Orthophosphate and Total P Orthophosphate reacts with ammoniummolybdate to a yellow-colored phosphorousmolybdate acid, that is reduced with ascorbic acid

in the presence of antimony to a strongly blue colored complex. This color is measured photometrically as described in Norwegian Standard (NS 4 !4". - #etermination of total phosphorous in water after digestion$dissolution of samples with potassium peroxidisulphate (%!S!O&" as described in Norwegian Standard (NS 4 !'". The method is applicable on freshwater and seawater samples, but is not applicable of for water with high organic carbon content. (aximum )-concentration is '** g ) +-,. Samples with higher concentrations ha-e to be diluted. #etection limit. , g ) +-,. Silicon and arsenic in the form of arsenate can interfere with the analysis, as these compounds also create a blue complex with molybdate PRINCIPLE Orthophosphate. /n a sulphuric acid solution ( *., mol +-," orthophosphate reacts with molybdate and antimony (Sb ///" forming a yellow-colored molybdatephosphorous complex. 0y reducing this complex by ascorbic acid a bluecolored heteropolycomplex (molybdenum blue" is formed. This coloured complex is determined spectrophotometrically at O# &&*nm. Samples with high organic carbon content need a stronger oxidation procedure. /nterference with free chlorine is eliminated by the ascorbic acid. Total-). 1omplex inorganic and organic )-compounds will be transformed to orthophosphate by addition of peroxidisulphate under acidic conditions by boiling the samples (in tefloncontainers" in an autocla-e. REAGENTS 2ll chemicals should be of )2 3uality. %!S!O&, 4!SO4, 154&O5, (N44"5(o O!444!O, %(SbO"1444O5*.'4!O, Na!S!O6'4!O, Na!1O6, %4!)O4, 41l, NaO4. 4( Sulphuric acid !!!m+ concentrated sulphuric acid (7'-7 8, density ,.&4 g m+-," is carefully diluted to '+ with d.d.d. water. The solution is stored at room temperature for , wee9. :ashing water 7'm+ of the 4( sulphuric acid is diluted to '+ with d.d.d. water. The solution may be stored at room temperature for , month. 2cid water To ,+ d.d.d. water ,*m+ 4( sulphuric acid is added. The solution is stored at room temperature for , month. 4ydrochloric acid for cleaning (,(" &*m+ conc. 4ydrochloric acid (41l, 6 8, density ,.,7 g m+ -," is diluted with d.d.d. to ,+. The solution is stored at room temperature for , year. 2scorbic acid solution (reagent 0" ,!,4g ascorbic acid (154&O5" is dissol-ed in ,***m+ d.d.d. water.

(olybdate reagent (reagent 2" !6!mg potassiumantimon(///"oxidetartrate hemihydrate (%(SbO"1444O5 ;4!O, 77.'8" is dissol-ed in ,5**m+ d.d.d. water. 6&,&m+ conc. Sulphuric acid is added while stirring and cooling. /t is important that the solution is completely cooled. Then 5g ammonium heptamolybdate ((N44"5(o O!4 44!O" is added before the solution is diluted to !***m+. The solution is stored at room temperature for ! months. The flas9 should be pac9ed in 2l-foil in order to pre-ent photo-degradation. )hosphate stoc9 solution, !**mg ) +-,. *,& &* *,***!g dried (,*'<1 for ! hours" potassium dihydrogen phosphate (%4 !)O4" is dissol-ed in d.d.d. water and diluted to ,***m+. The solution is stored at room temperature for , year. )hosphate wor9ing solution, ,* mg ) +-,. '*,**m+ of the ) stoc9 solution and ,m+ chloroform (141l 6" is diluted with d.d.d. water to ,***m+ in a -olumetric flas9. The solution is stored at room temperature for , year. )hosphate wor9ing solution, , mg ) +-,. '*,**m+ of the ) wor9ing solution ,* mg ) + -, is diluted with d.d.d. water to '**m+ in a -olumetric flas9. The solution cannot be stored. Standard solutions 1onc. of =inal g ) +-, m+ wor9ing -olume, solution m+ ! ! , ,*** ' ' , ,*** ,* ,* , ,*** !' !' , ,*** '* '* , ,*** ' ' , ,*** ,** ,* ,* ,*** !'* !' ,* ,*** 6'* 6' ,* ,*** '** '* ,* ,*** The calibration solution are added 7m+ sulphuric acid, 4(, prior to dilution and ,*m+ sulphuric acid. 4(, after dilution. The calibration solutions are not oxidised. The solutions are transferred to ,+ plastic bottles. The solution is stored at room temperature for 5 months. 1ontrol solutions Control stock solution, approx. 50 mg P L ! #issol-e *,&*'7g disodium-adenosin-'-monophosphate with 5 crystal water (1,*4,!N'Na!O )54!O" in d.d.d. water. 2dd ,*m+ sulphuric acid, 4(, and dilute with d.d.d. to ,+ in -olumetric flas9. The solution is stored at room temperature for , year. Control solutions The control stoc9 solution is diluted ,.,* and is used to ma9e three control solutions. ,**.,***m+ that after addition of ,*m+ sulphuric acid gi-es 4&' g ) +-,. ,*.,***m+ that after addition of ,*m+ sulphuric acid gi-es 4&,' g ) +-,. ,.,***m+ that after addition of ,*m+ sulphuric acid gi-es 4,&' g ) +-,. The solution is stored at room temperature for , year.

Samples are conser-ed by adding ,m+ 4( sulphuric acid to ,**m+ sample. The analysis should be performed within 6 months.

"#I$ATI"N Sha9e sample bottle before transferring !*m+ sample to a !*m+ scintillication -ial. 2dd *,!**,*4g potassiumperoxodisulphate. /nclude three blind samples. Transfer !*m+ d.d.d. to the scintillication -ials, add *,!*m+ 4( sulphuric acid and *,!* *,*4g potassiumperoxodisulphate. The control samples with 4, 4* and 4** g ) +-, are also oxidised. $ETER%INATI"N ) is determined in two calibration ranges. * > ,** g ) +-, and ,** > '**g ) +-,. The analysis start with the calibration solutions, then ! acid waters, 6 blind samples, control samples. Then ,* and ,* samples are analysed separated by ! acid waters. ?nd the analysis with a set of calibration standards. /n the * > ,** g ) +-, the 4 and 4*g ) +-, control sample is used. /n the ,** > '** g ) +-, the 4**g ) +-, control sample is used. The limits for acceptance of the results from the control samples are as follows. 4 g ) +-, control sample. 6.* > '.* g ) +-, 4* g ) +-, control sample. 6&,' > 4,,' g ) +-, 4** g ) +-, control sample. 67* > 4,* g ) +-, 44 measurements of a potassiumhydrogenphosphate solution of 4 @g ) +-, ga-e mean -alue. 6.&5 *., @g ) +-, (, S#". 1orrespondingly 4* measurements of standard solution of 4* @g ) +-, ga-e mean -alue. 4**.6 !.7 @g ) +-, (, S#".

&igur' !( Standard solutions with blue phosphate molybdate complex.