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2001-10-04,2001-11-23。*。GuangxiSciences2002,9(2):112～114-(-2,4--)-ChromogenicReactionofCr(Ⅵ)withDiantipyrinyl[p-(-2,4-Dinitrophenoxy-)-]PhenylMethane蒙丹军 叶龙军* 黄梅兰 苏艳华 林会松MengDanjun YeLongjun HuangMeilan SuYanhua LinHuisong(, 530227)(Dept.ofFoodEngineering,GuangxiVocational-TechnologyCollege,Mingyang,Nanning,Guangxi,530227,China) -(-2,4--)-(DApDNPPM),Cr(Ⅵ)。:485nm,1.00%DApDNPPM0.60ml,(1+4)H3PO43.00ml,0.40molL-1Mn(Ⅱ)8.00ml,85℃,8min。0.10～0.80μg/25ml,:A=1.036C(μg/25ml)-0.008,r=0.998。1.30×106Lmol-1.cm-1。Cr(Ⅵ),。 (Ⅵ) -(-2,4--)-(DApDNPPM) O614.611Abstract Diantipyrinyl[-p-(-2,4-Dinitrophenoxy-)-]phenylmethane(DApDNPPM)ispre-pared.Thebestconditionsofthechromogenicreactionofdiantipyrinyl[-p-(-2,4-dinitrophe-noxy-)-]phenylmethanewithCr(Ⅵ)aresortedoutbyorthogonaldesign.Withtheaddingsof0.60ml1.00%DApDNPPM,3.00ml(1+4)H3PO4,8.00ml0.40mol/LMn(Ⅱ)at85℃waterbathingfor8min,agoodlinearrelationisavailableintheCr(Ⅵ)concentrationrangefrom0.10to0.80μg/25ml.Thereisamaximumabsorbanceat485nm.ThelinearregressionequationisA=1.036C(μg/25ml)-0.008(r=0.998).Themolarabsorptivityis1.30×106Lmol-1.cm-1.TheproposedmethodisappliedtothedeterminationofCr(Ⅵ)inthesampleofwaterwithsatisfactoryresults.Keywords Chrome(Ⅵ),diantipyrinyl[-p-(-2,4-dinitrophenoxy-)-]phenylmethane(DApDNPPM),spectrophotometry (Ⅵ)、(Ⅴ)[1],。,。-(-2,4--)-,(Ⅵ),,。,。1 1.1 -(-2,4--)-(DApDNPPM) 0.1mol-(-2,4--)-10ml95%,0.2mol,5ml,。60℃112GuangxiSciences,Vol.9No.2,May2002DOI:10.13656/j.cnki.gxkx.2002.02.009。300ml,,。5%,。,():C,64.85(64.91);H,4.62(4.64);N,12.93(12.98)。(cm-1):1188,1069,γAr-O-Ar,γC-O;3053,γAr-H,;1542,1485,1394,γN=O,;1596,1584,1453,495,γC=C,-;1318,γC-N,;756,879,δAr-H;1651,γC=O,;2914,2820,1005,1069,γ-CH3,。,。1.2 UV1100(),1cm。()。 (Ⅵ):0.1414gK2Cr2O7,50ml。0.10μg.ml-1。 1.00%DApDNPPM(W/V):1.00gDApDNPPM,95%100ml,95%。 0.40molL-1Mn(Ⅱ):MnSO4H2O36.92g,H2SO4(1+3)1ml,500ml。 :(1+4)。 ,AR。1.3 0.50μg.ml-1Cr(Ⅵ)25ml,1.00%DApDNPPM0.60ml,(1+4)H3PO43.00ml,0.40molL-1Mn(Ⅱ)8.00ml,,。85℃8min,,,1cm485nmA,Cr(Ⅵ)。2 2.1 0.50μg(Ⅵ),,,1。485nm,。2.2 ,,H2SO4、HNO3,HCl、HAC,H3PO4。Tween20、Tween40、Tween60、Tween80、OP、SD、CTMAB。Mn(Ⅱ),Mn(Ⅱ),[2]。1 Fig.1 Absorptionspectra1 Reagentblank(Cr(Ⅵ)=0.00μg)a-gainstwater;2 Chromogenicreactionsystem(Cr(Ⅵ)=0.5μg)againstreagentblank2.3 ,,,。85℃,8min。2.4 ,0.5h1.5%,0.5h。2.5 [3] DApDNPPMCr(Ⅵ)5:DApDNPPM、Mn(II)、H3PO4、。5,:1.00%DApDNPPM2.00ml,0.60ml,3.00ml,0.20ml,1.00ml;(1+4)H3PO47.00ml,4.00ml,1.00ml,5.00ml,3.00ml;0.40molL-1Mn(Ⅱ)6.00ml,8.00ml,3.00ml,4.00ml,10.00ml;60℃,75℃,95℃,98℃,85℃;3min,5min,7min,8min,10min。L25(56),25,Cr(Ⅵ)0.50μg,。 ,,,,2～6。2～6,:1.00%DApDNPPM0.60ml;(1+4)H3PO4 3.00ml;0.40molL-1Mn(Ⅱ) 8.00ml;85℃;8min。,Cr(Ⅵ)0.50μg,A=0.515,,。113广西科学 2002年5月 第9卷第2期2 Fig.2 InfluenceofDApDNPPM(Cr(Ⅵ)=0.50μg)3 (1+4)H3PO4Fig.3 Influenceof(1+4)H3PO4(Cr(Ⅵ)=0.50μg)4 0.40molL-1Mn(Ⅱ)Fig.4 InfluenceofMn(Ⅱ)(Cr(Ⅵ)=0.50μg)5 Fig.5 Influenceoftemperature(Cr(Ⅵ)=0.50μg)6 Fig.6 Influenceofheatingtime(Cr(Ⅵ)=0.5μg)2.6 Cr(Ⅵ),Cr(Ⅵ)0.10～0.80μg(25ml)-1,A=1.036C(μg/25ml)-0.008,0.998,1.30×106Lmol-1cm-1。0.50μgCr(Ⅵ)5,(RSD)1.3%。2.7 ,0.50μgCr(Ⅵ)。,±5%,5000K+,Cl-,SO2-4,NO-,NH+4;1000Mg2+,Zn2+,Sr(Ⅲ),La(Ⅲ);500Ca2+,Ni2+,SiO2-3,F-;100Sb(Ⅲ),Hg2+,W(Ⅲ),Cr(Ⅲ);50Pb2+;10Mo(Ⅵ),Bi(Ⅲ);5Fe3+,V(V),Cu2+。。2.8 200ml,(ZnSO4.7H2O 8.0g100ml;NaOH2.4g120ml,)20ml20min,。10.00ml,。50.58μg/ml,0.56μg/ml,0.55μg/ml,0.58μg/ml,0.56μg/10ml,RSD2.4%。(Ⅵ)0.20μg/25ml,(Ⅵ)0.20μg/ml,0.19μg/ml,0.21μg/ml,0.21μg/ml,0.20μg/25ml,100%,95%,105%,105%,100%。1 , ,..,1994,14(6):5～9.2 ,,..,1993,15(3):146～148.3 ..:,1986.180～208.(:) 114GuangxiSciences,Vol.9No.2,May2002