Chapter 6

Preventive Maintenance

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Contents

1 Flame Systems Preventative Maintenance ............................................. 4

1.1 Safety .................................................................................................. 4
1.2 Initial Checks ...................................................................................... 4
1.3 Spray Chamber Maintenance ............................................................ 4
1.4 Dismantling the Spray Chamber ....................................................... 5
1.4.1 To re-assemble the spray chamber ........................................... 6
2 Nebuliser .................................................................................................... 6
2.1.1 To clean the Nebuliser ................................................................ 6
2.1.2 To measure the Nebuliser uptake rate ...................................... 6
3 Drain ........................................................................................................... 6
3.1 To empty and refill the Drain............................................................. 6
4 Gas Supply Hoses ..................................................................................... 7
4.1 Gas Leaks Test ................................................................................... 7
5 Flashbacks................................................................................................. 8
6 Burner(s) .................................................................................................... 8
7 Gas Piping/Leak Test ................................................................................ 9
7.1 Leak Test and Gas Flows ................................................................ 10
8 Lubrication............................................................................................... 10
9 Optics ....................................................................................................... 10
10 Wavelength Accuracy Test ................................................................. 11
11 Resolution Test.................................................................................... 11
12 Background Correction Balance ........................................................ 11
13 Electronics/Calibration........................................................................ 11
14 Chemical Tests .................................................................................... 11
15 Final Report.......................................................................................... 12
16 Flame Preventive Maintenance Checklist.......................................... 13
17 FAS Autosampler Preventive Maintenance ....................................... 14
17.1 FAS Preventive Maintenance Checklist ......................................... 15
18 GFS 33/35 Furnace Preventive Maintenance..................................... 16
18.1 GFS Furnace PSU............................................................................. 19
19 GFS35Z Preventive Maintenance........................................................ 20
Appendix - GFS 33/35..................................................................................... 24

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1 Flame Systems Preventative Maintenance
Test Equipment
SOLAAR Service Diagnostic Software for iCE 3000
DVM
Ni/Cr & Ca/Mg HCLs Standard Ni/Cr solution (10ppm Ni & 3pprn Cr) 131350647201
Super-lube - 4013 228 46751

1.1 Safety
Discuss with the customer any problems or difficulties and obtain information of the
potential hazards surrounding the machine and within the laboratory. Also ascertain
the type of samples that have been used on the machine and their likely hazards.
The drain system in particular may contain hazardous material and a routine
precaution before dismantling the system would be to flush it with water by pouring
200-300mls of water down the spray chamber stem. The wearing of protective gloves
is also advisable when dismantling burners and spray chamber. The kitchen area
may also be contaminated. If serious biological contamination is suspected, refer to
Appendix A which deals with cleaning instruments. If in any doubt, a CLEARANCE
CERTIFICATE should be filled in by the customer before work proceeds.

1.2 Initial Checks

1. Check the condition of the electrical supply cable, RS232 control cables, USB
cable and gas supply pipes.
2. Check the earthing of main instrument to the supply socket is less than 0.2 Ohms
resistance with a DVM.
3. Check that the drain container is made of a suitable shatter-proof material with
a wide neck.
4. Switch on the spectrometer and check that the indicator lights extinguish
correctly and number 1 starts to flash when the software is started.

1.3 Spray Chamber Maintenance

(a) If the precision of the instrument is poor, or if the memory effect has become
obvious it is advisable to clean the spray chamber. Should a flashback occur
it is essential that the spray chamber is thoroughly inspected, refurbished and
cleaned. (By a Factory trained Service engineer)
(b) Minor cleansing during operation can be achieved by aspirating a 2 to
5% solution of a proprietary laboratory cleaner (e.g. Decon solution) for
approximately 5 minutes, followed by aspiration of de-ionised water for
approximately 5 minutes.

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 (c) For more thorough cleaning, dismantle the spray chamber and wash through
with a 2 to 5% solution of proprietary laboratory cleanser. Rinse thoroughly with
de-ionised water.

1.4 Dismantling the Spray Chamber

WARNING: Before removing the burner, allow ten minutes for It to cool before
touching the burner.

To remove and dismantle the Spray Chamber

1. Use the system software commands to raise the Burner until the Burner Height
is less than 10mm.
2. Remove the Burner
3. Empty the Spray Chamber Drain.
4. Disconnect the gas lines to spray Chamber and disconnect the Drain tube.
5. Release the Burner Mount Clamp Screw by at least 3 full turns, and then
rotate the Spray Chamber downwards around the axis of the bayonet mount to
release it and the Clamp Ring/Mounting Bracket from the bayonet mount, and
remove the assembly.
6. Unscrew the 4 thumbscrews and remove the Spray Chamber Front Cap.
7. Unscrew the 3 Rear Clamp screws, and remove the Clamp ring/Mounting
Bracket and the Over - Pressure Disc.
8. Push the Baffle Assembly out of the Spray Chamber body towards the front.
9. Undo the Fuel Gas Coupling on the Spray Chamber body, and remove the
Gauze Disc assembly/spring and washer

To dismantle the Cap Assembly

1. Slacken the Impact Bead Clamp Adjusting Screw, and withdraw the Bead from
the Alumina Disc side of the Cap.
2. Remove the Seal and Alumina disc.
3. Undo the securing screws, and remove the Bead Adjustment Assembly.
4. Slacken the Nebuliser Retaining Clip screw, withdraw the Clip, and then
remove the nebuliser and O-ring.

To re-assemble the Cap Assembly

1. Fit the O-ring to the Nebuliser body; refit the Nebuliser to the Cap, and replace
the Clip and tighten the screw.
2. Lightly lubricate the Impact Bead stem with silicone grease (Superlube), pass it through
the Alumina Disc, and fit one O-ring over the stem.

Caution: Take great care not to contaminate the Bead itself or the
Alumina Disc with grease.

3. Fit the Alumina Disc to the Cap, passing the Impact Bead stem through the
hole in the Cap
4. Fit the second O-ring to the stem, slide the bead adjustment assembly on to
the stem, and secure it to the Cap.
5. Set the bead Adjuster to the fully out position.
6. Position the Impact bead so that the Bead is centrally located in the Nebuliser
Nose Cone and is as close as possible to the Nose Cone.
7. Tighten the bead Clamp screw.
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 8. Refit the Alumina Disc and Seal.

1.4.1 To re-assemble the spray chamber

1. Inspect, clean and replace any damaged components
2. Push the Baffle Assembly into the front of the Spray Chamber body, with the
Baffle to the rear, and a short Baffle Blade at the bottom. Push the assembly
into the Spray Chamber body taper until a slight resistance is felt.
3. Re-assembly and re-fit the Gauze Disc assembly, spring and Fuel Inlet Coupling.
4. Using a new Over-pressure Disc, refit the Disc and Clap Ring.
5. Re-fit the Cap Assembly, and tighten the thumbscrews.
6. Re-fit the Spray Chamber to the Spectrometer Mount, and re-connect the
Gas Lines, Drain and Burner. Ensure that the Burner Mount Clamp Screw is
fully tightened after the Spray Chamber is rotated into position in the bayonet
Mount.
7. Perform a Leak Test and rectify and leaks before lighting a flame.

2 Nebuliser

2.1.1 To clean the Nebuliser

1. Extinguish the flame

2. Remove the Nebuliser Uptake Capillary.
3. Push the Nebuliser Cleaning Probe trough the Nebuliser Capillary to remove
the blockage. Warning: Do not use any other tool or wire to clean the nebuliser
4. Replace the Nebuliser Uptake Tube, light an air/acetylene flame and check
Nebuliser uptake rate.

2.1.2 To measure the Nebuliser uptake rate

1. Fill a 10ml measuring cylinder with deionised water.

2. Fit a standard length (250mm) of 0.5mm ID Nebuliser Capillary.
3. Light an air/acetylene flame.
4. Aspirate the water from the measuring cylinder and note the volume aspirated
in 1 minute.
The normal Nebuliser uptake rate under these conditions should be between 4.5 and
5.5ml/min.

3 Drain
Periodically check the external Drain Tube and replace it if it is cracked or damaged.
If the Drain becomes blocked it can be cleaned by pouring dilute hydrochloric acid
(5%v/v) or laboratory detergent down the Spray Chamber Stem and leaving it to
soak. When the blockage has dissolved, empty the Drain, and refill it with clean
water.

3.1 To empty and refill the Drain

1. Turn off the fuel and nitrous oxide gas supplies at source, but leave the air
supply turned on.
2. Remove the Burner.

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 3. Ensure that a suitable container is positioned to receive the contents of the
Drain.
4. Block the top of the Spray Chamber with a suitable bung.
5. Vent the Gas System by holding down the Flame Off button for at least 30
seconds. This will cause the contents of the Drain to be blown out to waste.
6. Refill the Drain by pouring clean water or solvent into the top of the Spray Chamber
Stem until it flows freely from the Drain.

4 Gas Supply Hoses

• Inspect the Gas Supply hoses regularly, and replace any that are cracked or
damaged.
We recommended that all Gas Supply hoses are replaced every four years, the date
can be found attached to the hose
• Run the Gas Leak Test at least once every six months, and whenever the
instrument is moved, and rectify any leaks found.

4.1 Gas Leaks Test

The software command necessary to run the Gas Leak test are included in the
SOLAAR OQ Test Data Station application.

Fig. 4 - 1. Nebuliser and Spray Chamber Components

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5 Flashbacks
If the flowrate of gases through the burner is reduced below the rate of flame propagation,
the flame can flash back into the spray chamber, and a small explosion will result. A red hot
particle falling through the burner into the spray chamber could produce a similar effect.

Should a flashback occur, the fuel gas must be turned off as quickly as possible. The spray
chamber must be removed, dismantled and examined for damage. It is probable that the
alumina disc, the impact bead, the spider, baffle and the overpressure disc will all need to
be replaced. It is recommended, therefore, that the Spray Chamber Maintenance Procedure
should be carried out following a flashback.
Note: A Flashback report form should be filled in a returned to Technical Support Cambridge
.

6 Burner(s)
Introduction
Flame System maintenance must be performed at regular intervals to ensure
safe and reliable operation. Flame AAS involves high temperatures and corrosive
solutions; system cleanliness is most important.

iCE 3000 Series Spectrometers can accept both the Universal Finned (50mm) and the
100mm Titanium Burners. Both of these are cleaned and dismantled in
the same way.

Safety
Turn off all gas supplies and disconnect the spectrometer and accessories from the
mains supply before carrying out maintenance work.
Burner

Fig. 11 - 1. Universal titanium burner head

DO NOT ATTEMPT TO CLEAN THE BURNER WHILE A FLAME IS BURNING, AND

ENSURE THAT THE BURNER HAS COOLED BEFORE HANDLING IT.
To clean the external surfaces of the Burner
• Clean and polish the top surfaces using a mild abrasive soap cleaner.
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 • Clean the burner slot with the Burner Cleaning Tool supplied or a piece of stiff
card. Do NOT use an abrasive material inside the slot.
• Wash the Burner with detergent solution and rinse with deionised water. Dry
the Burner carefully before using it again.
To dismantle the Burner
.
• Turn the finned burner head half a turn anti-clockwise.
• Lift the Burner Head away from the Burner Base to separate the two parts.

To clean the internal surfaces of the Burner

• Use an ultrasonic bath filled with deionised water, dilute detergent solution or
5% v/v of nitric acid to clean the internal surfaces of the Burner Head.

Warning: Do NOT put the plastic Burner Base and Ignition Electrode assembly into
the ultrasonic bath. ▲

To re-assemble the Burner

• Push the Burner Head into the Burner Base and turn it half a turn clockwise until it
clicks into place.
To align the Ignition Electrode
• Refer to the figure, and place the Cleaning Tool/Setting Jig as shown, aligning
the bottom corner of the chamfer with the edge of the Ignition Well.
• Gently bend the Electrode until the tip touches the top corner of the chamfer on
the Setting Jig, as shown above.

7 Gas Piping/Leak Test

1. Check the flexible piping and seals in the kitchen area for hardening, cracks or wear –
replace if required.
2. Check the piping from the wall/cylinder to the instrument for wear/damage or
chemical attack, replace if required. Remove the right hand cover and check
the internal pipes for cracks or wear - replace if required. The red fuel hoses
should be replaced every four years.
3. Block off the acetylene and air lines at the spray chamber with the blanking
plug. The blanking plug for the air line is 4013 228 36581. The blanking plug for
the fuel line is 4013 166 91961.
4. From the OQ software, select the gas leak test and follow the instructions

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1
 5. After releasing the Flame Off button an audible hiss of air venting the reservoir/air lines
should be heard.
6. Remove the blanking plugs and check that the pressure on both supplies falls
to zero.
TRACE AND RECTIFY ANY LEAKS BEFORE CONTINUING THE SERVICE.

7.1 Leak Test and Gas Flows

1. Re-fit and re-connect the spray chamber to the instrument.
2. Fit the burner, and light an air acetylene flame.
3. Check around the chamber for leaks with soapy water.
4. Check the gas flow switches by increasing the fuel flow from 0.8 l/m to 1.4 l/m
in 0.1 l/m steps checking for a smooth change in flow.
5. Return to the gas setup page and select a fuel gas flow of 0.81/min.
6. Check that the flame stays alight. Also check that the flame turns luminous
when the fuel gas flow is changed from 1.1 to 1.31/min.
7. Check the fuel gas and air pressures if either condition is not achieved.
8. Using a small measuring cylinder check that the uptake rate of the nebuliser is
>4.5mls/min when using an 200mm length of standard uptake tube.

8 Lubrication
Remove both side panels the top cover.
Use super-lube, part number 4013 228 46751 in the following places.
1. Lamp Mirror Linear Actuator, clean contact surfaces and apply fresh super-
lube.
2. Polariser Linear Actuator (if fitted), clean contact surfaces and apply fresh
super-lube.
3. Burner Height Mechanism, clean and lubricate top adjustor screw, not the
bushes, these are designed to run dry.
4. D2 Lamp Mechanism - Check this moves from side to side freely and the return
spring is working properly. Apply super-lube as required.

9 Optics
All optical components within the optical base casting should not need cleaning,
since this is a sealed compartment.
Check the optical components outside the optical base, i.e the beam combiner, lamp
alignment mirror and windows.
Also check GFTV (if fitted) for alignment.

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10 Wavelength Accuracy Test
Use the service software to run the following tests.
Use a Ca/Mg Hollow Cathode Lamp at 75% max current and a bandpass of 0.2nm.
The wavelengths to use are:
285.21 nm
347.26nm
603.00nm
743.89nm
All wavelengths should be found to within ± 0.2nm.
If this is not the case, you will need to re-calibrate the monochromator.

11 Resolution Test
This is done at a wavelength of 393.37 with a 0.2nm bandpass.
The specification is 0.17nm - 0.225nm.

12 Background Correction Balance

Set up at 285.2nm with background correction on and check the balance is within
10%.

13 Electronics/Calibration
1. Check that the power supply voltages are within their nominal voltages.
2. Using neutral density Alters (either balanced across the burner or fitted to jig
4013 172 93401) and a Ni lamp set to 10-15mA, carry out the absorbance test.
3. Check the absorbance calibration using the 540.1 nm line to the following
spec:
0.0A - 0.4A 0.4A - 1.6A 1.6A - 2.8A
±0.005A ±2% ±3%

14 Chemical Tests
1. Start up the user software and using 10ppm Ni solution run the following sensitivity
tests.
2. Fit a Ni/Cr hollow cathode lamp to the turret, switch on and align.
3. Select Ni from the Spectrometer/Parameters page to set the defaults for Nickel,
and then modify the settings as follows:
System
Single Element
Spectrometer Parameters
Number of resamples: 10
Calibration
None or Off
Autosampler Off

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 Sequence (Delete Calibration if necessary)
Sample 1
Sample 2

4. Use Setup Optics and allow the lamp to warm up for 5 minutes.
5. Light the air acetylene flame and aspirate the standard solution.
6. Set up the burner rotation, horizontal position and impact bead for maximum
sensitivity.
7. Start the analysis and allow to set up.
8. Aspirate deionised water for a blank and then the standard solution. The result
should be greater than 0.5A, with an RSD of less than 1.0%, for a 50mm slot
burner and greater than 0.6A with a 100mm slot burner. If an autosampler is
fitted, check the correct autosampler is selected in the system box, check the
"Use autosampler"' box and load the samples in accordance with the ASLG.
Restart the analysis with the autosampler, the result should be greater than
0.35A (50mm) or 0.45A (100mm) and with an RSD of less than 1.5%.

9. If nitrous oxide is connected and a finned 50mm burner available, repeat for a 3ppm
solution of Cr using a nitrous oxide flame and the default settings modified as follows:
Spectrometer Parameters
Number of resamples: 10
Calibration None or Off
Autosampler Off
Sequence (Delete Calibration if necessary)
Sample 1
Sample 2
10. The result should be better than 0.16A with an RSD less than 1.5%.
11. Clean the keyboard and VDU screen.
12. Check the hard drive for excessive tmp files, advise customer of a problem if
several are found in either the root directory or the TEMP directory.
13. Exit Windows and run CHKDSK, check for any lost allocation units and
advise the customer. Do not fix and delete without backing up the disk and
unAinstalling the accessory software.
14. Check the remaining hard disk space is sufficient for continued use, and that
the SOLAAR\data directory does not contain more than 200 files. If there are
excessive files, suggest to the customer that they are either archived into
another directory or onto a floppy disk.
16. Emission Test. Using the instrument in the emission mode, aspirate a solution
of 5ppm sodium and ensure the wavelength is located correctly at 589.Onm.

15 Final Report
Discuss with the customer any remaining problems with the instrument, and any
problems likely to arise in the near future. Fill out the paperwork and leave the
customers copy along with the completed check list sheet.

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16 Flame Preventive Maintenance Checklist
√ or X
Initial Checks USB Cable [ ]
Mains cable(s) [ ]
RS232/USB cables [ ]
Flexible Gas Hoses [ ]
Earthing to socket [ ]
Spray Chamber "O"rings and seals replaced [ ]
Burner Burner cleaned and checked for corrosion [ ]
Burner igniter lead and plug [ ]
Igniter gap set [ ]
Gas Pipes /Leak Test Kitchen area pipes and seals checked/replaced [ ]
Acetylene gas leak test passed [ ]
Nitrous Oxide gas leak test passed [ ]
Internal Gas Pipes [ ]
Spray chamber leak test & gas Spray chamber leak test [ ]
flows Acetylene gas flow test [ ]
Nebulizer uptake rate > 4.0 mls/min [ ]
285.21 (0.2nm) [ ]
Optics
422.67 (0.2nm) [ ]
845.34 (0.2nm) [ ]
Resolution 0.2nm [ ]
Background Correction [ ]
Electronics/Calibration Power supplies in spec. [ ]
Absorbance calibration within spec. [ ]
Completion Cover earth continuity tests [ ]
Printer connected [ ]
Furnace connected [ ]
Chemical tests Nickel - absorbance > 0.6A (100mm burner) [ ]
or > 0.5A (50mm burner) [ ]
with an RSD of <1% [ ]
Chromium - absorbance > 0.16A [ ]
with an RSD of < 1.5% [ ]
Sodium - Wavelength found [ ]
Keyboard, VDU & Disks
Keyboard cleaned [ ]
VDU screen cleaned [ ]
Hard Disk checked [ ]

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17 FAS Autosampler Preventive Maintenance

Test Equipment
Service Diagnostic Software
PC.

Safety
Discuss with customer the safety precautions that should be taken when dismantling
the autosampler. Bear in mind that any spillage deposited on the inside and outside
of the sampler assembly may constitute a hazard. A minimum precaution of wearing
latex gloves is strongly suggested. If in doubt contact the company safety officer
before proceeding.

Checks
1 Disconnect gas line and control cable from furnace power supply.
Check condition of cable, drain tube and gas line.
Examine wash and waste bottles and lid seal for signs of cracking or
weakness, replace if required.

2. Check the capillary sample tube from the syringe to the arm for contamination
or wear, particularly at the "elbow" of the arm. Replace if required.

3. Remove turn-table and drip tray, check for blockage in top of drain.
Inspect for spillage inside unit and report any problems to customer.
Check the condition of sample uptake tube and replace if required.
Check condition of gas and water tubing pipes and connections.

4. Check for smooth syringe action with syringe test.

5. Run the arm test and check for smooth action. Check that arm stops in correct
position.

6. Carry out a turn-table test choosing cup positions in both inner and outer rings
of the turn-table.
Fit cups in the turn-table at test points and check for central lateral pick-up.
Adjust arm height if required.

7. Rebuild and connect.

Test wash solenoid from normal usage by doing a wash with empty wash cup.
Cup should start to overflow after 4 washes.
Check wash bottle gas pressure if insufficient wash water.

8. If balance available, weigh plastic weighing boat and note result.

With sampler standing on bench, program system to inject 20ml.Run program
and collect injection in weigh boat.
Repeat 5 times, ensuring a drip is not left on end of tube.
Re-weigh the boat, the difference should be .020 gms ±001.

9. Test with furnace system for correct operation and dilution.

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17.1 FAS Preventive Maintenance Checklist

CHECKS COMMENTS PASS/FAIL

Control cable condition
Drain tube
Gas supply pipe
Wash water bottle
Interior in clean condition
Interior gas pipe and joints
Interior water pipe
Sample uptake tube
Syringe action smooth
Arm action correct
Pick-up tube central in test cups
Wash action correct
Injection volume correct
Checked with furnace program

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18 GFS 33/35 Furnace Preventive Maintenance

Test Equipment
DVM, PC Service Diagnostic Software, Manganese HCL

Safety
Discuss with customer the precautions that should be taken when dismantling the
furnace head. Bear in mind that some of the samples will have been deposited
on the inside and outside of the head assembly during the drying phase and will
not have been subjected to high temperatures (e.g. bacterium and viruses from
human and animal samples). Also the products of ashing and atomising at high
temperatures may produce carcinogenic material which is deposited on the head.
A minimum precaution of wearing latex gloves is strongly suggested. If in doubt
contact the company safety officer before proceeding. If in any doubt a CLEARANCE
CERTIFICATE should be filled in by the customer before work proceeds.

1. Check condition of electrical supply cable, RS232 control cable, gas supply
pipes and water pipes.
Check earthing of FPSU is satisfactory.
Isolate furnace from supply.

2. Clean/replace water Filter situated on rear right-hand side on inlet pipe stub.

3. Remove top and rear furnace covers, check the condition and security of all
gas and water tubing in the FPSU.
With the water on full check that the flow is greater than 1 l/min using the
Customer Diagnostics. If faulty check water regulator valve for faults.

4. Remove furnace head centre block and check gas and water connections.

5. Remove and clean window in centre block. Check power braids (a sharp pull
will show if they are corroded) and replace if required.
Check red and blue voltage feedback wires.

6 Remove and clean windows, replace if damaged. Check condition of sealing

gasket at right-hand contact cone.

7. Remove temperature feedback system from rear of head. Remove white lens
holder, clean lens.
Remove optic fibre and clean end.
Reassemble and refit to head.

8. Clean and examine carbon cones at contact areas for damage and wear,
surface mating with contacts should be smooth and un-pitted, the area that
contacts the tube should be clean.
Advise customer if replacements required.

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 9. Refit centre block and window holders checking that gas supply pipes are not
kinked, align with tube alignment jig and fit new, uncoated graphite tube.
Re-connect mains to power supply.
Set the argon supply pressure to 15psi.
Check the gas flows using the Service Diagnostic Software.

Place the furnace head on its side, remove both gas supply pipes.
Check that on all phases gas is supplied from the lens supply.
Check that the inner gas flow increases correctly and shuts off properly. A
simple method of checking flow is to bubble through water or connect to a
rotameter if available.
Check the condition of the gas pipes and re-connect.
Check security and condition of the water pipes under the head.

10. Visually check the temperature calibration as follows:

2000 TEST
Phase Temp Time Ramp Gas Gas Commands
Type Flow
1 2000 10.0 2 0.2L/min
2 2000 5.0 2 0.2L/min TC
3 0 10.0 2 0.2L/min
4 0 3.0 2 0.2L/min RD
and with a white card held against the sample compartment exit window, check
that the brightness of the light emitted from the tube does not change considerably
between phases 1 and 2 apart from a slight dip at switch-over and check that the cuvette
does not emit too much smoke
3000 TEST
Phase Temp Time Ramp Gas Gas Commands
Type Flow
1 3000 5.0 2 0.2L/min TC
2 0 10.0 2 0.2L/min
3 0 3.0 2 0.2L/min RD

600 TEST.
Phase Temp Time Ramp Gas Gas Commands
Type Flow
1 600 40.0 2 0.2L/min TC
2 0 10.0 2 0.2L/min
3 0 3.0 2 0.2L/min RD
and check that the tube glows dull red and the temperature does not appear to
oscillate.If any of these tests fail re-check the contacts and connections at the head
and in the rear of the PSU.

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 11. Replace covers and check earth continuity between covers and earth.
12. Run a chemical test consisting of a blank and a 0.02ppm Manganese standard.
Use parameters listed in Appendix B.
Set up the furnace head and At a coated graphite tube.
Set up the autosampler with an injection depth of about 2mm from the bottom
of the tube.
Load the autosampler with a cup of blank and one of Mn standard, set the
Autosampler to /ON and press ANALYSE.
Check with a mirror that the blank dries without boiling and that drying is
complete before the end of the phase. The blank should be less than .010A
and the Mn standard should be greater than 0.8A with an RSD of less than 2%.

Final Report

Discuss with the customer any remaining problems with the instrument, and any problems
likely to arise in the near future.

Fill out the paperwork and leave the customer's copy along with the completed checklist
sheet.

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18.1 GFS Furnace PSU
Preventive Maintenance Checklist

CHECKS COMMENTS PASS/FAIL

Supply cable
RS232 cable
Gas supply pipes and clips
Water pipes and clips
Earth good
Water Alter cleaned/ replaced
Gas tubing in FPSU
Water tubing in FPSU
Water flow correct
Centre block window
Power braids
Voltage feedback wires
Windows cleaned/replaced
Sealing gasket
Lens cleaned
Optic fibre cleaned
Carbon contact cones
Gas flows at rear of head checked
Gas pipes on rear of head
Water pipes and clips on rear of head
2000°VC/2000°TC test
Smoke at 3000o acceptable
600° Test stable
Temperature set-up
Cover continuity check
Chemical test

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19 GFS35Z Preventive Maintenance
To allow access to the centre block, open the right-hand electrode, remove the
magnet clamp bolt and separate the two halves of the magnet. Use the rear magnet
latch to hold the rear magnet half in position. Tilt the complete head forwards on its
mount.

Remove the centre block by pulling to the right to disengage it from its mounting pins
and then lift vertically. This allows access to the window in the bottom of the block.

To remove the window unscrew the window holder and take care not to lose the
window which will then be released.

Access to the lens at the end of the fibre optic can be achieved by removing the 'O'
ring from the front of the lens.

The end windows may be removed by rotating and pulling outwards.

All windows and lenses may be cleaned using a cotton bud and alcohol before re-
assembly. Ensure that all soot deposits are removed from inside the centre block and
end contacts.

Note: Ensure that the window in the base of the centre block is fitted correctly
and does not leak! If this is not done, very short cuvette life will result.

Check the contact cones for wear and replace if necessary using the ZEEMAN
Furnace contact cone replacement tool.

To re-assemble the magnet release the rear catch and replace the clamp bolt. Do not
over-tighten the bolt to avoid damage to the graphite insert in the centre block. If the
bolt is too loose there will be excess noise from the vibrations of the magnet when
powered. A torque of between 6-10nM is recommended (approximately finger tight, plus
half a turn).

The Polariser Assembly

The polariser can be removed from its mount to enable the end windows to be
cleaned. Be sure to note its orientation since it must be replaced the correct way
round (the small vertical alignment hole away from the monochromator).

The polariser is adjusted to be in the correct position by means of the end stop and
rotation via the small hole at the end of the housing. The rotation will be correct when
the adjusting hole is vertical; use a long hex key in the hole to set it vertically and
tighten the clamp screw.

The end stop is set for maximum energy on the right hand light patch. The action of
the polariser will split the circular hollow cathode lamp image into two and the right
hand image as it falls onto the entrance slit of the monochromator is the one used in
the Zeeman mode.

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GFS35Z Zeeman furnace - centre block removed

GFS352 Zeeman furnace - magnet open

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 GFS35Z ZEEMAN FACTORY TEST SPECIFICATION

Removing the Power Supply Cover

Remove the power supply module from its packing. Remove the outer cover by
undoing the screws on the lower edge of the top cover.
Carefully lift the cover off ensuring that no wires or connectors become caught or
get pulled out in the process.

Cooling Water Tests

Water Pressure Leak Test

(i) Connect the water to the water system inlet (attach using jubilee clips
or similar), pump enough water through (head, conduit and power
supply) to fill the system then block the outlet by clamping a short
length of hose attached to the outlet pipe. Pressurise to 50 psig.

(ii) Check for water leaks around all connections in the water system. If
not completely leak tight, adjust the connections until all leaks have
been eliminated.

(iii) Release the pressure on the water and disconnect it.

(iv) Fill in production test record sheet.

Water Supply Pressure Regulator

(i) Fit the in-line pressure gauge after the water regulator in the water box.
(ii) Connect the inlet of the water recirculator to the outlet of the GF90. Connect
the regulator (with 0 - 60 psi gauge) between the outlet of the recirculator and
the inlet of the GFS35Z water box (the arrow on the back of the regulator
indicates the direction of water flow).
(iii) Vary the pressure in the inlet line between 20 and 60 psi by adjusting the in-
line regulator, and observe the reading on the water box pressure gauge. The
pressure should reach a maximum of 30 psi. If necessary adjust the pressure
using the regulator knob (pull to unlock, adjust, then push to lock once the
correct value has been set).

Nominal Cooling Water Flow

(i) Remove the regulator from the input line. Turn on the recirculator and check
that the pressure at the GFS35Z Zeeman water box is regulated correctly to
less than 30 psi and that there are no leaks.
(ii) Turn off the recirculator. Remove the pressure gauge from the water box
regulator, tighten the screws on the bracket and replace the blank.
(iii) Switch on the recirculator and check that the water box regulator does not
leak.
(iv) Switch off the recirculator and replace the regulator in the input line. Set the
input pressure to 20 psi.

Water Flow Sensor Test

The status of the cooling water flow is indicated by LED number 3.

(i) With water at 20 psi flowing check that the LED is ON. Switch off the
reciculator and check that the LED goes OFF.
(ii) Switch the DIL switches all back to the off position and press the red reset
button on the CPU pcb.

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 Gas Test

Select 'outer gas'. Turn on the outer gas flow in the power supply and the gas
will be heard to hiss lightly inside the furnace head.

Furnace Pressure Regulator Test

Note: The input pressure on the leak test gauge should still be set to give 15 psig
with a flow of 3 l/min.

(i) The pressure with a flow of 3 L/min should read 12 1 psig. If necessary adjust
the gas pressure regulator. Ensure that the gas is flowing during this test.
Ensure that the setting is locked after adjustment.
(ii) Record the gas pressure on record sheet.

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 Appendix - GFS 33/35
Furnace Commissioning Test

This test consists of running a manganese sample of 0.02ppm and a blank solution.

Align the Furnace Head and At a ridged coated cuvette. Fit the Furnace Autosampler
and set it to give an injection depth of 2mm from the bottom of the tube.

Load the Furnace Autosampler with a cup of blank solution and a cup of the Mn
0.02ppm sample.

Use the following parameters:

Wavelength 279.5nm
Slit width 0.2nm- reduced height
Lamp current Default
Background Correction On
Analysis Time 3.0sec
No of Resamples 5
Concentration Off
Standard Additions Off
Working Volume 10ml
Matrix mod Off
Sample prep None
Cuvette type ridged coated
Autoprobe Off
Injection temp

Set the following furnace program:

Furnace Program Time Ramp Gas Gas Commands
Phase Temp (°C) (s) (°C/s) Type Flow
1 90 1.0 40 2 0.2L/min
2 120 10.0 1 2 0.2L/min
3 700 20.0 250 2 0.2L/min
4 1800 3.0 2 0.0L/min RD, TC
5 2500 3.0 3 0.1L/min TC

Select Autosampler on and start the analysis. Check with a mirror that the blank dries
without boiling and that drying is complete before the end of the phase.

The blank should be less than 0.01A and the Mn sample should be greater than 0.8A
with an RSD of less than 2.0%.

Page 24 of 24 iCE 3000 Technical Support Manual Version 0.5