Sir Galahad User Manual G525M050 v1-3
Sir Galahad User Manual G525M050 v1-3
Sir Galahad User Manual G525M050 v1-3
P
PSA 10.525
SIR GALAHAD II
USER MANUAL
PSA 10.525 Sir Galahad II User Manual
Version Version
Update Description
No. Date
Revised to include amalgamation unit type D009 (Sections 1.1.0, 1.4.0 –
1.3 13 May 15
1.4.3, 3.1.0 & 3.1.1). Minor revisions.
Carrier gas specification updated (§2.9.1), Hazardous substance
information updated to reflect GHS terminology (§3.3.0). Changes due
1.2 10 Jun 14
to SGv3 software release: Minimum computer specification (§2.10.0);
software and software manual references revised (throughout).
1.1 05 Oct 12 Addition of Section 1.5.1. Minor revisions.
First Issue. Amalgamation of previous individual Sir Galahad
Manuals,(G525M002, G525M012, G525M013, G525M014 &
1.0 04 Nov 10
G525M015) with extensive updates and revisions. Manual applicable to
instruments with Serial Numbers 500+
Manual
Manual Description
Part No.
SGv3 Software G525M030
PSA OnLine Software C210M007
Sir Galahad Service G525M009
P S Analytical Ltd
Arthur House, Crayfields Industrial Estate,
Main Road, Orpington, Kent BR5 3HP,UK
Tel: +44 (0) 1689 891211 Fax: +44 (0) 1689 896009
E-mail: psa@psanalytical.com Website: www.psanalytical.com
© P S Analytical 2010-15
Note: Pressures in this manual are given in bar. Conversions to other units are given
below:
CONTENTS
SECTION 1 INTRODUCTION
1.1.0 Introduction
The P S Analytical 10.525 Sir Galahad II enables the determination of mercury in a wide
range of gaseous media, including; ambient air, natural gas and stack gases. The
Sir Galahad is based on amalgamation with atomic fluorescence spectrometry. Atomic
fluorescence provides inherently more sensitivity than atomic absorption and offers
advantages in terms of linearity, accuracy and precision.
The P S Analytical Merlin detector offers the sensitivity to be able to measure low levels
of elemental mercury with minimal sampling requirements. Combining the detector with
a specific gold amalgamation trapping mechanism using Amasil™ traps provides the key
to offering a complete monitoring system.
The PSA 10.525 Sir Galahad II analyser has been designed to support a wide range of
applications. To support this range of applications, a number of different models are
available. The different models are denoted by suffixes on the basic PSA 10.525 Part
Number, as shown in Table 1. The differences between the models are principally
confined to the configuration of the amalgamation unit (or “drawer”). All models
incorporate a PSA Merlin detector. The range of models available and the available
modes of operation and special features of each are shown in Table 1.
Note: The abbreviated part number 10.525/Dnnn is used in this manual to identify the
different Sir Galahad models unless identification of a particular Detector Type or
Purge Ready Status is also required.
Continuous Sequential
3
2
Rapid-cycle Dual
Online Sampling
Sour Gas Ready
Remote Sample
4
Amalgamation
Amalgamation
Amalgamation
Part No. Description
Online Single
Online Dual
Collection
G525D001 Standard Model
G525D005 Online Dual Amalgamation Ready
(Quartz Trap 2 module)
G525D500 Online Dual Amalgamation
(Long life ceramic Trap 2 heater module)
G525D510 Standard Ex p model
(Online Dual amalgamation with Long Life 5
Ceramic Trap 2 heater module and separated
waste streams for Ex p cabinets).
1
G525D520 Ex p model for sour gas applications
(Online Dual Amalgamation with Long Life
Ceramic Trap 2 Heater Module, separated
waste streams for Ex p cabinets and separate
5
Trap1/detector and Trap 2 carrier gas streams
for sour gas applications)
G525D006 “Quick” Online Dual Amalgamation
G525D007 Continuous Sequential Sampling
Online Single Amalgamation
G525D008 Dual Sample Inlet, Single
Amalgamation
(for low level online air sampling)
G525D009 Online Dual Amalgamation Ready
(Quartz Trap 2 heater module and separated 5
waste streams).
1
The G525D520 Unit also requires the G525K010 accessory to control the carrier gas flow.
2
Modified for online sample streams containing high H2S.
3
Equipped with two traps for continuous sample collection. (Mercury is collected on one trap
whilst mercury collected on the other trap is being analysed.)
4
Modified for a shorter online dual amalgamation cycle.
5
G525K510 Single Amalgamation Link Kit also required.
Note: Other naming conventions were previously used to indicate the Sir Galahad
configuration, below is a translation. Except where shown, use of a B700 optics
box was indicated by the addition of “H” to the end of the part number.
Previous Part No. New Part No.
10.525 10.525/D001/B300
10.526 10.525/D005/B300
10.525EX 10.525/D500/B300/EX (previously 10.525/D005/B300/EX)
10.525F 10.525/D007/B300
10.525K 10.525/D520/B700/EX
10.525Q 10.525/D006/B300
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PSA 10.525 Sir Galahad II User Manual
The PSA Sir Galahad is a highly flexible instrument. It can be readily transported and
will monitor one or numerous sample streams/locations in a local, online or remote basis.
(Online analysis when incorporated into an analyser system.)
The instrument has been widely used to measure mercury levels in many different gas
streams, including: ambient air, workroom air, hydrocarbon/petrochemical streams
(including sour gas streams), syngas, hydrogen, process streams and utility stack gases.
For stack gas applications, chemical pre-treatment can be used to distinguish between
the species of mercury being measured. The sensitivity of the detector allows for a
range of dilution and sample pre-treatment options.
The instrument includes all the necessary components to clean the argon or nitrogen or
air carrier gas, to control the carrier and cooling gas flows and to selectively analyse on a
continuous cycle, one sample stream or to allow the measurement of samples collected
remotely on a similar trapping system. (PSA 10.525/D006 & /D007 models do not
support remote sample collection.)
The system incorporates both the gold Amasil™ and atomic fluorescence techniques to
provide sensitive mercury determinations, combined with a series of valves to allow
different cycles to take place.
PMT Measures
Fluorescence a
PMT b
Mercury
Lamp
Sheath Gas (a)
Sample In (b)
Mercury Lamp
Causes Mercury
to Fluoresce
Lens
A flow of mercury entrained in carrier gas, passes a mercury source, and the
fluorescence produced is measured by a conventional photomultiplier tube (PMT).
Mercury absorbs and fluoresces at the same wavelength (253.7 nm), which assures
maximum sensitivity. Argon is preferred to nitrogen and air, as the molecular gases
quench the fluorescence signal. The inherent sensitivity of the Merlin detector means
that mercury can be accurately measured well below the limits imposed by current
legislation.
The presence of air and other gases has the effect of quenching the fluorescence and
reducing the detection levels attainable. The level of quenching depends on the
composition of the sample, thus, to apply this detector to measurements in air some
means of collecting the mercury and exchanging the gaseous sample medium for argon,
nitrogen or dry air is required. This is simply achieved by use of a valve switching
mechanism.
1. Mercury, typically from a known volume of sample gas, is collected on the Sir
Galahad’s Amasil™ trap
2. Carrier gas is flushed over the trap to remove any air or other gases present.
3. The heating coil is activated which heats the Amasil™ to a temperature greater
than 500ºC, desorbing the mercury which is carried by a stream of carrier gas
into the fluorescence detector.
4. The Amasil™ trap is rapidly cooled by compressed air ready for the next
sampling cycle.
The full analytical cycle employed in the Sir Galahad depends on the model being used
and the mode of operation. This is discussed in more detail in Section 1.4.0 Analytical
cycles.
AmasilTM Traps are largely insensitive to mercury speciation, efficiently collecting all
forms of gaseous mercury compounds. Collection efficiencies for a range of mercury
compounds are shown in Table 2, However, when the AmasilTM Trap is thermally
desorbed, regardless of the adsorbed species, the mercury vapour produced is in the
form Hg0(g), as required by the AFS detector for the fluorescence measurement.
AmasilTM Traps can also be used to collect samples at elevated temperatures. Collection
efficiency is not affected at temperatures of up to 200°C, as shown in Table 3. Collection
at elevated temperatures is particularly useful when sampling low dew point
petrochemical streams or sampling other wet gas streams.
The “Manual” calibration procedure involves the injection of known volumes of mercury
saturated air at a known temperature using a gas-tight syringe. This is a simple but
effective means of providing a primary standard which is more effective and economic
than many other calibration approaches.
“Automatic” calibration uses calibration gas from a PSA Calibration Gas Generator which
works on similar principles to the manual calibration approach but can easily be
automated and can be used to calibrate an entire sampling interface as well as the
analyser itself.
A series of injections, together with zero points where no mercury vapour is injected are
used to prepare a calibration graph of detector response against mass of mercury.
A series of calibration gas and zero gas samples are used to prepare a calibration graph
of detector response against mass of mercury.
The modes of operation applicable to the Sir Galahad for the different amalgamation unit
(drawer) configurations is shown in Table 4 below:
Trap 1 Trap 1
Waste
Carrier Carrier
gas gas
Injection Injection
port port
Sample In Sample In
(c) (d)
AFS
AFS
Detector Pump
Detector Pump
Flow
Flow
Control
Control
Trap 1 Trap 1
Carrier Carrier
gas gas
Injection Injection
port port
Sample In Sample In
Note: For Sir Galahad instruments fitted with a D510 or D009 Amalgamation Units: to
use Online Single Amalgamation mode, Use the G525K510 Single Amalgamation
Link Kit to tee together the “Pump” and “Waste 2” ports before connecting to a
flow control device and pump. For a D520 Amalgamation Unit, tee together
“Waste 2” and the pump line from the drawer.
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A four stage process is employed to sample gas or air directly onto Trap 1, when
sampling in the online single amalgamation mode:
1. Sampling A known volume of a gas/air sample passes over the
(Figure 2(a)) AmasilTM trap. Any mercury present in the sample is
adsorbed onto the gold surface of the trap. Generally,
sample is pulled over the trap by a downstream mass flow
controller and vacuum pump arrangement. (The volume may
be known by sampling a known flow rate for a known time
period.)
2. Flush The sample flow is diverted and carrier gas introduced to the
(Figure 2(b)) AmasilTM trap and detector. The carrier gas flow flushes out
any residual air or sample gas that may be present as this
would have a damping effect on the mercury fluorescence.
(Simultaneously, the detector baseline is measured.)
3. Analysis – Heating When the flush cycle is completed, the heating coil is
(Figure 2(c)) activated and heats the AmasilTM trap to > 500°C. This
desorbs mercury collected on the trap which is transferred to
the carrier gas stream and into the fluorescence detector.
4. Analysis – Cooling When the heating cycle is complete, cooling gas is directed
(Figure 2(d)) over the heater module and AmasilTM trap to rapidly cool it in
preparation for the next sampling period.
Note: Mercury desorbed from the AmasilTM trap starts to reach the detector at the end
of the heating period, continuing into the cooling period. The signal output from
the detector is monitored throughout the heating and cooling periods.
The cycle time is the Sampling Time + approximately 3 min analysis time. (Pre-flushing
of sample lines to ensure a representative is also required when different sample
streams are analysed.) With the average times for the complete cycle, including
sampling, ranging up to approximately 5 minutes, data can be returned in a meaningful
timescale. This allows a continuous update of the mercury levels.
Samples are collected remotely using specially designed AmasilTM traps. Mercury from
gas streams passed through the traps is adsorbed onto gold inside the trap. The tubes
are then capped and placed into a sealed container and transported to the analyser for
analysis.
The analytical cycle first transfers mercury from the remote trap to a fixed trap within the
analyser. This ensures the consistent analytical performance of the analyser, particularly
providing a consistent peak shape and height and a narrow peak. The permanent trap is
also used for analyser calibration.
The steps of the Remote Sampling analytical cycle are shown schematically in Figure 3.
Trap 1 Trap 1
Waste Waste
Carrier Carrier
gas gas
Injection Injection
port port
Trap 2 Trap 2
Trap 2 Trap 2
Carrier gas Carrier gas
(c) (d)
AFS AFS
Detector Detector
Waste Waste
Trap 1 Trap 1
Carrier Carrier
gas gas
Injection Injection
port port
Trap 2 Trap 2
Trap 2 Trap 2
Carrier gas Carrier gas
Note: Waste carrier gas from the transfer process exits through the port labelled
“Pump” on the rear of the instrument, except with D510, D520 and D009 Drawers
where it exits through the port labelled “Waste 2”
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PSA 10.525 Sir Galahad II User Manual
The analytical cycle first passes the sample stream over an AmasilTM trap (Trap 2),
collecting mercury from a measured volume of the sample onto the gold inside the trap.
It then transfers mercury from Trap 2 to Trap 1 before transferring the mercury to the
detector.
This mode of operation allows for the sample trap to be warmed during sample collection
to prevent the deposition of heavier hydrocarbons from the sample gas onto the trap. It
also further provides for easy replacement of the AmasilTM sample trap if required
(except10.525/D006). Dual amalgamation is also used for Online Stack Gas analysis
systems for certain sampling configurations where undiluted sample streams are
generated and the gas stream has not passed through a water-filled impinger.
The steps of the Online Dual Amalgamation analytical cycle are shown schematically in
Figure 4.
Trap 1
Trap 1
Carrier
gas Carrier
gas
Injection
port Injection
port
Trap 2
Trap 2
Trap 2
Carrier gas Trap 2
Carrier gas
Sample in Sample in
(c) (d)
AFS AFS
AFS
AFS Detector
Detector
Detector Detector
Pump Pump
Pump
Pump
Flow Flow
Control Control
Trap 1 Trap 1
Carrier Carrier
gas gas
Injection Injection
port port
Trap 2 Trap 2
Trap 2 Trap 2
Carrier gas Carrier gas
Sample in Sample in
Note: With the D510, D520 and D009 drawers, the line marked vents as a separate
waste (labelled “Waste 2”); it does not flow to the MFC and pump as shown
above.
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A four stage process is employed to sample gas or air when sampling in the online dual
amalgamation mode:
To monitor continuously for mercury in air or gas, two AmasilTM traps are employed in
parallel. While sample gas is pulled over one trap, to absorb any mercury present, the
second trap is analysed. The six stages of the Online Continuous Sampling analytical
cycle are shown schematically in Figure 5.
Argon Argon
(c) Sample Trap B, Cool Trap A (d) Sample Trap A, Flush Trap B
To Detector To Detector
Argon Argon
Figure continues…
Figure 5 (Continued)
(e) Sample Trap A, Heat Trap B (f) Sample Trap A, Cool Trap B
To Detector To Detector
Argon Argon
A continuously cycling six stage process is employed to collect and analyse samples on
traps A and B alternately using Online Continuous Sampling:
1. Trap A – Flush AmasilTM Trap A is purged with Carrier gas, flushing
Trap B – Sample out any residual air or sample gas that may be
(Figure 5(a)) present. (Sample was collected during the previous
cycle.)
Gas/air sample passes over Trap B. Any mercury
present in the sample is adsorbed onto the gold
surface of the trap. The total volume sampled is
known over the trap is measured.
2. Trap A – Analysis (Heating) The Trap A heating coil is activated and heats the
Trap B – Sample AmasilTM trap to > 500°C. This desorbs mercury from
(Figure 5(b) the trap, which is carried in a stream of carrier gas to
the detector.
Sampling continues on Trap B.
3. Trap A – Analysis (Cooling) Trap A is rapidly cooled by flowing cooling air over the
Trap B – Sample heating module in preparation, for the next sample
Figure 5(c) stage.
Sampling continues on Trap B. The total volume
sampled is measured.
4. Trap A – Sample Gas/air sample passes over AmasilTM Trap A. Any
Trap B – Flush mercury present in the sample is adsorbed onto the
(Figure 5(d)) gold surface of the trap. The total volume sampled is
known over the trap is measured.
Trap B is purged with Carrier gas, flushing out any
residual air or sample gas that may be present.
This approach allows the continuous updating of the mercury levels. The cycle time (for
two results) is equal to the Sampling Time (for two samples), with a minimum 90 s
between results (3 min cycle time).
Once the results have been collected, the software provides full collating and reporting
facilities. Full management information, including timed and dated results is provided as
standard. Using such an automated software package with the Sir Galahad provides
complete control of data and conditions, while the system of menus allows easy use.
Note: The Sir Galahad model 10.525/D007 can only be operated using the PSA Online
Software (Part No. C210S007). Unlike other Sir Galahad models it cannot be
used with PSA SGv3 Software (Part No. G525S302 (basic) or G525S303
(advanced)).
1.6.0 Applications
The PSA 10.525 Sir Galahad II can be used for a wide range of applications for gaseous
samples. The sensitivity of the system is down to one picogram which offers a number
of advantages to the user, namely in the reduction of the volume of gas required to
provide accurate measurement. The PSA software allows absolute calibration and
calculates the concentration of mercury based on the calibration curve obtained. Results
can be computed in a range of units as desired by the user. Application notes relating to
the Sir Galahad are being prepared on an on-going basis. Please contact P S Analytical
or your distributor for more information.
For more information on any applications of the Sir Galahad, please contact
P S Analytical or your local distributor.
For offline use, the Sir Galahad can be used to sample directly from sample bombs or
Tedlar bags or used to analyse Amasil Tubes from samples collected in the field. When
used in conjunction with the PSA 10.547 Offline Sample Interface (Dual Absorber), the
procedure is designed to be fully compliant with both the ISO 6978 part B and ASTM
6350 methods.
The PSA Sir Galahad can be incorporated into an Ex p purged enclosure and
accompanied by a Sampling System to reduce the gas pressure to perform online
analysis of the concentration of mercury in a range of petrochemical streams.
The Sir Galahad can also be used offline with the PSA 10.515 Preconcentration Unit to
measure the mercury concentration in low-boiling point petrochemical liquids such as
naphtha and condensates. An online implementation of this technology incorporated into
Ex p purged enclosures is also available.
For offline measurements, AmasilTM tubes can be used to sample flow rates as low as
100 ml min-1 for 1 to 4 weeks to obtain long term average mercury exposure levels. A
suitable filter is used to remove particulate from the gas stream prior to the AmasilTM
tube. Ambient air concentrations are typically in the ng m-3 range.
Online measurements utilise a similar filter and Teflon tube sampling configuration to
sample directly onto an AmasilTM tube located within the Sir Galahad. Higher sample
flow rates, typically 0.5-0.8 l min-1 are employed to maximise the volume of gas sampled
during each 30-60 min sampling period. Figure 6 shows a week typical results of
ambient air monitoring, sampling for 10 min periods at 0.8 l min-1 at an industrial estate in
a suburban location in southeast England.
The Sir Galahad has also been used to monitor transient mercury emissions in
crematory stacks and waste incinerators.
With an appropriate sample probe and sample conditioning system from the P S
Analytical range, the Sir Galahad can be used to provide reliable online mercury
concentration and speciation (Hg0 and total gas-phase mercury, HgCl2 being determined
by difference) data.
For technical assistance please contact your local distributor or P S Analytical directly.
Power: 192 VA
Class: 1
Voltage Tolerance: ± 10 %
Warning
This instrument must be earthed
Mains connection is by IEC lead (see Section 2.7.0 Voltage and Fuse Checks).
Temperature: 5º – 40ºC
Use: Indoors
Installation Category: II
Pollution Degree 2
Weight: 15.0 kg
2.5.0 Unpacking
Carefully unpack the Sir Galahad from the packing material. Visually inspect the unit for
any apparent damage. If any exists notify both the P S Analytical offices and the
shipping company. Check the contents against the packing list and notify PSA of any
discrepancies immediately.
2.6.0 Location
Because the instrument is self-contained and compact, the Sir Galahad can be placed
virtually anywhere on a laboratory bench, the Sir Galahad can also be incorporated in a
range of online analyser systems based on 19 in. racked enclosures. The area should,
however, be clean and free from pollutants.
Depending on proposed use, adequate ventilation and waste disposal facilities may need
to be provided.
Note: For installation in purged cabinets, the top cover must be removed to ensure
adequate purging. For other online cabinets PSA recommends that the top cover
is removed to provide additional ventilation.
Caution
Before any electrical checks are made, ensure that the instrument is switched off
and isolated from the mains electrical supply.
The instrument must not be connected to any other mains electrical supply than
that specified (see Specifications - Electrical Supply Section 2.2.0).
Before connecting the instrument into the electrical supply, check that the voltage
selector and fuse size are correct. Operator fuse replacement is restricted to the fuses in
the mains voltage selector unit.
The voltage selector, mains on/off switch and the mains input fuses are located on the
rear panel (see figure 7).
Figure 7 Voltage Selector, Mains On/Off and Mains Input Fuse Location
Voltage selection and access to the mains fuses is by removal of the rectangular panel
to the right hand side of the mains input unit.
Caution
Remove the mains input cable
The rectangular panel can be removed by the insertion of a suitable tool in the locating
hole on the left hand side of the rectangular panel. Access to the fuses and voltage
selector is now possible.
Voltage selection is obtained by accessing the red fuse holder on the right hand side of
the mains unit and rotating so that the desired voltage is visible through the window. A
small flat bladed screwdriver is needed to access and remove the fuse holder.
Fuse ratings:
F1 5A Type T
F2 5A Type T
The Sir Galahad contains other internal fusing which is not normally deemed operator
replaceable.
The Sir Galahad contains potential hazards to personnel when the covers are removed.
P S Analytical therefore recommends that only suitably trained or technically competent
personnel should remove these covers. If in any doubt please contact your local
distributor or P S Analytical.
Caution
Some of these fuses are mounted close to mains voltages
Warning
This instrument must be earthed
Important: The wires in the mains cable are coloured in accordance with the
following code:
Green/Yellow Earth
Blue Neutral
Brown Live
Carrier Gas
Cooling Gas
Purge Instruments used in Ex p purged enclosures only
(Trap 2 Carrier only with D520 drawer)
The requirements for the different gases are described in Sections 2.9.1-2.9.3. Different
gases are recommended for each gas supply. It can however be convenient to use a
single supply for the carrier gas and cooling gas. In this case, the common supply
should be regulated to approximately 3.5 bar (gauge).
Argon is the recommended carrier gas. Nitrogen and air may be used; however, these
reduce the net signal of fluorescence by 9 and 180 times respectively. (See Figure 8 for
the carrier gas input location).
Argon or nitrogen purity should be 99.99+%, compressed air should be to class 3.3.3:
Compressed Air Quality Classes to ISO 8573-1: Class 3.3.3
Category Class Definition
Solid Content 3 Particle size ≤ 5 µm
-3
Particle density ≤ 5 mg m
Humidity 3 Pressure dew point ≤ 5°C
-3
Oil Content 3 Total oil content ≤ 1 mg m
The carrier gas must also be free from mercury. An internal “clean up” system is
provided. As effective as this is, total reliance is not recommended.
Note: Sir Galahad Analysers fitted with the D520 drawer for determination of mercury in
sour gas have two carrier gas inputs. Argon or nitrogen should be used for the
port labelled “Carrier gas” (This is the Trap 1 and detector carrier gas.)
Compressed air must be used for the carrier gas port labelled “Trap 2 Carrier”.
(This is the Trap 2 carrier gas.) The Carrier Gas 2 port is a ¼ in. stainless steel
compression fitting.
Compressed air is the recommended cooling gas; however nitrogen or argon can also be
used. The input gas should be clean, dry and free from any compressor oil/mists.
Caution
Nitrogen and argon are asphyxiants. Cooling gas is vented to atmosphere.
Locate in a well-ventilated area before use if using nitrogen or argon cooling gas.
POWER
F1 5A(T)
1
0 HEATERS
TTL
F2 5A(T)
USB
PURGE
WASTE
GAS
COOLING PUMP
CARRIER
Warning
When installed in an Ex p purged enclosure, the purge gas line MUST always be
connected
* One RS485 port is required for Modbus® enabled instruments. The second
RS485 port is required if a PLC or DCS link is required.
** RS232 port only required for instruments with Serial Numbers below 500.
The minimum specification for PSA OnLine Software may differ. Consult the relevant
User Manual for more information.
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PSA 10.525 Sir Galahad II User Manual
For operation of the PSA Sir Galahad Software (PSA Part No. G525S302 (basic) or
G525S303 (advanced)) or PSA OnLine Software (PSA Part No. C210S007) please refer
to the appropriate manuals.
Computer connections for the Sir Galahad system are shown in Figure 9.
STATUS
POWER GAS 1
SERIAL GAS 2 HOT
TRAP 1 TRAP 2
COOL
TRAP1 TRAP2
ARGON ARGON
HEAT HEAT
COOL COOL
ANALYSIS CYCLE
CALIBRATION SAMPLE
PORT PORT
POWER
Computer
Sir Galahad
POWER
USB Port
F1 5A(T)
1
0 HEATERS
TTL
F2 5A(T)
USB
PURGE
WASTE
GAS
COOLING PUMP
CARRIER
SECTION 3 OPERATION
3.1.0 Front Panel Controls
Figure 10 PSA 10.525/D001 Sir Galahad II Front Panel Controls
F G H I J L M N O
A
STATUS HOT
Power Gas 1 TRAP 1 TRAP 2
COOL
Serial Gas 2
B
C TRAP1 TRAP 2
D Flush Flush
Heat Heat
Cool Cool
ANALYSIS CYCLE
E
POWER
K P Q R
Figure 11 PSA 10.525/D005, /D500, /D510, /D520 & D009 Sir Galahad II
Front Panel Controls
F G H I J S L M N O
A SAMPLE
STATUS TRAP
PORT 2 1 2
Power Gas 1
Serial Gas 2
B HOT
POWER
PORT
SAMPL
EPORT 1
REMOT
EPORT
K P Q R
A
STATUS HOT
TRAP 1 TRAP 2
Power Gas 1 COOL
Serial Gas 2
B CALIBRATION CALIBRATION
SAMPLE
C TRAP1 TRAP 2 PORT
TRAP 1
INLET
PORT
TRAP 2
D Flush
Heat
Flush
Heat
Cool Cool
ANALYSIS CYCLE
E
POWER
SIR GALAHAD
APPLYING THE POWER OF ATOMIC FLUORESCENCE
K P S T
A
STATUS HOT
TRAP 1 TRAP 2
Power Gas 1 COOL
Serial Gas 2
B
C TRAP1 TRAP 2
D Flush Flush
Heat Heat
Cool Cool
ANALYSIS CYCLE
E
CALIBRATION SAMPLE
PORT PORT
POWER
SIR GALAHAD
APPLYING THE POWER OF ATOMIC FLUORESCENCE
K P Q
POWER
F1 5A(T)
1
0 HEATERS
TTL
F2 5A(T)
USB
PURGE
WASTE
GAS
COOLING PUMP
CARRIER
E F K GH I J
Location Description
Mains power input socket with switch, voltage selector and fusing.
A Power Inlet
See Section 2.7.0 for further information.
B USB Port USB port used for communication to and from the host computer
Internal fusing for the trap heaters. See Section 2.7.1 for further
C Heater Fuses
information.
25-way male “D” connector used for accessory equipment, for example
D TTL Port
a stream selection unit. See Section 2.4.1 for pin outs.
E Identification Tag Quoting Part No., Serial No., VA rating etc.
¼ in. compression fitting connection for cooling gas supply. See
F Cooling Port
Section 2.9.2 for details.
¼ in. compression fitting connection for connecting a flow control
device and pump during online sampling.
G Pump Port (10.525/D520 only: the “Trap 2 Carrier” inlet is located here. The
pump connection is made to a ⅛ in. o.d. Teflon tube exiting the
Amalgamation Drawer directly.)
H Waste Port Outlet for waste carrier gas.
¼ in. push fit connection for carrier gas supply. See Section 2.9.1 for
I Carrier Port
details.
Purge gas inlet port. When the Sir Galahad is installed in an Ex p
J Purge Gas Port purged enclosure, this port must be connected to the purge gas
distribution system. The port is otherwise unused.
Unused except for 10.525/D510, /D520 & /D009 models where this
port vents carrier gas during the transfer stage and for online single
Waste 2 Port amalgamation must be teed to the “Pump” output (G for D510 and
K
(Location Marked) D009, line from drawer for D520) before connection to a flow control
device and pump. (For the D510 and D009 drawers, the G525D510
Single Amalgamation Link Kit should be used.)
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PSA 10.525 Sir Galahad II User Manual
Warning
The Sir Galahad may be used in conjunction with hazardous substances,
particularly mercury. Always use appropriate laboratory practices and comply
with all applicable risk assessments and SDS requirements when working with
hazardous substances.
The following summary is therefore provided for information only:
MERCURY
Toxic by inhalation
Danger of cumulative effects
Very toxic to aquatic organisms, may cause long term adverse effects in the
aquatic environment
Mercury must only be used, handled, stored and disposed of in strict accordance with
the SDS and risk assessment. Appropriate personal protective equipment (PPE) must
be worn, including eye protection and rubber or plastic gloves.
The calibration relies on the knowledge that at a fixed temperature the saturated vapour
pressure of mercury is known and a fixed volume of vapour will contain a known quantity
of mercury. This volume is adsorbed onto the continuous analytical gold trap (Trap 1)
and then revaporised into the detector where the peak height or peak area of the
response is measured. The PSA software has the necessary programs to operate the
Sir Galahad and also holds the calibration details. Once the temperature and volume
are provided the software computes the absolute level of mercury adsorbed onto the
trap.
To carry out these procedures reliably, good attention to detail is required; i.e., good
housekeeping and pure carrier gas supply. A specially designed glass vessel is also
required to hold the calibration mercury at a set temperature.
1. Place 20-30 g (1.5-2.2 cm3) of elemental mercury into the glass calibration vessel
via Port A. See Figure 15
Caution
Mercury compounds are highly TOXIC and should be handled with extreme care!
(See Section 3.3.0 Hazardous Substances)
2. Insert a thermometer into Port B and carefully tighten the fittings to hold the
thermometer in place. The bulb of the thermometer should be close to but not
touching the bottom of the vessel. See Figure 16.
3. Insert a septum into injection Port C and carefully tighten the fittings to hold the
septum in place. The septum should be inserted with the Teflon (red) side on the
bottom. The septum should be replaced every 30 injections. See Figure 16
Caution
Ensure that no elemental mercury comes into contact with this injection port.
This would result in severe contamination of the Sir Galahad instrument.
Thermometer
Capillary Tube
B C
Elemental
Hg
5. Carefully transfer the calibration vessel to a thermostatic bath and monitor the
temperature of the mercury vapour using the thermometer. Allow the vessel to
stabilise.
Note: The saturation concentration of atomic mercury in air is calculated using the
vapour pressures of mercury as a function of the temperature. The saturation
concentration can be calculated using the formula outlined in Section 1.3.1. This
calculation is automatically performed by the PSA SGv3 or PSA OnLine Software
during a calibration cycle.
7. Switch on the instrument and ensure that the Gas 1 and Gas 2 LEDs are not
flashing. Allow at least 30 minutes to warm up.
8. Set up the computer and load the PSA SGv3 or PSA OnLine Software. Once the
software has loaded initiate a calibration. A four-point calibration (including
blank) is recommended.
Note: For more information on operating SGv3 or PSA OnLine Software consult the
appropriate software user manual.
10. Enter the temperature of the mercury contained in the calibration vessel.
Note: 1 ml ≡ 1000 µl
11. The software will automatically calculate the mass of Hg based on the vapour
pressure of Hg using the equation shown in Section 1.3.1.
12. Carefully insert the syringe into the port of the calibration vessel and extract the
appropriate volume of gas to be injected. Take care not to touch the needle
against the side walls of the vessel. Syringes supplied will have a gas valve.
Green is open and red is closed.
Notes: To avoid blockages, side port needles are used with calibration syringes.
Syringes must be preconditioned. Before first use, fill with vapour from
the calibration vessel and leave for at least 20 min. To ensure syringes
are conditioned, store filled with Hg saturated air.
13. Inject the Hg vapour from the syringe into the calibration port of the Sir Galahad
and then press OK to start the cycle. The software will activate the sequence of
events.
14. Continue this procedure until a calibration is obtained. The temperature of the
calibration vessel may change, in which case input the temperature for each
injection.
Step:
1. Collect the remote samples noting the flow rate and the length of collection time
or the sample volume collected. Cap the ends of the sample tube after collection.
Flowmeter
Filter
Mercury Adsorber
AIR
Pump
TM
Amasil
Gold Impregnated Sand
(Gold coated silica)
When using a rotameter as shown in Figure 17, the gas/air volume sampled can be
calculated by multiplying the flow rate (l min-1) by the collection time (min). Alternatively,
replacing the rotameter with a volumetric flow meter/accumulator is equally acceptable.
When sampling a variable composition gas, such as a petrochemical stream, a matrix
independent flow meter, such as a wet gas flow meter, is preferable.
3. Introduce the remote sample tube into the remote port (Trap 2) of the instrument.
4. Remove the cap covering the sample port (this must be in place at all times when
the port is not in use).
5. Link the remote port output to the sample port using the adaptor/transfer line.
Avoid kinking the tubing.
6. Access the Results Page of the PSA Sir Galahad software and click the Analyse
Sample button.
7. Select Remote Method and enter the relevant data sample name and ID and the
sample volume acquired at collection. Other notes can be made using the memo
button if desired.
8. Click Analyse to determine the mercury collected on the remote sample tube.
Notes: It is recommended to measure the blank level on AmasilTM tubes before use.
When analysing samples collected using the PSA 10.547 Offline Sample
Interface in Series mode for petrochemical gas analysis, the SGv3 Software
“Series Mode” feature has been expressly prepared to perform the replicate
measurements and calculations required for compliance with ISO 6978 part B
and ASTM 6350. This feature is only available in G525S303 SGv3 advanced.
Additional sampling details are required to use this feature. For more information
on the Series Mode feature, see the SGv3 Software manual (Manual Part No.
G525M030).
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PSA 10.525 Sir Galahad II User Manual
2. Under normal working conditions, the AmasilTM traps will have an unlimited
lifetime. However, this may be significantly shortened by:
Similar principles and concepts to those described here apply when the Sir Galahad is
incorporated into a larger online analyser system, when PSA OnLine Software is used
and/or when Dual Amalgamation or Continuous Sampling mode are utilised. For more
information on the use of the Sir Galahad in an online analyser system, see the relevant
User Manual.
Note: Please read Sections 1.4.0 – 1.4.4 for an explanation of the principles of online
sampling. Refer to the PSA SGv3 Software or PSA OnLine Software Manuals
(as appropriate) for an extensive explanation of the software functions and
features (Manual Part Nos G525M030 and C210M007 respectively).
Step:
1. Calibrate the Sir Galahad as described in Section 3.4.2 Calibration Procedure.
2. For air sampling arrange for a pump or similar device to be connected to the
pump output at the rear of the instrument. In addition a rotameter or a volumetric
flow meter/accumulator is required in order to monitor the flow rate or sample
volume. Typical sample flow rates of 0.5 to 1.0 l min-1 should be employed. See
Figure 18.
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PSA 10.525 Sir Galahad II User Manual
F1 5A(T)
1
0 HEATERS
TTL
F2 5A(T)
USB
Pump
PURGE
WASTE
GAS
COOLING PUMP
CARRIER
Flowmeter
TRAP1 TRAP 2
Flush Flush
Heat Heat
Cool Cool
ANALYSIS CYCLE
POWER
Filter
To Sampling Point
Notes: If a rotameter is being used then calculation of the gas/air volume is performed by
multiplying the flow rate (l min-1) by the collection time (min).
Use of a downstream flow control device, as in Figure 18, can reduce the lifetime
of sample pumps. Configure sample flow control and measurement devices for
accurate flow measurement and as recommended by the pump manufacturer.
COOLING
WASTE
PUMP
PURGE
GAS
Volumetric
CARRIER
Flowmeter /
Accumulator
TRAP1 TRAP 2
Flush Flush
Heat Heat
Cool Cool
ANALYSIS CYCLE
SIR GALAHAD
CALIBRATION REMOTE
PORT PORT PORT
Filter
Valve
Cylinder
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PSA 10.525 Sir Galahad II User Manual
4. Remove the cap covering the sample port (this must be in place at all times when
not using the port). Attach an air filter (approximately 0.50 µm) in front of the
sample attachment to avoid aerosol contamination. If the sample is 'wet' the filter
must be replaced for each sample to avoid any possibility of carry-over. Keep the
length of input sampling tube to a minimum.
5. Arrange for the gas or air sample to be connected to the sample port on the front
panel of the instrument (see Figures 18 or 19).
6. Access the Results Page of the PSA Sir Galahad software and click the Analyse
Sample button.
a. Select Flow Time Method and enter the relevant data sample name and ID
and the sample flow rate and the desired collection time. Other notes can be
made using the memo button if desired.
b. Select the number of repeat analyses required.
c. Click Analyse. The software will collect sample for the selected time period,
then determine the mercury mass (and concentration) sampled.
d. If repeat analyses are selected, the analyser will automatically continue to
these.
a. Select Sample Volume Method and enter the relevant data sample name and
ID and the volume of gas to be sampled. Other notes can be made using the
memo button if desired.
b. Select the number of repeat analyses required. (Manual action will be
required to end each sampling period.)
c. Click Analyse. The software will display a prompt to click when the required
volume has been sampled. After this volume has been sampled, click OK on
the prompt to start the measurement cycle. The mercury mass (and
concentration) sampled will then be determined.
d. If repeat analyses are selected, the analyser will automatically continue to
these, however the end of sampling must be manually acknowledged each
time.
SECTION 4 MAINTENANCE
4.1.0 Introduction
It is strongly recommended that all replacement and spare parts are obtained from P S
Analytical or its representatives. The fitting of unauthorised spare parts may invalidate
any warranty or service contract covering the instrument.
4.2.0 Maintenance
Under normal conditions the Sir Galahad requires very little maintenance.
Maintenance Schedule
Daily:
Start Up
1. Run instrument through a Clean Up Cycle.
2. Change the Calibration Port Septum. (Teflon (white) side towards the analyser.)
Shut Down
1. Run instrument through a Clean Up Cycle.
Weekly:
As Daily
Monthly:
1. As Daily
2. Check detector Reference and Emission values, adjust as necessary.
Six Monthly:
1. As Monthly
2. Check that the analytical gold trap (Trap 1) is in good condition and is not dirty (see Gold
Trap Cleaning Section 4.3.1).
3. Leak check the analyser sample path
Yearly:
1. As Six Monthly
2. If necessary, replace Hg lamp
3. After the first year of use it is recommended that the Sir Galahad is inspected and
checked out according to the Service Manual by the P S Analytical Service Department or
by its authorised representatives.
4.3.0 Cleaning
Before undertaking any cleaning procedures disconnect the mains supply cable from the
Sir Galahad. Cleaning is only recommended for user accessible parts of the instrument
i.e. the outside case.
1. Clean the instrument with a damp cloth which has been previously immersed in
soapy water. Alternatively a suitable laboratory cleaning fluid may be used.
Avoid copious amounts of liquid coming into contact with the instrument.
Caution
Repeated heater activation without sufficient cooling may cause permanent
damage to the heater coil and gold trap.
Gas 1 LED flashing Carrier gas not present or Connect gas or increase pressure
pressure too low to 2.4 bar (gauge) minimum
Gas 2 LED flashing Cooling gas not present or Connect gas or increase pressure
pressure too low to 2.4 bar (gauge) minimum
Display over-range at all Contamination of the Flush out with argon (sheath gas)
times measuring chamber
No sample signal seen Heater coil open circuit Call PSA Service Dept
Faulty injection needle Replace Needle
Will not proceed through Incorrect mode selected Select correct mode
cycle Electronics problem Call PSA Service Dept
Double peaks on sample Uneven winding on the heater Trouble shoot the heater coil – call
coil the PSA Service Dept
Long “Tail” on sample No cooling or insufficient Trouble shoot the cooling gas
cooling pressure
Insufficient carrier gas flow rate Trouble shoot the carrier gas
Gold trap not positioned in the Trouble shoot the heater assembly
heater assembly correctly – call the PSA Service Dept
Insufficient vaporise time Increase vaporise time
This list of spare parts is for user replacement with care. If there is any doubt about
replacing parts, contact either your local distributor or P S Analytical.
This list of spare parts is for user replacement with care. If there is any doubt about
replacing parts, contact either your local distributor or P S Analytical.
Description Part No
Amalgamation Unit (Drawer) – See Section 1.1.0 for details Various
Hg Lamp M023L001
Activated Charcoal Refill: 5g M025C032
Activated Charcoal Filter Complete M025F100
TM
Cap for Amasil Traps (Pack of 10) G511C005
TM
Test Tube: Plastic (for Amasil Traps) (Pack of 10) G511T002
Test Tube Caps (pack of 10) G511C004
Needle: Side Port (pack of 3) Z360N052
Syringe: 0 - 50 µl Z360S524
Syringe: 0 - 250 µl Z360S531
Syringe: 0 - 1000 µl Z360S533
Syringe: 0 - 5000 µl Z360S535
Calibration Vessel Septa (Pack of 100) Z012S002
Thermometer: UKAS Certified Z550T002
Calibration Vessel G523V002
¼ in. o.d. Nylon Tubing (5m) Z026T107
5
¼ in. o.d., /32 in. i.d. Teflon Tubing (per metre) C533T004
1
⅛ in. o.d., /16 in. i.d. Teflon Tubing (5m) Z018T117
Air Sampling Pump A001S002
Wet Gas Flow Meter M001G002
Consumable Parts
Generally speaking components or parts, which are easily accessible and/or replaceable
without the aid of specialist knowledge, are considered operator replaceable parts. In
addition, components or parts which require changing on a regular basis due to the
nature of their use, are considered operator replaceable parts. Further, components or
parts, which have a defined lifetime dependent on use, are also considered operator
replaceable parts. If there is any doubt about replacing parts, please seek advice from
P S Analytical or your local distributor.
www.psanalytical.com
Thank You!