I-Hielscher Ultrasound Technology

I-EPA3550 i-Ultrasonic Extraction Guide

Isizinda se-Ultrasonic iyindlela enobungozi, engokwemvelo yemvelo engasetshenziswa kuma-sampuli amancane webhu kanye nokukhishwa kwamakhemikhali ayigugu ekulinganiseni kokukhiqiza kwezohwebo. I-United State Environmental Protection Agency (EPA) iphakamisa izindlela ezihlukahlukene zokuhlaziywa kwezindlela zokuhlola, izibonelo zokuhlola, ukuqinisekiswa kwezemvelo nokusekela ikhwalithi ekusekeleni uMthetho Wokugcinwa Kwemvelo Nokubuyiswa Kwemithombo (RCRA). Ngokuba isizinda se-ultrasonically-basizwa, i-EPA ikhishwe isiqondiso esilandelayo:

INDLELA 3550C – Isizinda se-Ultrasonic

1. Ububanzi kanye nesicelo

Qaphela: i-SW-846 ayihloselwe ukuba yincwadi yokuqeqesha yokuhlaziya. Ngakho-ke, izinqubo zendlela zilotshwe ngokusekelwe ekucatshangweni ukuthi zizokwenziwa ngabahlaziyi abaqeqeshiwe ngokomthetho okungenani izimiso eziyisisekelo zokuhlaziywa kwamakhemikhali kanye nokusetshenziswa kobuchwepheshe besifundo.
Ngaphezu kwalokho, izindlela ze-SW-846, ngaphandle kokusetshenziswa kwendlela edingekayo yokuhlaziywa kwemingcele echazwe ngendlela, zihloswe ukuba zibe izindlela zokuqondisa eziqukethe ulwazi jikelele mayelana nendlela yokwenza inqubo yokuhlaziya noma inqubo okuyi-laboratory engayisebenzisa njengendlela isisekelo sokuqala esisisekelo sokukhiqiza indlela yakhe ejwayelekile yokusebenza okujwayelekile (SOP), noma ngokusetshenziswa kwayo jikelele noma isicelo esithile sephrojekthi. Idatha yokusebenza ehlanganisiwe kule ndlela yenzelwe izinhloso zokuqondisa kuphela, futhi ayihloselwe ukuba ibe futhi ayifanele isetshenziswe njengendlela yokuvuma yokwamukela i-QC ngenhloso yokugunyazwa kwelabhutri.

1.1 Le ndlela ichaza inqubo yokukhipha izinhlanganisela eziphilayo ezingasetshenzisiwe kanye nezimila ezivela ezinqabeni ezinjengomhlabathi, amaskluji namadaka. Inqubo ye-ultrasonic iqinisekisa ukuthintana obuseduze kwesampuli sesampuli ne-solvent yezizinda.
1.2 Le ndlela ihlukaniswe ibe yizinqubo ezimbili, ngokusekelwe ekuhlungeni okulindelekile kwamakhemikhali. Inqubo yokuhlushwa ephansi (Isigaba 11.3) yilezi zakhi eziphilayo ezilindelekile ngaphansi kokulingana no-20 mg / kg bese zisebenzisa ubukhulu besampuli kanye neziqephu ezintathu eziyinkimbinkimbi (izingqinamba eziphansi kunzima kakhulu ukukhipha). Inqubo ye-concentration / medium high (Isigaba 11.4) yilezi zakhi eziphilayo ezilindelekile ezingaphezu kuka-20 mg / kg futhi zisebenzisa isampula encane kanye nesinye esisodwa.
1.3 Kunconywa kakhulu ukuthi lezi ziqhumane zingaphansi kwesimo sokuhlanza (isb., Ukusebenzisa indlela kusukela ochungechungeni lwama-3600) ngaphambi kokuhlaziywa.
1.4 Kubalulekile ukuthi le ndlela (kuhlanganise nemiyalelo yomkhiqizi) ilandelwe ngokucacile, ukuze kufezekiswe ukusebenza kahle kwesilinganiso. Bheka Isigaba. 11.0 ukuxoxisana ngezici ezibucayi zenqubo yokukhipha. Bheka imiyalelo yomkhiqizi mayelana nezilungiselelo ezithile zokusebenza.
1.5 Le ndlela ichaza okungenani izinhlelo ezintathu zokuxazulula izixazululo ezingahle ziqashwe amaqembu ahlukene abahlaziyi (bheka iSahluko 7.4). Amanye ama-solvent systems angaqashwa, uma nje ukusebenza okwanele kungaboniswa ngabahlaziyi bentshisekelo. Ukukhethwa kwe-solvent yesikhumba kuzoxhomeke kubalingisi benzuzo futhi akukho solvent eyodwa esebenza kuwo wonke amaqembu e-analyte. Ngenxa yokukhathazeka mayelana nokusebenza kahle kwesitokisi se-ultrasonic, ikakhulukazi ekugxilweni okungezansi noma ngezansi mayelana no-10 μg / kg, kubalulekile ukuthi umhlaziyizimboni abonise ukusebenza kwesistimu yokuxazulula izinkinga kanye nezimo zokusebenza zabahlaziyi abanentshisekelo kanye nokugxila inzalo. Lokhu kubonakala kusebenza kunoma yikuphi uhlelo lokuxazulula izinhlanzi oluqashiwe, kuhlanganise nalabo abalulwe ngqo kule ndlela. Okungenani, ukubonakaliswa okunjalo kuzohlanganisa ukubonakaliswa kokuqala kobuchwepheshe obuchazwe ku-Method 3500, besebenzisa i-matrix ecacile. Indlela 8000 ichaza izinqubo ezingasetshenziselwa ukuthuthukisa izindlela zokusebenza zemibukiso enjalo kanye ne-matrix spike kanye nemiphumela yesampula yokulawula isampula.
1.6 I-EPA iphawula ukuthi kunemininingwane ekhishwe eshicilelwe ngokusebenza kahle kwesakhiwo se-ultrasonic ngokuphathelene nezidakamizwa ze-organophosphorus ezingxenyeni eziphansi ezingamabhiliyoni (ppb) ezingezansi nangaphansi. Ngenxa yalokho, ukusetshenziswa kwalendlela kulezi zinhlanganisela ikakhulukazi kufanele kusekelwe ngedatha yokusebenza njengalezo ezixoxwe ngenhla naku-Method 3500.
1.7 Ngaphambi kokusebenzisa le ndlela, abahlaziyi bayelulekwa ukuthi baxoxe ngezindlela eziyisisekelo zenqubo ngayinye engasetshenziswa ekuhlaziyweni jikelele (isib. Izindlela 3500, 3600, 5000, no-8000) ngolwazi olwengeziwe mayelana nezinqubo zokulawula izinga, ukuthuthukiswa ye-QC yokwamukelwa, izibalo, kanye nokuqondiswa jikelele. Abahlaziyi kufanele futhi babonisane nesitatimende sokuzilahla phansi phambi kwebhukwana kanye nokwaziswa eSahlukweni sesibili ukuze uthole isiqondiso mayelana nokuguquguquka okuhloswe kukho ekukhethweni kwezindlela, izinto zokusebenza, izinto zokwenza izinto, izigulantshi nezibonelelo, kanye nemithwalo yemfanelo yomhlaziyi wokubonisa lokho amasu asetshenzisiwe afaneleka abahlaziyi bezintshisekelo, ku-matrix ezithakazelisayo, nasezindabeni zokukhathazeka.
Ngaphezu kwalokho, abahlaziyi kanye nabasebenzisi bezinhlelo zelulekwa ukuthi, ngaphandle uma kuchazwe ngokucacile emtsetfweni, ukusetshenziswa kwezindlela ze-SW-846 akumele kulandelwe izidingo zokuhlolwa zikahulumeni. Ulwazi oluqukethwe kule ndlela luhlinzekwa yi-EPA njengesiqondiso okufanele sisetshenziswe ngumhlaziyi kanye nomphakathi olawulwayo ekwenzeni izahlulelo ezidingekayo ukuze kutholakale imiphumela ehlangabezana nezinhloso zekhwalithi yedatha ngenhloso ehlosiwe.
1.8 Ukusebenzisa le ndlela kuvinjelwe ukusetshenziswa, noma ngaphansi kokuqondiswa, abahlaziyi abanokuhlangenwe nakho nabaqeqeshiwe. Umhlaziyi ngamunye kumele akhombise ikhono lokukhiqiza imiphumela eyamukelekayo ngale ndlela. Njengoba kuphawuliwe ngenhla, imiboniso enjalo iqondene nabahlaziyi bezintshisekelo kanye nesistimu ye-solvent esebenzisayo, kanye nezinqubo zamasampula okuhlushwa aphansi naphakathi / phezulu.

I-Sonification iyisinyathelo esivamile ngaphambi kokuhlaziywa (isib. GC, TLC, HPLC)

I-VialTweeter for ultrasonic isampula prep

2. Isifinyezo seMethod

2.1 Inqubo yokuhlushwa ephansi — Isampula ixubene ne-sodium sulfate ye-anhydrous ukuze yenze i-powder egeleza mahhala. Ingxube yenziwa nge-solvent kathathu, isebenzisa isizinda se-ultrasonic. Ukukhishwa kuhlukaniswe nesampula ngokuhlunga okuzenzakalelayo noma i-centrifugation. Ukukhishwa kusilungele ukugxila kokugcina, ukuhlanza, kanye / noma ukuhlaziywa.
2.2 Inqubo yokuhlushwa emaphakathi / phezulu — Isampula ixubene ne-sodium sulfate ye-anhydrous ukuze yenze i-powder egeleza mahhala. Lokhu kukhishwa nge-solvent once, ngokusebenzisa isizinda se-ultrasonic. Ingxenye yokukhishwa iqoqwe ukuhlanza kanye / noma ukuhlaziywa.

3. Izincazelo

Bheka iSahluko 1 kanye nemiyalelo yomkhiqizi ngezincazelo ezingase zifanele kule ndlela.

4. Izinkambiso

4.1 Amakhemikhali, ama-reagents, i-glassware, kanye nezinye izampula ze-hardware ezisebenzayo zingenza izici kanye / noma iziphazamiso zokuhlunga isampula. Zonke lezi zinto kufanele ziboniswe zingenasiphazamiso ngaphansi kwemibandela yokuhlaziywa ngokuhlaziya izinkomba zendlela.
Ukukhethwa okucacile kwama-reagents nokuhlanzwa kwe-solvents yi-distillation kuzo zonke izibuko-ingilazi kungadingeka. Bheka indlela ngayinye okufanele isetshenziselwe isiqondiso esithile mayelana nezinqubo zokulawula ikhwalithi kanye neSahluko Sesine ukuze uthole isiqondiso jikelele ngokuhlanzwa kwe-glassware.
4.2 Izintatheli zivame ukucaciswa kubahlaziyi abanentshisekelo. Ngakho-ke, bhekani ku-Method 3500 kanye nezindlela ezifanele zokunquma ukuqondisa okuqondile mayelana nokuphazamiseka kokukhipha.

5. Ukuphepha

Le ndlela ayihambisani nezinkinga zokuphepha ezihlobene nokusetshenziswa kwayo. I-laboratory inesibopho sokugcina indawo ephephile yomsebenzi kanye nefayela lokuqwashisa lwamanje ye-OSHA imithethonqubo mayelana nokuphathwa okuphephile kwamakhemikhali abhalwe ngale ndlela. Ifayela lokubhekisela lamaphepha emininingwane yokuphepha (MSDSs) kufanele itholakale kubo bonke abasebenzi abathintekayo kulezi zihlaziywa.

6. Izinsiza nokunikezwa

Ukushiwo ngamagama okuhweba noma imikhiqizo yezohwebo kulokhu kubhalwa ngenhloso yokufanekisa kuphela, futhi akuyona ukugunyazwa kwe-EPA noma izincomo ezikhethekile zokusetshenziswa. Imikhiqizo nezilungiselelo zensimbi ezibalwe ngezindlela ze-SW-846 zimelela lezo mikhiqizo kanye nezilungiselelo ezisetshenziselwa ukuthuthukiswa kwendlela noma kamuva zihlolwe yiSikhungo. I-Glassware, ama-reagents, imishini, imishini, kanye nezilungiselelo ngaphandle kwalezo ezibalwe kule ncwadi kungase iqashwe uma indlela yokusebenza efanelekile ekusetshenzisweni okuhlosiwe ibonisiwe futhi ibhalwe phansi.
Lesi sigaba asikho uhlu lwama-glassware evamile (isib., Abeakers and flasks).

Isicelo solwazi




Qaphela kwethu Inqubomgomo yobumfihlo.



Izinqubo ze-Ultrasonic:

    – Ukuhlanzwa

    – I-Sono-Leaching
    – Ukuchitheka
6.1 Izixhobo zokugaya amasampula omfucu owomile.
6.2 Ukulungiselela i-Ultrasonic — Idivayisi ephethe uphondo ifakwe ithiphu le-titanium, noma idivayisi eyokwenza ukusebenza okufanele, kufanele isetshenziswe. (isib UP200Ht noma UP200St)
6.2.1 Isiphazamisi se-ultrasonic — Isiphazamiso kufanele sibe namandla okulinganisa amandla angama-watts angu-300, nekhono lokususa. Idivaysi eyenzelwe ukunciphisa umsindo we-cavitation unconywa. Landela imiyalelo yabakhiqizi yokulungiselela ukuphazamiseka kokukhipha amasampuli ngezingqondo eziphansi neziphakathi / eziphezulu. (isib UP400S)
6.2.2 Sebenzisa uphondo lwe-3/4-intshi ngenqubo encane yokuhlushwa kwe-concentration kanye ne-microprop 1/8-inch tapered microtip ehlanganiswe nophondo oluphakathi kuka-1/2-intshi ngenqubo yokwenza umthamo ophakathi / ophezulu.
6.3 Ibhokisi lokuvikela umsindo - Ukuze ugweme ukulimala kokuzwa, ukusetshenziswa kwe-enlosure yokuvikela umsindo (isb. Ibhokisi lokuvikela umsindo SPB-L) Kunconywa. Ngalokho, umsindo wokucabangela wenqubo yomsindo unganciphisa kakhulu.

Izinsiza ezengeziwe

6.4 Amadivaysi ekunqumeni amaphesenti isisindo esomile
6.4.1 Ukushisa ihhavini — Iyakwazi ukugcina i-105 degC.
6.4.2 Desiccator.
6.4.3 Izibhamu — I-porcelain noma i-aluminium elahlwayo.
6.5 amaphuputha ePasteur — I-1-mL, ingilazi, ilahlwa.
6.7 Izixhobo zokuhlunga noma ukucindezela ukucindezela
6.7.1 umcibisholo we-Buchner
6.7.2 Iphepha lokuhlunga
6.8 Izixhobo zeDuderna-Danish (KD)
6.8.1 I-tube concentrator — 10-mL, iziqu. I-stopper-ground glass stopper isetshenziselwa ukuvimbela ukukhuphuka kwamashizi.
6.8.2 I-flask ye-evaporation — 500-mL. Namathisela i-flask ku-tube concentrator eneziphethu, izigubhu, noma okulinganayo.
6.8.3 ikholomu yeSnyder — I-ball-ball macro.
6.8.4 ikholomu yeSnyder — I-micro-ball micro.
6.8.5 Iziphethu — I-1/2 intshi.
6.9 Isistimu yokutakula isisindo se-Solvent.
QAPHELA: Le glassware Kunconywa ngenhloso yokuthola i-solvent ngesikhathi izinqubo zokuhlushwa ezidinga ukusetshenziswa Kuderna-Danish concentrators evaporative. Ukuhlanganiswa kwalezi zixhobo kungadingeka yiMithetho kahulumeni, kaHulumeni noma yendawo yendawo elawula ukukhishwa komoya kwezinto ezingokwemvelo. I-EPA itusa ukufakwa kwalolu hlobo lokubuyisela uhlelo njengendlela yokuqalisa uhlelo lokunciphisa ama-emissions. Ukutholwa kwe-solvent kuyindlela yokuhambisana nokuncishiswa kokudoba kanye nokuvimbela ukungcola.
6.10 Ama-chips abilayo — I-Solvent-ekhishwe, cishe ama-10/40 omeshini (i-silicon carbide noma ilingana).
6.11 Ukugeza amanzi — Ukufudumala, ngendwangu yokugqoka eyigugu, ekwazi ukulawula ukushisa ku-± 5 degC. Ibhuku kufanele lisetshenziswe kuhodo.
6.12 Ukulinganisa — Ukulayisha okuphezulu, okukwazi ukulinganisa ngokunembile ku-0.01 g.
6.13 izigqoko — I-2-mL, ye-GC autosampler, ifakwe i-polytetrafluoroethylene (PTFE) - i-screw caps noma i-crimp phezulu.
6.14 ama-glass scintillation — I-20-mL, enezikhwama ze-PTFE-lined screw scs.
6.15 Spatula — Insimbi engenalutho noma i-PTFE.
6.16 Ukoma ikholomu — I-ID ye-20-mm ye-borosilicate ingilazi ye-chromatographic ikholomu ne-glass wool ngezansi.
QAPHELA: Amakholomu ane-disk glass fritted kunzima ukuwohloka ngemuva kokuba asetshenzisiwe ukuma okwetshenziswe kakhulu. Amakholomu ngaphandle kwamafreyithi angathengwa.
Sebenzisa i-pad encane ye-glass wool ukuze ugcine i-adsorbent. Phakamisa i-glass wool pad nge-50 mL ye-acetone elandelwe yi-50 ml we-elution solvent ngaphambi kokupakisha ikholomu nge-adsorbent.
6.17 Amadivayisi we-nitrogen evaporation (ozikhethela) — I-N-Evap, indawo engu-12 noma engu-24 (I-Organomation Model 112, noma ilingana).

7. Ama-Reagents namazinga

7.1 Amakhemikhali e-reagent-grade kumele asetshenziswe kuzo zonke izivivinyo. Ngaphandle kokuthi kuboniswe ngenye indlela, kuhloswe ukuthi wonke ama-reagents ahambisana nezimpawu zeKomidi lamaReagents e-Analytical we-American Chemical Society, lapho imininingwane ekhona khona. Amanye amamaki angase asetshenziswe, uma kutholakala ukuthi kuqala ukuthi i-reagent ihlanzekile ngokwanele ukuvumela ukusetshenziswa kwayo ngaphandle kokunciphisa ukunemba kokuzimisela. Ama-reagents kufanele agcinwe ngilazi ukuze kuvinjelwe i-leaching ye-contaminants ezikhungweni zepulasitiki.
7.2 Amanzi asebenzayo angenalutho. Konke okubhekisela emanzini kule ndlela kubhekisela emanzini e-reagent angenalutho, njengoba kuchazwe eSahlukweni 1.
7.3 I-sulfate ye-sodium (i-granular, i-anhydrous), i-Na2SO4. Hlanza ngokushisa nge-400 degC amahora angu-4 endaweni ye-tray engajulile, noma ngokuguqula i-sodium sulfate nge-methylene chloride. Uma i-sulfate ye-sodium ihlanjululwa nge-methylene chloride, indlela engacacile kufanele ihlaziywe, ibonise ukuthi akukho ukuphazamiseka kwe-sodium sulfate.
7.4 izixazululo zokususa
Ama-sampuli kufanele akhishwe ngokusebenzisa uhlelo lokuxazulula izinhlanzi olunikeza ukuhlaziywa okungcono, okuphindaphindiwe kwama-analytes ezithakazelisayo kusukela kwisampuli yesampuli, ezindaweni ezithakazelisayo. Ukukhethwa kwe-solvent yesikhumba kuzoxhomeke kubalingisi benzuzo futhi akukho solvent eyodwa esebenza kuwo wonke amaqembu e-analyte. Kungakhathaliseki ukuthi kusetshenziselwa uhlelo lokuxazululwa kwegazi, kuhlanganise nalabo abalulwe kulolu hlelo, umhlaziyi kufanele abonise ukusebenza okwanele kwabahlaziyi bezithakazelo, emazingeni ezithakazelo. Okungenani, ukubonakaliswa okunjalo kuzohlanganisa ukubonakaliswa kokuqala kobuchwepheshe obuchazwe ku-Method 3500, besebenzisa i-matrix ecacile. Indlela 8000 ichaza izinqubo ezingasetshenziselwa ukuthuthukisa izindlela zokusebenza zemibukiso enjalo kanye ne-matrix spike kanye nemiphumela yesampula yokulawula isampula.
Amanethiwekhi amaningi okuxazulula izinto ahlongozwe ngezansi afaka ukuhlanganiswa kwamanzi okungahambisani kahle namanzi, njenge-acetone, ne-solvent immiscible solvent, efana ne-methylene chloride noma i-hexane. Inhloso yomsombuluko we-water-miscible ukusiza ukukhishwa kwama-solids amanzi ngokuvumela i-solvent exubekile ukungenelela koqweqwe lwamanzi ebusweni bezinhlayiya eziqinile. Amanzi-immiscible solvent akhipha amakhemikhali e-polarities afanayo. Ngakho-ke, i-solvent engeyona i-polar efana ne-hexane isetshenziselwa ukuhlaziywa okungewona ama-polar njengama-PCB, kuyilapho isisombululo se-polar njenge-methylene chloride singasetshenziselwa ukuhlaziywa kwe-polar. I-polarity ye-acetone ingasiza futhi ukukhipha ama-analytes e-polar ohlelweni oluxubene lwe-solvent.
Ithebulethi 1 inikeza idatha yokutakula isibonelo yezinhlanganisela ezikhethiwe zemvelo ezikhishwe ku-NIST SRM besebenzisa izinhlelo ezihlukahlukene zokuhlunga izizinda. Izigaba ezilandelayo zinikeza isiqondiso ekukhethweni kwezixazululo zamaqembu ahlukene abahlaziyi.
Zonke izixazululo kufanele zibe izinga lokubulala izibulala-zinambuzane noma okulinganayo. Izixazululo zingase zihlulwe ngaphambi kokusebenzisa.
7.4.1 I-acidone / hexane (1: 1, v / v CH3COCH3 / C6H14), i-acetone / methylene chloride (1: 1, v / vCH3COCH3 / CH2Cl2).
7.4.2 I-Organochlorine pesticides ingasuswa nge-acetone / hexane (1: 1, v / v CH3COCH3 / C6H14), noma i-acetone / methylene chloride (1: 1, v / vCH3COCH3 / CH2Cl2).
7.4.3 Ama-PCB angasuswa nge-acetone / hexane (1: 1, v / v CH3COCH3 / C6H14), noma i-acetone / methylene chloride (1: 1, v / vCH3COCH3 / CH2Cl2), noma i-hexane (C6H14).
7.4.4 Amanye ama-solvent systems angaqashwa, uma nje umhlaziyi angabonisa ukusebenza okwanele kwabahlaziyi bezithakazelo, ekugxilweni kwezintshisekelo, kwisampuli yesampuli (bheka indlela 3500).
7.5 Exchange solvents — Ngokusebenzisa ezinye izindlela zokunquma, i-solvent yesikhumba izodinga ukushintshaniswa ne-solvent ehambelana nensimbi esetshenziselwa leyo ndlela yokunquma. Bheka indlela yokunquma okufanele isetshenziselwe ukukhethwa kwe-solvent efanelekayo. Zonke izixazululo kumele zibe yizinga lesifo se-pesticide noma elilinganayo. Izibonelo ze-solvents yokushintshaniswa zinikezwa ngezansi.
7.5.1 Hexane, C6H14
7.5.2 2-Propanol, (CH3) 2CHOH
7.5.3 I-Cyclohexane, i-C6H12
7.5.4 i-Acetonitrile, i-CH3CN
7.5.5 I-Methanol, i-CH3OH
Ibhokisi lokuvikelwa komsindo lenziwe kusuka ingilazi ye-acrylic ukuze inqubo ye-sonication ingabonwa ngokubukeka. (Chofoza ukuze ukhulise!)

Ibhokisi lokuvikelwa komsindo i-SPB-L linciphisa umsindo wokucabangela we-sonication kakhulu.

8. Iqoqo leSampula, ukulondolozwa, nokuGcina

8.1 Bheka indaba engeniswa eSahlukweni Sine, “Ama-Analytics e-Organic” Indlela 3500, kanye nezindlela eziqondile zokuqashwa ezizosetshenziswa.
8.2 Amasampuli aqinile okumele akhishwe ngale nqubo kufanele aqoqwe futhi agcinwe njengamanye amasampuli aqinile aqukethe okwenziwe nge-semivolatile engokwemvelo.

9. Ukulawulwa Kwemithi

9.1 Bheka iSahluko Se-1 ukuze uthole isiqondiso esengeziwe mayelana nesiqiniseko sekhwalithi (QA) kanye nemigomo yokulawula ikhwalithi (QC). Uma ukungahambisani phakathi kwemihlahlandlela ye-QC, indlela ye-QC ethize ihamba phambili ngaphezu kokubili kwezinqubo eziqondene nezinqubo nezindlela ezihlinzekwe eSahlukweni 1, futhi izindlela ze-QC eziqondene nezobuchwepheshe zihamba phambili ngaphezu kweSahluko 1. Noma yimuphi umzamo ohilela ukuqoqwa kwedatha yokuhlaziya kufanele ufake ukuthuthukiswa kwedokhumenti ehleliwe ehleliwe, ehlelekile njengePhiko lokuQinisekiswa koMgangatho weQiniso (QAPP) noma uhlelo lokuSampula kanye nokuHlola (SAP), oluhumusha izinjongo zeprojekthi kanye nezincazelo eziqondisweni kulabo uzosebenzisa le phrojekthi futhi ahlole imiphumela. I-laboratory ngayinye kufanele igcine uhlelo oluqinisekisiwe lokuqinisekisa ikhwalithi. I-laboratory kufanele futhi igcine amarekhodi okubhalisa ikhwalithi yedatha eyenziwe. Yonke idatha yamashidi nedatha yokulawula ikhwalithi kufanele igcinwe ukubhekisela noma ukuhlolwa.
9.2 Ukuboniswa kokuqala kobuchwepheshe
I-laboratory ngayinye kufanele ikhombise ubuchwepheshe bokuqala ngokulungiselela isampula ngayinye kanye nenhlanganisela yenqubo yokuqapha isebenzisa ngokudala idatha yokwaziswa okulungile nokwaziswa ngokucwaninga okuhlosiwe ku-matrix ehlanzekile. I-laboratory kumele iphinde iphinde ibonise ukuqeqeshwa lapho abasebenzi abasha beqeqeshiwe noma izinguquko eziphawulekayo ekusebenziseni izinsimbi. Bona iMethod 8000 ngolwazi lokuthi ungayifeza kanjani ukubonakaliswa kobuchwepheshe.
9.3 Ekuqaleni, ngaphambi kokucubungula noma yikuphi amasampula, umhlaziyi kufanele akhombise ukuthi zonke izingxenye zomshini oxhumana naye nesampula zingenaphazamiso. Lokhu kufezwa ngokuhlaziywa kwendlela engenalutho. Njengesikebhe esiqhubekayo, amasampuli ngayinye akhishwa, ahlanzwa, ahlaziywe, futhi uma kukhona ushintsho kuma-reagents, indlela engenalutho kufanele ikhishwe futhi ihlaziywe ngamakhemikhali athakazelisayo njengokulondeka kokungcola okungavamile kwama-laboratory.
9.4 Noma yiziphi izikhalazo zezindlela, amasampuli ama-matrix spike, noma ama-sampuli aphindaphindiwe kufanele afakwe ezinkambisweni ezifanayo zokuhlaziya (Isigaba 11.0) njengalezo ezisetshenziselwa amasampuli langempela.
9.5 Imikhuba yokuqinisekisa ikhwalithi ejwayelekile kufanele isetshenziswe ngale ndlela njengoba ifakwe emibhalweni ehlelekile yokuhlela kanye nama-SOPs laboratory. Zonke izimo zokusebenza zokusebenza kufanele zirekhodwe.
9.6 Futhi ubhekisele ku-Method 3500 yezinqubo zokulawula ukukhishwa kwekhwalithi kanye nesampula yokulungisa ikhwalithi kanye nezindlela zokunquma ezizosetshenziselwa izinqubo ze-QC ezinquma.
9.7 Uma kubhalwe indlela efanele yokunquma, izindinganiso zokungena kufanele zengezwe kuzo zonke amasampuli ngaphambi kokukhipha. Bheka Izindlela 3500 no-8000, nezindlela ezifanele zokunquma ulwazi oluthe xaxa.
9.8 Njengoba kuphawuliwe ekuqaleni, ukusetshenziswa kwanoma yiluphi uhlelo lokucubungula, kufaka phakathi isizinda se-ultrasonic, kufanele lusekelwe ngedatha ebonisa ukusebenza kwesistimu ethile yokuxazulula izinhlanzi kanye nezimo zokusebenza zabahlaziyi bezintshisekelo, emazingeni ezithakazelo, kwisitatimende samatriki.

10. Ukulinganisa nokuma

Awekho izinyathelo zokulinganisela noma zokumisa ngokuqondile ezihlotshaniswa nale nqubo yenqubo yesampula.

11. Inqubo

Njengoba kuboniswe kuSec. 1.4, isizinda se-ultrasonic angeke sibe yindlela enamandla njengoba ezinye izindlela zokwenza izinhlabathi / izinsila. Ngakho-ke, kubalulekile ukuthi le ndlela ilandelwe ngokucacile (kufaka phakathi nemiyalelo yomkhiqizi) ukuze kufinyeleleke ekusebenzeni okuphezulu kwesilinganiso. Okungenani, ukuze usebenzise ngokuphumelelayo le nqubo:

  • Idivaysi yokukhipha kumele ibe nama-watts angama-300 amancane futhi ifakwe izimpondo eziphazamisayo zesayizi (bheka isigaba 6.2).
  • Uphondo kufanele lugcinwe kahle, kufaka phakathi ukulungiswa ngokulandela imiyalelo yomkhiqizi ngaphambi kokusetshenziswa, nokuhlola ithiphu lokuphenya ngokugqoka ngokweqile.
  • Isampula kufanele ilungiselelwe kahle ngokuyixuba ngokugcwele nge-sulfate ye-sodium, ukuze idale i-powder egeleza mahhala ngaphambi kokwengezwa kwe-solvent.
  • Izimpondo zesikhumba / i-sonotrodes esetshenziselwa ukuhlushwa okuphansi kanye nezinqubo eziphakeme zokuhlushwa (Izigaba 11.3 no 11.4, ngokulandelana) aziguquguquki. Imiphumela ibonisa ukuthi ukusetshenzwa kwempondo ka-3/4-intshi akufanelekile ngenqubo yokuhlushwa ephezulu, ikakhulukazi ngokukhipha izinhlanganisela ezingekho polar ezinjenge-PCBs, ezikhangisa kakhulu ematrix enhlabathini.
  • Ukuze uthole amasampuli aphansi, ukukhishwa okuthathu kwenziwa nge-solvent efanelekile, ukukhishwa kwenzelwa kwimodi ye-pulse ekhethiwe, futhi ithiphu le-sonotrode / uphondo libekwe phansi ngaphansi kwe-solvent, kodwa ngaphezu kwesampula. Indlela efanayo isetshenziselwa amasampula aphezulu okuhlushwa, ngaphandle kokuthi kungenziwa isidingo esisodwa kuphela.
  • Ukuxuba kakhulu kwesampula kanye ne-solvent kufanele kwenzeke lapho i-pulsay ultrasonic isebenze. Umhlaziyi kufanele aqaphele ukuxuba okunjalo ngesikhathi esithile ngesikhathi senqubo yokukhipha.
  • 11.1 Ukusingathwa kwesampula

    11.1.1 Amasampula omhlabathi / omhlabathi — I-Decant bese ulahla noma yiliphi uhlaka lwamanzi kwisampula sediment. Lahla noma yiziphi izinto zangaphandle ezifana nezinduku, amaqabunga, namadwala. Hlanganisa isampula kahle, ikakhulukazi amasampuli ahlanganisiwe.
    11.1.2 Amasampula wokuchitha — Amasampula anezigaba eziningi kufanele alungiswe ngaphambi kokukhipha isigaba sokuhlukaniswa kwesigaba esichazwe eSahlukweni sesiBili. Le nqubo yenqubo yesikhumba yilabo kuphela kuphela.
    11.1.3 Amasampula omfucumfucu owomile angasetshenziswa ukugaya — Gweba noma uhlukanise ngenye indlela udoti ukuze udlule ngesihluthulelo se-1-mm noma ungadluliselwa emgodini we-1-mm. Sethula isampula esanele kumadivayisi okugaya ukuze unikele okungenani 10 g ngemuva kokugaya.
    QAPHELA: Ukumisa nokugaya kufanele kwenziwe kwikhodi, ukugwema ukungcola kwelabhutrikhi.
    11.1.4 Izinto ezinamafutha, ama-fibrous, noma amafutha angenayo amandla okugaya — Sika, shred, noma ukunciphisa ngandlela-thile lezi zinto zokwakha ukuvumela ukuxuba nokwehliswa okuphezulu kwezakhiwo zesampula ze-extraction.
    11.2 Ukunqunywa kwesisindo somzimba owomile — Uma imiphumela yesampula kufanele ibalwe ngesisekelo sesisindo esomile, ingxenye ehlukile yesampula kufanele ilinganiswe ngesikhathi esifanayo nesabelo esisetshenziselwa ukuzimisela kokuhlaziya.
    QAPHELA: I-ovini yokumisa kufanele ilandelwe kwihood noma ivuliwe. Ukungcola okubaluleke kakhulu kwe-laboratory kungase kubangele isampula enobungozi enobungozi obuyingozi kakhulu.
    Ngokushesha ngemva kokulinganisa isakhi samanquot esikhwameni ukuze sikhiqizwe, silinganisa i-aliquot eyengeziwe ka-5- kuya ku-10-g yesampula ibe yi-crucible ehlanjululwe. Dry le aliquot ubusuku obuyi-105 degC. Vumela ukupholisa ku-desiccator ngaphambi kokulinganisa.
    Bala isisindo esomile sephesenti kanje:
    % isisindo esomile = (g sampula esomile / g isampula) x 100
    Le aliquot eyomile-ovini ayisetshenziselwa ukukhipha futhi kufanele ilahlwe ngendlela efanele uma isisindo esomile sinqunywa.

    11.3 Inqubo yezinga lokuhlushwa okuphansi

    Le nqubo isebenza kuma-sampuli aqinile okulindeleke ukuba aqukethe ngaphansi kuka-20 mg / kg okuhlaziya okuphilayo.

    Izinyathelo ngaphambi kwe-sonication

    QAPHELA: Engeza ama-surrogates kanye nama-matrix spiking compounds ku-aliquot yesampula ngaphambi kokuxuba isampuli ne-sodium sulfate drying agent. Ukukhipha isampula kuqala kwandisa isikhathi sokuxhumana samakhemikhali a-spiked kanye nesampuli sangempela sesampuli. Kumele kuholele ekuxubeni okungcono kwesisombululo sopikisi nesampula lapho isulfure sulfate nesampula zihlanganiswa kuze kube seqophelweni lokuhamba okukhululekile.
    11.3.1 Izinyathelo ezilandelayo kufanele zenziwe ngokushesha ukuze kugweme ukulahlekelwa yi-extractable engavamile.
    11.3.1.1 Cishe cishe 30 g yesampula ibe ngu-400-mL beaker. Qopha isisindo eseduze 0.1 g.
    11.3.1.2 Ukuze isampula ku-batch ngayinye ekhethiwe ukupenda, engeza i-1.0 mL yesisombululo se-matrix spiking. Xhumana no-Method 3500 ukuze uthole isiqondiso ekukhethweni okufaneleko kwe-matrix spiking compounds nama-concentrations. Bona futhi inothi ku-Sec. 11.3.
    11.3.1.3 Engeza i-1.0 mL yesisombululo esiphezulu se-surrogate kuwo wonke amasampuli, amasampuli a-spiked, ama-sampuli we-QC, nama-blank. Xhumana no-Method 3500 ukuze uthole isiqondiso ekukhethweni okufanele kwe-comprogate compounds kanye nokugxila. Bona futhi inothi ku-Sec. 11.3.
    11.3.1.4 Uma i-gel permeation ihlanza (bheka indlela 3640) kufanele isetshenziswe, umhlaziyi kufanele abe wengeze kabili ivolumu yesisombululo sokupaka (kanye nesisombululo se-matrix spiking, lapho kufanele khona), noma ugxilise ukukhipha kokugcina kube yingxenye yevolumu evamile , ukukhokhela isigamu sokukhishwa esilahlekile ngenxa yokulayisha kwekholomu ye-GPC. Bona futhi inothi ku-Sec. 11.3.
    11.3.1.5 Amasampuli angama-nonporous noma amanzi (uhlobo lwama-gummy noma ubumba) olungenawo umhlabathi olunezihlahla ezingenawo mahhala kufanele axutshwe nama-60 g we-sodium sulfate anhydrous, usebenzisa i-spatula. Uma kudingeka, i-sodium sulfate engaphezulu ingafakwa. Ngemuva kokungezwa kwe-sulfate ye-sodium, isampula kufanele ibe yi-free flow. Bona futhi inothi ku-Sec. 11.3.

    11.3.1.6 Masinyane wengeze i-100 ml ye-solvent yesikhumba noma ingxube ye-solvent (bheka iSahluko 7.4 noThebula 2 ngolwazi ngokukhetha kwamakhemikhali).
    11.3.2 Beka indawo engezansi yephuzu lomsindo wokuphazamisa u-3/4-intshi mayelana no-1/2-intshi ngaphansi kwesimo se-solvent, kodwa ngaphezu kwezingqimba zomhlabathi.
    QAPHELA: Qinisekisa ukuthi uphondo lwe-ultrasonic / i-sonotrode kahle lukhuni ngokuya imiyalelo yomkhiqizi.
    11.3.3 Khipha isampula nge-ultrasonically ngamaminithi angu-3, ​​ngokulawulwa kokukhipha okubekiwe ku-100% (amandla agcwele) noma ekusetshenzisweni kwamandla okuphakanyiswa komkhiqizi, ukushintsha kwemodi ku-Pulse (amandla okukhipha esikhundleni samandla okuqhubekayo), nomjikelezo womsebenzi wephesenti usethe ku-50% (amandla ngama-50% wesikhathi futhi aphule isikhathi se-50%). Ungasebenzisi probe ye-microtip.
    11.3.4 Ukunquma ukukhipha bese uyihlunga ngokusebenzisa iphepha lokuhlunga (isib. I-Whatman No. 41 noma ilingana) kumngcwabo we-Buchner ohlanganiswe nebhola lokuhlunga elihlanzekile le-500-mL. Ngaphandle kwalokho, i-decant ikhiphe ibhodlela le-centrifuge ne-centrifuge ngesivinini esincane ukuze ususe izinhlayiya.
    11.3.5 Phinda ukhiqize isiqephu izikhathi ezimbili ngokwengeziwe izingxenye eziyi-100-mL ezengeziwe ze-solvent ehlanzekile. Decant off the solvent emva isizinda ngasinye ultrasonic. Ngemuva kwesizinda sokugcina se-ultrasonic, uthele yonke isampula kumngcwabo weBuchner, susela i-beaker nge-solvent isizinda, bese ufaka isiphuzo emngceleni.

    Izinyathelo emva kokubeletha

    Faka i-vacuum ku-flask yokuhlunga, bese uqoqa ukukhishwa kwe-solvent. Qhubeka ukuhlunga kuze kube yilapho yonke i-solvent ebonakalayo isusiwe emgodini, kodwa ungazami ukuqina ngokuphelele isampula, njengoba ukuqhubeka kokusebenza kwe-vacuum kungaholela ekulahlekelweni kwamanye ama-analytes. Ngaphandle kwalokho, uma i-centrifugation isetshenziswe ku-Sec. 11.3.4, udlulisele isampula sonke kwibhodlela le-centrifuge. I-Centrifuge ngejubane eliphansi, bese ubeka umquba we-solvent ebhodleleni.
    11.3.6 Uma kunesidingo, gxila ekukhishwe ngaphambi kokuhlaziywa ngemuva kwenqubo ku-Sec.11.5. Uma kungenjalo, qhubeka ku-Sec. 11.7.
    Sonication yisinyathelo esibalulekile ngesikhathi sokulungiselela isampula

    UP200St nge-tip-micro ye-sonication yesampula

    Isicelo solwazi




    Qaphela kwethu Inqubomgomo yobumfihlo.


    11.4 Inqubo yesikhumba sezinga eliphakathi / eliphakeme

    Le nqubo isebenza kuma-sampuli aqinile okulindeleke ukuba aqukethe ngaphezulu kuka-20 mg / kg yezihlaziyi eziphilayo.

    Izinyathelo ngaphambi kwe-sonication

    11.4.1 Dlulisa cishe 2 g yesampula ku-20mL. Sula umlomo we-vial ngezicubu ukuze ususe noma iyiphi isampula. Thatha isikhala ngaphambi kokuqhubeka nesampula esilandelayo ukuze ugweme noma yikuphi ukungcola okuphambene. Qopha isisindo eseduze 0.1 g.
    11.4.2 Ukuze isampula kuqoqo ngalinye elikhethiwe ukupaka, faka i-1.0 mL yesisombululo se-matrix spiking. Xhumana no-Method 3500 ukuze uthole isiqondiso ekukhethweni okufaneleko kwe-matrix spiking compounds nama-concentrations. Bona futhi inothi ku-Sec. 11.3.
    11.4.3 Engeza i-1.0 mL yesisombululo sokwenza isiphakamiso esiphezulu kuzo zonke amasampuli, amasampuli aphethiwe, amasampuli e-QC, kanye nezikhala. Xhumana no-Method 3500 ukuze uthole isiqondiso ekukhethweni okufaneleko kwe-matrix spiking compounds nama-concentrations. Bona futhi inothi ku-Sec. 11.3.
    11.4.4 Uma i-gel permeation ihlanza (bheka indlela 3640) kufanele isetshenziswe, umhlaziyi kufanele abe wengeze kabili ivolumu yesisombululo sokuphenya (kanye nesisombululo se-matrix spiking, lapho kufanele khona), noma ugxilise ukukhipha kokugcina kube yingxenye yevolumu evamile , ukukhokhela isigamu sokukhishwa esilahlekile ngenxa yokulayisha kwekholomu ye-GPC.
    11.4.5 Amasampuli angama-nonporous noma amanzi (uhlobo lwama-gummy noma ubumba) olungenawo ukuthungwa kwehlabathi okungahambi kahle mahhala kufanele axutshwe no-2 g we-sodium sulfate anhydrous, besebenzisa i-spatula. Uma kudingeka, i-sodium sulfate engaphezulu ingafakwa. Ngemuva kokungezwa kwe-sulfate ye-sodium, isampula kufanele ikhululeke mahhala (bheka inothi ku-Sec. 11.3).
    11.4.6 Masinyane wengeze noma yiliphi ivolumu yokuxazulula kuyadingeka ukuze ulethe ivolumu yokugcina ibe ngu-10.0 mL, ucabangela umthamo owengeziwe wezinsizakalo nama-matrix spikes (bheka iSahluko 7.4 noThebula 2 ngolwazi ngokukhetha kwamakhemikhali).

    11.4.7 Susa isampula nge-s / ultra-inch tapered microtip ultrasonic probe ngamaminithi angu-2 ekulungiseleleni kokukhipha okukhiphayo 5 kanye nemodi yokushintsha emjikelezweni wokuphambana nomphesenti ku-50%.
    11.4.8 Phakamisa i-Pasteur ipipette elahlwe ngamasenti amabili kuya ku-3 we-glass wool. Hlunga isampula itholakale nge-wool ingilazi bese uqoqa ukukhishwa kwisitsha esifanele. Yonke imitha eyi-10 ye-solvent yokususwa ayikwazi ukutholakala esampheni. Ngakho-ke, umhlaziyi kufanele aqoqe ivolumu efanelekile ngobuzwe bendlela yokunquma okufanele isetshenziswe. Ngokwesibonelo, ngezindlela ezingadingi ukukhipha ukugxila phambili (isib. Indlela ye-Method 8081 isebenzisa umthamo wokugcina wokugcina we-10 mL), ukukhishwa kungase kuqoqwe ku-vial scintillation noma esinye isitsha esingasetshenziswa. Ukuze uthole ukukhishwa okuzodinga ukuhlushwa okuqhubekayo, kuhle ukuqoqa ivolumu evamile yazo zonke izibonelo ezinjalo ukuze kube lula ukubalwa kwemiphumela yesampula yokugcina. Ngokwesibonelo, qoqa u-5.0 mL wokukhishwa kwiphubhu ehlanzekile yokugxila. Leli volumu limelela ingxenye eyodwa yenani eliphelele le-extract sample. Uma kunesidingo, bhala i-akhawunti “ukulahleka” okuyingxenye yokukhishwa kwezibalo zokugcina zesampula, noma ugxilise ukukhishwa kokugcina kwesigamu somqulu wokugcina wokuqokwa (isib. 0.5 mL vs. 1.0 mL) ukukhokhela ukulahleka.
    11.4.9 Uma kunesidingo, gxila ekukhishwe ngaphambi kokuhlaziywa ngemuva kwenqubo kuSec. 11.5 noma iSec. 11.6. Uma kungenjalo, qhubeka ku-Sec. 11.7.

    Amasu okugxila

    Inqubo yokuhlushwa ye-Kuderna-Danish (KD)
    Lapho kudingekile ukuhlangabezana nenqubo yokuzwela, izitshalo zesampula ezivela emkhatsini ophansi noma emkhatsini wesikhulumi sezinga eliphezulu noma eziphakemeyo zingase zibhekiswe emtatsheni wokugcina okudingekayo ukuze kusetshenziswe indlela kanye nesicelo esithile okufanele sisetshenziswe, ngokusebenzisa uhlelo lwe-KD noma ukuthuthwa kwe-nitrogen.
    11.5.1 Hlanganisa i-Kuderna-Danish (KD) concentrator ngokufaka ithubhu ye-concentrator ye-10-mL ukuya esikhwameni sokuphuza.
    11.5.2 Yima umkhiqizo ngokuwudlulisa ngokusebenzisa ikholomu yokumisa equkethe cishe ama-10 g we-sodium sulfate anhydrous. Qoqa ukukhipha okomile ku-concentrator ye-KD.
    11.5.3 Hlanganisa i-tube yokuqoqa kanye nokomisa ikholomu ku-Flask KD ene-20-mL ingxenye engezansi ye-solvent ukuze kutholakale ukudluliselwa okulinganiselwe.
    11.5.4 Engeza i-chips eyodwa noma ezimbili ehlanzekile ebilisiwe ebhodini bese unamathisela ikholomu ye-ball Snyder. Namathisela i-glassware yokutakula i-glassware (i-condenser kanye nedivayisi yokuqoqa, bheka iSec 6.9) kukholomu le-Snyder lamadivayisi we-KD, ngokulandela imiyalelo yomkhiqizi. Hlanganisa ngaphambili ikholomu ye-Snyder ngokungeza cishe i-1 mL ye-methylene chloride (noma enye i-solvent efanele) kuze kube phezulu kwekholomu. Beka amadivaysi e-KD ngamanzi ashisayo okugeza (15 – I-EC engaphezu kwendawo yokubilisa ye-solvent) ukuze i-concentrator tube igxiliswe kancane emanzini ashisayo futhi yonke indawo engezansi engaphansi kwesibhakabhaka igezwa ngomoya oshisayo. Lungisa isikhundla esiqondile sama-apparatus kanye nokushisa kwamanzi njengoba kudingeka ukuze uqedele ukuhlushwa ngo-10 – 20 iminithi. Ngesilinganiso esifanele sokuphuza izidakamizwa, amabhola ekholomu azoxoxa ngentshiseko, kodwa amakamelo ngeke agcwalise. Uma ivolumu ebonakalayo yamanzi ifinyelela ku-1 mL, susa amadivaysi e-KD emanzini okugezela futhi uvumele ukuba idle futhi ipholile okungenani iminithi eyi-10.
    QAPHELA: Ungavumeli ukukhipha kuhambe, ngoba lokhu kuzoholela ekulahlekelweni okukhulu kwezihlaziyi ezithile. Izibulala-zinambuzane ze-Organophosphorus zitholakala ikakhulukazi ekulahlekelweni okunjalo.
    11.5.4.1 Uma kudingekile ukushintshaniswa kwe-solvent (njengoba kuboniswe kuThebula 2 noma indlela efanelekayo), susa okwesikhashana ikholomu ye-Snyder, engeza i-50 mL ye-solvent exchange kanye ne-chip entsha yokubilisa.
    11.5.4.2 Faka kabusha ikholomu yeSnyder. Gxila ekukhishwe, ukukhulisa izinga lokushisa kwamanzi okugeza, uma kunesidingo, ukugcina izinga lokuhlanza izidakamizwa.
    11.5.5 Susa ikholomu ye-Snyder. Hlanza isibhakela se-KD namalunga angaphansi kwekholomu ye-Snyder engxenyeni ye-concentrator ene-1 – 2 ml we-solvent. Ukukhishwa kungase kuqhutshekwe phambili ngokusebenzisa elinye lamasu akhishwe ku-Sec. 11.6, noma ulungiselelwe umthamo wokugcina we-5.0 – 10.0 mL usebenzisa i-solvent efanele (bheka ithebula 2 noma indlela efanele yokunquma). Uma kukhona amakristalu esulfure, qhubeka ku-Method 3660 ukuze uhlanzwe.
    11.6 Uma kukhona okunye okudingekayo, sebenzisa inqubo yekholomu encane (bheka iSigaba 11.6.1) noma inqubo yokuthuthwa kwe-nitrogen (bheka iSigaba 11.6.2).
    11.6.1 inqubo yekholomu ye-Micro-Snyder
    11.6.1.1 Engeza i-chip ehlanzekile yokubilisa emgodini we-concentrator bese unamathisela ikholomu emibili ye-micro-Snyder ngqo kwi-tube concentrator. Namathisela i-glassware yokuthola i-glassware yokutakula (i-condenser kanye nedivayisi yeqoqo) ekolini elincane le-Snyder lamadivayisi we-KD, ngokulandela imiyalelo yomkhiqizi. Hlanganisa ngaphambili ikholomu ye-Snyder ngokungeza u-0.5 mL we-methylene chloride noma isisombululo sokushintshanisa phezulu kwekholomu. Beka amakhemikhali amancane okuhlushwa emanzini ashisayo okugeza ukuze i-concentrator tube igxilwe emanzini ashisayo. Lungisa isikhundla esiqondile sama-apparatus kanye nokushisa kwamanzi, uma kudingekile, ukuqedela ukuhlushwa ku-5 – 10 iminithi. Ngesilinganiso esifanele sokuphuza izidakamizwa amabhola ekholomu azoxoxa ngentshiseko, kodwa amakamelo ngeke agcwalise.
    11.6.1.2 Uma ivolumu ebonakalayo yamanzi ifinyelela ku-0.5 mL, susa ama-apparatus emanzini okugezela futhi uvumele ukuba idle futhi ipholile okungenani iminithi eyi-10. Susa ikholomu ye-Snyder bese ugeza amalunga ayo aphansi engxenyeni ye-concentrator ene-0.2mL ye-solvent. Lungisa ivolumu yokukhipha kokugcina ibe yi-1.0 – I-2.0 mL.
    QAPHELA: Ungavumeli ukukhipha kuhambe, ngoba lokhu kuzoholela ekulahlekelweni okukhulu kwezihlaziyi ezithile. Izibulala-zinambuzane ze-Organophosphorus zitholakala ikakhulukazi ekulahlekelweni okunjalo.
    11.6.2 izinqubo zokufudumala kwe-nitrojeni
    11.6.2.1 Beka i-concentrator tube ekugezeni okufudumele (30 degC) futhi uchithe umthamo wokuxazulula u-0.5 mL usebenzisa umfudlana omile we nitrogen ohlanzekile, omile (ohlanjwe ngendwangu yesikhumba esebenzayo).
    QAPHELA: I-tubing entsha ye-plastiki akumele isetshenziswe phakathi kwesibambiso sekhabhoni nesampula, ngoba ingase iqalise ukuphazamiseka kwe-phthalate.
    11.6.2.2 Gcoba udonga lwangaphakathi lwe tube concentrator izikhathi eziningana nge-solvent ngesikhathi sokuhlushwa. Ngesikhathi se-evaporation, misa isikhumbi se-concentrator ukuze ugweme ukukhipha amanzi ngaphakathi. Ngaphansi kwezinqubo ezivamile, ukukhishwa akufanele kuvunyelwe ukuba kube omile.
    QAPHELA: Ungavumeli ukukhipha kuhambe, ngoba lokhu kuzoholela ekulahlekelweni okukhulu kwezihlaziyi ezithile. Izibulala-zinambuzane ze-Organophosphorus zitholakala ikakhulukazi ekulahlekelweni okunjalo.
    11.7 Ukukhishwa kungase kube khona ukuhlanza izinqubo noma ukuhlaziywa kwabahlaziyili abahlosiwe besebenzisa izinqubo ezifanele zokunquma. Uma ukuphathwa okukodwa kokukhipha ngeke kwenziwe ngokushesha, vimbela ithebhu ye-concentrator kanye nesitolo esiqandisini. Uma ukukhishwa kuzogcinwa isikhathi eside kunezinsuku ezingu-2, kufanele kudluliselwe ku-vial ene-PTFE-lined screw-cap, futhi ibhalwe ngokufanele.

    12. Ukuhlaziywa kwedatha kanye nezibalo

    Azikho izibalo ezihlotshaniswa ngokucacile nale nqubo yesikhumba. Bheka indlela efanele yokunquma ukubalwa kwemiphumela yesampula yokugcina.

    13. Indlela Yokusebenza

    Bheka izindlela ezifanele zokunquma izibonelo zedatha nokusebenza. Idatha yokusebenza nolwazi oluhlobene lunikezwa ngezindlela ze-SW-846 kuphela njengezibonelo nesiqondiso. Idatha ayimeleli ukusebenza okudingekayo kubasebenzisi bezindlela. Esikhundleni salokho, izindlela zokusebenza kufanele zenziwe ngesisekelo esithile sephrojekthi, futhi i-laboratory kufanele ibeke izindlela zokusebenza ngaphakathi kwe-QC yokusebenzisa le ndlela. Le datha yokusebenza ayihloselwe ukuba ibe futhi akumele isetshenziswe njengendlela yokuvuma yokwamukela i-QC ngokuphelele ngezinhloso zokugunyazwa kwelabhoratri.

    14. Ukungcola Ukuvimbela

    14.1 Ukuvimbela ukungcoliswa kwemvelo kuhlanganisa noma iyiphi indlela eyanciphisa noma ekuqedeni ubuningi kanye / noma ubuthi obuncithakalo ngesikhathi sokuzalwa. Amathuba amaningi okuvimbela ukungcola akhona ekusebenzeni kwama laboratory. I-EPA isungule ubuchwepheshe obuningi bokuphathwa kwemvelo okubeka ukuvimbela ukungcola njengendlela yokuphatha yokukhetha kokuqala. Noma nini lapho kungenzeka, abasebenzi be-laboratory kufanele basebenzise amasu okuvikela ukungcola ukubhekana nokukhiqiza imfucuza yabo. Ngenkathi imfucuza ingenakuhliswa ngokuyisisekelo emthonjeni, i-Agency itusa ukuvuselelwa njengendlela elandelayo engcono kakhulu.
    14.2 Ukuze uthole ulwazi mayelana nokuvimbela ukungcola okungase kusetshenziswe kuma-laboratories nezikhungo zokucwaninga uthintana nokuncane Kungcono: I-Laboratory Chemical Management Yokuncishiswa Kwemfucuza etholakala eMnyangweni Wezobudlelwano BobuHulumeni NoSayensi We-American Chemical Society, 1155 16th St., NW Washington, DC 20036 , https://www.acs.org.

    Ukuphathwa Kwemfucuza

    I-Environmental Protection Agency idinga ukuthi imikhuba yokuphathwa kwemfucuza ye-laboratory iqhutshwe ngokuhambisana nayo yonke imithetho esebenzayo kanye nemigomo. ISikhungo sinxusa ama-laboratories ukuvikela umoya, amanzi, kanye nomhlaba ngokunciphisa nokulawula konke okukhishwayo
    ama-hood kanye nemisebenzi yamabhentshi, ngokuhambisana nencwadi nemoya yanoma yiziphi izimvume nemithethonqubo yokukhishwa kwamanzi okuhambisa umkhumbi, futhi ngokuhambisana nayo yonke imithethonqubo enobungozi eqinile nenobungozi, ikakhulukazi imithethonqubo eyingozi yokuhlonza imfucuza kanye nemingcele yokulahla umhlaba. Ukuze uthole olunye ulwazi mayelana nokulawulwa kwemfucuza, thintana neNcwadi Yokulawulwa Kwemvelo yabasebenzi beLobhu Laboratory etholakale ku-American Chemical Society ekhelini elibalulwe kuSec. 14.2.

    Amaphuzu

    • US EPA, “Isifundo sokuqhathanisa okubambisana: Izindlela zeMikhiqizo enokuzenzekelayo neyimizuzu emibili,” I-Laboratory Monitoring Systems Laboratory, iHhovisi Lokucwaninga Nokuthuthukiswa, Las Vegas, NV, EPA 600 / 4-84-027, 1984.
    • CS Hein, uPJ Marsden, AS Shurtleff, “Ukuhlola Izindlela 3540 (Soxhlet) no-3550 (Sonication) yokuHlola kweSithasiselo IX Ukuhlaziywa okuvela kumaSampuli aqinile,” S-CUBED, Umbiko we-EPA Contract 68-03-33-75, Isabelo Somsebenzi No. 03, Document No. SSS-R- 88-9436, Okthoba, 1988.

    Xhumana Nathi / Cela Ukwaziswa Olwengeziwe

    Khuluma nathi mayelana nezidingo zakho zokucubungula. Sizosikisela ukusetha nokulungiswa kwemingcele efanele yephrojekthi yakho.





    Sicela uqaphele wethu Inqubomgomo yobumfihlo.




    Amaqiniso Okufanele Ukwazi

    I-ultrasonic izicubu ze-homogenizers ngokuvamile ibizwa ngokuthi i-sonicator yesondlo, i-lyser ye-sonic, i-ultrasound ephazamisayo, i-grinder ye-ultrasonic, i-sono-ruptor, i-sonifier, i-sonic dismembrator, i-cell disrupter, i-ultrasonic disperser noma i-dissolver. Amagama ahlukene avela ezinhlobonhlobo zokusebenza ezingagcwaliseka nge-sonication.

    Abahlukahlukene sonotrode osayizi nomumo izinhlelo zokusebenza ahlukahlukene.

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    Isicelo solwazi




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