set
up like a chemical laboratory. The location must meet the following conditions:
The installation site must be devoid of dust, draft air currents, vibrations and caus-
tic fumes.
Do not place the novAA 800 near sources of electromagnetic interference.
Avoid direct sunlight and heater radiation on the novAA 800. In extreme cases,
provide air conditioning in the room.
A separate room is recommended for sample preparation and storing chemicals.
The following ambient conditions must be met by the operating room of the no-
vAA 800:
The ambient conditions for the novAA 800 are identical for operation and storage.
39
Installation and initial start-up novAA 800
WARNING
Observe the mains connection!
During electrical installation, observe any local regulations! The mains supply must be
correctly earthed. Do not use an adapter in the mains cabling.
novAA 800 D + G The models novAA 800 D and novAA 800 G are operated on a single-phase alternat-
ing current network. The current load at the maximum heating rate can reach up to
40 A for a short period (1 s). The mains voltage at the novAA 800 P should not de-
crease by more than 6 % during this period. In case of deviations from these values,
please contact the Analytik Jena service department. Appropriate accessories can be
supplied.
Optimum device function strongly depends on a correct mains connection with ade-
quate cable cross-section. The mains connection must be protected by a 35 A slow-
blow fuse on the input (building) side and must be installed prior to delivery of the
novAA 800 near the assembly point. The length of the instrument cable is 3 m. The
CEE surface socket (two-pole + E Blue 5UR 3 206-2 220/32, Siemens) is supplied
according to the terms of delivery.
The auxiliary components that are to communicate with each other, for example PC,
monitor, printer and hydride system, have to be connected to the power strip that is
supplied with the device. The power strip is plugged into the rear of the novAA 800 D
and G and is connected to the same phase as the base device itself. The compressor
needs a separate power supply.
If you use your own PC printer configuration, and if it is connected via the 5-socket
power strip, please observe the limit of the permitted line current. To avoid sudden
voltage fluctuations, do not connect the novAA 800 to the same electrical circuit as
other power-intensive devices.
Conditions for Supply voltage 230 V ~
switching on
Frequency 50 / 60 Hz
Mains fuse 35 A, safety fuse, slow blow, single phased
installation in the
building
Power consumption 2600 VA (basic device: 1400 VA + output socket: 1200 VA)
Maximum current 28 A for a period of 8 s or 40 A for 1 s
consumption
Output socket Same as input voltage
For connection of accessories: PC, monitor, printer, hydride
system, cooling unit
Power consumption of the 650 VA while heating the cell
hydride system 400 VA in continuous operation
novAA 800 F The novAA 800 F is operated on single-phase alternating current. Optimum device
function strongly depends on a correct mains connection. The mains connection must
be protected by a 16 A slow-blow fuse on the input (building) side. The length of the
instrument cable is 2 m.
40
novAA 800 Installation and initial start-up
The auxiliary components that are to communicate with each other, for example PC,
monitor, printer and hydride system, have to be connected to the power strip that is
supplied with the device. The power strip is plugged into the rear of the novAA 800 F
and is connected to the same phase as the base device itself. The compressor and cool-
ing unit need a separate power supply.
If you use your own PC printer configuration and connect the printer to the 5-socket
power strip, observe the maximum permissible operating current. To avoid sudden
voltage fluctuations, do not connect the novAA 800 to the same electrical circuit as
other power-intensive devices.
Conditions for Supply voltage 230 V ~
switching on
Frequency 50 / 60 Hz
Mains fuse 16 A, single phase
installation in the
building
Power consumption 1350 VA (basic device: 150 VA + output socket: 1200 VA)
Output socket Same as input voltage
For connection of accessories: PC, monitor, printer, hydride
system
Power consumption of the 650 VA while heating the cell
hydride system 400 VA in continuous operation
WARNING
Risk of explosion due to leaking acetylene! Risk of the build-up of an oxygen-deficient
atmosphere caused by leaking gas!
The operator must ensure that the connector type used on the outlet side of the gas
pressure controller complies with the national requirements.
The operator must carry out the necessary safety leakage tests on all gas supply lines
and connectors including those on the device on a weekly basis. For this, possible pres-
sure losses from closed systems and lines under pressure are to be determined. The
leak is to be localized and corrected immediately. If the gas is supplied via compressed
gas cylinders, these must be attached to the wall with cylinder mounts in an upright
position outside the laboratory.
Gases in the The inert gas argon is used to protect the graphite components of the atomizer which
graphite tube technique are subjected to extreme temperatures. The inert gas is also used as a means of
transport for the pyrolysis components accrued during the analysis. The purity of the
inert gas is extremely important for the analysis and for the useful life of the graphite
tube.
Introducing an auxiliary gas during the pyrolysis (e.g. compressed air), can accelerate
the ashing of the sample, i.e. the removal of the matrix components. The auxiliary gas
is fed in through the "Gas Auxiliary" connection (item 2 in Fig. 28 on page 50) at the
rear of the device.
The inlet pressure on the spectrometer must be 600 to 700 kPa.
41
Installation and initial start-up novAA 800
The pressure hose for argon is included in the delivery. The standard length of the
hose is 5 m. Other hose lengths can be provided upon request. Please contact the Ana-
lytik Jena service department.
Gases in The flame technique requires an oxidant (compressed air or nitrous oxide) and acety-
flame technique lene as a fuel gas. On request Analytik Jena can also supply accessories to use propane
as a fuel gas.
The purity of the gases is extremely important for the analysis. The piston compressor
PLANET L-S50-15 can be used to supply the compressed air. If compressed air is sup-
plied via an in-house compressed air supply system, please consult the service depart-
ment at Analytik Jena. Nitrous oxide and acetylene are supplied via compressed gas
cylinders or an in-house supply system.
The pressure hoses are supplied. The pressure reducing valves are optional.
Length of the hose for cylinder connection 5m
Length of the hose for compressor 5m
It is also possible to connect other hose lengths. Please consult the service department
at Analytik Jena.
CAUTION
Risk of poisoning due to leaking gases!
Switch on the exhaust unit prior to starting the novAA 800. Extract the exhaust air
from the laboratory and prevent congestion!
42
novAA 800 Installation and initial start-up
Correct extraction can only be ensured by an exhaust hood that is installed directly
above the sample chamber.
The exhaust unit should remove health-damaging combustion residues of the flame as
well as any ozone that is produced during combustion. Ozone is produced when air
reacts with UV radiation from the hollow cathode lamps and the burner flame. Use a
suction device made of heat-resistant and corrosion-resistant material. The first 6 m of
the exhaust air system should be made of metal.
Parameter Properties
Material V2A
Exhaust performance for graphite tube Approx. 1 m3/min
technique
Exhaust performance for nitrous oxide Approx. 8 to 10 m3/min
flame
Exhaust performance for air flame Approx. 5 m3/min
Hood opening Approx. 300 x 300 mm
Distance to the upper edge of the device Approx. 200 to 300 mm
Tube diameter Approx. 100 to 120 mm
The novAA 800 is a compact device conceived to be mounted on a table. The required
space depends on the number of components needed for measurement. When placing
the device and system components observe a minimum clearance of 15 cm to walls
and neighboring installations.
The PC with the monitor, the printer and the keyboard are arranged beside the base
device. The PC and printer may also be placed on a separate side table.
The workbench must be positioned in a way that allows easy access from all sides. In
addition to that, the workbench must meet the following requirements:
Minimum dimensions:
1800 x 700 mm, select the height based on ergonomic aspects.
Load capacity of the workbench: min. 180 kg
Table surfaces: resistant to wiping, scraping, corrosion and water
The autosamplers for flame mode AS-F or AS-FD are mounted in the sample chamber
of the novAA 800. The storage bottle for the washing liquid of the AS-F or the Fluidics
module of the AS-FD are placed next to the AAS device.
The autosampler AS-GF for the graphite furnace technique is mounted in the sample
chamber.
The accessories for the hydride technique (e.g. HS 60 modular) are placed on a sepa-
rate table in front of the novAA 800. The Air Purge Kit can be placed next to the no-
vAA 800 or on a separate side table (length of the connecting hose: 2 m).
43
Installation and initial start-up novAA 800
44
novAA 800 Installation and initial start-up
Fig. 21 Dimensions of the novAA 800 (with AS-FD and Fluidics module)
45
Installation and initial start-up novAA 800
46
novAA 800 Installation and initial start-up
47
Installation and initial start-up novAA 800
The supply lines are connected by the technicians of the Analytik Jena service depart-
ment during the installation of the novAA 800.
The mains switch is located on the right side of the novAA 800. The right device side
also contains an easily accessible connection panel with interfaces for PC and accesso-
ries. The media connections for gases, cooling water and electricity as well as the fuses
are located on the rear panel. The mains connection for the power strip supplied to
connect the accessories is equally located at the rear.
A pair of carrying handles is fastened to the left and the right for transport and instal-
lation. After installation the handles are unscrewed and the openings sealed with the
plugs supplied with the device.
48
novAA 800 Installation and initial start-up
49
Installation and initial start-up novAA 800
The novAA 800 D is equipped with connections for the following gases: Inert gas (ar-
gon) and auxiliary gas (e.g. compressed air) for graphite furnace technique and fuel
gas (acetylene), nitrous oxide and compressed air for flame technique. The no-
vAA 800 G does not have any connections for the flame gases. The novAA 800 F does
not have the connections for inert gas and auxiliary gas.
1 Connection inert gas (argon)
2 Connection auxiliary gas
3 Connection Air Purge Kit
4 Cooling water return flow "Water out"
5 Cooling water inlet "Water in"
50
novAA 800 Installation and initial start-up
Type plate The type plate is located on the rear of the device. The type plate contains the serial
number and the electrical connection data.
Device type and model AAS novAA 800 D AAS novAA 800 F
AAS novAA 800 G
Voltage / Frequency 230 V ~ 230 V ~
50 / 60 Hz 50 / 60 Hz
Power consumption 2600 VA 1350 VA
Max. current consumption max. 28 A/8 s or n/a
max. 40 A/1 s
Serial number S-NR 10-1430D-AQXXX (D – model specification)
The serial number is also attached to the top of the lamp chamber.
NOTICE
Removing the transport locks! The transport locks must be removed by Analytik Jena
service engineers or technical personnel authorized by Analytik Jena during the initial
device installation.
Transport lock on the For transportation, the monochromator of the novAA 800 is protected by a securing
monochromator device. In addition to that, the graphite furnace of the combined device novAA 800 D
and the novAA 800 G is tilted backwards and secured in parking position by a
transport lock (red foam).
The two transport locks must be removed prior to commissioning the novAA 800.
51
Installation and initial start-up novAA 800
1. Unscrew and remove the clamps of the device cover on the left and right side walls
(item 1 in Fig. 24).
2. Remove the device cover.
3. Unscrew the red-marked transport lock (arrow in Fig. 29) from the mesh lever and
remove it from the spectrometer chamber.
Retain the transport locks for future use.
4. Cover the opening in the photometer hood with non-transparent black adhesive
tape.
5. Place the device cover and fasten the clamps on the left and right side walls.
Transport locks on the
graphite furnace
Pull out the red and white transport lock from the sample chamber of the no-
vAA 800 D or the novAA 800 G and retain them for future use.
After unlocking the graphite furnace it can be tilted forwards into the optical axis (→
section "Changing the atomization technique" on page 60).
52
novAA 800 Installation and initial start-up
Installing and launching the software program ASpect LS are described in the "AS-
pect LS" manual.
WARNING
Risk of skin and eye damage caused by UV radiation! Turn off the lamp current before
opening the lamp chamber.
To do so, open the section OPTICAL PARAMETERS in the SPECTROMETER / CONTROL window
of the ASpect LS software and set the lamp current [mA] to zero. Open the drop-down
list BACKGROUND CORRECTION and select the option NO BACKGROUND. Click [SET]. Negate
the error message.
53
Installation and initial start-up novAA 800
CAUTION
Risk of burns! Allow lamps to cool down before replacing them.
NOTICE
Risk of damage to the lamp! Do not touch the lamp window. Remove and install lamps
only when the device is de-energized.
The 8-lamp turret should preferably be loaded with coded hollow cathode lamps. The
use of uncoded lamps is possible.
The lamp turret is usually de-energized before it is loaded. However, lamps can also be
loaded or replaced while the turret is energized.
1 Bracket of the deuterium
hollow cathode lamp
2 Deuterium hollow cathode
lamp
3 Base plate of the lamp turret
4 Hollow cathode lamp (position
of the lamp turret for
removal and installation)
5 Tension spring
The 8-lamp turret and the deuterium hollow cathode lamp are located behind the left
front door in the lamp chamber of the novAA 800. The unit can also be accessed via
the left side wall after removing the cover plate.
54
novAA 800 Installation and initial start-up
In energized state In energized state, it is possible to move the lamp turret to the desired position using
the control software. Furthermore, it is possible to configure uncoded lamps for
mounting and dismounting in ASpect LS (→ section "Configuring the lamp turret in
ASpect LS" on page 56).
1. Click the icon to open the SPECTROMETER window and go to the CONTROL
tab.
2. Use the [LAMP TURRET] button to open the corresponding window.
3. Highlight the position that is to be mounted with a lamp or which is to be changed.
4. Click [CHANGE LAMP] to move the lamp turret to the desired position.
5. Replace the lamp (see above).
6. Configure the uncoded lamp in ASpect LS.
7. Exit the LAMP TURRET window by clicking on [CLOSE].
The lamp turret is automatically initialized with the newly loaded lamps.
55
Installation and initial start-up novAA 800
1,3,5
Securing nuts of the
lamp holder
2 Adjustment screws
4 Attachment screws for the
safety bracket of the
lamp holder
Coded lamps If coded lamps are available, the relevant data for the method of analysis which are
saved on the transponder, such as the lamp type, elements, maximum and recom-
mended lamp current as well as maximum and recommended boost current, are read
during initialization and assigned to the lamp position.
56
novAA 800 Installation and initial start-up
Uncoded lamps
NOTICE
Observe the lamp position! If you use uncoded hollow cathode lamps, make sure that
the position data in the software matches the actual loading position in the turret.
1. Click the icon to open the SPECTROMETER window and go to the CONTROL
tab.
2. Use the [LAMP TURRET] button to open the corresponding window.
3. Highlight the position that is to be mounted with a lamp or which is to be changed.
4. Use [CHANGE] to open the SELECT LAMP/ELEMENT window.
57
Installation and initial start-up novAA 800
For M-HCL it is possible to select several elements. Clicking the symbol of the ele-
ment again will clear the selection. Selected elements are shown in the adjacent
table.
6. Click [OK] to exit the SELECT LAMP/ELEMENT window and return to the LAMP TURRET
window.
The new lamp specification is automatically loaded to the table of the LAMP TURRET
window.
7. Exit the LAMP TURRET window by clicking [CLOSE].
The lamp turret is automatically initialized with the newly loaded lamps.
Fine adjusting the lamps is generally required only once after a new installation of the
lamp.
Maximizing the The useful life of the lamp strongly depends on the current setting for the lamp. The
useful life of the lamp recommended operating current varies from lamp type to lamp type. For the following
adjustment, observe the instructions in the cookbook of the ASpect LS software, the
Analytik Jena operating instructions for the various lamps and the information sup-
plied with the lamp.
Adjusting the
line source 1. Click the icon to open the SPECTROMETER window and go to the CONTROL
tab.
2. Use the [LAMP TURRET] button to open the corresponding window.
58
novAA 800 Installation and initial start-up
The lamp is then automatically adjusted relative to a pitch circle. In the lamp align-
ment area, the energy is displayed as a blue bar during the adjustment.
Adjusting the deuterium
hollow cathode lamp 1. Click the icon to open the SPECTROMETER window and go to the CONTROL
tab.
2. Click the [ELEMENT] button to open the SELECT ELEMENT/LINE window.
3. Click on the blue button to select the element. Select the wavelength range 190-
350 nm from the Line table. Click on [OK] to close the window.
4. Open the drop-down list BACKGROUND CORRECTION and select the option ONLY D2
BACKGROUND.
7. Initiate the energy measurement by clicking on [START]. Wait until the D2-HCL has
started.
8. Set the energy level to a maximum value:
With focus adjusting: Move the lamp holder up or down slightly before tightening
the securing nuts (items 1, 3, 5 in Fig. 33 on page 56).
With axis adjustment: Adjust the adjustment screws (item 2 in Fig. 33).
9. Stop the adjustment process by clicking on [STOP] and click [CLOSE] to exit the
dialog.
The D2-HCL is adjusted.
59
Installation and initial start-up novAA 800
NOTICE
Always switch off the novAA 800 before installing or removing the autosampler or the
hydride system! Connecting or disconnecting electrical contacts may damage the sensi-
tive electronic components of the novAA 800.
novAA 800 D In the combined device novAA 800 D the flame atomizer and the graphite furnace are
both attached to a bracket on the height adjustment that can be tilted by 60°.
Proceed as follows to change the atomization technique:
Push up the locking lever (item 1 in Fig. 38) and unlatch it.
When doing so, use the tilt lever (item 2 in Fig. 38) to tilt the graphite furnace
backwards or forwards until it reaches the stop. Bring the atomizer into the desired
working position.
1 Locking lever
2 Tilt lever
For the flame technique, it is possible to adjust the position of the stop using the set-
screw (→ section "Aligning the atomizer within the beam path" on page 105).
Changing from one atomization technique to the next only requires a few additional
steps such as removing the autosampler.
Changing from graphite 1. Close the control software ASpect LS. Shut down the PC and novAA 800. Uninstall
furnace to flame atomizer the autosampler AS-GF and remove the depth-adjustable stop.
2. Tilt the graphite furnace backwards to bring the mixing-chamber-nebulizer system
into working position.
3. Fill the siphon with water via the mixing chamber tube until the water starts run-
ning off via the outlet tube.
4. Install the burner on the mixing chamber tube and clamp it to the stop.
5. Mount the safety glass pane.
60
novAA 800 Installation and initial start-up
NOTICE
After removal of the burner, close the mixing chamber tube with the safety stopper.
Otherwise, acid fumes could escape from the siphon and damage the novAA 800. Fur-
thermore, the water in the siphon can not leak out when you tilt the mixing-chamber-
nebulizer system backwards.
novAA 800 G The novAA 800 G can be used for graphite furnace, HydrEA and hydride technique.
Together with a clamped connector, the graphite furnace is attached to a height ad-
justable bracket that can be tilted by 60°. The connecting piece serves as a receptacle
for the cell unit of the hydride system.
To change over to the hydride technique:
Push up the locking lever (item 1 in Fig. 38) and unlatch it.
When doing so, use the tilt lever (item 2 in Fig. 38) to tilt the graphite furnace
backwards until it reaches the stop. Bring the clamped connector into the desired
operating position.
Attach the cell unit to the connector and use the attachment screws to lock it in
that position.
Follow the separate operating instructions to install the hydride system. Take care
to switch off the novAA 800 before installing the hydride system.
First switch on the PC, then the novAA 800.
Open the window MAIN SETTINGS in the ASpect LS to select the hydride technique.
Initialize the device.
61
Installation and initial start-up novAA 800
4.8.1 Connections in the sample chamber for the graphite tube technique
Fig. 39 Elements in the sample chamber for the graphite furnace technique
1 Plastic pin for attaching the safety glass pane 3 Graphite furnace with connections
(flame technique only) 4 Height-adjustable stop for AS-GF
2 AS-GF receptacle on the right sample chamber 5 AS-GF hinge on the right sample chamber
62
novAA 800 Installation and initial start-up
The connections for gas, cooling water and electric current are permanently installed
on the graphite tube furnace.
Open the MAIN SETTINGS window in the ASpect LS software to set the options for the
graphite furnace technique. The user interface of the software is updated with the
method and device parameters after initialization.
63
Installation and initial start-up novAA 800
The following options are available for the graphite furnace technique:
The height of the graphite furnace is automatically adjusted to the different graphite
furnace models (automatic detection).
64
novAA 800 Installation and initial start-up
NOTICE
The graphite tubes of the novAA 800 are custom-made and must be ordered from
Analytik Jena. Do not use any other graphite tube. Other graphite tubes can damage
the novAA 800.
Never touch the graphite tube with your bare fingers! Fingerprints burn into the sur-
face, and this causes premature damage to the pyrolysis coating of the tube.
Inserting the
1. Use the button in the ASpect LS to open the FURNACE window. Go to the
graphite tube
CONTROL tab.
65
Installation and initial start-up novAA 800
CAUTION
Risk of burns!
Allow the graphite tube furnace to cool down before removing the graphite tube.
NOTICE
Never touch the graphite tube with your bare fingers!
Fingerprints burn into the surface, and this causes premature damage to the pyrolysis
coating of the tube.
1. Use the [OPEN FURNACE] button in the FURNACE / CONTROL window to open the
graphite furnace (Fig. 42 on page 65).
2. Remove the graphite tube with tweezers. Use gloves when removing the tube by
hand.
3. Insert the new graphite tube and use the [CLOSE FURNACE] button to close the fur-
nace.
66
novAA 800 Installation and initial start-up
1. Use the button in the ASpect LS to open the FURNACE / CONTROL window.
2. Enter the data for the current graphite tube in the FURNACE / CONTROL window:
Used graphite tube Heat cycles Current value of the graphite tube
Life time Current value of the graphite tube
67
Installation and initial start-up novAA 800
1. Use the button in the ASpect LS to open the FURNACE / CONTROL window.
2. Set the following parameters in the group box CLEAN FURNACE:
HydrEA method The following temperature program must be used for baking out gold-coated and
iridium-coated graphite tubes (also refer to the operating instructions for the hydride
system). A higher final temperature is required to evaporate the metal coating.
ELEMENT Au Ir Au Ir
TEMP. [°C] 1000 2200 1800 ≤ T ≤ 2600 ≤ 2600
RAMP [°C/S] 500s 500
HOLD [S] 10 10
Do not select a longer dwell time to avoid excessive load on the furnace.
NOTICE
Always switch off the novAA 800 before installing or removing the AS-GF!
Connecting or disconnecting electrical contacts may damage the sensitive electronic
components of the novAA 800.
Choose a safe location for the completion of the AS-GF. The device can tilt easily.
68
novAA 800 Installation and initial start-up
69
Installation and initial start-up novAA 800
7. Hang the AS-GF into the receptacles of the sample chamber (items 1 and 7 in Fig.
44). Check whether the autosampler is horizontally aligned. If necessary, adjust the
position of the autosampler using the depth-adjustable stop.
8. If necessary, align the AS-GF with the furnace (coarse adjustment):
Manually move the autosampler arm above the dosing opening of the graphite
tube. If the dosing tube does not reach the opening, move the suspension of the
autosampler backwards or forwards (in y-direction). Remove the autosampler from
the sample chamber to do this. Use the adjustment screw 1 and the setscrew (2, 4
in Fig. 45) to move the left and the right suspension. The setscrews must be ad-
justed with a screwdriver. Fit the autosampler back on the suspension and check
the coarse adjustment. Repeat the procedure as required.
9. Plug the control cable into the socket on the connection panel of the AAS device
(autosampler graphite connection, item 1 in Fig. 25 on page 49).
10. Place and fix the sample tray on the axis of the AS-GF.
11. Place the sample cover until it sits in the guide rail.
12. If applicable, mount the dosing syringe to the dosing unit (→ section "Replacing
the dosing syringe" on page 110).
13. Switch on the PC and the novAA 800, wait until the end of the spectrometer initial-
ization, start the ASpect LS software and initialize the system.
The autosampler AS-GF is installed in the sample chamber.
Preparing the novAA 800 Prior to installing the HydrEA technique the graphite tube must be coated with iridium
for the HydrEA technique or gold (see hydride system manual). To do this, use the autosampler AS-GF with the
dosing tube used during graphite operation. Alternatively, pipette the iridium or gold
stock solution (c = 1 g/L) into the graphite tube by hand.
1. Use the autosampler to coat the graphite tube with iridium or gold.
70
novAA 800 Installation and initial start-up
Notice!
Do not use the titanium cannula for the coating.
2. Switch off the novAA 800 and install the hydride system (e.g. HS 60 modular).
3. For the HydrEA technique, loosen the clamp nut of the hose guide and pull out the
dosing tube. Remove the dosing tube from the tube holder on the autosampler
arm.
4. Insert the titanium tube into the hose guide until it protrudes from the bottom by
8 mm. Attach the titanium cannula with the clamp nut.
5. Attach the reaction gas tube (from the hydride system) to the titanium cannula.
Suitable autosamplers for the continuous introduction of samples into the hydride
system HS 60 modular are the AS-F and the AS-FD.
The AS-GF has already been installed in the sample chamber in accordance with sec-
tion "Installing the autosampler" on page 68. The fine alignment of the AS-GF to the
furnace is carried out in a software-controlled process. During this autosampler align-
ment, the dosing tube is put to the ideal position to deliver the samples in the graphite
tube without touching the dosing insert, for instance. The injection depth for the sam-
ple is set in the same process.
1. Start the ASpect LS software, click on the symbol to open the AUTOSAMPLER
window and switch to the TECHN. PARAMETERS tab.
2. Click the [ALIGN SAMPLER TO FURNACE] button to start the alignment.
3. Follow the prompts in the dialog fields of the software.
71
Installation and initial start-up novAA 800
Further configurations of the autosampler can be found in the "ASpect LS" manual in
the section "Technical autosampler parameters".
72
novAA 800 Installation and initial start-up
1. Observe the sequence for switching off the novAA 800 and its accessories and turn
the devices off.
2. For HydrEA coupling:
Remove the reaction gas tube from the titanium cannula. Loosen the clamp nut
before pulling the titanium cannula off the tube guide.
3. Remove the control cable from the socket in the right side wall of the AAS device
(autosampler graphite connection).
4. Loosen the adjustment screws 2 and 3 and remove the autosampler AS-GF from
the sample chamber.
5. Remove the depth-adjustable stop from the sample chamber.
6. Screw the plastic pins back in.
73
Installation and initial start-up novAA 800
1 Suspension for injection module SFS 6 4 Connection for injection module SFS 6
2 Suspension for autosampler, right side 5 Siphon monitoring connection
3 Scraper connection 6 Suspension for autosampler, left side
74
novAA 800 Installation and initial start-up
Set the option FLAME in the TECHNIQUE group of the MAIN SETTINGS window of the AS-
pect LS software.
The user interface of the software is updated with the method and device parameters
after initialization.
With manual sample introduction the sample is loaded directly to the burner-nebulizer
system. It is possible to use the injection module SFS 6.
NOTICE
Switch off the novAA 800 prior to installation! Connecting or disconnecting electrical
plug-in contacts may damage the sensitive electronic components of the novAA 800.
1. Observe the sequence for switching off the novAA 800 and its accessories and turn
the devices off.
2. Check that the mixing-chamber-nebulizer system properly sits in the retainer of
the height adjustment. The plate of the mixing chamber tube must have contact.
The white marking on the mixing chamber tube must be positioned above the
edge of the retainer (item 2 in Fig. 50).
75
Installation and initial start-up novAA 800
1. Attach the outlet tube to the connector of the siphon and the corresponding open-
ing in the lid of the waste bottle.
Note: Route the outlet tube in a constant downward slope. If necessary shorten the
tube. The tube must not dip into the liquid.
2. Fill the siphon with water via the mixing chamber tube until water flows out via
the outlet tube.
3. Plug the connector of the siphon sensor to the connection on the right sample
chamber wall (item 5 in Fig. 48 on page 74).
4. Push the collection tray underneath the burner-nebulizer system in the sample
chamber.
5. Connecting the gas supply:
Fuel gas hose (red) at the top of the mixing chamber head
Oxidant hose (blue) at the side of the nebulizer
Auxiliary oxidant hose (black) at the side of the mixing chamber
Only tighten the knurled-head screws finger tight.
6. Plug the nebulizer into the mixing chamber head and lock it with the ring.
7. Attach the aspiration tube to the nebulizer cannula.
76
novAA 800 Installation and initial start-up
8. Attach the required burner (50 mm or 100 mm) to the mixing chamber tube, turn
to the stop position and clamp. Ensure that the burner is positioned correctly.
There are markings on the mixing chamber tube and the retainer.
9. Injection module SFS 6
If you are working with the injection module SFS 6, install the injection module
SFS 6 (→ section "Installing the injection module SFS 6" on page 81).
10. Place the sample or purge cups in front of the device or on a separate side table.
11. Hang the safety glass in and slide it in front of the burner.
12. Switch on the novAA 800 and start the ASpect LS software.
The burner-nebulizer system is installed and prepared for manual sample in-
troduction.
Steps 1. Observe the sequence for switching off the novAA 800 and turn the device off.
Demounting
2. If you worked with the injection module SFS 6, put the injection module SFS 6 out
of operation (→section "Installing the injection module SFS 6" on page 81).
3. Remove sample cups and purge cups.
In continuous working mode, the samples are loaded via the autosampler AS-F
or AS-FD.
77
Installation and initial start-up novAA 800
Installing the burner- 1. Observe the sequence for switching off the novAA 800 and its accessories and turn
nebulizer system the devices off.
2. Check that the mixing-chamber-nebulizer system properly sits in the retainer of
the height adjustment. The plate of the mixing chamber tube must have contact.
The mixing chamber must be aligned to the height adjustment, the marking on the
connector must be above the edge of the holding fixture (item 2 in Fig. 50 on
page 76).
3. Attach the waste tube to the connector of the siphon and the corresponding open-
ing in the lid of the waste bottle.
Note: Route the outlet tube in a constant downward slope. If necessary shorten the
tube. The tube must not dip into the liquid.
4. Fill the siphon with water via the mixing chamber tube until water flows out via
the waste hose.
5. Plug the connector of the siphon sensor to the connection on the right sample
chamber wall (item 5 in Fig. 48 on page 74).
6. Push the collection tray underneath the burner-nebulizer system in the sample
chamber.
7. Connecting the gas supply:
Fuel gas hose (red) at the top of the mixing chamber head
Oxidant hose (blue) at the side of the nebulizer
Auxiliary oxidant hose (black) at the side of the mixing chamber
Only tighten the knurled-head screws finger tight.
8. Plug the nebulizer into the mixing chamber head and lock it with the ring.
9. Attach the required burner (50 mm or 100 mm) to the mixing chamber tube, turn
to the stop position and clamp. Ensure that the burner is positioned correctly.
There are markings on the mixing chamber tube and the retainer.
Installing the If you are working with injection module SFS 6, install injection module SFS 6 (section
injection module "Installing the injection module SFS 6" on page 81).
Installing the 1. Hang the autosampler in the corresponding receptacles of the sample chamber
autosampler (items 2, 6 in Fig. 48 on page 74). Adjust the adjustment screw on the right sus-
pension so that the autosampler cannot slip out of the mounting hole (item 3 in
Fig. 52 on page 79).
2. Place the Fluidics module (for AS-FD) or storage bottle for washing liquid (for AS-
F) next to the AAS device.
3. Plug the control cables for connecting the autosampler to the Fluidics module and
the AAS device into the connections on the rear of the autosampler and lock them
in place (items 1 and 2 in Fig. 52 on page 79). If necessary, unhinge the right side
of the autosampler to do this.
4. Plug the control cable into the "Sampler flame" connection on the right side wall of
the novAA 800 (item 2 in Fig. 25 on page 49) and lock it in place.
5. Attach the outlet tube to the outlet connector of the autosampler (rear panel,
item 4 in Fig. 52 on page 79). Attach the outlet tube to the respective opening of
the lid of the collecting bottle.
78
novAA 800 Installation and initial start-up
Note: Route the outlet tube in a constant downward slope. If necessary shorten the
tube. Tube must not dip in the liquid.
6. Screw the tube for the purging liquid into the rear of the autosampler (item 5 in
Fig. 52 on page 79).
Note: In the AS-FD the tubes for connecting the autosampler with the Fluidics
module are numbered and attached to each other by a jacket. The tubes are at-
tached to the rear of the autosampler using the attachment lug. Marking Wash
tube "2".
7. Feed the dosing tube for the diluent (marking "1") in the AS-FD through the tube
guide on the autosampler arm and attach it to the thicker cannula of the au-
tosampler arm.
Note: The autosampler arm can be moved manually when the device is switched
off.
8. Stick the sample aspiration tube onto the nebulizer cannula.
9. Route the sample intake tube through the tube guide at the autosampler arm and
plug it onto the thin cannula of the autosampler arm.
10. Lay the sample tray on the autosampler casing, make sure it clicks into place.
11. Place the sample cover until it sits in the guide rail.
1 Fluidics module connection
2 AAS connection
3 Suspension mount with adjust-
ment screw
4 Connector for outlet tube
5 Screw for purge tube
6 Suspension for injection module
SFS 6
79
Installation and initial start-up novAA 800
12. If applicable, mount the dosing syringe to the dosing unit (→ section "Replacing
the dosing syringe" on page 110).
13. Place the storage bottles for the washing liquid (left) and diluent (right) into the
bottle holders of the Fluidics module.
14. Immerse the short tube (marking at the tube "3") into the storage bottle for the
diluent. Screw the second tube end to the valve (item 2 in Fig. 53).
15. Screw the dosing tube for the diluent (sheathed, marking "1") to the second con-
nection of the valve (item 3 in Fig. 53).
16. Immerse the hose for the washing liquid (marking "2") into the storage bottle.
Uninstalling the 1. Observe the sequence for switching off the novAA 800 and turn the device off.
autosampler
2. Detach the sample aspiration tube from the thin cannula of the autosampler arm
and pull it off the tube guide.
3. Detach the tube for the wash liquid at the rear of the autosampler.
4. For the AS-FD, detach the dosing tube for the diluent from the thicker cannula and
pull it off the tube guide. Pull the two encased tubes out of the attachment lug at
the rear of the autosampler.
5. Pull the outlet tube from the connector of the autosampler (backplate).
6. Detach both control cables at the rear of the autosampler.
7. Take the autosampler out of the sample chamber.
Uninstalling the If you are working with the injection module, put the injection module SFS 6 out of
injection module operation (→ section "Uninstalling " on page 82).
80
novAA 800 Installation and initial start-up
81
Installation and initial start-up novAA 800
Uninstalling the injection 1. Remove the aspiration tubes from the washing liquid bottle and the sample cup
module (for manual operation), or pull them off the aspiration cannula of the autosampler
to allow the system to drain.
2. Pull off the short piece of tube from the nebulizer cannula.
3. Detach the control cable of the SFS 6 from the AAS, remove the injection module.
CAUTION
Risk of burns!
To remove the hot burner, use the burner bracket (optional accessory). Otherwise wait
until the burner has cooled down.
When working with the nitrous oxide flame the use of a scraper is recommended
which automatically removes carbon deposits from the burner head in nitrous oxide
operation. Alternatively, carbon deposits can be manually removed from the burner
slot with the scraper. Upon request, the scraper can be mounted to the 50-mm burner
in the factory before delivery. It can also be retrofitted on a 50 mm burner.
NOTICE
For fuel gas flows > 250 NL/h, pay attention to stubborn deposits. Remove these
where necessary to ensure the functionality of the scraper.
1. Unscrew the screws from the front burner jaw (arrow in Fig. 55) (the screw for
fastening the burner on the mixing chamber tube is also located on the side of the
front burner jaw).
2. Unscrew the fastening rail (item 1 in Fig. 56) with the knurled head screws (item 3
in Fig. 56) from the scraper.
The captive knurled head screws remain attached in their holder in the scraper.
3. Mount the fastening rail to the burner body as shown in Fig. 56. Use the three
longer titanium screws and the nuts that were supplied with the equipment to
mount the rail. Insert the screws from the top through the front burner jaw and
screw down the fastening rail with nuts.
82
novAA 800 Installation and initial start-up
4. Attach the scraper to the guide pins of the fastening rail (item 2 in Fig. 56) and
tighten it with knurled head screws (item 3 in Fig. 56).
NOTICE
The mobile cooling unit KM5 is controlled by the novAA 800 and is therefore not
switched on and off manually.
83
Installation and initial start-up novAA 800
1. Close the control software ASpect LS on the PC: Click the menu item FILE EXIT.
2. For unsaved values decide whether data or information should be saved before
exiting the program.
3. Shut down the PC.
4. Use the respective mains switches to switch off (in this order):
Compressor
AAS accessories (e.g. hydride system)
novAA 800
Printer
PC
The AAS system is now switched off.
84
novAA 800 Service and maintenance
WARNING
Electric shock! The novAA 800 must be switched off before carrying out any mainte-
nance work. Pull the mains plug. The safe disconnection of the novAA 800 from the
mains can only be achieved by pulling the mains plug. Power is still supplied to both
certain areas of the spectrometer, as well as the output socket, after the device has
been switched off at the main switch.
The only exception to this are maintenance tasks that must be carried out while the
AAS device and the control software are running, such as the baking out of the graph-
ite tube.
WARNING
Risk of skin and eye damage caused by UV radiation!
HCL, D2-HCL, the heated graphite tube (T > 1000 °C) and the flame of the burner
transmit radiation in the UV range. Do not look into the rays emitted by the lamp, the
graphite tube or the flame without UV protection goggles. Protect the skin against
radiation.
Switch off the lamp by means of the control and analysis software ASpect LS before
opening the lamp door: To do so, open the section OPTICAL PARAMETERS in the
SPECTROMETER / CONTROL window of the ASpect LS software and set the lamp current
[mA] to zero. Open the drop-down list BACKGROUND CORRECTION and select the option
NO BACKGROUND. Click [SET]. Negate the error message.
To observe the placement of the samples or the drying of liquid samples, the dental
mirror may only be inserted into the beam path from the left side of the graphite fur-
nace. When observing on the right side of the furnace, UV radiation may be reflected.
WARNING
The operator is responsible for ensuring the proper decontamination of the device
before maintenance and repair works. This applies to any case in which the inside or
the outside of the device have been contaminated with hazardous substances.
CAUTION
The operator must not undertake any service or maintenance work to this device and
its components other than those specified and described in this chapter.
Please observe the notes in section "Safety instructions" on page 9. Compliance with
the safety instructions is a prerequisite for the error-free operation of the device. Al-
ways observe all warnings and instructions that are displayed on the device itself or
indicated by the control and analysis software ASpect LS.
To guarantee faultless and safe functioning, the novAA 800 should be inspected on an
annual basis by the Analytik Jena service department.
CAUTION
Risk of burns from touching hot surfaces! Observe the required cooling times before
starting any maintenance tasks on the graphite furnace and the burner-nebulizer
system.
85
Service and maintenance novAA 800
Pipetting insert Clean and wash. May be necessary on a daily basis, depending
on the type of samples.
86
novAA 800 Service and maintenance
87
Service and maintenance novAA 800
WARNING
Risk of electric shock!
Prior to replacing the fuses in the novAA 800 always switch off the device with the
mains switch and pull the plug.
The power supply fuses (F1, F2) of the novAA 800 D and G may only be replaced by
Analytik Jena service engineers or by technical personnel authorized by Analytik Jena.
novAA 800 D + G The fuses of the novAA 800 D and G can be found on the rear panel of the device and
within the sample chamber. They are marked.
Fuses Refer to Fig. 27 on page 50 for the fuses
rear panel
Fuse number Type Protected circuit
F3 T 6.3 A/H Socket for external accessories
F4 T 6.3 A/H Socket for external accessories
F5 T 2.5 A/H Transformer, primary side, NTL
F6 T 2.5 A/H Transformer, primary side, NTL
F7 T 0.08 A D2-HCL
F8 T 0.25 A HCLs
F9 T 3.15 A Filament
Fuse for the furnace Refer to item 7 in Fig. 40 on page 63 for the furnace fuse
novAA 800 F The fuses of the novAA 800 F can be found on the rear side of the device (Fig. 27 on
page 50).
88
novAA 800 Service and maintenance
1. Clean the sample chamber regularly using a lint-free cloth moistened with alcohol.
2. In case of residual fluid in the collection tray underneath the mixing-chamber-
nebulizer system (e.g. from the siphon outlet), carefully remove and empty the tray
and rinse it under the tap.
3. Clean the radiation entrance and exit windows of the sample chambers if energy
losses are detected:
Turn the windows to unscrew them from the bayonet lock.
Notice!
Do not clean the furnace windows in an ultrasonic bath. This may lower the UV
permeability of the windows.
Wipe the windows with a lint-free cloth soaked in alcohol (optical cloth) with-
out leaving streaks.
Re-insert the windows to the sample chamber.
Note: After cleaning the window with alcohol, it takes about 1 h before the UV trans-
mission is completely restored.
The gas connectors (on the rear panel of the device) must be checked for leaks:
Weekly in form of a safety check.
If a gas connection is opened when operation is started up again.
To check for leaks, close the stopcock of the gas supply system and observe the pres-
sure reading on the downstream manometer. If the pressure drops significantly, search
and fix the gas leak using the following method:
1. Brush connections with a heavily foaming liquid (e.g., soap solution). If bubbles
form when opening the gas connection, switch off the novAA 800 and disconnect
the gas supply.
2. Unscrew the untight gas connections and check whether they are properly posi-
tioned. Replace worn out sealing rings. Cut off worn out hose ends.
3. Screw on the gas connectors by hand or using a suitable open-end wrench. When
doing so, make sure that the connector is properly placed on the port.
4. Re-check the gas connections for leaks.
After a prolonged operation time, sample residues, modifiers and sublimated carbon
from the graphite tube are deposited on the contact surfaces of the electrodes, the
furnace shroud and the pipetting insert. Such deposits may lead to deviations in the
effective tube temperature and contaminate the samples.
Damages to furnace, ceramic ring, graphite tube or electrodes may be the reason for
poor analysis results, too.
89
Service and maintenance novAA 800
CAUTION
Risk of burning at the hot furnace!
Allow the graphite tube furnace to cool down before attempting any service or
maintenance work.
NOTICE
Do not touch the quartz panes of the furnace windows with your bare hands. Finger-
prints burn in.
Do not clean the furnace windows in an ultrasonic bath. This may lower the UV perme-
ability of the windows.
Danger of embrittlement of the rubber seals. When cleaning the furnace windows with
a cloth soaked in alcohol, make sure that the rubber seals do not come in contact with
the alcohol!
The furnace windows must be cleaned every week with a lint-free cloth soaked in al-
cohol (optical cloth) without leaving streaks. Note: After cleaning the furnace window
with alcohol, it takes about 1 h before the UV transmission is completely restored.
Use a mild surfactant to remove stubborn soiling. Preparing the cleaning solution: Use
a mixture of demineralized water and 1 vol.% cleaning solution.
1. Pull off the furnace windows by hand in a rotating movement. Do not touch the
windows!
2. Fill so much cleaning solution into a beaker that the furnace windows can be com-
pletely submerged in the solution.
3. Let the windows soak in the solution for approx. 30 min at a temperature between
25 and 30 °C.
4. Remove the furnace windows from the cleaning solution (e.g. using plastic pliers,
do not hold the window by the optical surfaces) and rinse them with demineralized
water (σ < 1 µS/cm).
5. Use compressed air or argon to blow dry the windows.
6. Re-insert the furnace windows.
Identical markings must point upwards (→ Fig. 57 on page 91)!
If the furnace windows are too loose or if the sealing rings of the furnace windows
exhibit brittleness and cracks, replace the sealing rings.
The furnace windows are cleaned and re-installed.
90
novAA 800 Service and maintenance
The graphite surfaces must be cleaned every day after using the device.
1. Switch on the novAA 800 and start the ASpect LS software (the movable furnace
part must be pressurized to be opened/closed).
2. Use the button in the ASpect LS to open the FURNACE window. Open the
CONTROL tab.
3. Use the [OPEN FURNACE] button to open the furnace.
4. Remove the pipetting insert from the furnace shroud and clean it in
0.1 to 1 modular HNO3.
Then rinse well with slightly acidic or demineralized water.
5. Clean the contact surfaces of the electrode on the movable part of the furnace with
a cotton swab, a lint-free cloth soaked in alcohol, or nonwoven paper.
6. Clean inner surfaces of the furnace shroud with a cotton swab.
7. Use the [CLOSE FURNACE] button to close the graphite furnace.
The graphite furnace is ready for operation again.
Clean the graphite tube Bake out the graphite tube every day to clean it.
Refer to chapter "Cleaning / baking out the graphite tube" on page 68 for the required
steps.
Cleaning the coated For the HydrEA technique, bake out the graphite tube every day to clean it.
graphite tube
Refer to chapter "Cleaning / baking out the graphite tube" on page 68 for the required
steps.
Evaporating the Evaporate the iridium or gold coating after approx. 500 atomizations or before
iridium coating recoating.
Refer to chapter "Cleaning / baking out the graphite tube" on page 68 for the required
steps.
Replacing the The graphite tube must be replaced if it shows significant burn-up or if it no longer
graphite tube meets analytical requirements. In that case, the pyrolysis layer is run down.
91
Service and maintenance novAA 800
Refer to chapter "Inserting the graphite tube into the furnace" on page 65 for the re-
quired steps.
Electrodes and furnace shroud must be replaced if the device persistently yields poor
analytical results which cannot be adjusted by cleaning or replacing the graphite tube.
1, 3 Electrodes
2 Furnace shroud
These tasks can be completed by the service department in the course of the regular
maintenance. If you wish to perform the maintenance work yourself, you will need the
furnace tools that are available as an option.
1 Insertion tool for
furnace shroud
2 Extractor
3 Insertion tool for
electrodes
4 Allen wrench
5 Ratchet wrench
6 Key wrench
NOTICE
The graphite furnace shown in the following photo series has been removed from the
device to ensure a good view on the individual work steps. However, the graphite fur-
nace does not need to be removed from the sample chamber of the novAA 800 to
perform this maintenance work.
1. Switch on the novAA 800 and start the Aspect LS software (the movable furnace
part must be pressurized to be opened/closed).
92
novAA 800 Service and maintenance
2. Use the button in the ASpect LS graphite furnace technique to open the
FURNACE / CONTROL window.
3. Use the [OPEN FURNACE] button to open the furnace.
4. Use a pair of tweezers to remove the graphite tube from the opened graphite fur-
nace. Wear gloves when removing the tube by hand.
5. Unscrew the cover screw from the mov-
able part of the furnace.
93
Service and maintenance novAA 800
94
novAA 800 Service and maintenance
95
Service and maintenance novAA 800
96
novAA 800 Service and maintenance
97
Service and maintenance novAA 800
Insert the graphite tube into the furnace before re-starting the furnace (→ section
"Inserting the graphite tube into the furnace" on page 65). Form the graphite tube.
The burner-nebulizer system must be cleaned at regular intervals. The following con-
ditions indicate when the system needs to be cleaned:
Irregularities in the flame hem of the burner flame. Washing with diluted acid in
the active program and blowing the burner out does not bring about any improve-
ment.
The sensitivity given in the cookbook for an individual element is not achieved
despite changing the composition of the gas.
Hard deposits on the burner slit occurring during the analysis of solutions with a
high salt content cannot be removed with the cleaning strip.
CAUTION
Risk of burns! Allow the burner to cool down before attempting any service or mainte-
nance work.
98
novAA 800 Service and maintenance
99
Service and maintenance novAA 800
1. Loosen the retaining screw (item 2 in Fig. 60 on page 99) on the burner and re-
move the burner from the connector.
2. Unscrew the screwed tube connections on the mixing chamber head and the nebu-
lizer (items 10 and 11 in Fig. 60) and pull the sample uptake tube off the nebuliz-
er.
3. Turn the locking ring of the nebulizer (item 4 in Fig. 60) to open the locking. With-
draw the nebulizer from the mixing chamber head, holding the nebulizer in the
groove (Fig. 62).
Risk of breaking the connector!
Connector for gas connection may break when being pulled.
4. Unscrew the siphon sensor cable from the connection in the sample chamber
(item 8 in Fig. 60) and pull it off.
5. Remove the outlet tube from the outlet connector of the siphon (item 7 in Fig. 60).
6. Loosen the clamp screw of the siphon and pull off the siphon towards the bottom.
Empty the siphon.
Caution
The solution in the siphon is acidic. Wear protective goggles and clothing.
7. Unscrew the insert of the siphon sensor and remove the sensor from the siphon
(item 11 in Fig. 61).
8. Hold the system tightly, loosen the knurled head screw on the holding bow of the
mixing chamber tube (item 12 in Fig. 60), push the retaining clip backwards and
remove the system.
9. Withdraw the safety plug (item 1 in Fig. 61) from the mixing chamber.
10. Loosen the four screw joints of the mixing chamber (item 5 in Fig. 60) and disas-
semble the mixing chamber into the chamber head and the chamber tube.
11. Remove the impeller (item 3 in Fig. 61) from the chamber tube.
12. Unscrew the gas connections for fuel gas and auxiliary oxidant (item 5 in Fig. 61)
from the mixing chamber head.
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novAA 800 Service and maintenance
Removing Perform the following working steps only when hard deposits haven´t been removed
hard deposits by the procedure described above.
1. Undo the fittings (item 2 in Fig. 63) of the burner jaws on the burner body and
remove the burner jaws.
2. Undo the fittings of the burner jaws against each other (item 1 and 3 in Fig. 63).
3. Remove the burnt residue deposits with burner cleaner (paper strips).
4. Clean the burner jaws in 0.1 molar HNO3, and then wash with distilled water.
5. Screw the burner jaws together and make sure that the ends of the spacers on the
burner slit extension and the end faces are flush.
Note: The spacers must not protrude beyond the upper side of the burner jaws (ar-
row in Fig. 65)! The scraper would get caught on the edges.
6. Screw the burner jaws onto the burner body. The dowel pins (item 4 in Fig. 63) on
the burner ensure correct positioning.
NOTICE
Risk of destroying the scraper!
If the spacers protrude beyond the upper side of the burner jaws, the scraper can get
caught and burn away!
101
Service and maintenance novAA 800
1. Place the nebulizer for several minutes into an ultrasonic bath with approx. 1 % of
HNO3 or organic solvent (isopropyl alcohol).
2. Slightly turn the baffle ball (item 7 in Fig. 61 on page 99) and pull it off the nebu-
lizer. If the baffle ball is seized, place the nebulizer back into the ultrasonic bath for
another few minutes.
3. Insert the cleaning wire into the nebulizer canula and clean the canula by moving it
up and down several times.
4. Attach the baffle ball on the nebulizer and lock it by turning slightly.
Clean the mixing chamber consisting of the chamber tube and the chamber head. Pro-
ceed as follows:
1. Remove the sealing rings from the chamber head.
102
novAA 800 Service and maintenance
2. Use diluted mineral acid (HNO3, HCl, H2SO4) or, depending on the analyzed sub-
stances an appropriate organic solvent, for cleaning the component.
3. If the mixing chamber is cleaned with a diluted mineral acid, wash thoroughly with
distilled water after cleaning.
1. Use nitric acid, diluted mineral acid, or an appropriate organic solvent matching
the analyzed substances for cleaning the component. Clean the channels and the
float tank with a circular brush.
2. If the siphon is cleaned with a diluted mineral acid, wash thoroughly with distilled
water after cleaning.
WARNING
Risk of explosion due to leaking gas connections!
When connecting the supply tubes, ensure correct connection. Insert the sealing rings
and test their tightness. Only hand-tighten all screwed connections.
1. Check all sealing rings of the chamber head, connections and the nebulizer, replace
worn out sealing rings, pull on seals and ensure correct positioning.
2. Hold the impeller at its handle (item 3 in Fig. 61 on page 99) and insert it into the
mixing chamber tube. Lock by pressing slightly.
3. Mate the mixing chamber parts (chamber tube and chamber head), align the sides
so that they are flush and screw them together (item 2 in Fig. 61). Ensure that the
sealing rings are seated correctly.
4. Screw the siphon sensor (item 11 in Fig. 61) into the siphon. Attach the siphon to
the chamber head ensuring that the float tank is inclined towards the front (refer
to Fig. 60 on page 99 for the correct positioning). Attach the siphon using the
clamp screw (item 9 in Fig. 61).
5. Attach the safety plug (item 1 in Fig. 61) on the chamber tube.
6. Screw the connections for fuel gas and auxiliary oxidant (item 5 in Fig. 61) with
the sealing rings into the mixing chamber head. Only tighten the knurled-head
screws finger tight.
7. Attach the nebulizer (item 8 in Fig. 61) to the chamber head and fasten it using
the locking ring (item 6 in Fig. 61).
Note: If the nebulizer cannot be stuck easily into the chamber head, slightly grease
the sealing rings with the lubricant supplied (Apiezon grease).
8. Attach the mixing chamber nebulizer system to the height adjustment using the
retaining clip (item 12 in Fig. 60). The white marking must be above the edge of
the holding fixture. The plate of the mixing chamber tube must rest evenly on the
height adjustment. Screw the knurled head screw at the holding bow tightly.
103
Service and maintenance novAA 800
9. Plug the cable of the siphon sensor (item 8 in Fig. 60) into the connection on the
sample chamber wall (mind the lug) and screw tight.
10. Attach the outlet tube to the outlet connector of the siphon (item 7 in Fig. 60).
Route the outlet tube to the waste bottle in a constant downward slope.
11. Fill the siphon with water via the mixing chamber tube until the water starts run-
ning off via the outlet tube.
12. Set the burner on the mixing chamber tube and turn against the 0° stop. Clamp
with retaining screw (item 2 in Fig. 60).
13. Connect the gas supply:
Screw the fuel gas hose (red) onto the connector at the top of the mixing
chamber head (item 11 in Fig. 60).
Screw the oxidant hose (blue) onto the nebulizer connector (item 10 in Fig.
60).
Screw the auxiliary oxidant hose (black) onto the connector on the side of the
mixing chamber (item 10 in Fig. 60).
Only tighten the knurled-head screws finger tight.
14. Hang the safety glass in and slide it in front of the burner.
Sensitivity control /
adjustment 1. In the ASpect LS software for flame technique, use the button to open the
FLAME / CONTROL window.
2. Set the ratio between gas C2H2 – oxidant (air or N2O) in the group field SETTINGS.
3. Align the burner to the height of and parallel to the optical axis.
4. Use the [IGNITE FLAME] button to ignite the flame.
5. Open the MANUAL OPTIMIZATION tab.
6. Select an element line, e.g. Cu324, and click [SET].
7. Aspirate a test solution, e.g., Cu / 2 mg/L, via the nebulizer and initiate the contin-
uous display of the measured values by clicking [START]. Evaluate the signal.
8. If the sensitivity is too low, adjust the nebulizer in such a way that the absorbance
attains its maximum at the selected item line:
Loosen the lock nut (item 2 in Fig. 66).
Use the adjustment nut to adjust the depth of the canula (item 3 in Fig. 66).
9. After completing the adjustment, secure the adjustment with lock nut (item 2 in
Fig. 66).
The burner-nebulizer system is cleaned and installed.
104
novAA 800 Service and maintenance
1 Baffle ball
2 Lock nut
3 Adjustment nut for cannula
4 Inner cannula
5 Connection for oxidant
The novAA 800 D has an adjustment screw to align the burner-nebulizer system in the
sample chamber depth. For adjusting the system, the stop of the tilting bracket is re-
set.
1. In the ASpect LS software for flame technique, use the button to open the
FLAME / CONTROL window.
2. Set the ratio between gas C2H2 – oxidant (air or N2O) in the group field SETTINGS.
3. Use the [IGNITE FLAME] button to ignite the flame.
4. Open the MANUAL OPTIMIZATION tab.
5. Select an element line, e.g. Cu324, and click [SET].
6. Aspirate a test solution, e.g., Cu / 2 mg/L, via the nebulizer and initiate the contin-
uous display of the measured values by clicking [START]. Evaluate the signal.
7. Change the setting of the adjustment screw with an Allen key (M 3.0) until the
absorbance has reached its maximum for the selected element line.
105
Service and maintenance novAA 800
For the models novAA 800 G + F it is possible to use the factory-set configuration for
all measurement tasks.
In addition to that, the control and analysis software ASpect LS automatically sets the
height of the atomizer for all models of the novAA 800 product family after selecting
the atomization technique in the MAIN SETTINGS window.
A sensor system monitors whether the burner is placed on the mixing chamber neck
before igniting the flame. The openings of the sensor system must be cleaned, if
there are deposits in the opening (e.g. salt incrustation)
the program produces an error message even though the burner is mounted on the
tube of the mixing chamber.
1. Hold the burner-nebulizer system tightly, loosen the knurled head screw on the
retaining clip of the mixing chamber tube (item 12 in Fig. 60), rotate the retaining
clip backwards and remove the system.
2. Use a small brush (toothbrush) with alcohol, e.g. isopropyl alcohol, to gently clean
the sensor openings.
3. Allow the sensor openings to dry.
4. Remount the burner-nebulizer system into the height adjustment.
106
novAA 800 Service and maintenance
The dosing tube must be purged prior to and after work. To do this, purge solution is
taken from the storage bottle, pumped via the dosing syringe into the dosing tube and
dispensed into the purge cup.
1. Switch on the novAA 800 and start the ASpect LS software / graphite furnace
technique.
If one method is active, the number of wash cycles specified for this method will be
executed after pressing the [WASH] button in the AUTOSAMPLER window.
107
Service and maintenance novAA 800
Cleaning the The dosing tube requires cleaning, dependent on the sample material, when:
dosing tube
The pH levels of the sample, the wash liquid and the air bubble are blurred, or if
the bubble is segmented.
The sample is carried over because the tube's interior is contaminated.
108
novAA 800 Service and maintenance
3. In ASpect LS use to open the AUTOSAMPLER window. Open the FUNCTION TESTS
tab (Fig. 69 on page 107).
4. Enter "101" in the TRACKER/ROTATOR field and enable the option CUP NO.
The autosampler arm moves to position "101".
5. Use the arrow keys to lower the autosampler arm into the special cup (ap-
prox. 50 mm) in the DEPTH list field of the DIPPING ARM area.
Note: The autosampler is only lowered if the arrow keys are used. After entering
the value directly into the list field, click the arrow keys once again!
6. Use the arrow keys to set the volume to be taken (100 to 200 µL) in the
VOLUME [µL] list field of the PIPETTER area. The volume can be set in steps of 50 µL.
7. Press the button [TAKE UP]. The autosampler fills the dosing tube with the cleaning
liquid.
8. Allow the cleaning liquid to react for approx. 20 min.
9. In the area TRACKER/ROTATOR enable the option WASH POSITION.
10. The autosampler arm moves to the wash position.
11. Use the arrow keys to lower the autosampler arm into the purge cup (ap-
prox. 40 mm) in the DEPTH list field of the DIPPING ARM area. When entering the
value directly into the list field, click the arrow keys once again!
12. Click the [DISPENSE] button to empty the dosing tube into the purge cup.
13. Start 5 wash cycles. (Click the [WASH] button 5 times).
The dosing tube is cleaned.
Shortening the 1. Loosen the clamp nut at the tube guide (item 6 in Fig. 71) and remove the dosing
dosing tube tube by pulling upwards.
2. Cut approx. 70 mm of the dosing tube with a razor blade or a scalpel at an angle of
10° to 15°.
3. Push the dosing tube as far as possible into the tube guide until the dosing tube
protrudes by approx. 8 mm beyond the bottom.
4. Lock the dosing tube with the clamp nut.
5. Readjust the injection depth of the sample (→ section "Adjusting the sampler" on
page 71).
The autosampler is ready for operation again after contaminated or damaged
parts of the tube were removed.
Replace the dosing tube 1. Loosen the clamp nut at the tube guide (item 6 in Fig. 71) and pull out the tube.
Remove the tube from the tube holders at the autosampler arm and the back of
the autosampler (items 1 and 3 in Fig. 71).
109
Service and maintenance novAA 800
2. Detach the screw top from the T valve of the dosing unit (item 4 in Fig. 71 ).
3. Screw the new dosing tube to the valve and feed it through the tube holders.
4. Push the dosing tube as far as possible into the tube guide until the dosing tube
protrudes by 8 mm underneath. Lock with the clamp nut.
5. Readjust the injection depth of the sample (→ section "Adjusting the sampler" on
page 71).
The autosampler is ready for operation with a new dosing tube.
The details below apply to the samplers AS-GF (graphite furnace technique) and AS-
FD (flame technique). The dosing units only differ in the size of the dosing syringe
(500 or 5000 µL).
1 T valve
2 Dosing syringe, consisting of piston and glass cylinder
3 Attachment screw
4 Drive rod
1. Switch on the novAA 800 and start the ASpect LS software. Select the technique in
the MAIN SETTINGS window: GRAPHITE FURNACE (AS-GF) or FLAME (AS-FD).
2. Use to open the AUTOSAMPLER window. Open the FUNCTION TESTS tab.
3. Use the arrow keys to set a volume to be taken in the VOLUME [µL] list field in the
PIPETTER area (AS-GF: 500 µL; AS-FD: 5000 µL). Increase the speed to 6-7.
4. Press the button [TAKE UP].
The piston of the dosing syringe moves down.
5. Unscrew the fixing screw (item 3 in Fig. 72).
6. Unscrew and remove the dosing syringe (item 2 in Fig. 72).
7. Screw the new dosing syringe to the valve.
8. Carefully pull the piston down until the eyelet at the piston end is aligned with the
hole in the drive rod.
Screw the piston with the attachment screw finger-tight to the drive rod.
Caution
Excessive force can lead to material damage! Do not tighten the screw too much.
110
novAA 800 Service and maintenance
If during the process a purge cup has overflowed, immediately interrupt the process
and clean the device.
1. Instantly abort the analysis process.
2. Take up the liquid with cellulose wadding or cloth. Wipe the device surface dry.
3. Ensure that the outlet can be drained, i.e., remove any kinks in the outlet tube and
make sure that the outlet tube does not dip into the liquid in the waste bottle.
The analysis process can be continued.
Contamination on the tray and the casing can be removed with a dry cloth on a daily
basis as required. In addition according to conditions:
Washing the sample path
Washing the mixing cup
Replace the cannula(s) at the autosampler arm
Replace the aspiration tube and dosing tube
Replace the dosing syringe (→ section "Replacing the dosing syringe" on page 110)
Clean, after a wash or mixing cup has overflowed.
1. Use the button to open the FLAME window in the software Aspect LS and
ignite the flame.
111
Service and maintenance novAA 800
The mixing cup must be washed before and after the operation to prevent adhesion
and scaling.
Before preparing the first standard / first sample the mixing cup is washed automati-
cally. Further washing processes might be useful during continuous operation.
Washing the system If salts were added to the diluent (bidistilled or acidic bidistilled water), the dosing unit
before shutting down the and valve must be washed with methanol or ethanol before the device is put out of
device for an extended service for an extended period of time. Otherwise scaling and blocking may also occur.
period
1. Fill the storage bottle for the diluent with methanol or ethanol.
2. Perform the wash cycle as described in Section "Washing the system prior to and
after the measurement". Repeat the washing process several times.
5.6.3 Replacing the cannulas and guide on the autosampler arm of the AS-FD
The cannulas and guide must be replaced in case of significant contamination or me-
chanical damage (detectable by large standard deviations in the measurements).
112
novAA 800 Service and maintenance
The cannula for picking up the sample (thin cannula) must be replaced in case of sig-
nificant contamination or mechanical damage (detectable by large standard deviations
in the measurements).
1. Pull the dosing tube for the diluent off the thicker cannula on the autosampler arm
and feed it through the tube guide (item 6 in Fig. 52 on page 79).
2. Detach the tube for the washing liquid at the rear of the autosampler (item 5 in
Fig. 52 on page 79).
3. Pull the encased tubes out of the attachment lug at the rear of the autosampler.
4. Pull the tube for the washing liquid off the storage bottle.
5. Unscrew the dosing tube from the change-over valve (item 3 in Fig. 53 on pa-
ge 80).
6. Screw the new tube set with dosing tube (marking "1") to the change-over valve
and attach the encased tubes with the attachment lug to the rear of the au-
tosampler.
7. Insert the tube with the marking "2" into the storage bottle for the washing liquid.
8. Screw the tube for the washing liquid to the rear of the autosampler.
9. Slide the other end of the dosing tube through the tube guide onto the thicker
cannula of the autosampler arm.
113
Service and maintenance novAA 800
If the purge cup or mixing cup (when using the AS-FD) overflows during the analysis
process, immediately interrupt the analysis and clean the device.
3. Use to open the AUTOSAMPLER window. Open the FUNCTION TESTS tab.
Check the MIX CUP PUMP checkbox in the PUMPS section to start the pump.
Run the pump until the liquid is pumped out. If necessary, activate and deactivate
the pump several times.
Filling and venting 1. Open the top of the KM 5 and remove the lid of the fill opening.
2. Fill up with 5 liters of softened water using a funnel (up to approx. 5 cm below the
lid).
3. Place the back flow tube in the coolant container of the KM 5.
4. Switch on the KM 5. Allow the water cooler pump to run until the returning water
is free of air. Switch the KM 5 on and off several times, as required.
5. Switch off the KM 5. Reconnect the back flow tube to the KM 5. Close the filling
opening and the lid of the KM 5.
114
novAA 800 Service and maintenance
The furnace is under pressure. To avoid splashing of liquid, attach a hose to the
cock and slowly open the cock to carefully drain the liquid into a waste bottle.
Drain oily condensation water from the pressure reducer every week by pressing
the pin at the bottom of the liquid separator.
Suction filter:
Check the filter every month. Clean or replace the filter every six month.
Oil:
Only use the special oil SE-32! Dispose of the used oil according to the applicable
regulations.
Check the oil level on the inspection glass every week. Refill oil, if necessary.
Change the oil every 12 months.
Unscrew the 4 screws and remove the ribbed cover to do this.
Tilt the tank far enough to allow the oil to drain from the tank. Hold the motor
block with one hand while draining the oil to prevent it from falling out.
Remove any contaminations from the housing.
Check the O ring on the ribbed cover and replace it, if required. Clean the seal-
ing surfaces.
Top up about 0.6 L of oil (SE-32).
Remount the ribbed cover. Check the tightness of the ribbed cover when the
device is in operation.
115
Troubleshooting novAA 800
6 Troubleshooting
The following chapter describes a number of possible problems that the user can par-
tially remedy independently. If such problems occur frequently, the operator must
inform the Analytik Jena service department.
A system monitoring process is initiated as soon as the novAA 800 is switched on. Any
errors that occur are displayed in a window after start-up.
The user must acknowledge the error messages by clicking the [OK] button.
NOTICE
Risk of device damage!
If the errors below cannot be remedied using the corresponding troubleshooting notes,
the operator must inform the service department at Analytik Jena. This also applies for
the repeated occurrence of individual faults.
Error on the gas supply Check the gas supply (air, fuel gas)
Gas supply closed before reaching the Check the gas supply, open the gas sup-
device connection ply before the gas connection
Cause Remedy
Transformer temperature too high Allow the device to cool down for at least
1 h. If necessary, reduce the thermal load
in the temperature-time program
4233 Cooling system sensor error (status)
Cause Remedy
Insufficient filling level of the coolant Check the water level in the cooling unit
reservoir. and top up the cooling water, if required.
116
novAA 800 Troubleshooting
Cause Remedy
Cause Remedy
Cause Remedy
Fluctuations of the HCL energy are too Start up the HCL and wait for 5 to
big 15 minutes before manually repeating an
energy alignment and a peak search
Check the calibration state of the HCL
and the atomizer
Increase the slit width and the lamp
current
Choose a more energy intensive HCL line
Check the aging (blackening) of the HCL
and replace the HCL, if required
5006 Background radiator signal too low
Cause Remedy
Energy of the D2 HCL too low Increase the slit width or select a HCL
analysis line with a shorter wavelength
Check the alignment and aging
(blackening) of the D2-HCL
Check the calibration distance of the
atomizer
If necessary, do without the background
compensation
117
Troubleshooting novAA 800
5008 Energy drift or energy fluctuations in the background radiator too big
Cause Remedy
Fluctuations of the D2-HCL energy are Increase the slit width or select an analy-
too big sis line with a shorter wavelength
Check the alignment and aging
(blackening) of the D2-HCL
Check the calibration distance of the
atomizer
5009 Too much energy during the zero balance (AZ phase)
Cause Remedy
Drift of the HCL energy level too big Start up the HCL and wait for 5 to
Inappropriate moment in the measure- 15 minutes before manually repeating an
ment process for the AZ phase energy alignment and a peak search
5010 Too little energy during the zero balance (AZ phase)
Cause Remedy
Drift of the HCL energy level too big Start up the HCL and wait for 5 to
AZ phase disturbed (fogged window, un- 15 minutes before manually repeating an
spec. ABS signal) energy alignment and a peak search
Atomizer is not ideally aligned with the Cleaning the windows
beam path Check the calibration distance of the
atomizer
5012 Baseline drift during the AZ phase (total absorption)
Cause Remedy
Drift of the HCL energy level too big Start up the HCL and wait for 5 to
15 minutes before manually repeating an
energy alignment and a peak search
Cause Remedy
The flow of the cooling water is too low Check the cooling water level in the
Partial obstruction of the cooling water cooling unit
channels Top up the cooling water
Contact the customer service in case of
obstructions
118
novAA 800 Troubleshooting
Other problems not detected by the system monitoring can also occur. Starting a
measurement is possible. Such errors are usually detected on the basis of implausible
measuring results (analytical problems). Often, such errors are also clearly recogniza-
ble in the equipment technology. If the suggested solutions are not successful, inform
the service department.
119
Troubleshooting novAA 800
120
novAA 800 Troubleshooting
Contamination / carry-over in the Check the flow through the nebulizer and clean
nebulizer (flame technique) it
If necessary, filter the sample solutions
The nebulizer gas flow is not opti- Optimize the nebulizer gas flow
mal
(flame technique)
Drift
Cause Remedy
Atmospheric oxygen in the graph- Perform a formation of the graphite tube be-
ite tube at the beginning of the fore starting the measurement
measurement
121
Transport and storage novAA 800
CAUTION
Risk of injury!
The various different models of the novAA 800 product family weigh between 95 kg
and 130 kg. The device must be transported by at least 4 persons using the fixed
screw-in carrying handles.
CAUTION
Risk of burns from touching hot surfaces! Observe the required cooling times of the
novAA 800 before preparing the device for transport.
NOTICE
Using improper packaging material and omitting the transport locks may cause dam-
age to the device!
Always use the original packaging when transporting the novAA 800. When transport-
ing the novAA 800 D and G, insert the transport lock into the sample chamber to se-
cure the graphite furnace in parking position. In addition to that, use a transport lock
to secure the monochromator.
1. Close the control and analysis software ASpect LS. Observe the sequence for
switching off the PC and the novAA 800 and turn them off (→ section "Switching
off sequence" on page 84).
2. Detach all components and accessories (→ section "Installation and initial start-up"
on page 38). Remove the autosampler from the sample chamber.
3. Flame technique: Remove the outlet tube of the siphon and the safety glass pane.
4. Empty the waste bottle and dispose of the waste.
5. Close the gas supply upstream of the device connections.
6. Detach the gas connectors on the rear of the novAA 800:
Manually detach the gas connectors for the inert gas (argon) and the auxiliary
gas, if applicable.
Manually detach the tubes for compressed air and nitrous oxide.
For the acetylene gas connector, use a 17-mm open-end wrench.
Left hand thread!
7. Undo the electrical connections.
8. Graphite furnace technique: Detach the quick-release connectors of the coolant
hoses on the novAA 800. Drain the mobile cooling unit (→ section "Cooling unit
KM 5" on page 114).
122
novAA 800 Transport and storage
9. Insert the transport lock for the monochromator (→ section "Removing the
transport locks" on page 51):
Remove the device cover.
Screw the transport lock that is marked red into the mesh lever.
Reattach the device cover.
10. novAA 800 D + G: Use the pivoting mechanism to tilt the graphite furnace back-
wards. Insert the transport lock into the opening in the back of the sample cham-
ber so that the wedge locks the graphite furnace in parking position.
11. Remove the four plugs (provided with the device) from the holes for the handles
on both sides of the device and keep retain them for future use.
12. Screw the four handles securely into the holes as far as the end stops.
The novAA 800 is prepared for transport
Observe the safety instructions in the section "Safety instructions, transport and instal-
lation" on page 11. Transport the novAA 800 and its components with care to prevent
damage from impact or vibration. The device should be transported in such a way that
major temperature fluctuations are avoided and the formation of condensate is thus
prevented.
123
Disposal novAA 800
The following ambient conditions must be met when transporting and storing the
device:
Temperature range
Transport -40 °C to +70 °C
Storage +5 °C to +40 °C
Max. humidity: 90% at 40 °C
If the novAA 800 and add-on devices are not installed immediately after delivery or
are not required for a prolonged period of time, store them in their original packaging.
A suitable desiccant should be added to the packaging to prevent damage from mois-
ture.
8 Disposal
Atom absorption spectrometry usually creates only liquid waste. The liquid waste con-
tains metal ions or heavy metal ions, but mostly different mineral acids which were
used during sample preparation.
For safe disposal of this waste, all solutions must be neutralized with an alkaline solu-
tion such as a diluted sodium hydroxide solution. The neutralized waste must be dis-
posed of correctly in accordance with statutory regulations.
At the end of its service life, the novAA 800 and all its electronic components must be
disposed of as electronic waste in accordance with the applicable regulations.
Dispose of the hollow cathode lamps in accordance with the local requirements or
contact the Analytik Jena service department.
124
novAA 800 Specification
9 Specification
Photometer Dual-beam arrangement with beam splitter and rotating sector mirror for coupling
in the reference beam path
High light yield and base line stability
Quartz-improved mirror optics
Silicon-hydride receiver S 12749
Optics purging: Optional purging of the optics with purified compressed air for op-
eration in environments with large quantities of dust (in combination with an Air
Purge Kit – APK).
Monochromator Installation Modified Czerny-Turner layout with an flat hologrid, auto-
matic setting of the wavelength and the slit
Wavelength range 185 to 900 nm
Slit width 0.2 nm, 0.3 nm, 0.5 nm, 0.8 nm, 1.2 nm
Lamp turret for HCL PC-controlled 8-lamp turret for fully automated operation with a write/read unit for the use
of coded lamps.
125
Specification novAA 800
Deuterium hollow- Lamp type: Glow discharge lamp with continuum radiation in the UV range
cathode lamp D2-HCL
Lamp current 30 mA
Mode electrical timing 50 Hz
126
novAA 800 Specification
127
Specification novAA 800
Instrument fuses The fuses of the power supply may only be changed by service engineers from Analytik Jena
or by technical personnel authorized by Analytik Jena.
Fittings for gL-fuses (10×38 mm²) according to 60947-3.
Fuse number Type Protected circuit
F1 25 A/T Power supply
F2 25 A/T Power supply
128
novAA 800 Specification
Instrument fuses Fittings for G-fuses (5×20 mm²) according to IEC 60127.
Fuse number Type Protected circuit
F1 T 6.3 A/H Socket for external accessories
F2 T 6.3 A/H Socket for external accessories
F3 T 2.5 A/H Transformer on the primary side, SNT
F4 T 2.5 A/H Transformer on the primary side, SNT
F5 T 0.08 A D2-HCL
F6 T 0.25 A HCLs
F8 T 3.15 A Filament
Dimensions and weights The models of the novAA 800 product family have identical dimensions but different
weights.
Mass novAA 800 D 130 kg
novAA 800 G 125 kg
novAA 800 F 95 kg
Dimensions 820 mm x 600 mm x 770 mm
(W x H x D):
Transport of device Mandatory use of the accompanying, securely screwed on car-
rying handles.
129
Specification novAA 800
Adjusting the furnace Software-controlled height adjustment of the graphite furnace in the beam path
Height 4 to 18 mm, automated
Depth Factory preset
130
novAA 800 Specification
Oxidant Compressed air and N2O (ni- Inlet pressure: 400 to 600 kPa
trous oxide)
Nebulizer flow
Air 400 to 600 NL/h
N2 O 320 to 480 NL/h
Auxiliary oxidant (air or N2O)
Air 3 levels: 75 / 150 / 225 NL/h
N2O 3 stages: 60 / 120 / 180 NL/h
Siphon Integrated monitoring of the correct filling level (80 mm water column)
Mode of action Float, corrosion proof
131
Specification novAA 800
132
novAA 800 Specification
Piston compressor Model: PLANET L-S50-15 Standard, Compressed air supply for the flame technique
Tank capacity 15 L
Dimensions (diameter x height) 400 mm x 480 mm
Power supply 230 V, 50 Hz or
230 V, 60 Hz
Mass 27 kg
Max. operating pressure 800 kPa
Scraper Automatic burner head cleaning device for nitrous-oxide flame, PC-controlled
Power supply Via AAS basic instrument
Air Purge Kit (APK) Purging of the spectrometer with purified air
Dimensions (H x W x D) 245 mm x 265 mm x 260 mm
Power supply 100 – 240 V
50/60 Hz
Power consumption Max. 15 VA
Fuse 2 x T1.6 AH
Mass 3.2 kg
For further information refer to the operating instructions for the Air Purge Kit (APK).
Hydride system Chemical generation of hydride in flow injection and batch mode; devices with modular de-
sign for easy adaptation to changing requirements
Models HS 60 modular, HS 55 modular, HS 50
Techniques Hydride technique, mercury-cold-vapor technique and
HydrEA
For further information refer to the operating instructions of the hydride system.
133
Specification novAA 800
Protection class and The novAA 800 has the protection class I.
protection rating The casing has the protection rating IP 20.
Device safety The novAA 800 complies with the safety standards
DIN EN 61010-1 (VDE 0411T.1; IEC 61010-1)
DIN EN 61010-2-061 (IEC 61010-2-061)
EMC compatibility The novAA 800 is tested for suppression of radio interference, noise immunity and
interference emission in accordance with class A of the standard DIN EN 55011 and
fulfils the respective requirements
DIN EN 61326
Environmental The novAA 800 has been tested for environmental compatibility and fulfills the re-
compatibility quirements stipulated by
DIN ISO 9022-3:2000
DIN ISO 9022-32-03-0
DIN ISO 9022-2:2003/01
Directives for China The device contains restricted substances (according to directive "Management Meth-
ods for the Restriction of the Use of Hazardous Substances in Electrical and Electronic
Products"). Analytik Jena guarantees, that those hazardous substances may not leak
out during the next 25 years when the device is used in accordance with its intended
purpose.
EU directives The novAA 800 is built and tested according to standards that fulfill the requirements
stipulated by the EU directives 2014/35/EU, 2014/30/EU and 2011/65/EU.
Each device leaves the manufacturer in a pristine and technically safe state. To main-
tain this condition and to ensure safe operation, the operator must strictly observe the
safety and operating instructions contained in this manual. For accessories which have
also been supplied, and system components from other manufacturers, their operating
instructions should be referred to.
134
novAA 800 CE Declaration of Conformity
10 CE Declaration of Conformity
135
Index novAA 800
11 Index
A C
Acetylene
Canula
safety instructions 14
replacement 112
Adjustment
Change
atomizer 105
atomizer 60
Air Purge Kit 37
Compressed air supply Refer to Piston
Air purge of the spectrometer 37
compressor
Analysis
Compressed gas cylinder 14
problems 119
Computer 129
AS-F, AS-FD
Confidence interval 127
installation 78
Cooling unit
maintenance 111
installation 53
replacing the dosing syringe 110
maintenance 114
technical data 132
technical data 133
uninstall 80
AS-F,AS-FD D
replacing the cannula 112 Decontamination measures 16
AS-GF Device layout 43
adjustment 71 Device safety 134
functioning 27 Disposal 124
installation 69 Dosing syringe
maintenance 106 replacement 110
replacing the dosing syringe 110 Double-beam operation 19
technical data 132
uninstall 73 E
ASpect LS Electrode See graphite electrode
installation 53 EMC compatibility 134
Atomization technique 18 Emergency
Atomizer behavior 16
adjustment 105 Environmental compatibility 134
Automatic gas control 29 Environmental conditions 129
Autosampler graphite See AS-GF Equipment fault 116
Error message
B ASpect LS 116
Burner Exhaust unit 43
cleaning 101
cleaning the burner detection 106 F
installation 77, 78 Flame technique
replacement 82 configuration in ASpect LS 75
Burner adjustment 131 functioning 29
Burner detection maintenance 98
cleaning 106 technical data 131
Burner head cleaner See Scraper Fluidics module
Burner-nebulizer system installation 80
assembling 103 Fuel gas 131
cleaning 98 Function
disassembly 100 autosampler AS-GF 27
functioning 30 burner-nebulizer system 30
installation 75, 78 flame technique 29
furnace camera 27
graphite furnace technique 22
136
novAA 800 Index
137
Index novAA 800
P cleaning 103
Personnel 11 installation 76, 78
Piston compressor Siphon monitoring 131
functioning 35 Software See ASpect LS
maintenance 115 Space requirement 43
technical data 133 Storage 122
Planet L-S50-15 Refer to Piston compressor Switching off sequence 84
Power supply 40 Switching on sequence 83
technical data 127, 128 Symbols
Problem device 9
analytical 119 manual 7
Protection type 134
T
R Technical data 125
Radiation sensor 27 autosampler AS-F, AS-FD 132
Reference beam 19 autosampler AS-GF 132
Repair 17 computer 129
cooling unit 133
S graphite furnace technique 130
Safety circuits 131 injection module SFS 6 132
Safety class 134 optics 125
Safety instructions piston compressor 133
electrical equipment 12 power supply 127, 128
exhaust unit 14 Technical date
explosion protection 12 flame technique 131
gas supply 14 Temperature
graphite furnace technique/flame operation 39
technique 13 Temperature sensor 23
hazardous substances 15 Transport 122
operation 12 Transport lock
service and repair 17 installation 123
transport 11 removal 51
Safety shutdown 23 Troubleshooting 116
Sampling compartment Type plate 51
clean 89 Types of flame 131
Scraper
functioning 36 U
installation 82 Use 8
Serial number 51 User manual conventions 7
SFS 6
W
functioning 35
Warranty 8
installation 81
Water connection
technical data 132
installation 53
uninstall 82
Single-beam operation 19
Siphon
138