| method |
Sulfate
and chloride are detected using a HPLC system with an anion separation
column and indirect UV-detection. The eluent has a high UV adsorption
which is "diluted" by chromatographically separated ions.
Detection is performed at approximately 288nm. Chromatograms examined
by integrator or PC-integrator. |
| setup |
|
| pump
|
Thermo
Separation Products P100 |
| flow
|
2
ml/min |
| detector
|
KNAUER
variable wavelength monitor @ 288nm |
| autosampler
|
KNAUER
Autosampler 7500 |
| column
|
WESCAN
Anion-R 10 µm, 250 x 4.1 mm |
| capillary
|
UPCHURCH,
1.6x0.5 mm I.D PEEK |
| peak
integration |
KNAUER
Eurochrome 2000 software and interface box (1V integrator output to
RS 232) |
| solutions
|
|
| eluent
|
KHP
potassium-hydrogen-phtalate, 3mM, pH 6.8, methanol (p.a.) 5ml/L added
for sterilization |
|
standard
stock
|
seawater
standard (Cox & Culkin 1966) |
| work
standards |
standards
with lower concentration are prepared by diluting seawater standard
with sulfate-free artificial seawater. |
| sample
dilution |
both
samples and work standards are diluted 1 : 20 with pure water |
| retention
time |
approx.
8 min for sulfate |
| analysis
time |
approx.
10 min per sample |
| tips
+ tricks |
standards
have to be adjusted to expected concentrations. Chloride is measured
but usually only used for correction. Other anions are below detection
limit due to chloride peak tailing and 1:20 dilution necessary for
sulfate detection |