海水养殖废水中氨氮测定方法的影响因素及改进研究石芳永

石芳永1,张延青1,徐　洋1,刘　鹰2,刘明星2(1,266033;2,266071):采用酒石酸钾钠溶液—氢氧化钠溶液作为屏蔽剂排除海水中钙、镁离子对测定的干扰,将纳氏试剂比色法用于对海水养殖废水中氨氮的测定,最佳测定条件为200g/L的氢氧化钠溶液用量2.5mL,纳氏试剂1.5mL,显色时间25min。该方法对盐度为10～32的海水可以直接测定,氨氮质量浓度在0.01～0.04mg/L符合比尔定律,检出限为0.01mg/L,加标回收率在91%～108%。:海水养殖;氨氮测定;次溴酸盐氧化法;纳氏试剂比色法:X832　　　:A　　　:1007-9580(2009)02-20-05:2009-03-20;:2009-04-09:“863”(2006AA100305);(30671620);(2006BAD09A03):(1983—),,,。E-mail:[e-mail]:(1964—),,,,。E-mail:[e-mail]　　[1]。。[2],,、。,、,,。,。,[3],,。1　1.1(GB17378.4—1998),0～0.080mg/L。0.64mg/L,,[2],:(mg/L)(/):0/0,0.02/0.047,0.04/0.111,0.08/0.210,0.12/0.315,0.16/0.405,0.20/0.522,0.24/0.638,0.32/0.840,0.40/0.892,0.48/0.884,0.64/1.166。1。1　Fig.1　Scatterplotofconcentrationandabsorbance,0.32mg/L、0.840,:y=0.3803x+0.0006,R2=0.9995;,。,,NH3-N,,NH3-N,。20《》2009362　,0.6mg/L,,,。,,,NH3-N,。1.2　NH3-N,。750mL,NH3-N(10μg/mL)0.5mL,0.1%0,0.5,1.5,2.5,5.0,25.0,50.0mL,(),,(1)。1,NH3-N,。,,。[4]。1　Tab.1　Amountofglucosesolutionwithdifferentabsorbance(mL)0.00.51.52.55.025.050.00.3360.3510.3360.1230.3030.2360.7501.3　,。50mL,5mL,30min5mL,5min1mL,15min,0.245。(ε=3.9×104),100μg/L,0.280,[4]。,50mL,2,1,2KBr-KBrO31,。2。2　Tab.2　Resultsofdilutiontestfordifferentoxidantsused(mL)510152025303540455010.2000.3450.4610.4450.4100.3710.3550.3200.2900.24520.1400.2430.3400.4480.5610.6600.7300.7510.7200.690　　2,2,25mL50mL,0.245,0.410,。,,115mL,235mL,1,15mLNH3-N;2,35mLNH3-N。,:NH3-NNO2-N,,NO2-N,。,,—NH3-N,;NH3-N,。。15mL,NH3-N,NH3-N,;15mL,NH3-N21《》2009362　,,NH3-N,NH3-N,。,[4],,。1.4　,,。[5][1]。0.45μm,,。4℃、-20℃3,,—,,,4℃。2.9%,,;,,,。2　2.1UNICO723;,500g/L,10.0mg/L,[6];200g/L;。2.2　2.2.1　校准曲线　10.0mg/L0.00,0.10,0.20,0.60,1.00,1.40,2.00mL150mL,,500g/L1mL,。1100mL,500g/L1mL,200g/LNaOH2.5mL,。,,1.5mL,,25min,,420nm5cm,。2.2.2　样品测定和计算　0.45μm50mL,,500g/L1mL,。。ρ=m/V:ρ—,mg/L;m—,μg;V—,mL。2.3　2.3.1　吸收曲线　10.0mg/L1.0mL50mL,。5cm350～470nm。[7],370nm,,420nm。2.3.2　水样盐度对氢氧化钠溶液用量的影响　、。,。1L0,5,10,15,20,25,32(),200g/L0.0,0.5,1.0,1.5,2.0,2.5,3.0,3.5,4.0mL。10.0mg/L1.0mL50mL,,,3。3　、Tab.3　Therelationshipsbetweenabsorbanceandsodiumhydroxideamount,salinity00.2050.2060.20650.2070.2090.2080.207100.2090.2070.2080.2080.2080.2060.207150.2080.2070.2080.2080.2070.2080.207200.2060.2080.2080.2080.2080.2060.206250.2070.2070.2080.2100.2080.208320.2090.2060.2080.2070.2100.00.51.01.52.02.53.03.54.0V(mL)22《》2009362　　　,、。,,,,。10,50mL,200g/L1mL,,[6],1mL2mL,。10,。4,50mL200g/L2.5mL,10,2.5mL。2.3.3　氢氧化钠溶液用量的影响　。32200g/L,2,2.5mL,,2.5mL。2.3.4　显色剂用量的选择　,。2.0mL50mL,32,0.5、0.8、1.0、1.2、1.5、2.02.5mL,,3。,1.0～2.5mL,1.5mL。2　Fig.2　Effectsofsodiumhydroxideamountonabsorbance2.3.5　显色时间　,(32),,4。4,25min,,,2h。3　Fig.3　Effectsofreagentamountonabsorbance4　Fig　4　Stabilitytestofsamplecolor2.3.6　线性范围、检出限、精密度及加标回收率　[3],0.01～0.40mg/L,10b0.019～0.022,a≤0.005,R20.9990～0.9996。0.01mg/L,0.40mg/L。10,9%,91%～108%,、。,—,,,,、、,[8]。3　,、,NH3-N,。—,,、,,23《》2009362　。、,、,、。◆[1],,,.[J].,2005(4);35,41.[2]《》.[M].:,1991:265-270.[3],,.[J].,200315(3):23-25.[4].NH4-N[J].,1991(5):73-75.[5],,.[J].,2007(5):117-118.[6]《》.[M].4.:,2002:279-281.[7]《》.()[M].:,1990:133-140.[8],.———[J].,200536(7):34-35.StudyontheinfluencingfactorsandimprovementofNH3-NdeterminationinmariculturewaterSHIFang-yong1,ZHANGYan-qing1,XUYang1,LIUYing2,LIUMing-xing2(1QingdaoTechnologicalUniversity,Qingdao2660003,China;2InstituteofOceanology,ChineseAcademyofSciences,Qingdao266071,China)Abstract:HypobromiteOxidationprocesscannotapplytoNH3-Ndeterminationinmariculturewater,thisismainlybecausethehighNH3-Nconcentrationisoutoftherangeofstandardcurve.Furthermere,theconcen-trationoforganicmattersandreducingsubstancesaretoohigh,NH3-Ncannotachievecompleteoxidationduetothelackofoxidant.Thetestsindicatedthat,withpotassiumsodiumtartrateandsodiumhydroxidesolutionasshieldingagentforeliminatingtheinterferenceofcalciumandmagnesiumions,HypobromiteOxidationpros-esscanbeusedtodetermineNH3-N.Thebestconditionsinthelabwereasfollows:thedosageofsodiumhy-droxidesolutionwas2.5mLatitsconcentrationof200g/L,thedosageofNessler'sReagentwas1.5mL,andthebestcolor-developingtimewas25minutes.Thismethodissuitableforseawaterwithsalinityat10～32.Bear'slawisobeyedforNH3-Nintherangeof0.01～0.04mg/L,thedetectionlimitis0.01mg/Landtherecoveryofstandardadditionisintherangeof91%～108%.Thismethodisconvenient,goodsensitivity,col-orfastandstable,anditfullymeetstherequirementsofNH3-Ndeterminationinmariculturewater.Keywords:mariculturewater,NH3-Ndetermination,HypobromiteOxidationprocess,nessler'sreagentcolori-metry(上接第28页)Anovelfries-countingmethodbasedonmachinevisiontechniqueZHUCong-rong(CollegeofMechanicalEngineering,ZhejiangOceanUniversity,Zhoushan316004,China)Abstract:Anovelfries-countingmethodbasedonmachinevisiontechniqueisputforwardinthispaper.Thegrey-scalemapsoffriesareobtained,andtherelationshipbetweenthepixelnumbersoffriesinthesemapsandthenumbersoffries,namedcountingequation,issetupwithdatafittingmethod.Thenumberoffriesiscoun-tedwiththefittedcountingequation.AcommercialCCDcameraandself-compiledimageprocessingsoftwareareusedtosetupanexperimentalfries-countingsystem,andthecountingprocessisdescribed.Theexperimen-talresultsindicatethattheac