Ma. Nanny et Ra. Minear, USE OF LANTHANIDE SHIFT-REAGENTS WITH P-31 FT-NMR SPECTROSCOPY TO ANALYZE CONCENTRATED LAKE-WATER SAMPLES, Environmental science & technology, 28(8), 1994, pp. 1521-1527
Several lanthanide shift reagents (LSR) were synthesized from praseody
mium, europium, dysprosium, and terbium using ethylenediaminetetraacet
ic acid, trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid, and
diethylenetriaminepentaacetic acid for the purpose of separating overl
apping P-31 FT-NMR spectral signals of dissolved organic phosphorus co
mpounds present in concentrated lake-water samples. The extent of chan
ge in signal position and line width of several known phosphorus compo
unds dissolved in pure water was examined as a function of solution pH
and the molar ratio of LSR to phosphorus. Praseodymium ethylenediamin
etetraacetate (PrEDTA) was determined to be the most effective LSR. Co
ncentrated lake-water samples mixed with PrEDTA were examined with P-3
1 FT-NMR. The use. of PrEDTA provided separation of overlapping signal
s, indicated that phosphorus compounds were becoming isolated from the
solution environment during sample concentration, enhanced the sensit
ivity of certain signals by possibly acting as a T1 relaxation agent,
and did not precipitate in the presence of a high concentration of hum
ic and fulvic acids.