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Muchidzidzo ichi, imwe nzira yakagadziridzwa yekutemerwa panguva imwe chete yezvinoputika phenols, cyanides, anionic surfactants uye ammonia nitrogen mumvura yekunwa uchishandisa inoyerera analyzer.Sampuli dzakatanga kunyungudutswa pa145°C.Iyo phenol mu distillate inobva yaita nebasic ferricyanide uye 4-aminoantipyrine kuti iite red complex, iyo inopimwa colorimetrically pa505 nm.Iyo cyanide iri mu distillate inobva yasangana ne chloramine T kuita cyanochloride, iyo inobva yaita blue complex ine pyridinecarboxylic acid, iyo inopimwa colorimetrically pa630 nm.Anionic surfactants inobata nebasic methylene blue kuita komboni inotorwa nechloroform yogezwa neacidic methylene blue kubvisa zvinhu zvinovhiringa.Mishonga yebhuruu muchloroform yakatemwa colorimetrically pa660 nm.Munzvimbo ine alkaline ine wavelength ye660 nm, ammonia inopindirana ne salicylate uye chlorine mu dichloroisocyanuric acid kuita indophenol blue pa 37 °C.Pahuwandu hwehuwandu hwemhepo inopisa uye cyanides muhuwandu hwe 2-100 µg / l, kuenzanisa kwemaitiro kwakasiyana kwaiva 0.75-6.10% uye 0.36-5.41%, zvichienderana, uye maitiro ekudzorera aiva 96.2-103.6% uye 96.0-102.4% .%.Linear coefficient yekubatanidza ≥ 0.9999, miganhu yekuona 1.2 µg/L uye 0.9 µg/L.Relative standard deviations aive 0.27–4.86% uye 0.33–5.39%, uye kudzoreredzwa kwaive 93.7–107.0% uye 94.4–101.7%.Pahuwandu hwehuwandu hweanionic surfactants uye ammonia nitrogen 10 ~ 1000 μg / l.Linear coefficients yekubatanidza yaive 0.9995 uye 0.9999, miganhu yekuona yaive 10.7 µg/l uye 7.3 µg/l, zvichiteerana.Pakanga pasina misiyano yenhamba kana ichienzaniswa neyenyika chiyero nzira.Iyo nzira inochengetedza nguva nekuedza, ine yakaderera yekuona muganho, yakakwirira kurongeka uye kurongeka, kushoma kusvibiswa, uye inonyanya kukodzera kuongororwa uye kutsunga kwehukuru vhoriyamu samples.
Volatile phenols, cyanides, anionic surfactants uye ammonium nitrogen1 zviratidzo zve organoleptic, muviri uye metalloid zvinhu mumvura yekunwa.Phenolic makomisheni akakosha emakemikari ekuvaka zvidhinha kune akawanda maapplication, asi phenol nemahomologues ayo ane muchetura uye anonetsa ku biodegrade.Iwo anoburitswa panguva dzakawanda maindasitiri maitiro uye ave akajairika kusvibisa kwezvakatipoteredza2,3.Yakanyanya chepfu phenolic zvinhu zvinogona kunyudzwa mumuviri kuburikidza neganda uye nhengo dzekufema.Vazhinji vavo vanorasikirwa nehuturu hwavo panguva yedetoxification process mushure mekupinda mumuviri wemunhu, vozobuda muweti.Nekudaro, kana simba remuviri rekubvisa detoxification rakapfuura, zvikamu zvakawandisa zvinogona kuungana mumitezo yakasiyana-siyana uye matishu, zvichitungamira muchetura usingaperi, kutemwa nemusoro, mapundu, kuputika kweganda, kufunganya kwepfungwa, kupererwa neropa, uye zviratidzo zvakasiyana zvetsinga 4, 5, 6,7.Cyanide inokuvadza zvakanyanya, asi yakapararira mune zvakasikwa.Zvokudya zvakawanda uye zvirimwa zvine cyanide, inogona kugadzirwa nemamwe mabhakitiriya, fungi kana algae8,9.Muzvigadzirwa zvekugezesa zvakaita seshamposi uye kugeza muviri, anionic surfactants anowanzo shandiswa kufambisa kuchenesa nekuti vanopa zvigadzirwa izvi nemhando yepamusoro yelather uye furo inotsvakwa nevatengi.Nekudaro, akawanda ma surfactants anogona kutsamwisa ganda10,11.Mvura yekunwa, pasi pevhu, pamusoro pemvura uye tsvina ine nitrogen muchimiro chemahara ammonia (NH3) uye ammonium munyu (NH4+), inozivikanwa seammoniacal nitrogen (NH3-N).Zvigadzirwa zvekuora zve nitrogen-ine organic matter mumvura yetsvina yemumba netupukanana zvinonyanya kubva mumvura yetsvina yemaindasitiri senge coking uye synthetic ammonia, inoumba chikamu cheammoniacal nitrogen mumvura12,13,14.Nzira dzakawanda, kusanganisira spectrophotometry15,16,17, chromatography18,19,20,21 uye jekiseni rekuyerera15,22,23,24 inogona kushandiswa kuyera izvi zvinosvibisa izvi mumvura.Kuenzaniswa nedzimwe nzira, spectrophotometry ndiyo inonyanya kufarirwa1.Ichi chidzidzo chakashandisa mana maviri-channel mamodule kuti panguva imwe chete aongorore volatile phenols, cyanides, anionic surfactants, uye sulfides.
An AA500 inoramba ichiyerera analyzer (SEAL, Germany), SL252 electronic balance (Shanghai Mingqiao Electronic Instrument Factory, China), uye Milli-Q ultrapure mvura mita (Merck Millipore, USA) yakashandiswa.Makemikari ese akashandiswa mubasa iri aive egiredhi rekuongorora, uye mvura yakasvibiswa yakashandiswa mukuedzwa kwese.Hydrochloric acid, sulfuric acid, phosphoric acid, boric acid, chloroform, ethanol, sodium tetraborate, isonicotinic acid uye 4-aminoantipyrine yakatengwa kubva kuSinopharm Chemical Reagent Co., Ltd. (China).Triton X-100, sodium hydroxide uye potassium chloride zvakatengwa kubva kuTianjin Damao Chemical Reagent Factory (China).Potassium ferricyanide, sodium nitroprusside, sodium salicylate uye N, N-dimethylformamide yakapiwa neTianjin Tianli Chemical Reagent Co., Ltd. (China).Potassium dihydrogen phosphate, disodium hydrogen phosphate, pyrazolone uye methylene blue trihydrate yakatengwa kubva kuTianjin Kemiou Chemical Reagent Co., Ltd. (China).Trisodium citrate dihydrate, polyoxyethylene lauryl ether uye sodium dichloroisocyanurate yakatengwa kubva kuShanghai Aladdin Biochemical Technology Co., Ltd. (China).Mishonga yakajairika yemaphenols, macyanides, anionic surfactants, uye aqueous ammonia nitrogen yakatengwa kubva kuChina Institute of Metrology.
Distillation Reagent: Dilute 160 ml yephosphoric acid kusvika 1000 ml nemvura yakasvibiswa.Reserve buffer: Weresa 9 g ye boric acid, 5 g ye sodium hydroxide uye 10 g ye potassium chloride uye wedzera 1000 ml nemvura yakasvibiswa.Absorption Reagent (inovandudzwa vhiki nevhiki): Nyatsoyera 200 ml stock buffer, wedzera 1 ml 50% Triton X-100 (v/v, Triton X-100/ethanol) uye shandisa mushure mekusefa kuburikidza ne0.45 µm sefa membrane.Potassium ferricyanide (inovandudzwa svondo rega rega): Weresa 0.15 g ye potassium ferricyanide woinyungudutsa mu200 ml ye reserve buffer, wedzera 1 ml ye50% Triton X-100, sefa ne 0.45 µm sefa membrane usati washandisa.4-Aminoantipyrine (inovandudzwa vhiki nevhiki): Huremu 0.2 g ye4-aminoantipyrine uye inonyungudika mu200 ml ye stock buffer, wedzera 1 ml ye50% Triton X-100, sefa nepakati pe 0.45 µm sefa membrane.
Reagent ye distillation: volatile phenol.Mushonga webuffer: Weresa 3 g potassium dihydrogen phosphate, 15 g disodium hydrogen phosphate uye 3 g trisodium citrate dihydrate wodzikinura kusvika pa1000 ml nemvura ine deionized.Wobva wawedzera 2 ml ye50% Triton X-100.Chloramine T: Wema 0,2 g yechloramine T uye wedzera kusvika 200 ml nemvura yakasvibiswa.Chromogenic reagent: Chromogenic reagent A: Kunyungudutsa zvachose 1.5 g yepyrazolone mu 20 ml yeN, N-dimethylformamide.Mugadziri B: Dissolve 3.5 g ye hisonicotinic acid uye 6 ml ye5 M NaOH mu 100 ml yemvura yakasvibiswa.Sanganisa Mugadziri A uye Mugadziri B usati washandisa, gadzirisa pH kusvika 7.0 neNaOH mhinduro kana HCl mhinduro, wozodzikisa kusvika ku200 ml nemvura ine deionized uye sefa yekushandisa gare gare.
Buffer solution: Dissolve 10 g sodium tetraborate uye 2 g sodium hydroxide mumvura ine deionized uye diluted kusvika 1000 ml.0.025% methylene blue solution: Dissolve 0.05 g yemethylene blue trihydrate mumvura yakasvibiswa uye gadzira kusvika ku200 ml.Methylene blue stock buffer (inovandudzwa zuva nezuva): dilute 20 ml ye0.025% methylene blue solution kusvika 100 ml ine stock buffer.Endesa kune inoparadzanisa funnel, geza ne 20 ml ye chloroform, bvisa chloroform yakashandiswa uye ugeze nekloroform itsva kusvikira ruvara rutsvuku rwe chloroform layer rwanyangarika (kazhinji katatu), wozosefa.Basic Methylene Blue: Dilute 60 ml yakasefa methylene blue stock solution kune 200 ml stock solution, wedzera 20 ml ethanol, sanganisa zvakanaka uye degas.Acid methylene blue: Wedzera 2 ml ye0.025% methylene blue solution kune inenge 150 ml yemvura yakasvibiswa, wedzera 1.0 ml ye1% H2SO4 uye wozoderedza kusvika ku200 ml nemvura yakasvibiswa.Zvadaro wobva wawedzera 80 ml ethanol, sanganisa zvakanaka uye degas.
20% polyoxyethylene lauryl ether mhinduro: Yeresa 20 g ye polyoxyethylene lauryl ether uye dilue kusvika ku1000 ml nemvura yakasvibiswa.Buffer: Weresa 20 g ye trisodium citrate, dilue kusvika pa500 ml nemvura yakasvibiswa uye wowedzera 1.0 ml ye20% polyoxyethylene lauryl ether.Sodium salicylate solution (inovandudzwa vhiki nevhiki): Wera 20 g ye sodium salicylate uye 0.5 g ye potassium ferricyanide nitrite uye inonyunguduka mu 500 ml yemvura yakasvibiswa.Sodium dichloroisocyanurate solution (inovandudzwa vhiki nevhiki): Weresa 10 g ye sodium hydroxide uye 1.5 g ye sodium dichloroisocyanurate uye uzvinyungudise mu 500 ml yemvura yakasvibiswa.
Volatile phenol uye cyanide zviyero zvakagadzirirwa semhinduro dze0 µg/l, 2 µg/l, 5 µg/l, 10 µg/l, 25 µg/l, 50 µg/l, 75 µg/l uye 100 µg/l, uchishandisa. 0.01 M sodium hydroxide solution.Anionic surfactant uye ammonia nitrogen chiyero chakagadzirirwa uchishandisa mvura yakasvibiswa 0 µg/L, 10 µg/L, 50 µg/L, 100 µg/L, 250 µg/L, 500 µg/L, 750 µg00 mc/l uye 1g/l. .mhinduro.
Tanga kutonhora kutenderera tangi, ipapo (mukurongeka) vhura komputa, sampler uye simba kune iyo AA500 host, tarisa kuti pombi yakabatana nemazvo, isa mhepo hose muvharuvhu yemhepo, vhara iyo yekumanikidza ndiro yepombi peristaltic, isa reagent pombi mumvura yakachena pakati.Mhanyai software, shandisai inoenderana chiteshi hwindo uye tarisa kana mapombi ekubatanidza akabatana zvakachengeteka uye kana paine mapundu kana kudonha kwemhepo.Kana pasina kuvuza, tsvaga reagent yakakodzera.Mushure meiyo yekutanga yehwindo yechiteshi ichigadzikana, sarudza uye mhanyisa yakatsanangurwa nzira faira yekutsvaga uye kuongororwa.Mamiriro ezviridzwa anoratidzwa muTafura 1.
Mune iyi otomatiki nzira yekugadzirisa phenol uye cyanide, samples dzinotanga kunyungudutswa pa145 ° C.Iyo phenol mu distillate inobva yaita nebasic ferricyanide uye 4-aminoantipyrine kuti iite red complex, iyo inopimwa colorimetrically pa505 nm.Iyo cyanide iri mu distillate inobva yasangana ne chloramine T kuita cyanochloride, inoumba blue complex ine pyridinecarboxylic acid, iyo inopimwa colorimetrically pa630 nm.Anionic surfactants inopindirana neiyo basic methylene bhuruu kugadzira makomisheni ayo anotorwa nechloroform uye anoparadzaniswa nechikamu chinoparadzanisa.Chikamu chechloroform chakazogezwa neacidic methylene bhuruu kubvisa zvinhu zvinokanganisa uye kuparadzaniswa zvakare muchikamu chechipiri chekuparadzanisa.Colorimetric kutsunga kwebhuruu komisheni mu chloroform pa660 nm.Kubva pakuita kweBerthelot, ammonia inopindirana ne salicylate uye chlorine mu dichloroisocyanuric acid mu alkaline medium pa 37 °C kuita indophenol blue.Sodium nitroprusside yakashandiswa sechinhu chinokonzeresa mukuita, uye ruvara rwakazobuda rwakayerwa pa660 nm.Nheyo yeiyi nzira inoratidzwa muMufananidzo 1.
Schematic dhayagiramu yekuenderera mberi sampling nzira yekutemerwa kweanoputika phenols, cyanides, anionic surfactants uye ammoniacal nitrogen.
Iko kusanganiswa kwepenols uye cyanides kubva ku2 kusvika ku100 µg / l, mutsara wekugadzirisa coefficient 1.000, regression equation y = (3.888331E + 005) x + (9.938599E + 003).Iyo corelation coefficient ye cyanide i1.000 uye regression equation ndeye y = (3.551656E + 005) x + (9.951319E + 003).Anionic surfactant ine mutsara wakanaka wekutsamira pahuwandu hweammonia nitrogen muhuwandu hwe10-1000 µg/L.Iyo corelation coefficients yeanionic surfactants uye ammonia nitrogen yaive 0.9995 uye 0.9999, zvichiteerana.Regression equations: y = (2.181170E + 004) x + (1.144847E + 004) uye y = (2.375085E + 004) x + (9.631056E + 003), maererano.Sampu yekudzora yakaramba ichiyerwa 11 nguva, uye muganho wekuonekwa kweiyo nzira yakakamurwa ne3 yakajairwa kutsauka kweiyo sampu yekudzora pamateru eyakajairwa curve.Miganho yekuona yemhepo inopisa phenols, cyanides, anionic surfactants, uye ammonia nitrogen yaive 1.2 µg/l, 0.9 µg/l, 10.7 µg/l, uye 7.3 µg/l, zvichiteerana.Muganho wekuona wakadzikira pane nzira yenyika, ona Tafura 2 yeruzivo.
Wedzera yakakwira, yepakati, uye yakaderera mwero mhinduro kumasampuli emvura asina maronda evanoongorora.Intraday uye yepakati kupora uye kurongeka kwakaverengerwa mushure mezviyero zvinomwe zvakatevedzana.Sezvinoratidzwa muTebhurari 3, intraday uye intraday volatile phenol extractions yaiva 98.0-103.6% uye 96.2-102.0%, pamwe chete, pamwe nekutsauka kwemaitiro e0.75-2.80% uye 1. 27-6.10%.The intraday uye interday cyanide kupora aiva 101.0-102.0% uye 96.0-102.4%, ukuwo, uye hama mwero kutsauka aiva 0.36-2.26% uye 2.36-5.41%, ukuwo.Pamusoro pezvo, kutorwa kweanionic surfactants intraday uye yepakati pemazuva aive 94.3-107.0% uye 93.7-101.6%, zvichiteerana, ine mwero wakatsauka we0.27-0.96% uye 4.44-4.86%.Pakupedzisira, intra- uye yepakati-yemazuva ammonia nitrogen kudzoreredza yaive 98.0-101.7% uye 94.4-97.8%, zvichiteerana, ine mwero kutsauka kwe0.33-3.13% uye 4.45-5.39%, zvichiteerana.sezvinoratidzwa muTable 3.
Nzira dzinoverengeka dzekuyedza, kusanganisira spectrophotometry15,16,17 uye chromatography25,26, inogona kushandiswa kuyera iyo ina inosvibisa mumvura.Chemical spectrophotometry inzira ichangobva kuongororwa yekuona izvi zvinosvibisa, izvo zvinodiwa nemitemo yenyika 27, 28, 29, 30, 31. Inoda matanho akadai se distillation uye kubviswa, zvichiita kuti iite nguva yakareba nekusakwana kwekunzwa uye kunyatso.Zvakanaka, zvakaipa zvakarurama.Kushandiswa kwakapararira kwemakemikari ane organic kunogona kuunza njodzi kune hutano kune vanoedza.Kunyange zvazvo chromatography inokurumidza, iri nyore, inoshanda, uye ine miganho yekuona yakaderera, haigoni kuona makomisheni mana panguva imwe chete.Nekudaro, zvisiri-equilibrium dynamic mamiriro anoshandiswa mukuongorora kemikari uchishandisa inoenderera kuyerera spectrophotometry, iyo inoenderana nekuenderera kuyerera kwegasi panguva yekuyerera kwemhinduro yemuenzaniso, kuwedzera reagents muchiyero chakakodzera uye kutevedzana uchipedzisa kuita kuburikidza nekusanganisa loop. uye kuiona mu spectrophotometer, yakambobvisa mabhuru emhepo.Nekuda kwekuti maitiro ekutsvaga ari otomatiki, masampuli anodirwa uye anodzoserwa pamhepo munzvimbo yakavharwa.Iyo nzira inovandudza zvakanyanya kushanda kwekushanda, inowedzera kuderedza nguva yekuona, inorerutsa mashandiro, inoderedza reagent kusvibiswa, inowedzera sensitivity uye yekuona muganho weiyo nzira.
Iyo anionic surfactant uye ammonia nitrogen zvakasanganisirwa mune yakasanganiswa bvunzo chigadzirwa pakusangana kwe250 µg/L.Shandisa iyo yakajairwa chinhu kushandura inovhuvhuta phenol uye cyanide kune inoyedzwa chinhu pachikamu che10 µg/L.Pakuongorora uye kuona, nzira yenyika uye nzira iyi yakashandiswa (6 parallel experiments).Mhedzisiro yenzira mbiri idzi dzakaenzaniswa uchishandisa yakazvimirira t-bvunzo.Sezvinoratidzwa muTable 4, pakanga pasina musiyano mukuru pakati penzira mbiri (P> 0.05).
Ichi chidzidzo chakashandisa chinoramba chichiyerera analyzer yekuongorora panguva imwe chete uye kuonekwa kwemhepo inopisa phenols, cyanides, anionic surfactants uye ammonia nitrogen.Mhedzisiro yebvunzo inoratidza kuti vhoriyamu yemuenzaniso inoshandiswa neinoenderera inoyerera analyzer yakaderera pane yenyika standard nzira.Iyo ine zvakare yakaderera yekuona miganhu, inoshandisa 80% mashoma reagents, inoda kushoma yekugadzirisa nguva yemasampuli ega, uye inoshandisa zvakanyanya kushoma carcinogenic chloroform.Kugadziriswa kwepamhepo kunosanganiswa uye otomatiki.Iyo inoenderera ichiyerera inongoerekana yashuvira mareagents uye masampuli, yobva yasanganisa kuburikidza nedunhu rekusanganisa, inodziya otomatiki, inobvisa uye kuverenga ine colorimetry.Iyo yekuyedza maitiro inoitwa yakavharwa sisitimu, iyo inomhanyisa nguva yekuongorora, inoderedza kusvibiswa kwezvakatipoteredza, uye inobatsira kuve nechokwadi chekuchengetedza kwevanoedza.Matanho ekushanda akaomarara akadai semanyorero distillation uye kuburitsa hazvidiwe22,32.Nekudaro, piping yezviridzwa uye zvishongedzo zvakaomesesa, uye mhinduro dzebvunzo dzinopesvedzerwa nezvinhu zvakawanda zvinogona kukonzera kusagadzikana system nyore.Pane matanho akakosha aungatora kuti uvandudze huchokwadi hwezvawawana uye kudzivirira kuvhiringwa nekuedza kwako.(1) Iyo pH kukosha kwemhinduro kunofanirwa kuverengerwa pakusarudza volatile phenols uye cyanides.Iyo pH inofanira kunge yakatenderedza 2 isati yapinda mucoil ye distillation.Pa pH> 3, maamine anonhuwirira anogona zvakare kunyungudutswa, uye kuita ne 4-aminoantipyrine kunogona kupa kukanganisa.Zvakare pa pH> 2.5, kudzoreredza kweK3[Fe(CN)6] kunenge kuri pasi pe90%.Samples ine munyu unopfuura 10 g/l inogona kuvhara iyo distillation coil uye kukonzera matambudziko.Muchiitiko ichi, mvura yakachena inofanira kuwedzerwa kuderedza munyu wemuenzaniso33.(2) Zvinhu zvinotevera zvinogona kukanganisa kuzivikanwa kweanionic surfactants: Makemikari eCationic anogona kuumba majoini ane simba ane anionic surfactants.Migumisiro inogonawo kuva yakarerekera muhupo hwe: humic acid concentrations yakakura kudarika 20 mg/l;makomisheni ane basa repamusoro pamusoro (semuenzaniso mamwe ma surfactants) > 50 mg/l;zvinhu zvine simba rekudzikisa simba (SO32-, S2O32- uye OCl-);zvinhu zvinoumba mamorekuru ane mavara, soluble mu chloroform nechero reagent;mamwe anion inorganic (chloride, bromide uye nitrate) mumvura ine tsvina34,35.(3) Paunenge uchiverenga ammonia nitrogen, yakaderera molecular weight amines inofanirwa kuverengerwa, sezvo maitiro avo neammonia akafanana, uye mhedzisiro ichave yakakwirira.Kukanganisa kunogona kuitika kana iyo pH yemusanganiswa wekuita iri pazasi 12.6 mushure mekunge mhinduro dzese reagent dzawedzerwa.Yakanyanya acidic uye yakavharwa samples inowanzokonzera izvi.Metal ions iyo inonaya se hydroxides pahupamhi hwepamusoro inogonawo kutungamirira kukushaya kuberekazve36,37.
Mhedzisiro yacho yakaratidza kuti iyo inoenderera inoyerera yekuongorora nzira yekusimbisa panguva imwe chete yekusagadzikana kwephenols, cyanides, anionic surfactants uye ammonia nitrogen mumvura yekunwa ine mutsara wakanaka, yakaderera yekuona muganhu, kunaka kwakanaka uye kupora.Hapana misiyano yakakosha neiyo yenyika standard nzira.Iyi nzira inopa nzira inokurumidza, inonzwisisika, yakarurama uye iri nyore-kushandisa yekuongorora uye kusarudza kwenhamba yakawanda yemasampuli emvura.Inonyanya kukodzera pakuona zvikamu zvina panguva imwe chete, uye kushanda kwekuona kunovandudzwa zvikuru.
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Nguva yekutumira: Feb-22-2023