Flame Atomic Absorption

Maintenance and Safety

 Objectives

• Outline a suitable protocol for routine maintenance

covering:
– Gas supplies
– Atomization system
– Instrument body
– Key accessories

• Maintain instrument performance

• Review safety considerations

2
 Results of Poor Maintenance

• Degradation of performance

• Unsafe operation

3
 Basic Flame Maintenance

Light Sources
Gas Supplies
Burner Nebulizer Assembly
Instrument Body
Accessories

4
 Maintain Written Logbook

5
 Acetylene

• MUST be Stabilized

• NEVER Operate with

cylinder pressure below
700 kPa (100 psig)

• Or line pressure above

105 kPa (15 psig)

• NEVER use copper lines

or fittings

6
 Nitrous Oxide Regulator

• It may FREEZE!

• NEVER Lubricate “O”

rings with grease

• It is stored as liquid -
Cylinder pressure does
NOT indicate contents!

7
 Check Delivery Pressure

Normal

8
 Gas Flow and Burning Velocity

Flame Burning Down

Gas flowing Up

9
 Nitrous Oxide - Acetylene Gas Flow

Acetylene Nitrous Oxide

2.0
5

1.8
10

1.6
1
Varian AA
1.4 10 Gas Flow
Flash Back Region
Fuel/Oxidant Ratio

1.2

1.0
Region 15

0.8
5
0.6 20

0.4

0.2
1

0.0
0.0 5.0 10.0 15.0 20.0 25.0 30.0
Total Gas Flow Litre/Min

10
 Maintenance Tasks

Check Exhaust System

Clean Burner Compartment & Instrument
Clean Windows

11
 Daily Maintenance Tasks

• Empty waste container

• Check exhaust system

• Clean burner compartment & instrument

• Check the gas delivery pressures & cylinder contents

• Check the nebulizer uptake rate

12
 Check Exhaust

13
 Clean Spills

14
 Measure Uptake Rate

Listen to the sound of the

nebulizer it should hiss! And
there should be a change in
pitch when sample is aspirated

15
 Low Uptake Rate

 

6 mL/min 3.4 mL/min

16
 Mini-Vacuum Cleaner

Lint or sample particle blockages

Lint or sample particle blockages

17
 Aspirate D.I. Water

distilled
water Rinse regularly and at
the end of a set of
samples +/- 200ml

18
 Recommended Procedures at End of the day

1. Aspirate distilled water for a few minutes before shutting off

flame (200 mL)

3. Allow burner to cool

5. Remove burner and clean by running tap water through it

7. Dry burner by shaking

9. Pour half a litre of water into spray chamber, through burner

socket

11. Replace burner

13. Empty waste vessel

19
 Periodic Maintenance Tasks

• Check condition of O rings in atomization system

• Check condition of the impact bead

• Clean burner

• Clean windows in sample compartment

20
 Check O-rings

Lubricate with water or Non-

ionic detergent ie Triton X-100
ONLY

21
 Clean Burner

Keep slot clean and polished

22
 Clean Windows

YES, YOU MUST DO THE WINDOWS!

23
 SIPS Operation

24
 SIPS Pump Maintenance

• Clean Rollers and Band regularly

– Use Alcohol and tissue

• Clean and rinse T piece

• Replace capillary tubing if blocked

• Wipe down case with damp cloth

• Ensure adequate ventilation around control unit

25
 The SIPS pump head

26
 Autosampler Maintenance

Check interconnecting tubing

and probe capillary in good
condition
Clean any spills

27
 Capillary Connections

Capillary to Nebulizer

Connection Free of Dead

Volume

Capillary to
Autosampler or
SIPS

28
 Vapor Generation System Maintenance

Clean up spills
Check pump tubing
Check pump Rollers

29
 Stretched Tubing

30
 Pump Roller Clips

31
Check for Gas Leaks
 Overnight Leak Check

5:00 PM 8:00 AM

Watch the PRIMARY Gauge!

33
 Grease O-rings

DO NOT use grease on “O” rings in spray chamber

Hi-
Vacuu
m
Grease

TOO MUCH
GREASE!!!!!!!!!!!!

34
 AA Maintenance Guide

Useful reference guide to maintenance provided on the

CD
See document called
AA Maintenance Guide

35
 Summary

• Check gas supplies

• Check exhaust system
• Check uptake rate
• Clean dirty components & spills
• Maintain accessories
• Empty waste container
• Aspirate 200 mL D.I. water after analysis

36
 How do you prove that an instrument is working ok?

Validation

37