Endress+Hauser analytikjena HS 55 User manual

Operating Manual
HS 55 (Batch Mode)
Hg/Hydride System
HydrEA System

Manufacturer Analytik Jena GmbH
Konrad-Zuse-Strasse 1
07745 Jena / Germany
Phone: [phone]
Fax: [phone]
Email: [email protected]
Technical Service AnalytikJenaGmbH
Konrad-Zuse-Strasse 1
07745 Jena / Germany
Phone: [phone]
Fax: [phone]
Email: [email protected]
General Information http://www.analytik-jena.com
Documentation Number 10-1700-002-23
Edition C (11/2021)
Technical Documentation Analytik Jena GmbH
© Copyright 2021, Analytik Jena GmbH
For a proper and safe use of this product follow the instructions. Keep the
operating manual for future reference.

HS 55 (Batch Mode) Table of contents
3
Table of contents
1 Basic information............................................................................................................................................................ 5
1.1 About this operating manual........................................................................................................................... 5
1.2 Intended use ..................................................................................................................................................... 6
2 Security............................................................................................................................................................................ 7
2.1 Safety labeling on the device ........................................................................................................................... 7
2.2 Requirements for the operating personnel..................................................................................................... 8
2.3 Safety instructions– transport and installation.............................................................................................. 8
2.4 Safety instructions – operation........................................................................................................................ 8
2.4.1 Safety instructions – protection against explosion and fire........................................................................... 9
2.4.2 Safety instructions– electrical equipment ...................................................................................................... 9
2.4.3 Safety instructions for the operation of compressed gas containers and compressed gas systems............ 10
2.4.4 Handling of auxiliary and operating materials ............................................................................................... 10
2.5 Safety instructions – maintenance and repair ................................................................................................ 11
2.6 Behavior during emergencies .......................................................................................................................... 11
3 Function and design ....................................................................................................................................................... 12
3.1 Function and measuring principle ................................................................................................................... 12
3.2 Design................................................................................................................................................................ 13
3.2.1 Hose pump........................................................................................................................................................ 15
3.2.2 Batch module.................................................................................................................................................... 15
3.2.3 4-valve group for gas control........................................................................................................................... 16
3.2.4 Hg Plus Upgrade Modul (optional).................................................................................................................. 17
3.2.5 Type plate.......................................................................................................................................................... 18
3.3 Measuring process............................................................................................................................................ 18
4 Installation and commissioning..................................................................................................................................... 20
4.1 Installing the hydride and Hg cold vapor systems .......................................................................................... 20
4.1.1 Installing the cell unit....................................................................................................................................... 20
4.1.2 Installing the Hg/hydride system on the AAS................................................................................................. 23
4.1.3 Changing between operating modes............................................................................................................... 27
4.2 Retrofitting the Hg Plus Upgrade Modul......................................................................................................... 28
4.3 Installing the HydrEA system........................................................................................................................... 30
4.3.1 Preparing the analysis system for the HydrEA system ................................................................................... 30
4.3.2 Coating the graphite tube ................................................................................................................................ 31
4.3.3 Installing the Hg/hydride system on the AAS................................................................................................. 32
4.3.4 Adjusting the autosampler for the graphite tube furnace with the titanium cannula ................................. 34
5 Operation ........................................................................................................................................................................ 35
5.1 Preparing operating materials and standards ................................................................................................ 35
5.2 Switching the device on and off....................................................................................................................... 37
6 Maintenance and care.................................................................................................................................................... 38
6.1 Maintenance overview..................................................................................................................................... 38
6.2 Replacing the fuses........................................................................................................................................... 38
6.3 Cleaning the cell and the cell windows ........................................................................................................... 39
6.4 Inspecting and replacing the pump hose ........................................................................................................ 40

Table of contents HS 55 (Batch Mode)
4
6.5 Inspecting and replacing the flange seal in the batch module ...................................................................... 41
6.6 Replacing the hose dryer.................................................................................................................................. 41
6.7 Replacing the gold collector............................................................................................................................. 41
6.8 Maintaining the HydrEA system...................................................................................................................... 42
6.8.1 Cleaning the coated graphite tube .................................................................................................................. 42
6.8.2 Evaporating the iridium or gold coat............................................................................................................... 43
7 Troubleshooting.............................................................................................................................................................. 44
8 Transport and storage .................................................................................................................................................... 45
8.1 Transport........................................................................................................................................................... 45
8.1.1 Preparing the device for transport................................................................................................................... 45
8.1.2 Moving the device in the laboratory................................................................................................................ 46
8.1.3 Returning the device for servicing ................................................................................................................... 46
8.2 Storage .............................................................................................................................................................. 47
9 Disposal ........................................................................................................................................................................... 48
10 Specifications .................................................................................................................................................................. 49
10.1 Technical data................................................................................................................................................... 49
10.2 Standards and directives .................................................................................................................................. 50
11 Revision overview ........................................................................................................................................................... 51

HS 55 (Batch Mode) Basic information
5
1 Basic information
1.1 About this operating manual
Content This operating manual describes the HS55 Hg/hydride system.
The device is intended to be operated by qualified specialist personnel observing the op-
erating manual.
The operating manual provides information about the design and operation of the de-
vice and provides operating personnel the necessary know-how for the safe handling of
the device and its components. Furthermore, the operating manual includes information
on the maintenance and servicing of the device as well as hints on potential causes of
malfunctions and their correction.
Conventions Instructions for actions occurring in chronological order are numbered and combined
into action units.
Warnings are indicated by a warning triangle and a signal word. The type, source and
consequences of the hazard are stated together with notes on preventing the hazard.
Elements of the control and analysis program are indicated as follows:
¡Program terms are in bold (e.g., the System menu).
¡Buttons are indicated by square brackets (e.g., [OK]).
¡Menu items are separated by vertical lines (e.g., System | Device).
Symbols and signal words used
in this manual
The user manual uses the following symbols and signal words to indicate hazards or in-
structions. These warnings are always placed before an action.
WARNING
Indicates a potentially hazardous situation which can cause death or very serious (possi-
bly permanent) injury.
CAUTION
Indicates a potentially hazardous situation which can cause slight or minor injuries.
NOTICE
Provides information on potential material or environmental damage.

Basic information HS 55 (Batch Mode)
6
1.2 Intended use
The Hg/hydride system must only be used in connection with an atomic absorption
spectrometer by Analytik Jena.
The device and its components may only be used for the analyses listed in the user man-
ual. Only this specified use is regarded as the intended use, ensuring the safety of the
user and the device.

HS 55 (Batch Mode) Security
7
2 Security
For your own safety and to ensure error-free and safe operation of the device, please
read this chapter carefully before commissioning.
Observe all safety instructions listed in this user manual and all messages and infor-
mation displayed on the monitor by the control and analysis software.
2.1 Safety labeling on the device
Warning and mandatory action labels have been attached to the device and must al-
ways be observed.
Damaged or missing warning and mandatory action labels can cause incorrect ac-
tions leading to personal injury or material damage. The labels must not be removed.
Damaged warning and mandatory action labels must be replaced immediately!
The following warning and mandatory action labels have been attached to the de-
vice:
Warning symbol Meaning Comment
Warning against a haz-
ard location
On the cell heating connection: dan-
gerous electrical voltage warning. Only
connect and disconnect the connec-
tion cable when the device is switched
off.
Warning about hot sur-
face
On the red device hood: there is a risk
of burns on the Hg Plus Upgrade
Modul (optional). Allow the module to
cool down before opening the hood.
"Caution Hot" warn-
ing sign
Warning about hot sur-
face
On the cell heating: risk of burns at
the cell heating. Keep a safety distance
during operation.
Mandatory action
labels/information
symbols
Meaning Comment
Disconnect the power
plug prior to assembly
or disassembly and
opening of the device.
On the power switch/power input:
Switch off the device and disconnect
the power plug from the power con-
nection prior to assembly or disassem-
bly and opening of the device.
For People's Republic of
China only
The device contains controlled sub-
stances. Analytik Jena GmbH warrants
that these substances will not be re-
leased from the device within the next
25years provided the device is em-
ployed as intended.

Security HS 55 (Batch Mode)
8
2.2 Requirements for the operating personnel
The device must only be operated by qualified specialist personnel instructed in the
use of the device. This instruction also include teaching the contents of this user
manual and of the user manuals of the connected system components. We recom-
mend training by qualified employees of Analytik Jena or its representatives.
In addition to the safety instructions in this user manual, the general applicable
safety and accident prevention regulations of the respective country the device is op-
erated in must be observed and adhered to. The operator must ensure the latest ver-
sion of these regulations.
The user manual must be accessible to the operating and service personnel.
2.3 Safety instructions– transport and installation
Incorrect installation can create serious hazards. This may cause an electric shock.
¡Only the Analytik Jena GmbH customer service or specialist personnel trained
and authorized by them is allowed to install and commission the device and its
system components.
¡Unauthorized assembly and installation is not permitted.
To prevent health damage, the following must be observed when moving the device
in the laboratory (lifting and carrying):
¡The device has no carrying handles. To transport the device, grip the device
firmly at the bottom with both hands and lift it.
¡Ensure that the device is completely empty. Flush the pump and metering hoses
thoroughly to prevent reduction agent solution from dripping out. The solution is
corrosive and harmful to health and damages clothing.
¡Remove the storage bottle for reduction agent. Empty the bottle before trans-
port.
¡Insufficiently secured components pose a risk of injury. During transport, secure
the device components as specified in this operating manual.
¡Risk of damage to health due to improper decontamination! Perform a profes-
sional and documented decontamination of the device before returning it to An-
alytik Jena. The decontamination report is available from Service when register-
ing the return. Service must refuse acceptance of contaminated devices. The
sender may be liable for damage caused by inadequate decontamination of the
device.
2.4 Safety instructions – operation
The operator must make sure that the device and its safety equipment is in sound
condition each time before starting up the device. This applies in particular after
each modification or extension of the device or its repair.
Observe the following:
¡The device may only be operated if all items of protective equipment (e.g. covers
in front of electronic components) are in place, properly installed and fully oper-
ational.
¡The sound condition of the protection and safety equipment must be checked
regularly. Any defects must be corrected as soon as they occur.

HS 55 (Batch Mode) Security
9
¡Protective and safety equipment must never be removed, modified or switched
off during operation.
¡Free access to the power switch on the right side panel must be ensured during
operation.
¡Modifications, conversions and extensions to the device are only permitted after
consultation with Analytik Jena. Unauthorized modifications can jeopardize the
device’s operational safety and may lead to limitations regarding the warranty
and access to customer service.
¡The ventilation equipment on the device must be in good working condition.
Covered ventilation grilles or slots etc. may cause the device to break down or
may cause damage to it.
¡The cell unit becomes very hot during operation. Hot components must not be
touched during or directly after the operation of the device. The cooling times to
room temperature (at least 1hour) must be observed.
¡Keep flammable materials away from the cell unit.
¡The gold collector (Hg Plus Upgrade Modul, optional) also becomes very hot dur-
ing operation. Only open the red device hood when the module has cooled
down.
¡Caution when handling glass components. Risk of broken glass and therefore risk
of injury!
¡During operation, there is a risk of crushing at the hose pump. Long hair and
baggy clothing can become caught in the pump and drawn in. Wear suitable hair
protections and tight-fitting clothing.
2.4.1 Safety instructions – protection against explosion and fire
The device may not be operated in an explosive environment.
Smoking or handling open flames are prohibited in the room in which the device is
operated!
2.4.2 Safety instructions– electrical equipment
Lethal voltages may occur in the device! Contact with live components may cause
death, serious injury or painful electrical shock.
¡The power plug must be connected to a proper power outlet 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 rating
plate of the equipment. Do not replace the removable power cable of the device
with a power cable that does not meet the specifications (with no protective
ground conductor). Extensions of the supply cable are not permitted!
¡The basic module and the system components may only be connected to the
mains when they are switched off.
¡Electrical connection cables between the basic module and the system compo-
nents may only be connected or disconnected when the device is switched off.
¡Before opening the device, the device must be switched off via the main switch
and the power plug must be disconnected from the power outlet!
¡Work on the electronics may only be carried out by the customer service of Ana-
lytik Jena and specially authorized technicians.

Security HS 55 (Batch Mode)
10
2.4.3 Safety instructions for the operation of compressed gas containers and compressed gas
systems
¡The operating gases are taken from compressed gas containers or local com-
pressed gas systems. The operating gases must have the required purity.
¡Work on compressed gas containers and systems may only be carried out by indi-
viduals with specialist knowledge and experience in compressed gas systems.
¡Compressed air hoses and pressure reducers may only be used for the assigned
gases.
¡Pipes, hoses, screw connections and pressure reducers for oxygen must be kept
free from grease.
¡Check all pipes, hoses and screw connections regularly for leaks and externally
visible damage. Repair leaks and damage without delay.
¡Shut off the gas supply to the device prior to any maintenance and repair work
on the compressed gas containers.
¡After successful repair and maintenance of the components of the compressed
gas containers or system, the device must be checked for proper operation prior
to recommissioning.
¡Unauthorized assembly and installation are not permitted!
2.4.4 Handling of auxiliary and operating materials
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 hazardous substances, the locally applicable safety instructions and
instructions in the safety data sheets from the manufacturers of the auxiliary and op-
erating materials must be complied with.
¡Only operate the device when the exhaust unit is active. Ensure good room ven-
tilation in working rooms.
¡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.
¡When measuring cyanide-containing material, ensure that prussic acid cannot be
generated in the waste bottle.
Protective goggles and rubber gloves have to be worn when handing reagents.
¡Sodium borohydride (NaBH4) and sodium hydroxide (NaOH) are strongly corro-
sive, hygroscopic and, in solution, extremely aggressive.
Hydrogen is released by the reaction of sodium borohydride with the acidic sample
solution. The formation of a hot, explosive hydrogen-air mixture in the cells must be
excluded. The gas lines from the reaction beaker to the cell outlet must be kept oxy-
gen-free. To this end take the following measures:
¡Always ensure that the cell with the windows is closed and gastight. Replace the
cell even in the case of small cracks or damage to the front sides.
¡Guide the gas from the cell outlet to the exhaust unit.
Observe the following:
¡The operator is responsible for carrying out suitable decontamination should the
device become contaminated externally or internally with dangerous substances.
¡Splashes, drops or larger liquid spillages should be removed using an absorbent
material such as cotton wool, laboratory wipes or cellulose.
¡For biological contamination, wipe the affected area with a suitable disinfectant,
such as an Incidin Plus solution. Then wipe the cleaned areas so that they are
dry.

HS 55 (Batch Mode) Security
11
¡The only suitable cleaning method for the housing is wipe disinfection. If the dis-
infectant has a spray nozzle, apply disinfectant to a suitable cloth before using it
on the device.
Particular care must be taken if infectious materials are analyzed with the device,
as the device cannot be decontaminated as a single unit.
¡Before using a cleaning or decontamination procedure other than that pre-
scribed by the manufacturer, the user is required to check with the manufacturer
that the intended procedure will not damage the device. Safety labels attached
to the device must not have methanol applied.
2.5 Safety instructions – maintenance and repair
The device is generally maintained by the customer service department of Analytik
Jena or specialist personnel trained and authorized by them.
Unauthorized maintenance can damage the device. For this reason, only the activi-
ties described in the user manual in the "Maintenance and care" chapter may be per-
formed by the operator.
¡Only clean the exterior of the device with a slightly moistened, non-dripping
cloth. Use only water and, if required, customary surfactants.
¡All maintenance and repair work on the device must only be carried out when
the device is switched off (unless specified otherwise).
¡The gas supply must be shut off before performing any maintenance or repair
work (unless specified otherwise).
¡Allow the device to cool down before any maintenance work or replacement of
system components.
¡Use only original spare parts, wear parts and consumables. They have been
tested and ensure safe operation. Glass part are wear parts and are not subject
to the warranty.
¡All protective equipment must be reinstalled and checked for proper function
when the maintenance or repair work is complete.
2.6 Behavior during emergencies
¡If there is no immediate risk of injury, switch off the device and the connected
system components immediately in hazardous situations or in the event of an
accident and/or disconnect the power plugs from the power outlets.
¡Close the gas supply as soon as possible after switching off the devices.

Function and design HS 55 (Batch Mode)
12
3 Function and design
3.1 Function and measuring principle
Hydride method The hydride method enables the matrix-free detection of the elements As; Bi; Sb; Se; Sn;
Te. It is based on the formation of gaseous metal hydrides through reduction of the
acidic samples with sodium borohydride (NaBH4). The carrier gas and the released hy-
drogen transport the metal hydrides to the quartz cell. There they gradually decompose
through collisions with gas particles and the glass wall at temperatures of 850to950°C.
The free metal atoms absorb the primary radiation on the resonance line.
With the hydride method spectral interference is practically eliminated, because only the
element to be detected reaches the atomizer as gaseous metal hydride.
Cold vapor method The cold vapor method is used to detect mercury. Besides sodium borohydride (NaBH4),
tin(II) chloride (SnCl2) is also used as a reduction agent. During the reaction with the
acidic sample solution, atomic Hg vapor forms, which is transported to the Hg cell by the
carrier gas argon. The free Hg atoms absorb the primary radiation on the resonance line.
The heating of the cell from room temperature to 150°C can reduce background inter-
ference due to moisture.
HydrEA method The HydrEA method combines the hydride or Hg cold vapor method with the graphite
tube method. It is used for the highly sensitive selective detection of the hydride-form-
ing elements As; Bi; Sb; Se; Sn; Te or Hg with the graphite tube furnace.
The Hg/hydride system generates the gaseous metal hydrides or the atomic Hg vapor,
respectively. The autosampler for the graphite tube furnace (AS-GF) transfers the ana-
lytes with the carrier gas argon into the graphite tube furnace. There the metal hydrides
are enriched on the iridium-coated standard tube for wall atomization at a preheating
temperature of 300°C. They decompose in this process. At a temperature of 2100°C,
the deposited metal atoms atomize again. The generated atom vapor cloud absorbs the
primary radiation on the resonance line.
The atomic Hg vapor is enriched on the gold-coated standard tube at 65°C. At a temper-
ature of 950°C, the Hg atoms atomize again.
Overview of Hg/hydride sys-
tems
Hg/hydride system Function
HS 50 Simplest batch system with pneumatic operating principle
The quartz cell is heated by the acetylene-air flame.
HS 55 Batch system with electrically heated cell unit
The user fills the sample solution manually into the reaction
beaker of the Hg/hydride system. The reduction agent solution
is automatically metered by a 1-channel hose pump.
HS 60 Hg/hydride system for flow injection operation with electrically
heated cell unit
Sample and reduction agent solution, acid and waste are trans-
ported through the system by means of hose pumps.
The AS-F and AS-FD autosamplers can supply the sample solu-
tions to the Hg/hydride system in a fully automatic manner.
All Hg/hydride systems allow the detection of the hydride-forming elements and mer-
cury using the hydride and cold vapor methods.

HS 55 (Batch Mode) Function and design
13
You can extend the functionality of the HS 55 and HS 60 Hg/hydride systems with the
following accessories and modules:
Module Function
Hg cell ("tulip") Tulip-shaped cell for higher sensitivity for Hg detection
Hg Plus Upgrade Modul Enrichment of mercury on a gold collector for ultra-trace analy-
sis
HydrEA Upgrade Kit Coupling of the Hg/hydride systems to the graphite tube AAS
for ultra-trace analysis of the hydride-forming elements and
mercury
An AS-GF autosampler must be used to supply the samples to
the AAS.
You can retrofit these accessories and modules yourself.
3.2 Design
The Hg/hydride system consists of a basic module, the functional module and an op-
tional module for mercury enrichment. The three modules are plugged on top of each
other and electrically connected through mixed plug connectors.
The Hg/hydride system can be used with the following AAS devices:
¡ZEEnit700P, ZEEnit700Q, ZEEnit650P
¡contrAA800 series
¡novAA800 series, novAA350i
For information on using the Hg/hydride systems with older Analytik Jena AAS models,
please contact customer service.
Detailed information on the design of the AAS devices and on the analysis process can
be found in the AAS device manuals.
Figure1 Hg/hydride system with AAS device

Function and design HS 55 (Batch Mode)
14
All functionally relevant assemblies are located on the front plate of the batch functional
module:
¡1-channel hose pump for the reduction agent transport
¡Batch module as reaction unit
¡Push button to start the measuring process
The pump hose is also located here. It is easily accessible and can be replaced by the
user. The colored line on the front plate identifies the hose routing and thereby facili-
tates maintenance.
Figure2 Front view with main assemblies
1 Batch module with reaction beaker 2 1-channel hose pump
3 "Start" push button 4 Basic module
The 4-valve group for gas supply is located on the inside of the functional module. On
the right-hand side of the device is the storage bottle for the reduction agent in a
holder. The electrical connections are also located here.
The optional mercury enrichment module is inserted into the functional module from
above and electrically connected to it. The hoses are routed to the frame of the func-
tional module and from there to the front plate. When changing between the "Hydride
(batch)"/"Hg without enrichment (batch)" and "Hg with enrichment (batch)" modes, you
only change the hose routing on the front plate.
Supply the sample manually into the Hg/hydride system. To do so, pipette a volume of
1to20ml into the reaction beaker and clamp the reaction beaker to the head of the
batch module with a slight rotation so that it is gastight.
After the analysis has started, the 1-channel hose pump meters the reduction agent au-
tomatically into the reaction beaker. The fast and partly vigorous reaction releases
gaseous metal hydride or atomic Hg vapor. Hydrogen is formed as a by-product during
the reaction with NaBH4.
Argon is used as the carrier and purge gas. The argon flow transports the reaction prod-
ucts either directly to the AAS device or to a gold collector for Hg enrichment. The en-
riched mercury is released during the bake-out of the gold collector and transported to
the atomizer by a directly connected argon flow.

HS 55 (Batch Mode) Function and design
15
Remove the reaction beaker after the measuring process, rinse it and refill it with sam-
ple.
4-valve group
Purge gas
1-channel hose pump
Reduction agent
Cell
(in the AAS)
Gold collector
Solenoid
valve
Drying
hose
Gas outlet
Transport gas
Reaction beaker
Figure3 Functional diagram
The Hg/hydride system normally works with sodium borohydride (NaBH4) as the reduc-
tion agent. Alternatively, you can use tin(II) chloride (SnCl2) for Hg detection.
NOTICE
High workload when changing the reduction agent
Changing the reduction agent requires major maintenance work.
¡Renew all hoses that have come into contact with the reduction agent.
¡Flush the Hg/hydride system thoroughly before loading samples the next time.
3.2.1 Hose pump
The 1-channel hose pump is equipped with an adjustable snap-in cartridge and an
Ismaprene pump hose with an inner diameter of 2.06mm. The pump only runs during
the pump time and transports reduction agent in 4 selectable speed stages.
3.2.2 Batch module
The batch module consists of a reaction beaker with a conical bottom for sample vol-
umes of 1to20ml and the head.
The head contains:
¡purge gas supply (marked "purge gas" at the head), argon gas flow 15l/h
¡transport gas supply (marked "transp. gas"), argon gas flows 6l/h and 25l/h
¡gas outlet to the cell (marked "to cell")
¡flange seal for reaction beaker
¡Metering tip

Function and design HS 55 (Batch Mode)
16
Figure4 Batch module
1 "purge gas" gas supply 2 "transp. gas" gas supply
3 Metering hose for reduction agent 4 "to cell" gas outlet
5 Head 6 Reaction beaker
Reduction agent and purge gas are transported through the metering tip to the bottom
of the reaction beaker. The reaction with the sample initially takes place in the lower
part of the reaction beaker. The released reaction gas and the purge gas accelerate the
reaction. The purge gas drives the released metal hydride or Hg vapor out of the sample
solution. The transport gas ("transp. gas") enters the reaction beaker at the top. The
transport gas transports the metal hydride or the Hg vapor from the reaction beaker to
the atomizer in the AAS device or to the gold collector.
3.2.3 4-valve group for gas control
The 4-valve group provides fixed gas flows controlled by the software:
Valve MV2 Gas flow F2 with a flow of 15l/h
¡Constant purge gas flow through the pipette tip of the batch
module
Valves MV3/MV4 Gas flow F3 with a flow of 6l/h and gas flow F4 with a flow of
25l/h
¡Transport gas flow: the flows can be selected individually or
as a total gas flow (31l/h).
Valve MV5 The valve switches gas flows F3 and F4 either to the batch mod-
ule or to the gold collector to expel the released mercury.

HS 55 (Batch Mode) Function and design
17
3.2.4 Hg Plus Upgrade Modul (optional)
The optional module is located in a compartment at the top of the Hg/hydride system.
You can open the red cover of the Hg/hydride system and access the module.
The module consists of the following components:
¡quartz tube with the gold collector
¡infrared sensor
¡fan
¡3/2-way solenoid valve (at the inlet)
The solenoid valve switches the following gas flows to the gold collector:
¡reaction gas for loading the gold collector
¡direct gas flow for expelling the enriched mercury
The gold collector is the core of the module. It contains a loosely rolled-up gold/plat-
inum mesh which is approx. 20mm wide. The mesh is secured in the quartz tube.
The gold collector enriches the mercury from the reaction gas on its surface by means of
amalgamation. Mercury is only released again from the gold collector when heated to a
temperature of approx. 630°C during bake-out.
The quartz tube is surrounded by a heating coil. The heating coil supplies heat to the
gold collector from the outside during bake-out. An infrared sensor monitors the tem-
perature. After bake-out, the axial fan cools the quartz tube with air. This way, the Hg/
hydride system prepares the gold collector for the next measurement.
Figure5 Gold collector
1 Gas inlet 2 Heating wire
3 Gas outlet 4 Heating connection
5 Infrared sensor 6 Heating connection

Function and design HS 55 (Batch Mode)
18
3.2.5 Type plate
The type plate is located on the rear of the device. The type plate contains the following
information:
¡company name and complete address of the manufacturer
¡device designation: type designation and trade name
¡model and serial number
3.3 Measuring process
You can start the measurement either by pressing the "Start" button on the Hg/hydride
system or via the control and analysis software of the AAS.
Start the measurement immediately after you have filled a new sample into the reaction
beaker and attached the reaction beaker in a gastight manner. The Hg/hydride system
first purges the reaction beaker with argon to remove any air. After a certain waiting
time, the software registers the zero value (AZ = Auto Zero).
After the baseline adjustment, the hose pump starts pumping reduction agent into the
reaction beaker. After a short time, the purge flow starts: the carrier gas argon trans-
ports the metal hydrides formed or the elementary mercury to the AAS. Atomic vapor
forms in the quartz cell or the graphite tube furnace, respectively. The metal hydrides
decompose due to collisions.
In mercury detection, the pre-wash time and the AZ waiting time are omitted to prevent
the highly volatile mercury from being expelled from the sample too early. The zero
value is determined over a period of 2s instead of 4s.
Measuring process with enrich-
ment
Before a sample is supplied to the atomizer of the AAS device, the Hg/hydride system
enriches mercury from one or more samples on the gold collector. The gold collector re-
leases the mercury again during bake-out. With the subsequent cooling, the Hg/hydride
system prepares the gold collector for the next measurement.
Operation times In the control and analysis software, you can define the following operation times in a
method for the Hg/hydride system:
Option Description
Prewash time Time for purging the beaker with argon before the reaction (for hy-
dride formers)
The pre-wash time is used to expel air to prevent an oxyhydrogen re-
action during the subsequent reaction.
Pump time In this time, the reduction agent is pumped into the beaker in order to
start a reaction.
AZ wait time Time directly preceding the baseline adjustment (AZ = auto zero).
Wash time The wash times are needed to transport the reaction gas with the ar-
gon flow. The transport paths can be graphically displayed.
Heat. time collector During this time, the heater runs to release the enriched mercury
from the gold collector.
Cool. time collector During this time, the gold collector is cooled to make it ready for the
next enrichment.
Graphical display To open the graphical display of the gas paths, click on Plot in the Method |Hydride
window. The window displays the operations that run partially simultaneously during
the individual phases of the measurement.

HS 55 (Batch Mode) Function and design
19
Plot
Graphic for
first measurement
Parameters
React. GLS Coll. Cell
Batch
Phase
Sample pump
Sample valve
Reagents
Measurement
Collector
Time [s]
Take up sample
Take up reductant
Take up wash sol.
Sample valve to reactor
Reagent transport
Autozero
Delay time
Measurement
Heat collector
Cool collector
AZ Wash 2
Close
Gas paths and flows
Line
6
Pump time
Figure6 Graphical display: gas paths and measuring process

Installation and commissioning HS 55 (Batch Mode)
20
4 Installation and commissioning
Normally, the Hg/hydride system is installed by the Analytik Jena customer service or
persons authorized by Analytik Jena together with the AAS device. If the Hg/hydride sys-
tem is delivered separately at a later time, you can also install it yourself.
When installing and commissioning the system, observe the information in the "Safety
instructions" section. Compliance with these safety instructions is a requirement for the
error-free installation and the proper functioning of your measuring station. Observe all
warnings and instructions that are attached to the device itself or displayed by the con-
trol and analysis program.
To ensure trouble-free operation, please make sure that the installation conditions are
observed. To do so, check the installation conditions specified in the manual for your
AAS device.
4.1 Installing the hydride and Hg cold vapor systems
NOTICE
Continuous beeping tone in the case of incomplete installation
If the installation is incomplete, the device emits a continuous beeping tone.
¡In this case review the installation steps carried out.
Information on the AAS device can be found in the separate operating manual.
4.1.1 Installing the cell unit
WARNING
Risk of oxyhydrogen formation
The cell must be sealed gastight for the hydride system as otherwise an oxyhydrogen
mixture which could explode at high temperatures would form in the cell.
¡Inspect the polished end faces of the cell.
¡Even if you notice only minor damage, replace the cell.
NOTICE
Risk of corrosion
If acid residues remain in the siphon of the mixing chamber/nebulizer system, there is a
risk of corrosion of the cell unit due to the acid vapors.
¡Flush the siphon with 500ml of water via the mixing chamber connection before
placing the cell unit on the mixing chamber connection.
}Remove the burner head from the burner block.
}Flush the siphon with 500ml of water via the mixing chamber neck.
}Attach the cell unit to the burner block and lock it.