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Marine Geochemistry - Laboratory Methods

Phosphate detection with Auto-Analyzer
method In acid solution and in the presence of molybdate-ions, ortho-phosphate forms a complex which is reduced to phosphorous-molybdenium-blue with ascorbic acid. Phosphate is detected photometrically at 880 nm using an auto-analyzer. (alternatively use Photometer method)
setup Autosampler SKALARmeasuring blockME photometerperistaltic pump
solutions  
reagent

51 mM/L ammonium-molybdate (NH4)2MoO4, 1.4 mM potassium-antimony-tartrate (C4H4KO7Sb, Merck #108092) in 1.2M H2SO4
Dissolve 10g ammonium-molybdate in pure water. Dissolve 0.46 g KSb-tartrate in approx. 20 ml pure water. Put together both solutions and fill up to approx. 500 ml with pure water. Carefully add 134 ml 49% H2SO4. Let solution cool off and fill up to 1 L.

ascorbic acid 45.4 mM/L ascorbic acid(C6H8O6) in pure water with 0.2% Levor 4 (Aerosol 22, Sigma Aldrich #A9753):
0.8g ascorbic acid is dissolved in 100 ml pure water add 200µL Levor 4. Store cool in a brown glass bottle.
standard stock 1000 ppm Phosphate Standard Merck #19898
work solution 1 mM/L (or 100 ppm) PO4
work standards 2.5 - 5 - 7.5 10 µM/L PO4 ( or 0.25 -0.5 - 0.75 - 1.0 ppm) in phosphate-free natural or artificial seawater.
analysis conditions 4cm flow-through cuvette, linear range up to approx.10 µM/L (or 1ppm) PO4
pump peristaltic pump Ismatec
detection ME flow-through Photometer with IR LED(880 nm)
recording strip chart recorder 5V
analysis time approx. 90 sec.per sample
setup scheme ME photometerreaction coilIsmatec IPC pump
pump tubes sample
air
ascorbic acid
reagent
yellow-blue
white-orange
white orange
white orange
1.52 mm I.D.
0.64 mm I.D.
0.64 mm I.D.
0.64 mm I.D.
rinse rinsing between samples with seawater (or - according to samples - diluted seawater) with 1ml/L 25% H2SO4.
At dilutions greater than 1:10 rinse with 0.4% Levor 4 solution
tips + tricks All bottles and vials should be glass. Do not use plastic unless absolutely necessary (pump tubes). Rinse all glassware with 1.5% HCl followed by pure water prior to use in order to reduce phosphate background from detergents
If needed, the length of the final reaction coils may be increased in order to get higher sensitivity

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