AAS dan AES Analisis Instrumen I

OVERVIEW

Atomic Absorption Spectroscopy

(AAS) adalah suatu tehnik
analisis untuk menetapkan
konsentrasi suatu unsur
(logam) dalam suatu sampel.

AAS pertama kali

dikembangkan oleh
Sir Alan Walsh pada
tahun 1950
AAS dan AES Analisis Instrumen I

OVERVIEW
Proses dalam AAS melibatkan 2 langkah, yaitu:

1. Atomisasi sampel

2. Absorpsi radiasi dari sumber sinar oleh atom bebas.

• Sampel, biasanya berupa cairan atau padatan, terlebih dahulu

diubah menjadi atom lebih dulu, oleh perangkat atomisasi
(berupa nyala atau tungku grafit).
• Selama proses absorpsi sinar UV-Vis, atom bebas akan
mengalami transisi elektronik dari ground state ke exited
stated.
• Banyaknya atom yang mengalami transisi elektronik
bergantung pada temperatur, dirumuskan dalam Persamaan
Boltzmann:
AAS dan AES Analisis Instrumen I

OVERVIEW

Atom (logam) yang bisa dianalisis menggunakan AAS

AAS dan AES Analisis Instrumen I

OVERVIEW
Keuntungan AAS:
• Specific
• Sensitivity
• Low Cost Analysis
• Low Capital Cost (?)
• Can Analyze Many Samples in Short Time for Screening
of a Single Analyte Metal.

Kerugian AAS:
• Single Element at a Time.
• Requires more Set-up time between Elements.
• Not the preferred method for screening samples for
numerous elemental content

~ Arie BS ~
AAS dan AES Analisis Instrumen I

ABSORPSI VS EMISI
Pengukuran spektroskopik secara umum dibedakan dalam 2 golongan:
absorpsi dan emisi

Transisi elektronik terjadi bila suatu elektron

berpindah dari tingkat energi satu ke tingkat energi
yang lain.

ABSORPSI
Jika elektron menyerap (mengabsorpsi) foton
sehingga elektron berpindah dari orbital dengan
tingkat energi rendah ke tingkat energi tinggi.
EMISI
Jika elektron berpindah dari tingkat energi tinggi
ke tingkat energi rendah sehingga foton
dipancarkan sebanding dengan perbedaan
tingkat energi tsb.
~ Arie BS ~
AAS dan AES Analisis Instrumen I

ABSORPSI VS EMISI

ABSORPSI

EMISI

~ Arie BS ~
AAS dan AES Analisis Instrumen I

SPEKTRA EMISI ATOMIK

~ Arie BS ~
AAS dan AES Analisis Instrumen I

SPEKTRA EMISI ATOMIK

• Atomic spectra: single external

electron

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI
AAS terdiri dari 5 komponen utama.
Komponen-komponen ini dikontrol oleh piranti lunak komputer.

Single-Beam Atomic
Absorption Spectrometer

Double-Beam Atomic
Absorption Spectrometer

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

Hollow Cathode Lamp Electrodeless Discharege Lamp

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

Proses emisi pada Hollow Cathode Lamp

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

Tungsten Anode Analyte Hollow Cathode

Ne or Ar
Glass shield

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

~ Arie BS ~
AAS dan AES Analisis Instrumen I

Atomization
• Flame
• Electrothermal
– Graphite furnace
• Hydride
– As, Sb, Sn, Se, Bi, and Pb
• Cold-vapor
– Hg (ambient temperature vapor
pressure)

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

~ Arie BS ~
AAS dan AES Analisis Instrumen I

FLAME ATOMIZATION

Nebulization - Conversion of the liquid

sample to a fine spray.

Desolvation - Solid atoms are mixed with

the gaseous fuel.

Volatilization - Solid atoms are converted

to a vapor in the flame.

There are three types of particles that

exist in the flame:
1) Atoms
2) Ions
3) Molecules

~ Arie BS ~
AAS dan AES Analisis Instrumen I

FLAME ATOMIZATION

~ Arie BS ~
AAS dan AES Analisis Instrumen I

FLAME ATOMIZATION
Nebulizer

SAMPLE
AEROSOL

~ Arie BS ~
AAS dan AES Analisis Instrumen I

FLAME ATOMIZATION

~ Arie BS ~
AAS dan AES Analisis Instrumen I

FLAME ATOMIZATION
Fuel / Oxidant Temperature
H-C≡C-H acetylene / air 2100 °C – 2400 °C (most common)
acetylene / N2O 2600 °C – 2800 °C
acetylene / O2 3050 °C – 3150 °C
• Pemilihan jenis nyala bergantung pada temperatut penguapan atom yang
dianalisis.

Pengaruh ketinggian burner

terhadap absorbansi

~ Arie BS ~
AAS dan AES Analisis Instrumen I

ELECTROTHERMAL ATOMIZATION (ETA)

Graphite Furnace
• Sampel cair dialirkan pada tabung
silindris grafit yang dilapisi bahan yang
mencegah sampel terserap pada tabung.

Step Temperature Time

Drying 50° - 150°C ~ 60 s
Ashing 150° - 600°C ~ 60 s
Atomization 2000° - 3000°C ~5s

~ Arie BS ~
AAS dan AES Analisis Instrumen I

ELECTROTHERMAL ATOMIZATION (ETA)

Hydride Generation AAS (HGAAS)

~ Arie BS ~
AAS dan AES Analisis Instrumen I

PERBANDINGAN FLAME DAN FURNACE AAS

• Flame lebih sederhana

• Furnace lebih sensitif
• Furnace memiliki lebih banyak interferensi
• Furnace lebih sedikit membutuhkan
sampel
• Perangkat Furnace lebih mahal

~ Arie BS ~
AAS dan AES Analisis Instrumen I

PERBANDINGAN FLAME DAN FURNACE AAS

Limit deteksi (ng/mL)
Element AAS Flame AAS Electrothermal • Accuracy:
Al 30 0.005 – Relative error of flame AA
As 100 0.02 is ~1–2%
Ca 1 0.02 – Can be lowered with
Cd 1 0.0001
special precautions
Cr 3 0.01
– Electrothermal atomization
Cu 2 0.002
has 5–10 times higher
Fe 5 0.005
Hg 500 0.1
error than flame AA
Mg 0.1 0.00002
Mn 2 0.0002
Mo 30 0.005
Na 2 0.0002
Ni 5 0.02
Pb 10 0.002
Sn 20 0.1
V 20 0.1
Zn 2 0.00005

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

Dengan mengubah sudut grating akan menghasilkan

fokus pada panjang gelombang yang berbeda.

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

Pemilihan panjang gelombang bergantung pada:

- Unsur yang dianalisis
- Sensitivitas
- Limit deteksi

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

~ Arie BS ~
AAS dan AES Analisis Instrumen I

INSTRUMENTASI

~ Arie BS ~
AAS dan AES Analisis Instrumen I

APLIKASI
Preparasi Sampel
Timbang ± 2,5 g sampel, masukkan ke dalam gelas beker.
Tambahkan 25 mL HNO3 pekat, tutup dengan gelas arloji,
CARA BASAH didihkan selama 30 – 45 menit untuk mengoksidasi senyawa
organik. Dinginkan larutan secara perlahan, tambahkan 10
mL HClO4 70%. Didihkan kembali hingga larutan menjadi
jernih.

Timbang ± 2,5 g sampel, masukkan ke dalam porselin.

Panaskan dalam oven hingga suhu 550 oC selama 4 jam.
CARA KERING Dinginkan, tambahkan 10 mL HCl 3 N. Tutup dengan gelas
arloji, didihkan selama 10 menit. Dinginkan, saring dan
masukkan ke dalam labu takar 100 mL, encerkan hingga
batas dengan air bebas ion.

~ Arie BS ~
AAS dan AES Analisis Instrumen I

APLIKASI
Metode Seri Standar (Standar eksternal)
1. Ukur absorbansi dari seri larutan standar yang telah
diketahui konsentrasinya.
2. Buat kurva hubungan antara absorbansi versus
konsentrasi (Kurva Kalibrasi).
3. Dengan metode analisis regresi linier, turunkan
persamaan regresi linier, y = mx + c

Hasil plotting ke persamaan regresi:

Konsentrasi Cr = 3,45 ppm
~ Arie BS ~
AAS dan AES Analisis Instrumen I

APLIKASI
Metode Adisi Standar
1. Siapka dua buah larutan sampel yang identik.
2. Tambahkan sejumlah volume tertentu larutan standar
pada salah satu larutan sampel.
3. Ukur absorbansi masing-masing larutan.
4. Hitung konsentrasi analit dengan persamaan berikut.

~ Arie BS ~
AAS dan AES Analisis Instrumen I

APLIKASI

Kegunaan AAS:

1. Analisis Klinik Analisis logam dalam cairan biologis (darah, urine)

2. Analisis Lingkungan Monitoring lingkungan, memantau berbagai undur di

sungai, perairan laut, air minum, udara, minyak, dan
minuman (anggur/wine, bir, jus buah)
3. Farmasi Dalam proses industri sering digunakan katalis
(biasanya logam), yang seringkali terikut dalam
produk akhir. Dengan AAS, unsur tsb dapat
ditetapkan.
4. Industri Melakukan pengecekan apakah bahan baku
mengandung logam berat yang bersifat toksik.

5. Pertambangan Menetapkan kandungan logam dalam batuan.

AAS dan AES Analisis Instrumen I

INTERFERENSI DALAM AAS

• Ada 2 jenis interferensi yang terjadi dalam AAS:
A) Spectral Interferences
B) Chemical Interferences
A. Spectral Interferences
• garis emisi dari spesies lain overlap/sangat dekat dengan garis absorpsi
analit, sehingga pemisahan dengan monokromator sulit dilakukan.
• Sources of Spectral Interference
1. Overlapping AA or AE lines
• Jenis interferensi ini jarang terjadi.
• Selisih antar garis spektra harus < 0.01 nm untuk bisa menimbulkan
interferensi ini.
• Dapat diatasi dengan metode adisi standar.
2. Background interference
• Disebabkan oleh scattering sumber sinar atau adanya absorpsi molekular.
• Background interference menghsilkan peningkatan sinyal output.
• Background correction digunakan untuk mengeliminasi interferensi jenis
ini.
AAS dan AES Analisis Instrumen I

INTERFERENSI DALAM AAS

B. Chemical interferences
Hasil dari berbagai proses yang terjadi selama atomisasi result from
various processes occurring during atomization yang mengubah
karakteristik absorpsi analit.
1. Pembentukan senyawa dengan volatilitas rendah
• Anion yg terdapat dalam flame atau furnace dapat mebentuk senyawa
dengan volatilitas rendah dengan kation analit.
• metode yg biasa digunakan untuk mengatasi masalah ini adalah
dengan menambahkan release agents atau protective agents pada
matriks sampel.
Release Agent - bereaksi dengan zat yang menyebabkan interferensi dalam
matriks sampel.
Protective Agent - bereaksi dengan analit tetapi menghasilkan senyawa
volatil.
AAS dan AES Analisis Instrumen I

INTERFERENSI DALAM AAS

B. Chemical interferences
2. Kesetimbangan dissosiasi
• melibatkan pembentukan dan dissosiasi senyawa oksida logam dasi
sampel.
• Contoh: MO ↔ M + O
M(OH)2 ↔ M + 2OH
• Pergeseran kesetimbangan ke arah oksida logam akan menghasilkan
penurunan absorpsi radiasi oleh analit logam.
• Proses ini sangat tergantung pada kondisi nyala (bahan bakar,
temperatur nyala)
AAS dan AES Analisis Instrumen I

INTERFERENSI DALAM AAS

C. Chemical interferences
3. Ionisasi
• Pembentukan ion logam (kation) dalam nyala.
• Ionisasi logam akan menyebabkan peningkatan temperatur.
• dapat diminimalkan dengan penambahan ionization suppressant pada
matriks sampel yg akan menghasilkan konsentrasi elektron tinggi
dalam nyala yg dapat menekan pembentukan ion logam.
Guidelines for
Trouble Shooting
and Maintenance of
AA Systems

AA Maintenance & Trouble Shooting Feb. 2014

Common AA Problems Reported by Customers
Sensitivity:
• Sensitivity is worse than it used to be
• I have a new application and I can’t get the sensitivity I need
• How come I can’t get the instrument to meet published detection limits?

Precision
• Sensitivity is acceptable but precision is terrible

High noise
• Can get the “right answers”, but very noisy signal – this is also giving bad precision.

Accuracy
• Instrument does not give the “right” results.

Poor Sample Throughput

• The instrument throughput needs to improve
• Burner blocks too quickly

AA Maintenance & Trouble Shooting Feb. 2014

2
 Causes of Poor Flame AA Sensitivity

Flame Blocked nebulizer

atomization Dirty burner (reducing pathlength)
system
Broken impact bead
Poor optimization
Optimization Optics setting – using right wavelength/slit?
Wrong burner type
Interferences
High blank level
Standard
(& sample) Standards prepared correctly?
preparation
Samples prepared correctly? – ionization suppressant
Low acetylene gas pressure – acetone carryover

AA Maintenance & Trouble Shooting Feb. 2014

3
 Causes of Poor Flame AA Precision
Dirty burner (“ragged”
Flame
atomization
flame) Impact bead
system
adjustment Impact bead
condition
Not fitting mixing
Optimization
paddles Burner
alignment
Poor optimization
Standard
(& sample) High nebulizer flow rate
preparation
Gas purity
AA Maintenance & Trouble Shooting Feb. 2014

Wash-out (memory effects) 4

 Causes of High Noise in Flame AA
Dirty burner (“ragged” flame)
Flame
atomization Impact bead adjustment
system Impact bead condition
Not fitting mixing paddles
Burner alignment
Optimization Poor optimization – especially the HC lamp
Wrong lamp operating current
High nebulizer flow rate
Dirty optics
Gas purity
Standard
(& sample) Incomplete digestion – particles in solution
preparation
AA Maintenance & Trouble Shooting Feb. 2014

5
Flame Atomization System Tips

Do: Don’t:
Check optimization each analysis
Assume system is still optimized
Check/monitor the nebulizer uptake
Assume nebulizer flow rate is the same
Check/adjust the impact bead
Check the blank reading
Rinse between samples & at the end of Use a simple water blank
the run
- Rinse should match sample matrix
Clean the burner/spray chamber Wait until you have blockage before
regularly cleaning
- Inspect condition of the impact bead
Follow analytical recommendations in
“cookbook”

AA Maintenance & Trouble Shooting Feb. 2014

6
Burner Alignment Tips
Burner
• Burner position must be optimized
(vertical, horizontal & rotational
positioning)

• Use “target area” on burner alignment

card to ensure light beam runs
parallel to burner slot

Optimum viewing height for Ca

• Adjust burner height while aspirating a
standard and optimize for maximum
signal
- Optimum height varies depending on flame
chemistry

• Burner type changes path length

(for air/acetylene elements)

AA Maintenance & Trouble Shooting Feb. 2014

7
Optimization of the Nitrous Oxide/Acetylene Flame

Lean Stoichiometric Rich

Reduce acetylene flow Add extra acetylene

AA Maintenance & Trouble Shooting Feb. 2014

8
Cleaning the Atomization System

Cleaning the burner:

• Polish with metal polish like “Brasso”
- Watch the video (#4)

Cleaning the spray chamber:

• Wash in detergent solution
• Check the impact bead condition & setting
- Replace if badly pitted

Removing nebulizer blockage:

• Disassemble completely and wash in detergent
• Reassemble and test
AA Maintenance & Trouble Shooting Feb. 2014

9
Impact Bead Setting

Loosen bead securing screw

Turn external adjuster fully
clockwise
Set the bead position
• 2 critical settings
- Bead should be centred in front of
venturi
- Distance between bead & venturi
should be ~0.1mm (thickness of
sheet of paper)

Tighten adjuster to lock bead in

place

AA Maintenance & Trouble Shooting Feb. 2014

10
Flame Atomization – Rec. Settings
For most flame AA applications:
• Fit the mixing paddles
• Optimize the impact bead for best sensitivity
• Use narrow bore capillary tubing

For highest flame AA sensitivity:

• Remove mixing paddles
• Adjust impact bead further away from the nebulizer
• Use wide bore capillary tubing (highest uptake rate)

For higher TDS samples:

• Fit the mixing paddles
• Adjust impact bead ½ to 1 turn clockwise (towards nebulizer) from optimum sensitivity position
• Use wide bore capillary tubing (to reduce chance of blockage)

AA Maintenance & Trouble Shooting Feb. 2014

11
Recommended Procedures at End of the day

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

2. Allow burner to cool

3. Remove burner and clean by running water through it

4. Dry burner by shaking

5. Pour 500 mL of water into spray chamber, through burner socket

6. Replace burner

7. Empty waste vessel

AA Maintenance & Trouble Shooting Feb. 2014

12
 Flame AA Performance – Benefits
Flexibility, Ease of Use & Superior Flame Performance

Tunable performance means…

• Highest flame sensitivity:
> 0.9 Abs. for 5 mg/L Cu
• Best precision: < 0.5 % RSD
using 10 x 5 s readings
• Extended operation with
difficult samples
• No loose gas hoses and
no tools required for gas
connection
• Fast change-over to furnace
operation (manual - < 30 s)

AA Maintenance & Trouble Shooting Feb. 2014

13
 Causes of Poor Furnace AA Sensitivity
Missed injection
Furnace
workhead Aged (or damaged) tube in use
Wrong electrodes fitted
Poor optimization – esp. drying conditions
Workhead incorrectly aligned
Optimization
Optics setting – using right wavelength/slit?
No modifier (or incorrect) modifier used
Use of nitrogen as inert gas
No acid in solution
Standard High blank level
(& sample)
preparation Standards prepared & stored correctly?
Samples prepared correctly – digestion?

AA Maintenance & Trouble Shooting Feb. 2014

14
 Causes of Poor Furnace AA Precision
Missed injection
Bubble formation in syringe
Furnace
workhead
Dirty dispensing capillary
Using non-Agilent graphite tubes
Graphite components excessively worn – poor electrical contact
Wrong dispensing height
Optimization
Poor optimization – esp. drying conditions
Missing a cooldown step (esp. with platforms)
Gas purity
No acid or detergent in rinse (memory effects)
Standard
(& sample) No acid in solution
preparation Incomplete digestion – particles in solution

AA Maintenance & Trouble Shooting Feb. 2014

15
 Causes of High Noise in Furnace AA

Furnace Dirty windows in workhead

workead
Use of platforms
High background levels
High absorbance signals
Optimization
Wrong lamp operating current
Workhead incorrectly aligned
Poor optimization – especially the HC lamp
Dirty optics
Gas purity
Standard
(& sample) Incomplete digestion – particles in solution
preparation

AA Maintenance & Trouble Shooting Feb. 2014

16
Furnace AA System Tips

Do: Don’t:
Check optimization each analysis Assume system is still optimized
Check/monitor the dispensing height Assume dispensing height is the same

Ensure the rinse solution has 10 drops
conc. HNO3 + 5 drops Triton X-100
Remove residue from the dispensing
capillary
Check/monitor the graphite tube
Use a simple water rinse
Start analysis with a dirty capillary tip
Start analysis with a tube near the end

Check the blank reading of

it’s life
Clean the workhead regularly
- Inspect condition of the graphite components
Follow analytical recommendations in
“cookbook”

AA Maintenance & Trouble Shooting Feb. 2014

17
Furnace AA System Tips - Workhead Alignment
Furnace workhead
• Workhead position must be optimized
(want light beam to pass through centre of
graphite tube)
- Align lamp first (no workhead),
then place workhead in position and align

Sample Dispenser settings

• Carefully adjust injection depth – easy with the furnace camera

Light Beam Aligned

Through Center of
Graphite Tube

AA Maintenance & Trouble Shooting Feb. 2014

18
Furnace AA System Tips - Setting Injection Depth
Correct dispensing
Capillary tip must remain in contact
with solution during dispensing

Reduce dispensing height if sample

spreads due to low surface tension þ
Ensure there is no liquid on the
outside of the capillary after
Pipet tip too low!
dispensing

Ensure there is no liquid inside the

ý
capillary tip after dispensing
Pipet tip too high!

ý
Sample should remain as a drop in
the centre of the tube

AA Maintenance & Trouble Shooting Feb. 2014

19
Furnace AA System Tips – Tube Conditioning
Why condition the tubes before use?
• Helps remove residual contamination
• Gently “beds” a new tube in
- Important when determining concentrations near detection limit
- Also important with some complex matrices
• Critical when using modifiers
- Helps to build up coating inside the tube
- Improves efficiency of the modifier
• Improves reproducibility

Recommended process
• Use “Tube Condition” facility (or otherwise, fire tube 5-10 times using
either reagent blank or representative sample)
AA Maintenance & Trouble Shooting Feb. 2014

20
Furnace AA System Tips – Method Parameters
What to Check?
- Furnace parameters
• Set appropriate drying temperature and time (2-3 sec/uL of solution injected)
• Optimize ashing temperature using ashing study – use SRM optimization
• Ensure inner gas flow “off” just prior to atomization

Does the sample sizzle or

splatter during the dry stage?

• Listen for the

sound
• Use the mirror or
furnace video to monitor
the sample drying

AA Maintenance & Trouble Shooting Feb. 2014

21
Furnace AA System Tips – Method Optimization
• SRM “Wizard” automates furnace
optimization

• Optimizes absorbance as a function of

ashing and atomization temperature

• Automatically creates a method using

recommended conditions

• Reduces training requirements for new

users

Optimization
results for Pb
determination
using phosphate
modifier
AA Maintenance & Trouble Shooting Feb. 2014

22
Furnace AA System Tips – Reducing Sensitivity
May be required due to sensitivity of this technique:

• Switch to an alternate wavelength

- Select a less sensitive wavelength (if available)
• Reduce sample volume
• Use slower ramp rate to atomization
- Aim to broaden the peak during atomization
• Use low gas flow during the atomization step

AA Maintenance & Trouble Shooting Feb. 2014

23
Furnace AA System Tips – Factors Influencing Tube
Lifetimes
Graphite components excessively worn – poor electrical contact
No tube preconditioning (or always using Tube Clean)
Sample matrix
Inert gas used
• Argon gives longest life
• Nitrogen degrades tube faster due to oxygen presence
Temperature program used Type Zeeman Tube Lifetime
30 0.20
of chemical modifiers used 25
0.18

CCV Concentration ug/L

0.16

• Powerful oxidizing agents degrade tube faster 0.14

Absorbance
20 Firings Conc
0.12
Abs 2.453501
- Perchloric acid 15 CCV
CCV
209
CCV Concentration
212
512 25.4518 0.10
520 25.4837 0.08
0.1492
0.1495
CCV Abs orbance
- Perchlorates 10 CCV
CCV
215
218
527 25.3244
534 25.4040
0.1486
0.06
0.1490
CCV 221 542 25.7384 0.040.1508
- Sodium nitrate 5
CCV 224 549 25.4200 0.020.1491
CCV 225 552 25.6141 0.000.1499
0
CCV 228 559 25.7588 0.1507
0 1000 2000 3000 4000 5000
CCV 231 566 25.6141 0.1498
Number of Firings
CCV 234 574 25.7588 0.1506

AA Maintenance & Trouble Shooting Feb. 2014

24
Tips to Improve Standard Preparation
- How are they prepared?
• Ensure purchased standards are still within “Use By” date
• Use calibrated pipettes and class ‘A’ volumetric flasks for dilutions
- Periodically, check accuracy & reproducibility of your pipettes
• Use de-ionized water (Type I - conductivity > 18 Md/cm3)
- Lower grades may have contamination
• Use serial dilutions for preparing low concentrations from 1,000 ppm stock
- Please don’t do large dilutions (> 1:10,000) in 1 step

- What concentration are they?

• Low concentration standards have a finite life
- Prepare ppb (ug/L) concentration standards daily from high conc. stock
- Prepare low ppm (mg/L) concentration standards weekly

- How are they stored?

• Plastic vessels ensure better stability
• Stabilize with acid – low pH ensures better stability

AA Maintenance & Trouble Shooting Feb. 2014

25
Tips to Reduce Contamination
Contamination can come from anything that comes into
contact with your sample during storage, digestion
(dilution) and analysis
• Check reagent purity
- Always buy the best reagents
- Always check the certificate of analysis for
elevated levels
- Caution if buying in large quantities
• Worst case – can use contaminated acid for cleaning
• Ensure still within “use by” date
- Reseal immediately after use

• Other common contamination sources

- Reagent water
- Clean glassware?
- Airborne dust in the lab.
- Pipette tips
• Don’t insert pipette tips into your acids
• Use natural tips – colored tips may increase
contamination (Cu, Fe, Zn, Cd)
- Powdered gloves (esp. for Zn)

AA Maintenance & Trouble Shooting Feb. 2014

26
Tips to Improve Accuracy of Results
- Sample preparation
• Is the most appropriate digestion being used?
• Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved?
- Many digestions are only partial extracts – efficiency will vary with the sample
matrix
- Some volatile analytes may be “lost” during digestion
• Confirm by taking a solid certified reference material through your preparation and
analysis procedure

• Is the digest stable – or are you seeing any precipitates or a suspension?

• Do you see any potential contamination from either reagents or the digestion
equipment? e.g. especially with Si, B or Ca
• Include a “Reagent Blank” with every sample batch to monitor

AA Maintenance & Trouble Shooting Feb. 2014

27
Tips for Cleaning Dirty Optics

Monitor the windows regularly

- Check lamp for fingerprints
- Check sample compartment windows for build-up
of film/chemical residue

Smudges or chemical residue reduces throughput

light and increases noise

Cleaning the windows?

- Wipe clean with an optical tissue
(as you would use to clean a camera lens) Cleaning end windows
- If necessary, use optical tissue moistened with ethanol from furnace
workhead

AA Maintenance & Trouble Shooting Feb. 2014

28
Flame AA – Recommended Maintenance Schedule
Daily:
• Check the gas delivery pressures & cylinder contents (esp. acetylene)
• Check exhaust system
• Check the nebulizer uptake rate and burner condition
• Clean burner compartment & instrument
• Empty waste container

Weekly:
• Clean burner (or earlier if required)
• Disassemble flame atomization system and clean
- Check condition of O rings and impact bead (no pitting)

Monthly:
• Check windows in sample compartment (clean if necessary)

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Furnace AA – Rec. Maintenance Schedule
Daily:
• Check the gas delivery pressures & cylinder contents
• Check exhaust system
• Check condition of the graphite tube – replace as necessary
- When replacing the tube, check the condition of the electrodes
• Check dispensing capillary “free” and syringe
• Top up rinse reservoir as required
• Clean the workhead around the sample injection hole
• Empty waste container

Weekly:
• Check furnace workhead windows (clean if necessary)

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