Al Atomic Number 13
Matrix 0.1% Nitric Acid Atomizer Pyrolytic Platform
Furnace Operating Conditions
Step No. Temp.
(°C) Time (sec) Gas Flow (L/min) Gas Type CommandRead 1 300 30 3.0 Normal No 2 300 60 3.0 Normal No 3 1000 10 3.0 Normal No 4 1000 10 3.0 Normal No 5 1000 2 0 Normal No 6 2700 1.1 0 Normal Yes 7 2700 2 0 Normal Yes 8 2700 2 3.0 Normal No 9 40 2 3.0 Normal No Instrument Parameters Lamp Current 10 mA Spectral Bandwidth 0.5 nm Wavelength 396.2 nm Maximum Absorbance 2 MSR% 100%
Alternative Wavelengths Spectral Bandwidths
(nm) (nm) 309.3 0.5 237.3 0.5 257.4 0.5 256.8 0.5 Performance Data
Characteristic Mass (in argon): Peak Height 2.8 pg Peak Area 12 pg Maximum Ash Temperature: 1400 °C
Typical Peak Height Response (Argon): 10 µL of 14 ng/mL gives about 0.2 Abs.
An ash step at 1000 °C may be useful in obtaining a smooth peak shape.
The 309.3 nm line gives and MSR of 88% with a MAX ABS of 0.8 and a slightly poorer sensitivity than at 396.2 nm.
As Atomic Number 33
Matrix 0.1% Nitric Acid Atomizer Pyrolytic Platform
Furnace Operating Conditions
Step No. Temp.
(°C) (sec) Time Gas Flow (L/min) Gas Type CommandRead 1 300 30 3.0 Normal No 2 300 60 3.0 Normal No 3 500 10 3.0 Normal No 4 500 10 3.0 Normal No 5 500 2 0 Normal No 6 2600 1.1 0 Normal Yes 7 2600 2 0 Normal Yes 8 2600 2 3.0 Normal No 9 40 11.8 3.0 Normal No Instrument Parameters Lamp Current 10 mA Spectral Bandwidth 0.2 nm Wavelength 193.7 nm Maximum Absorbance 0.95 MSR% 86%
Alternative Wavelengths Spectral Bandwidths
(nm) (nm)
197.2 1.0
Performance Data
Characteristic Mass (in argon): Peak Height 15 pg* Peak Area 46 pg* Maximum Ash Temperature: 1500 °C* Recommended Chemical Modifiers Palladium (10 µL of 500 µg/L) or
Palladium solution (500-2000 µg/mL) plus reducing agent such as ascorbic acid (368)
or
Nickel solution (50 µg/mL)
Typical Peak Height Response (Argon): 10 µL of 114 ng/mL gives about 0.2 Abs.
Hg Atomic Number 80 Matrix 1.0% Nitric Acid
Atomizer Pyrolytic Platform
Furnace Operating Conditions
Step No. Temp.
(°C) Time (sec) Gas Flow (L/min) Gas Type CommandRead 1 300 30 3.0 Normal No 2 300 60 3.0 Normal No 3 500 10 3.0 Normal No 4 500 10 3.0 Normal No 5 500 2 0 Normal No 6 2600 1.1 0 Normal Yes 7 2600 2 0 Normal Yes 8 2600 2 3.0 Normal No 9 40 12.8 3.0 Normal No Instrument Parameters Lamp Current 4 mA Spectral Bandwidth 0.5 nm Wavelength 253.7 nm Maximum Absorbance 0.35 MSR% 69% Performance Data
Characteristic Mass (in argon): Peak Height 150 pg* Peak Area 250 pg* Maximum Ash Temperature: 500 °C* Recommended Chemical Modifiers Pd solution (1000 µg/mL)* or
Palladium solution (500-2000 µg/mL) plus reducing agent such as ascorbic acid (368) or
Diammonium sulphide in excess.
Typical Peak Height Response (Argon): 10 µL of 505 ng/mL gives about 0.2 Abs.
*Pd modifier used to obtain these results.
The palladium modifier is pre-injected, and taken to step 3. The palladium modifier permits the use of a higher ashing temperature and enhances the signal.
The diammonium sulphide modifier stabilizes the mercury signal.
Fresh dilutions of mercury standards should be prepared each day as the standards are not very stable.
Pb Atomic Number 82
Matrix 0.1% Nitric Acid Atomizer Pyrolytic Platform
Furnace Operating Conditions
Step No. Temp.
(°C) (sec) Time Gas Flow (L/min) Gas Type CommandRead 1 300 30 3.0 Normal No 2 300 60 3.0 Normal No 3 500 10 3.0 Normal No 4 500 10 3.0 Normal No 5 500 2 0 Normal No 6 2400 1 0 Normal Yes 7 2400 2 0 Normal Yes 8 2400 2 3.0 Normal No 9 40 11.8 3.0 Normal No Instrument Parameters Lamp Current 5 mA Spectral Bandwidth 0.5 nm Wavelength 283.3 nm Maximum Absorbance 1.4 MSR% 92%
Alternative Wavelengths Spectral Bandwidths
(nm) (nm)
217.0 1.0
261.4 0.5
Performance Data
Characteristic Mass (in argon): Peak Height 5 pg* Peak Area 15 pg* Maximum Ash Temperature: 600 °C* Recommended Chemical Modifiers
Ammonium dihydrogen orthophosphate (5 mg/mL)* or Orthophosphoric acid (1000 µg/mL) or
EDTA, citrate, oxalate (0.5 – 1% v/v) – See Chapter One or Palladium solution (500-2000 µg/mL) plus reducing agent such as ascorbic acid (368).
Typical Peak Height Response (Argon): 10 µL of 25 ng/mL gives about 0.2 Abs.
*Ammonium phosphate modifier used to obtain these results.
Phosphate chemical modifiers permit the use of a higher ashing temperature and stabilize the lead signal. The use of EDTA, citrate or oxalate stabilizes the lead allowing it to atomize at a lower temperature than does a nitrate or chloride matrix. The palladium chemical modifier permits the use of a higher ashing temperature.
Lead is a common contaminant in reagents and it is essential that a representative blank is measured before proceeding with the analytical program.
The atomization temperature can be altered by chemical modifiers. The chemical matrix plays an important role in determining optimum ash and atomizing conditions. It is
Sn Atomic Number 50 Matrix 0.1% Nitric Acid
Atomizer Pyrolytic Platform
Furnace Operating Conditions
Step No. Temp.
(°C) Time (sec) Gas Flow (L/min) Gas Type CommandRead 1 300 30 3.0 Normal No 2 300 60 3.0 Normal No 3 500 10 3.0 Normal No 4 500 10 3.0 Normal No 5 500 2 0 Normal No 6 2900 1.2 0 Normal Yes 7 2900 1.0 0 Normal Yes 8 2900 1.0 3.0 Normal No 9 40 14.3 3.0 Normal No Instrument Parameters Lamp Current 7 mA Spectral Bandwidth 0.5 nm Wavelength 286.3 nm Maximum Absorbance 1.6 MSR% 93%
Alternative Wavelengths Spectral Bandwidths
(nm) (nm)
235.5 0.5
300.9 0.5
266.1 0.5
Performance Data
Characteristic Mass (in argon): Peak Height 12 pg* Peak Area 60 pg* Maximum Ash Temperature: 800 °C* Recommended Chemical Modifiers Palladium solution (5 µL of 100 µg/mL)* or
Palladium solution (500-2000 µg/mL) plus reducing agent such as ascorbic acid (368).
Typical Peak Height Response (Argon): 10 µL of 60 ng/mL gives about 0.2 Abs.*
* Palladium modifier used to obtain these results. The use of palladium as the chemical modifier permits the use of higher ashing temperatures and enhances the signal. The addition of diammonium hydrogen citrate
(0.1% solution) to a tin (II) chloride solution also stabilizes the tin in solution and facilitates production of a single atomization peak.
Other complexing agents have also been used, among these are trisodium citrate and EDTA.
Chemical modification of the sample is necessary when analyzing tin in sodium chloride matrices.
5. Standard and Sample Preparation
Analysts must recognize that the graphite furnace technique demands a
particularly high standard of care in all activities which affect the accuracy and precision of the analytical result. Scrupulous cleanliness is essential in all
laboratory procedures. Standards and samples must be meticulously prepared and carefully handled. Ideally, the laboratory should be air-conditioned and dust free, preferably draught free as well. Unless the laboratory has been correctly prepared, satisfactory results may never be obtained with microanalytical techniques using graphite tube atomizers.
Strict precautions must be taken to avoid contamination of apparatus, and even though laboratory ware is stored under ideal conditions, it should be thoroughly rewashed before use (see 'Apparatus' below). Strict care should also be taken to avoid contamination of all reagents and distilled water. Ideally, reagents should be entirely free of the element of interest, but this is obviously impossible for all analyte elements in all reagents (see also 'Blank Solutions', 'Water', 'Reagents').