Method / Description ICP-AES
Generally:
Determination of the main and trace elements with atomic emission spectroscopy with inductively coupled plasma (ICP)-AES.
An atomic emission spectrometer with inductively coupled plasma contains a high frequency generator, a plasma torch, a high resolution spectrometer and a computer to control the instruments and the data output. An induction coil, fed by a high frequency generator, generates a strong, oscillating magnetic field at the IC-plasma torch (inductively, coupled). Argon is supplied to the burner, wich is lit with the help of a tesla coil. The high frequency generator with induction coil, supplies the energy for the ionization work in the plasma. The energy stands in direct relation to plasma-density and temperature. The plasma torch is connected with an atomizer (sprayer) system. The sample is transported to the plasma with the help of an argon-carrier-gas. The flowing argon gas generates a tunnel inside the plasma, where the sample is evaporated and stimulated (at high temperatures and longer residence time). The spectrometer receives the radiation from the observation zone above the live plasma zone. In the spectrometer the light is spectrally separated. The light intensities are measured sequentially (monochromator) or simultaneously (polychromator). All standards are diluted in a matrix similar to the sample-matrix.
1. Porewater samples
2. Gashydrat samples and other samples with lower concentration
3. Acid digestions of sediments (main elements)
4. Acid digestions of sediments (trace elements)
1. Porewater samples
ICP-AES: JY 170 ULTRACE
Sprayer: Cross-Flow-sprayer
Reagents: HCl suprapur 30%
NaCl p.a.
NaCl-St.Solution: 163,3475g NaCl p.a./1000ml
standard solution (in water). from Spex:
Ca | 10000mg/l |
K | 10000mg/l |
Mg | 10000mg/l |
Sr | 1000mg/l |
Mn | 1000mg/l |
B | 1000mg/l |
Ba | 1000mg/l |
Li | 1000mg/l |
Si | 10000mg/l |
Fe | 10000mg/l |
Y | 10000mg/l |
Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modus:
Element | Wave- length | STD 0 | STD 0 | STD1 | STD1 | STD2 | STD2 | STD3 | STD3 | HV | Mess.- mode |
| nm | mg/l | mmol/l | mg/l | mmol/l | mg/l | mmol/l | mg/l | mmol/l | V | |
K | 766.490 | 0 | 0 | 100 | 2.558 | 200 | 5.115 | 500 | 12.79 | 993 | sequential |
Ca | 317.933 | 0 | 0 | 100 | 2.495 | 200 | 4.99 | 500 | 12.48 | 455 | simultaneous |
Mg | 383.231 | 0 | 0 | 500 | 20.57 | 1000 | 41.14 | 2000 | 82.29 | 625 | sequential |
Na | 330.237 | | 599 | | 279.5 | | 559 | | 559 | 723 | sequential |
B | 249.773 | 0 | 0 | 1.00 | 0.0925 | 5.00 | 0.4625 | 10.0 | 0.925 | 783 | sequential |
| | mg/l | µmol/l | mg/l | µmol/l | mg/l | µmol/l | mg/l | µmol/l | | |
Sr | 407.771 | 0 | 0 | 2.00 | 22.83 | 5.00 | 57.06 | 10.0 | 114.1 | 676 | simultaneous |
Mn | 257.610 | 0 | 0 | 0.1000 | 1.82 | 0.200 | 3.64 | 0.500 | 9.1 | 903 | sequential |
Li | 670.784 | 0 | 0 | 0.100 | 14.41 | 0.200 | 28.81 | 0.500 | 72.04 | 993 | sequential |
Sil | 251.611 | 0 | 0 | 2.00 | 71.21 | 10.0 | 356 | 20.0 | 712 | 953 | sequential |
Fe | 238.204 | 0 | 0 | 0.100 | 1.791 | 0.5000 | 8.953 | 1.00 | 17.91 | 923 | sequential |
| | µg/l | nmol/l | µg/l | nmol/l | µg/l | nmol/l | µg/l | nmol/l | | |
Ba | 455.500 | 0 | 0 | 20.0 | 145.6 | 50.0 | 364.1 | 100 | 728 | 993 | sequetial |
-diluted in 100ml volumetric flask with 500µl HCl
Preparation of the sample:
On board: 3ml of the porewater sample and 30µl HCl are filled into 3ml-bottels(Zinsser), right after squeezing.
In the lab: all standards and samples are diluted in the relation 1:10 with a special solution: 3ml HCl and 1.1111ml Y-standard in 1000ml pure water.
Seawater standard (IAPSO) is measured as a control standard.
2. Gashydrat water samples or other samples with lower salinity:
ICP-AES: JY 170 ULTRACE
Sprayer: Cross-Flow-sprayer
Reagents: HCl suprapur 30%
NaCl p.a.
NaCl-St.Solution: 163,3475g NaCl p.a./1000ml which is 2795mmolNa/l
standard solution (in water). from Spex:
Ca | 10000mg/l |
K | 10000mg/l |
Mg | 10000mg/l |
Sr | 1000mg/l |
Mn | 1000mg/l |
B | 1000mg/l |
Ba | 1000mg/l |
Y | 10000mg/l |
Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modes:
Element | Wave- length | STD0 | STD0 | STD1 | STD1 | STD2 | STD2 | STD3 | STD3 | STD4 | STD4 | HV | Mess.- mode |
| nm | mg/l | µmol/l | mg/l | µmol/l | mg/l | µmol/l | mg/l | µmol/l | mg/l | µmol/l | V | |
B | 249.773 | 0 | 0 | 0.100 | 9.25 | 0.500 | 46.249 | 2.00 | 184.997 | 5.00 | 462.492 | 903 | sequential |
Mn | 257.610 | 0 | 0 | 0.0005 | 0.0910 | 0.020 | 0.3640 | 0.100 | 1.820 | 0.500 | 9.101 | 903 | sequential |
Ca | 317.933 | 0 | 0 | 5.00 | 124.76 | 20.0 | 499.03 | 50.0 | 1247.6 | 10.0 | 2495.1 | 455 | simultaneous |
Na | 330.237 | 0 | 0 | | 13975 | | 27950 | | 559000 | | 83850 | 903 | sequential |
Mg | 383.231 | 0 | 0 | 20.0 | 822.88 | 50.0 | 2057.2 | 200 | 8228.8 | 500 | 20571 | 625 | sequential |
Sr | 407.771 | 0 | 0 | 0.050 | 0.5706 | 0.200 | 2.2826 | 1.00 | 11.413 | 5.00 | 57.065 | 676 | simultaneous |
K | 766.490 | 0 | 0 | 10.0 | 255.8 | 20.0 | 511.5 | 50.0 | 1.2788 | 100 | 2.5577 | 993 | sequential |
| | µg/l | nmol/l | µg/l | nmol/l | µg/l | nmol/l | µg/l | nmol/l | µg/l | nmol/l | | |
Ba | 455.500 | 0 | 0 | 5.00 | 36.409 | 20 | 145.63 | 200 | 1456.3 | 500 | 3640.9 | 993 | sequential |
-diluted in 100ml volumetric flask with 500µl HCl
Preparation of the sample:
On board: 3ml of the porewater sample and 30µl HCl are filled into 3ml-bottels(Zinsser), right after squeezing.
In the lab: all standards and samples are diluted in the relation 1:10 with a special solution: 3ml HCl and 1.1111ml Y-standard in 1000ml pure water.
Seawater standard (IAPSO) is measured as a control standard.
3. Acid digestions of sediments (main elements):
read the method of the acid digestion under: description acid-digestion
ICP-AES: JY 170 ULTRACE
Sprayer: Cross-Flow-sprayer
Reagents: HNO3 suprapur 60%
standard solution(in water). from Spex:
Ca | 10000mg/l |
K | 10000mg/l |
Mg | 10000mg/l |
Sr | 1000mg/l |
Mn | 1000mg/l |
Li | 1000mg/l |
Ba | 1000mg/l |
Al | 10000mg/l |
Ti | 1000mg/l |
Fe | 10000mg/l |
Na | 10000mg/l |
Y | 10000mg/l |
Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modus:
Element | Wave- length | STD0 | STD1 | STD2 | STD3 | STD4 | STD5 | HV | Mess.- mode |
| nm | mg/l | mg/l | mg/l | mg/l | mg/l | mg/l | V | |
Fe | 238.204 | 0 | 100 | 200 | 500 | 1000 | 50 | 676 | simultaneous |
Mn | 257.610 | 0 | 1.00 | 2.00 | 10.0 | 50.0 | | 872 | simultaneous |
Mg | 383.231 | 0 | 50.0 | 100 | 200 | 500 | 10.0 | 625 | sequential |
Al | 308.215 | 0 | 100 | 200 | 500 | 1000 | | 455 | simultaneous |
Ca | 317.933 | 0 | 10.0 | 20.0 | 50.0 | 200 | | 455 | simultaneous |
Na | 330.237 | 0 | 50.0 | 100 | 200 | 500 | | 923 | sequential |
Sr | 407.771 | 0 | 0.500 | 1.00 | 5.00 | 10.0 | | 676 | simultaneous |
Ba | 455.500 | 0 | 0.500 | 1.00 | 5.00 | 20.0 | | 383 | sequential |
Li | 670.784 | 0 | 0.10 | 0.200 | 0.500 | 1.00 | | 993 | sequential |
K | 766.490 | 0 | 25.0 | 50.0 | 200 | 500 | | 993 | sequential |
Ti | 334.941 | 0 | 1.00 | 2.00 | 5.00 | 10.0 | | 583 | sequential |
-diluted in 100ml volumetric flask with 3ml HNO3
Preparation of the sample:
All standards and samples are diluted in the relation 1:10 with a special solution: 3ml HNO3 and 1.1111ml Y-standard in 1000ml pure water.
A sediment standard (MAG) is measured as a control standard.
4. Acid digestions of sediments (trace elements):
read the method of the acid digestion under: description acid-digestion
ICP-AES: JY 170 ULTRACE
Sprayer: Meinhard-sprayer
Reagents: HNO3 suprapur 60%
standard solution (in water). from Spex:
Cr | 1000mg/l |
Mo | 1000mg/l |
Ni | 1000mg/l |
Zn | 1000mg/l |
Cu | 1000mg/l |
V | 1000mg/l |
Y | 10000mg/l |
l
Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modus:
Element | Wave- length | STD0 | STD1 | STD2 | STD3 | STD4 | STD5 | HV | Measuring- mode |
| nm | µg/l | µg/l | µg/l | µg/l | µg/l | µg/l | V | |
Cr | 284.325 | 0 | 10.0 | 50.0 | 100 | 500 | 1000 | 853 | sequential |
Mo | 202.030 | 0 | 10.0 | 20.0 | 50.0 | 200 | | 903 | sequential |
Ni | 231.604 | 0 | 10.0 | 50.0 | 100 | 500 | 1000 | 993 | sequential |
Zn | 213.856 | 0 | 10.0 | 50.0 | 100 | 500 | | 753 | sequential |
Cu | 324.754 | 0 | 20.0 | 50.0 | 100 | 500 | | 993 | sequential |
V | 290.882 | 0 | 10.0 | 50.0 | 100 | 500 | | 853 | sequential |
-diluted in 100ml volumetric flask with 3ml HNO3
Preparation of the sample:
The Y-srandard is diluted in the relation 1:10.
5ml of all standards and all samples are mixed with 50µl of the diluted Y-standard before they are measured.
A sediment standard (MAG) is measured as a control standard.
5. Detection- and quantification limits:
Element | Conz. | Pore- water | Pore- water | Gashydrat- water | Gashydrat- water | Acid digestion of sediment (main elements) | Acid digestion of sediment (main elements) | Acid degestion of sediment (trace elements) | Acid degestion of sediment (trace elements) |
| | DL | QL | DL | QL | DL | QL | DL | QL |
Ca | mg/l | 2.00 | 6.00 | 0.60 | 2.00 | 0.05 | 0.20 | | |
Mg | mg/l | 6.00 | 20.0 | 2.00 | 6.00 | 0.15 | 0.50 | | |
K | mg/l | 4.00 | 12.0 | 2.00 | 6.00 | 0.60 | 2.00 | | |
Fe | mg/l | | | | | 0.20 | 0.50 | | |
Al | mg/l | | | | | 0.80 | 2.50 | | |
Ti | mg/l | | | | | 1.50 | 5.00 | | |
Sr | µg/l | 25.0 | 80.0 | 1.50 | 4.00 | 0.30 | 0.80 | | |
Ba | µg/l | 6.00 | 20.0 | 0.60 | 2.00 | 3.00 | 10.0 | | |
Li | µg/l | 25.0 | 80.0 | | | 2.00 | 6.00 | | |
Mn | µg/l | 5.00 | 15.0 | 5.00 | 15.0 | 8.00 | 30.0 | | |
B | µg/l | 40.0 | 150 | 10.0 | 30.0 | | | | |
Mo | µg/l | | | | | | | 5.00 | 20.0 |
Zn | µg/l | | | | | | | 6.00 | 20.0 |
Ni | µg/l | | | | | | | 15.0 | 50.0 |
Cr | µg/l | | | | | | | 5.00 | 1.0 |
V | µg/l | | | | | | | 5.00 | 15.0 |
Cu | µg/l | | | | | | | 6.00 | 20.0 |
DL=Detection limit
QL=Quantification limit