Analytical Method: Palladium in water and waste water

Instruments and Reagents:
Cat.No. 173016  Spectroquant® VIS Spectrophotometer Prove 100 or
Cat.No. 173017  Spectroquant® UV/VIS Spectrophotometer Prove 300 or
Cat.No. 173018  Spectroquant® UV/VIS Spectrophotometer Prove 600 or
Cat.No. 109751  Spectroquant® Photometer NOVA 60
Cat.No. 106268  Sodium acetate trihydrate for analysis
Cat.No. 100063  Acetic acid for analysis
Cat.No. 116754  Water for analysis
Cat.No. 820162  4.4'-Bis(dimethylamino)-thiobenzophenone (Michler's thioketone)
Cat.No. 103053  N.N-Dimethylformamide for analysis
Cat.No. 100979  Isoamylalcohol for analysis
Cat.No. 106649  Sodium sulfate water free for analysis
Cat.No. 109531  MColorpHastTM pH-indicator strips pH 0 - 6
Cat.No. 109137  Sodium hydroxide solution 1 mol/l
Cat.No. 109072  Sulfuric acid 0.5 mol/l
Cat.No. 114724  Empty round cells 16 mm with screw cap
 
Reagent 1:
Dissolve 83 g sodium acetate trihydrate about 500 ml water for analysis, adjust at the pH-meter to pH 3.0 with acetic acid and fill up to 1 l with water for analysis.
 
Reagent 2:
Dissolve 100 mg 4.4'-bis(dimethylamino)-thiobenzophenone in 100 ml N.N-dimethylformamide.
 
Reaction:
Palladium reacts with Michler's thioketone at pH 3.0 ± 0.2 under formation of a purple-red complex, which is extractable by isoamylalcohol. This reaction can be used for the extraction photometric determination of palladium.
 
Measurement range:
Method no. 133
0.05 - 1.25 mg/l Pd at cell length 10 mm and 525 nm
 
Analysis:
In an empty round cell mix 5.0 ml of the sample (weakly acidic) with 1.0 ml reagent 1 and check the pH-value with pH-indicator strips (set point pH 3.0; correction with NaOH 1 mol/l or H2SO4 0.5 mol/l resp.). After that add 0.20 ml reagent 2 as well as 5.0 ml isoamylalcohol and shake for one 1 min. Separate the organic phase, dry it by using a spatula-tipful of sodium sulfate and then determine in the photometer against a blank.
 
Interferences:
According to the literature mentioned below interfering cations are maskable by Titriplex® III.
 
Measurement:
In the photometers Prove 100, Prove 300, Prove 600, Pharo 100, Pharo 300 and NOVA 60 the method is stored.
For the measurement select method no. 133 on the instrument.
 
Literature:
Cheng, K.L. - B.L. Goydisch: Microchem. J. 10, 158 (1966)

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