OR/14/067 Reagent required for silver phosphate precipitation

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Lapworth, D J, Surridge, B, Williams, P J, Heaton, T H E, and Gooddy, D C. 2014. Method for analysing phosphate 18O/16O ratios for waters with high C:P ratios. British Geological Survey Internal Report, OR/14/067.

Initial preparation

  • Dowex 1X8–200 anion exchange resin (Sigma Aldrich) Approx. 50 g per sample
  • Dax-8 resin (Supelco, Supelite) Approx. 50 g per sample
  • Methanol (Analar) For preparing and cleaning Dax-8 resin — volume needed can be estimated according to requirements
  • Hydrochloric acid (Aristar) For preparing and cleaning Dowex anion exchange resin — volume needed can be estimated according to requirements
  • Potassium Chloride (Analar) 44.73 g required to make up 1litre — Two litres needed ideally just to elute for PO4
  • Potassium phosphate (KH2PO4) used to make up a PO4 standard

Magic precipitation

  • Magnesium Chloride (MgCl2.6H20) (Analysis grade) 2 g per sample
  • Sodium Hydroxide (Analysis grade) 0.4 g per sample

Cerium precipitation

  • Acetic acid, glacial (Analar) At least 2 ml per sample
  • Nitric acid (Arsitar) At least 1 ml per sample
  • Potassium acetate (Analar) Approx. 0.49 g needed to make up 0.5 M solution for 10 samples
  • Potassium hydroxide (may be necessary for adjusting pH)
  • Cerium (III) nitrate hexahydrate (From Merck described as ‘Extra pure’) 400 mg per sample

Cation resin

  • Dowex 50W X-8 cation exchange resin (Sigma Aldrich) Approx. 4 g per sample
  • Nitric acid (Aristar) For preparing and cleaning Dowex cation exchange resin — volume needed can be estimated according to requirements

Silver phosphate precipitation

  • Silver nitrate (AgNO3) (Analar) Approx. 2.54 g required to make up solution per 10 samples
  • Ammonium nitrate (NH4NO3) (Analar) Approx. 4.3 g required to make up solution per 10 samples
  • Ammonium hydroxide (NH4OH) (Analytical grade — From Fluka described as ‘for trace analysis’) Approx. 7–8 ml required per 10 samples

Removal of residual organics from silver phosphate

  • Hydrogen peroxide (H2O2) (Analar) 0.25 ml required per sample