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A cikin wannan binciken, an ƙirƙiri wata hanya don ƙayyade lokaci guda na phenols masu canzawa, cyanides, anionic surfactants da ammonia nitrogen a cikin ruwan sha ta amfani da mai nazarin kwarara.An fara distilled samfurori a 145 ° C.A phenol a cikin distillate sa'an nan ya amsa tare da asali ferricyanide da 4-aminoantipyrine don samar da wani hadadden ja, wanda aka auna launi a 505 nm.Cyanide a cikin distillate sai ya amsa da chloramine T don samar da cyanochloride, wanda ya samar da wani hadadden blue tare da pyridinecarboxylic acid, wanda aka auna da launi a 630 nm.Anionic surfactants suna amsawa tare da ainihin methylene blue don samar da wani fili wanda aka fitar da chloroform kuma an wanke shi da ruwan shuɗi na acidic methylene don cire abubuwa masu shiga tsakani.Abubuwan haɗin shuɗi a cikin chloroform an ƙaddara masu launi a 660 nm.A cikin yanayin alkaline tare da tsawon 660 nm, ammonia yana amsawa tare da salicylate da chlorine a cikin dichloroisocyanuric acid don samar da indophenol blue a 37 ° C.A yawan adadin phenols masu canzawa da cyanides a cikin kewayon 2-100 µg/l, madaidaitan daidaitattun ma'auni sun kasance 0.75-6.10% da 0.36-5.41%, bi da bi, kuma adadin dawowa ya kasance 96.2-103.6% da 96.0-102. .%.Matsakaicin daidaituwa na layi ≥ 0.9999, iyakokin ganowa 1.2 µg/L da 0.9 μg/L.Matsakaicin ma'auni na dangi shine 0.27-4.86% da 0.33-5.39%, kuma an dawo dasu sune 93.7-107.0% da 94.4-101.7%.A taro taro na anionic surfactants da ammonia nitrogen 10 ~ 1000 μg / l.Matsakaicin daidaitawar layi sune 0.9995 da 0.9999, iyakokin ganowa sune 10.7 µg/l da 7.3 μg/l, bi da bi.Babu bambance-bambancen ƙididdiga idan aka kwatanta da daidaitattun hanyar ƙasa.Hanyar tana adana lokaci da ƙoƙari, yana da ƙarancin ganowa, mafi girman daidaito da daidaito, ƙarancin gurɓatawa, kuma ya fi dacewa da bincike da ƙaddara manyan samfuran girma.
Volatile phenols, cyanides, anionic surfactants da ammonium nitrogen1 alamomi ne na organoleptic, jiki da abubuwan metalloid a cikin ruwan sha.Abubuwan da ake amfani da su na phenolic sune tushen ginin sinadarai don aikace-aikace da yawa, amma phenol da homologues suma masu guba ne kuma suna da wahala ga biodegrade.Ana fitar da su yayin tafiyar da masana'antu da yawa kuma sun zama gurɓataccen muhalli na gama gari2,3.Ana iya shigar da abubuwa phenolic masu guba a cikin jiki ta fata da gabobin numfashi.Yawancinsu suna rasa gubar su yayin aikin detoxification bayan sun shiga jikin ɗan adam, sannan su fita cikin fitsari.Duk da haka, a lokacin da jiki ta al'ada detoxification damar da aka wuce, wuce haddi abubuwa iya tara a cikin daban-daban gabobin da kyallen takarda, haifar da kullum guba, ciwon kai, kurji, fata itching, hankali damuwa, anemia, da kuma daban-daban neurological bayyanar cututtuka 4, 5, 6,7.Cyanide yana da matukar cutarwa, amma yaduwa a yanayi.Yawancin abinci da shuke-shuke sun ƙunshi cyanide, wanda wasu kwayoyin cuta, fungi ko algae8,9 za su iya samarwa.A cikin samfuran wanke-wanke irin su shamfu da wankin jiki, ana amfani da surfactants anionic sau da yawa don sauƙaƙe tsaftacewa saboda suna samar da waɗannan samfuran tare da ingantacciyar kumfa da ingancin kumfa waɗanda masu siye ke nema.Duk da haka, da yawa surfactants iya fusatar da fata10,11.Ruwan sha, ruwan ƙasa, ruwan sama da ruwan datti suna ɗauke da nitrogen a cikin nau'in ammonia kyauta (NH3) da gishirin ammonium (NH4+), wanda aka sani da ammoniacal nitrogen (NH3-N).Samfuran bazuwar kwayoyin halitta masu ɗauke da nitrogen a cikin ruwan sharar gida ta ƙananan ƙwayoyin cuta galibi suna fitowa ne daga ruwan sharar masana'antu kamar coking da ammonia na roba, waɗanda ke zama wani ɓangare na nitrogen ammoniacal a cikin ruwa12,13,14.Hanyoyi da yawa, ciki har da spectrophotometry15,16,17, chromatography18,19,20,21 da allura mai gudana15,22,23,24 ana iya amfani da su don auna waɗannan gurɓataccen ruwa guda huɗu.Idan aka kwatanta da sauran hanyoyin, spectrophotometry shine mafi mashahuri1.Wannan binciken ya yi amfani da nau'ikan tashoshi biyu-biyu don kimanta phenols masu canzawa lokaci guda, cyanides, anionic surfactants, da sulfides.
An yi amfani da AA500 mai ci gaba da kwarara mai gudana (SEAL, Jamus), ma'aunin lantarki na SL252 (Shanghai Mingqiao Electronic Instrument Factory, China), da Milli-Q ultrapure watermeter (Merck Millipore, Amurka).Dukkan sinadarai da aka yi amfani da su a cikin wannan aikin sun kasance na ƙididdiga, kuma an yi amfani da ruwan da aka lalata a duk gwaje-gwaje.Hydrochloric acid, sulfuric acid, phosphoric acid, boric acid, chloroform, ethanol, sodium tetraborate, isonicotinic acid da 4-aminoantipyrine aka saya daga Sinopharm Chemical Reagent Co., Ltd. (China).An sayi Triton X-100, sodium hydroxide da potassium chloride daga Tianjin Damao Chemical Reagent Factory (China).Potassium ferricyanide, sodium nitroprusside, sodium salicylate da N, N-dimethylformamide sun samar da Tianjin Tianli Chemical Reagent Co., Ltd. (China).Potassium dihydrogen phosphate, disodium hydrogen phosphate, pyrazolone da methylene blue trihydrate aka saya daga Tianjin Kemiou Chemical Reagent Co., Ltd. (China).Trisodium citrate dihydrate, polyoxyethylene lauryl ether da sodium dichloroisocyanurate an saya daga Shanghai Aladdin Biochemical Technology Co., Ltd. (China).Daidaitaccen mafita na phenols masu canzawa, cyanides, anionic surfactants, da ammonia nitrogen mai ruwa da tsaki an siyi su daga Cibiyar nazarin awo na kasar Sin.
Distillation Reagent: Tsarma 160 ml na phosphoric acid zuwa 1000 ml tare da deionized ruwa.Matsakaicin ajiya: Auna 9 g na boric acid, 5 g na sodium hydroxide da 10 g na potassium chloride da tsarma zuwa 1000 ml tare da ruwa mai narkewa.Reagent Absorption (sabunta mako-mako): Daidai auna 200 ml stock buffer, ƙara 1 ml 50% Triton X-100 (v/v, Triton X-100/ethanol) da amfani bayan tacewa ta hanyar 0.45 µm tace membrane.Potassium ferricyanide (sabunta mako-mako): Auna 0.15 g na potassium ferricyanide kuma narkar da shi a cikin 200 ml na ajiyar ajiya, ƙara 1 ml na 50% Triton X-100, tace ta hanyar 0.45 µm tace membrane kafin amfani.4-Aminoantipyrine (sabunta mako-mako): Auna 0.2 g na 4-aminoantipyrine kuma narkar da a cikin 200 ml na stock buffer, ƙara 1 ml na 50% Triton X-100, tace ta hanyar 0.45 µm tace membrane.
Reagent don distillation: m phenol.Maganin buffer: Auna 3 g potassium dihydrogen phosphate, 15 g disodium hydrogen phosphate da 3 g trisodium citrate dihydrate da tsarma zuwa 1000 ml tare da deionized ruwa.Sa'an nan kuma ƙara 2 ml na 50% Triton X-100.Chloramine T: Auna 0.2 g na chloramine T kuma tsarma zuwa 200 ml tare da ruwa mai narkewa.Chromogenic reagent: Chromogenic reagent A: Gaba ɗaya narke 1.5 g na pyrazolone a cikin 20 ml na N, N-dimethylformamide.Developer B: Narkar da 3.5 g na hisonicotinic acid da 6 ml na 5 M NaOH a cikin 100 ml na ruwa mai lalata.Mix Developer A da Developer B kafin amfani, daidaita pH zuwa 7.0 tare da NaOH bayani ko HCl bayani, sa'an nan a tsoma zuwa 200 ml da deionized ruwa da tace don amfani daga baya.
Maganin buffer: Narkar da 10 g sodium tetraborate da 2 g sodium hydroxide a cikin ruwa mai tsarma kuma tsarma zuwa 1000 ml.0.025% methylene blue bayani: Narkar da 0.05 g na methylene blue trihydrate a cikin deionized ruwa da yin har zuwa 200 ml.Methylene blue stock buffer (sabuwar yau da kullum): tsarma 20 ml na 0.025% methylene blue maganin zuwa 100 ml tare da hannun jari.Canja wurin mazurari, a wanke da 20 ml na chloroform, jefar da chloroform da aka yi amfani da shi kuma a wanke tare da sabo chloroform har sai launin ja na chloroform ya ɓace (yawanci sau 3), sannan tace.Basic Methylene Blue: Tsarma 60 ml tace methylene blue stock bayani zuwa 200 ml stock bayani, ƙara 20 ml ethanol, Mix da kyau da kuma degas.Acid methylene blue: Ƙara 2 ml na 0.025% methylene blue bayani zuwa kimanin 150 ml na ruwa mai laushi, ƙara 1.0 ml na 1% H2SO4 sannan a tsoma zuwa 200 ml tare da ruwa mai tsabta.Sa'an nan kuma ƙara 80 ml na ethanol, Mix da kyau da kuma degas.
20% polyoxyethylene lauryl ether bayani: auna 20 g na polyoxyethylene lauryl ether da kuma tsarma zuwa 1000 ml tare da deionized ruwa.Buffer: Auna 20 g na trisodium citrate, tsarma zuwa 500 ml tare da deionized ruwa da kuma ƙara 1.0 ml na 20% polyoxyethylene lauryl ether.Maganin sodium salicylate (sabuwar mako-mako): Auna 20 g na sodium salicylate da 0.5 g na potassium ferricyanide nitrite kuma narke a cikin 500 ml na ruwa mai narkewa.Maganin Sodium dichloroisocyanurate (sabuwar mako-mako): Auna 10 g na sodium hydroxide da 1.5 g na sodium dichloroisocyanurate da narkar da su a cikin 500 ml na ruwa deionized.
Volatile phenol da cyanide matsayin da aka shirya azaman mafita na 0 µg/l, 2 μg/l, 5 µg/l, 10 µg/l, 25 µg/l, 50 µg/l, 75 µg/l da 100 µg/l, ta amfani da 0.01 M sodium hydroxide bayani.Anionic surfactant da ammonia nitrogen misali an shirya ta amfani da deionized ruwa 0 µg/L, 10 μg/L, 50 µg/L, 100 µg/L, 250 µg/L, 500 µg/L, 750 µg/L, 750 µg/L da 1000 mc .mafita.
Fara tank sake zagayowar sanyaya, sa'an nan (domin) kunna kwamfuta, sampler da iko zuwa AA500 rundunar, duba cewa bututu an haɗa daidai, saka iska tiyo a cikin iska bawul, rufe da matsa lamba farantin na peristaltic famfo, saka bututun reagent cikin ruwa mai tsabta a tsakiya.Guda software ɗin, kunna taga tasha mai dacewa kuma bincika idan bututun haɗin suna da alaƙa ta amintaccen kuma idan akwai wasu gibi ko ɗigon iska.Idan babu yayyo, nemi reagent da ya dace.Bayan tushen tushen taga tashar ta zama tsayayye, zaɓi kuma gudanar da ƙayyadadden fayil ɗin hanyar don ganowa da bincike.Ana nuna yanayin kayan aiki a Tebur 1.
A cikin wannan hanya ta atomatik don ƙayyade phenol da cyanide, ana fara distilled samfurori a 145 ° C.A phenol a cikin distillate sa'an nan ya amsa tare da asali ferricyanide da 4-aminoantipyrine don samar da wani hadadden ja, wanda aka auna launi a 505 nm.Cyanide a cikin distillate sai ya amsa da chloramine T don samar da cyanochloride, wanda ya samar da wani hadadden blue tare da pyridinecarboxylic acid, wanda aka auna ta launi a 630 nm.Anionic surfactants suna amsawa tare da ainihin methylene blue don samar da mahadi waɗanda aka fitar da chloroform kuma an raba su ta hanyar mai raba lokaci.Sa'an nan kuma an wanke lokaci na chloroform tare da acidic methylene blue don cire abubuwan da ke shiga tsakani kuma a sake rabuwa a cikin mai raba kashi na biyu.Ƙirar launi na mahadi masu launin shuɗi a cikin chloroform a 660 nm.Dangane da halayen Berthelot, ammonia yana amsawa tare da salicylate da chlorine a cikin dichloroisocyanuric acid a cikin matsakaiciyar alkaline a 37 ° C don samar da indophenol blue.Sodium nitroprusside da aka yi amfani a matsayin mai kara kuzari a cikin dauki, da sakamakon launi da aka auna a 660 nm.Ana nuna ƙa'idar wannan hanyar a cikin hoto 1.
Zane mai tsari na ci gaba da yin samfur don tantance phenols masu canzawa, cyanides, anionic surfactants da nitrogen ammoniacal.
Matsakaicin phenols masu canzawa da cyanides sun kasance daga 2 zuwa 100 µg/l, daidaitaccen daidaituwa na layi 1.000, equation regression y = (3.888331E + 005) x + (9.938599E + 003).Matsakaicin daidaituwa don cyanide shine 1.000 kuma ma'auni na regression shine y = (3.551656E + 005) x + (9.951319E + 003).Anionic surfactant yana da ingantacciyar dogaro na linzamin kwamfuta akan tattarawar nitrogen ammonia a cikin kewayon 10-1000 µg/L.Matsakaicin daidaitawa na anionic surfactants da nitrogen ammonia sun kasance 0.9995 da 0.9999, bi da bi.Matsakaicin koma baya: y = (2.181170E + 004) x + (1.144847E + 004) da y = (2.375085E + 004) x + (9.631056E + 003), bi da bi.An ci gaba da auna samfurin sarrafawa sau 11, kuma an raba iyakar gano hanyar ta hanyar 3 daidaitattun sauye-sauye na samfurin sarrafawa ta kowane gangara na daidaitattun ma'auni.Iyakokin ganowa na phenols masu canzawa, cyanides, anionic surfactants, da ammonia nitrogen sune 1.2 µg/l, 0.9 µg/l, 10.7 µg/l, da 7.3 μg/l, bi da bi.Iyakar ganowa ya yi ƙasa da tsarin ƙa'idar ƙasa, duba Table 2 don cikakkun bayanai.
Ƙara maɗaukaki, matsakaici, da ƙananan ƙayyadaddun mafita ga samfuran ruwa ba tare da alamun masu bincike ba.An ƙididdige murmurewa a ciki da tsakar rana bayan ma'auni bakwai a jere.Kamar yadda aka nuna a cikin Table 3, abubuwan da aka cire na phenol na intraday da intraday sun kasance 98.0-103.6% da 96.2-102.0%, bi da bi, tare da daidaitattun ma'auni na 0.75-2.80% da 1. 27-6.10%.Farfadowar cyanide na cikin rana da tsakar rana shine 101.0-102.0% da 96.0-102.4%, bi da bi, kuma madaidaicin ma'auni shine 0.36-2.26% da 2.36-5.41%, bi da bi.Bugu da kari, da intraday da interday extractions na anionic surfactants sun kasance 94.3-107.0% da 93.7-101.6%, bi da bi, tare da zumunta daidaitattun sabawa na 0.27-0.96% da 4.44-4.86%.A ƙarshe, dawo da nitrogen a cikin- da tsaka-tsaki na ammoniya ya kasance 98.0-101.7% da 94.4-97.8%, bi da bi, tare da ƙayyadaddun ma'auni na 0.33-3.13% da 4.45-5.39%, bi da bi.kamar yadda aka nuna a Table 3.
Yawancin hanyoyin gwaji, gami da spectrophotometry15,16,17 da chromatography25,26, ana iya amfani da su don auna gurɓataccen gurɓataccen ruwa guda huɗu.Chemical spectrophotometry wata sabuwar hanyar bincike ce don gano waɗannan gurɓatattun abubuwa, wanda ake buƙata ta ka'idodin ƙasa 27, 28, 29, 30, 31. Yana buƙatar matakai kamar distillation da cirewa, yana haifar da dogon tsari tare da rashin isasshen hankali da daidaito.Da kyau, mummunan daidaito.Yin amfani da sinadarai masu yaɗuwa na iya haifar da haɗari ga lafiya ga masu gwaji.Kodayake chromatography yana da sauri, mai sauƙi, inganci, kuma yana da ƙananan iyakoki, ba zai iya gano mahadi guda huɗu a lokaci guda ba.Koyaya, ana amfani da yanayin kuzarin da ba daidai ba a cikin binciken sinadarai ta amfani da ci gaba da kwarara spectrophotometry, wanda ya dogara da ci gaba da kwararar iskar gas a cikin tazara mai gudana na maganin samfurin, ƙara reagents a cikin ma'auni masu dacewa da jeri yayin kammala amsa ta hanyar madauki mai haɗawa. da gano shi a cikin spectrophotometer, a baya cire kumfa mai iska.Saboda tsarin ganowa yana sarrafa kansa, ana cire samfuran kuma ana dawo da su akan layi a cikin yanayin rufaffiyar.Hanyar yana inganta ingantaccen aiki sosai, yana ƙara rage lokacin ganowa, sauƙaƙe ayyuka, rage gurɓataccen reagent, ƙara haɓakar hankali da iyakan gano hanyar.
An haɗa da anionic surfactant da ammonia nitrogen a cikin haɗe-haɗe samfurin gwajin a taro na 250 µg/L.Yi amfani da daidaitaccen abu don juyar da phenol da cyanide mai canzawa zuwa abun gwajin a matakin 10 µg/L.Don bincike da ganowa, an yi amfani da hanyar daidaitattun ƙasa da wannan hanyar (6 gwaje-gwajen layi daya).An kwatanta sakamakon hanyoyin biyu ta amfani da t-gwajin mai zaman kanta.Kamar yadda aka nuna a cikin Table 4, babu wani bambanci mai mahimmanci tsakanin hanyoyin biyu (P> 0.05).
Wannan binciken ya yi amfani da na'urar nazari mai ci gaba da gudana don bincike na lokaci guda da gano phenols masu canzawa, cyanides, anionic surfactants da ammonia nitrogen.Sakamakon gwajin ya nuna cewa ƙarar samfurin da ake amfani da shi ta hanyar ci gaba da nazarin kwarara ya yi ƙasa da tsarin daidaitaccen tsarin ƙasa.Hakanan yana da ƙananan iyakokin ganowa, yana amfani da ƙarancin reagents 80%, yana buƙatar ƙarancin lokacin sarrafawa don samfuran mutum ɗaya, kuma yana amfani da ƙarancin chloroform na carcinogenic.Ana haɗa sarrafa kan layi kuma ana sarrafa shi ta atomatik.Ci gaba da gudana ta atomatik yana neman reagents da samfurori, sannan ya gauraya ta hanyar da'ira, yana zafi ta atomatik, cirewa da ƙidaya tare da launi.Ana aiwatar da tsarin gwaji a cikin rufaffiyar tsarin, wanda ke haɓaka lokacin bincike, rage gurɓataccen muhalli, kuma yana taimakawa tabbatar da amincin masu gwaji.Matakan aiki masu rikitarwa kamar distillation na hannu da hakar ba a buƙata22,32.Koyaya, bututun kayan aiki da na'urorin haɗi suna da ɗan rikitarwa, kuma sakamakon gwaji yana tasiri da abubuwa da yawa waɗanda zasu iya haifar da rashin daidaituwar tsarin cikin sauƙi.Akwai matakai masu mahimmanci da yawa da zaku iya ɗauka don inganta daidaiton sakamakonku da hana tsangwama ga gwajin ku.(1) Ya kamata a yi la'akari da ƙimar pH na maganin lokacin da aka ƙayyade phenols da cyanides masu canzawa.Dole ne pH ya kasance a kusa da 2 kafin ya shiga cikin coil distillation.A pH> 3, amines masu ƙanshi kuma za a iya kashe su, kuma amsawar 4-aminoantipyrine na iya ba da kurakurai.Hakanan a pH> 2.5, dawo da K3[Fe (CN) 6] zai zama ƙasa da 90%.Samfurori tare da abun ciki na gishiri fiye da 10 g/l na iya toshe coil ɗin distillation kuma ya haifar da matsala.A wannan yanayin, ya kamata a ƙara ruwa mai tsabta don rage yawan gishiri na samfurin33.(2) Abubuwan da ke biyo baya na iya yin tasiri ga gano abubuwan da ke cikin anionic: Sinadarai na cationic na iya samar da nau'i-nau'i mai ƙarfi na ion tare da masu surfactants anionic.Sakamako kuma na iya zama mai ban sha'awa a gaban: adadin humic acid fiye da 20 mg/l;mahadi tare da high surface aiki (misali sauran surfactants)> 50 MG / l;abubuwa tare da ƙarfin ragewa mai ƙarfi (SO32-, S2O32- da OCl-);abubuwan da ke samar da kwayoyin launi, masu narkewa a cikin chloroform tare da kowane reagent;wasu inorganic anions (chloride, bromide da nitrate) a cikin ruwan sharar gida34,35.(3) Lokacin da ake ƙididdige nitrogen ammonia, yakamata a yi la'akari da aminin ƙananan ƙwayoyin ƙwayoyin cuta, tunda halayensu da ammoniya iri ɗaya ne, kuma sakamakon zai kasance mafi girma.Tsangwama na iya faruwa idan pH na cakuda amsa ya kasance ƙasa da 12.6 bayan an ƙara duk hanyoyin magance reagent.Samfurori masu yawan acidic da buffered suna haifar da wannan.Ƙarfe ions da ke hazo a matsayin hydroxides a babban taro kuma na iya haifar da rashin daidaituwa36,37.
Sakamakon ya nuna cewa hanyar binciken ci gaba da gudana don ƙayyade lokaci guda na phenols masu canzawa, cyanides, anionic surfactants da ammonia nitrogen a cikin ruwan sha yana da layi mai kyau, ƙarancin ganowa, daidaitattun daidaito da dawowa.Babu wani bambanci mai mahimmanci tare da daidaitattun hanyar ƙasa.Wannan hanyar tana ba da hanya mai sauri, mai mahimmanci, daidai kuma mai sauƙi don amfani don bincike da ƙayyade yawan adadin ruwa.Ya dace musamman don gano abubuwa hudu a lokaci guda, kuma ana samun ingantaccen aikin ganowa sosai.
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