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
K10000mg/l
Mg10000mg/l
Sr1000mg/l
Mn1000mg/l
B1000mg/l
Ba1000mg/l
Li1000mg/l
Si10000mg/l
Fe10000mg/l
Y10000mg/l

Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modus:

ElementWave-
length
STD 0STD 0STD1STD1STD2STD2STD3STD3HVMess.-
mode
 nmmg/lmmol/lmg/lmmol/lmg/lmmol/lmg/lmmol/lV 
K766.490001002.5582005.11550012.79993sequential
Ca317.933001002.4952004.9950012.48455simultaneous
Mg 383.2310050020.57100041.14200082.29625sequential
Na330.237 599 279.5 559 559723sequential
B249.773001.000.09255.000.462510.00.925783sequential
  mg/lµmol/lmg/lµmol/lmg/lµmol/lmg/lµmol/l  
Sr407.771002.0022.835.0057.0610.0114.1676simultaneous
Mn257.610000.10001.820.2003.640.5009.1903sequential
Li670.784000.10014.410.20028.810.50072.04993sequential
Sil251.611002.0071.2110.035620.0712953sequential
Fe238.204000.1001.7910.50008.9531.0017.91923sequential
 

 

µg/lnmol/lµg/lnmol/lµg/lnmol/lµg/lnmol/l

 

 

Ba455.5000020.0145.650.0364.1100728993sequetial

-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
K10000mg/l
Mg10000mg/l
Sr1000mg/l
Mn1000mg/l
B1000mg/l
Ba1000mg/l
Y10000mg/l

Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modes:

ElementWave-
length
STD0STD0STD1STD1STD2STD2STD3STD3STD4STD4HVMess.-
mode
 nmmg/lµmol/lmg/lµmol/lmg/lµmol/lmg/lµmol/lmg/lµmol/lV 
B249.773000.1009.250.50046.2492.00184.9975.00462.492903sequential
Mn257.610000.00050.09100.0200.36400.1001.8200.5009.101903sequential
Ca317.933005.00124.7620.0499.0350.01247.610.02495.1455simultaneous
Na330.23700 13975 27950 559000 83850903sequential
Mg383.2310020.0822.8850.02057.22008228.850020571625sequential
Sr407.771000.0500.57060.2002.28261.0011.4135.0057.065676simultaneous
K766.4900010.0255.820.0511.550.01.27881002.5577993sequential
  µg/lnmol/lµg/lnmol/lµg/lnmol/lµg/lnmol/lµg/lnmol/l  
Ba455.500005.0036.40920145.632001456.35003640.9993sequential

-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
K10000mg/l
Mg10000mg/l
Sr1000mg/l
Mn1000mg/l
Li1000mg/l
Ba1000mg/l
Al10000mg/l
Ti1000mg/l
Fe 10000mg/l
Na10000mg/l
10000mg/l

Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modus:

ElementWave-
length
STD0STD1STD2STD3STD4STD5HVMess.-
mode
 nmmg/lmg/lmg/lmg/lmg/lmg/lV 
Fe238.2040100200500100050676simultaneous
Mn257.61001.002.0010.050.0 872simultaneous
Mg383.231050.010020050010.0625sequential
Al308.21501002005001000 455simultaneous
Ca317.933010.020.050.0200 455simultaneous
Na330.237050.0100200500 923sequential
Sr407.77100.5001.005.0010.0 676simultaneous
Ba455.50000.5001.005.0020.0 383sequential
Li670.78400.100.2000.5001.00 993sequential
K766.490025.050.0200500 993sequential
Ti334.94101.002.005.0010.0 583sequential

-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
Mo1000mg/l
Ni1000mg/l
Zn1000mg/l
Cu1000mg/l
V1000mg/l
Y10000mg/l

l
Standards, wavelengths, adjustments at the photomultiplier(HV) and measuring modus:

ElementWave-
length
STD0STD1STD2STD3STD4STD5HVMeasuring-
mode
 nmµg/lµg/lµg/lµg/lµg/lµg/lV 
Cr284.325010.050.01005001000853sequential
Mo202.030010.020.050.0200 903sequential
Ni231.604010.050.01005001000993sequential
Zn213.856010.050.0100500 753sequential
Cu324.754020.050.0100500 993sequential
V290.882010.050.0100500 853sequential

-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:

ElementConz.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)

 

 

DLQLDLQLDLQLDLQL
Camg/l2.006.000.602.000.050.20

 

 

Mgmg/l6.0020.02.006.000.150.50

 

 

Kmg/l4.0012.02.006.000.602.00

 

 

Femg/l

 

 

 

 

0.200.50

 

 

Almg/l

 

 

 

 

0.802.50

 

 

Timg/l

 

 

 

 

1.505.00

 

 

Srµg/l25.080.01.504.000.300.80

 

 

Baµg/l6.0020.00.602.003.0010.0

 

 

Liµg/l25.080.0

 

 

2.006.00

 

 

Mnµg/l5.0015.05.0015.08.0030.0

 

 

Bµg/l40.015010.030.0

 

 

 

 

Moµg/l

 

 

 

 

 

 

5.0020.0
Znµg/l

 

 

 

 

 

 

6.0020.0
Niµg/l

 

 

 

 

 

 

15.050.0
Crµg/l

 

 

 

 

 

 

5.001.0
Vµg/l

 

 

 

 

 

 

5.0015.0
Cuµg/l

 

 

 

 

 

 

6.0020.0

DL=Detection limit
QL=Quantification limit

 

  • Head:

    <link mitarbeiter fb2 mg kwallmann _blank einen externen link in einem neuen>Prof. Dr. Klaus Wallmann
    Tel.: 0431-600 2287
    Fax: 0431-600 2928

    Technique /Operator

    <link de mitarbeiter fb2 mg bdomeyer _blank einen externen link in einem neuen>Bettina Domeyer
    Tel.: 0431-600 2230
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    <link de mitarbeiter fb2 mg ableyer _blank einen externen link in einem neuen>Anke Bleyer
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    <link typo3 null _blank einen externen link in einem neuen>Regina Surberg
    Tel.: 0431-600 2211
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