17.2 Ukunqunywa Okufanelekile Kwesitashi KumaPolymer Ancibilikayo Amanzi
17.2.1 Isimiso
17.2.1.1 Inhloso yalokhu kuhlola ukuthola ukuba khona kwesitashi noma okuphuma kokunye kwesitashi kumapholima ayimpuphu noma ayimbudumbudu ancibilika emanzini njenge-PAC-LV.
17.2.1.2.Ukutholwa kwesisombululo se-PAC-LV ngokungeza isisombululo semineral/iodide*
Uma i-amylose ikhona, ihunyushwa ibe yinkimbinkimbi enemibala.
17.2.2 Ama-reagents nezinto zokwakha
a) Amanzi akhiqiziwe noma agayiwe
b) Isixazululo se-Nitrate, isb Merck 1.09.089.1000 (CAS No. 7553-56-2) 7) 0.05.
c) Iodide ye-Potassium 1 Merck 1.0504 3.0250 PA (CAS No. 7681-11-0
d) I-sodium hydroxide (NaOH) (i-CAS No. 1310-73-2): isisombululo se-dilute, 0.1% -0.5%.
17.2.3 Izinsiza
17.2.3.1 I-Stirrer 1ta Model 98 Multi-shaft Stirrers ifakwe impeller engu-9B29X noma iblade efanayo nenye
i-waveform ye-sinusoidal,blade ububanzi approx.25 mm (i-lin, ubuso obushaywe ngesibhakela phezulu).
17.2.3.2 Inkomishi enyakazayo inosayizi ocishe ube ngu-180 mm (7.1 in) ukujula, 97 mm (3-5/6 in) ububanzi
umlomo ophezulu,kanye no-70 mm (2.75 in) ububanzi besisekelo esiphansi (isb. uhlobo lwe-M110-D i-Hamilton Beachinkomishi enyakazayo
noma into efanayo).(Ingilazi engu-600 ml nayo ingasetshenziswa esikhundleni.)
17.2.3.3 Izinkezo zaselabhorethri.
17.2.3.4 I-Scraper.
17.2.3.5 Ibhalansi: Ukunemba ngu-0.01 g.
17.2.3.6 amaflask eVolumetric 100ml
17.2.3.7 Amapayipi e-Pasteur noma amapulasitiki adonsayo.
17.2.3.8 Isikhathi: Imishini noma i-electronic, ukunemba 0.1 imiz.17.2.3.9 pH amamitha nama-electrode e-pH:
isb Thermo Russell thayipha KDCW1 19)
17.2.3.10 Amadivayisi e-Polymeric feeding (isb. Fann 10) noma 0Fl uhlobo 11))
17.2.3.11 Amashubhu okuhlola.
17.2.4 Inqubo - Ukulungiswa Kwesixazululo se-Iodine/Potassium Iodide
17.2.4.1 Engeza u-10 μl ± 0.1 ml wesisombululo se-iodine esingu-0.05 mol / l ku-100 ml ± 0.1 ml yefulaski yevolumu.
17.2.4.2 Engeza u-0.60 g±..01 g I-Potassium iodide (KI), nyakazisa iflaski ukuze uyincibilikise.
17.2.4.3 Engeza amanzi akhishwe i-deionized kumaki angu-100 ml bese uxuba kahle.Qopha usuku lokulungiselela.
17.2.4.4 Isixazululo se-iodine/iodide esakhiwe sigcinwa esitsheni esivaliwe bese sigcinwa endaweni emnyama, epholile neyomile.
Idethi yokuphelelwa yisikhathi ifinyelela ezinyangeni ezintathu futhi kufanele ilahlwe futhi yakhiwe kabusha.
17.2.5 Inqubo - Ukulungiselelwa Kwesixazululo Se-PAC-LV Nokutholwa Kwesitashi
17.2.5.1 Lungiselela isixazululo samanzi esingu-596 se-PAC-LV esizohlolwa.
Engeza u-380 g ± 0.1 g wamanzi akhishiwe enkomishini yokuxuba, engeza u-2 g ± 0.1 g we-PAC-LV ngesivinini esifanayo
ngenkathi ugqugquzela i-stirrer,futhi isikhathi sokwengeza kufanele siqhubeke amasekhondi angama-60 kuye kwangama-120.
Isampula kufanele yengezwe kusiphithiphithi enkomishini yokuxuba, futhi ugweme ukunyakazisa shaft ukunciphisa uthuli.
Kungcono ukusebenzisa idivayisi yokushaja ye-polymer ku-17.2.3.10.
17.2.5.2 Ngemva kokugqugquzela imizuzu emi-5 ± 0.1 iminithi, susa inkomishi enyakazayo kusivusi bese uklebhula wonke ama-PAC-LV anamathiselwe kuwo.
udonga lwenkomishi nge-spatula.Wonke ama-PAC-LV anamathele ku-scraper axutshwe esixazululweni.
17.2.5.3 Kala i-pH yesisombululo.Uma i-pH ingaphansi kuka-10, engeza isixazululo esixubile se-NaOH dropwise.
Khuphula i-pH ibe ngu-10
17.2.5.4.Buyisela inkomishi enyakazayo ku-stirrer futhi uqhubeke ugqugquzela.Isikhathi esiphelele sokunyakazisa kufanele sibe imizuzu engama-20 ± 1 Min.
17.2.5.5 Faka u-2 ml wesixazululo sesampula eshubhuni lokuhlola bese wengeza amaconsi ama-3 esixazululo se-iodine/iodide,
kuze kufike kumaconsi angama-30.
17.2.5.6 Lungiselela izivivinyo ezintathu ezingenalutho ngamanzi acwecwe.Faka amaconsi ama-3, amathonsi ayi-9, amathonsi angama-30 esixazululo se-iodine/iodide
amashubhu okuhlola ukuqhathanisa.
17.2.5.7 Ngemva kokwengeza amaconsi angu-3 esixazululo isikhathi ngasinye, nyakazisa ithubhu ukuze uqhathanise umbala wesixazululo sesampula.
ngokuhlolwa okungenalutho.Ukuqhathaniswa kwemibala kufanele kwenziwe ngokumelene nesizinda esimhlophe.
17.2.6 Ukuzimisela - Ukutholwa Kwesitashi se-PAC-LV
17.2.6.1 Uma isampula lesixazululo esizohlolwa sibonisa umbala ophuzi ofanayo nowesivivinyo esingenalutho, isampula alikwenzi lokho.
iqukethe noma yisiphi isitashi noma okuphuma kwesitashi.
17.2.6.2 Uma kukhona omunye umbala, kukhonjiswa ngokuqinile ukuthi kukhona okuphumayo kwesitashi noma kwesitashi.
17.2.6.3 Uma umbala ubonakala unyamalala ngokushesha, okubonisa ukuba khona kwe-ejenti yokunciphisa, kulokhu,
qhubeka nokwengeza i-dropwise iodine / iodide Isixazululo, ukuqhathanisa umbala nokuhlolwa okungenalutho, bheka 17.2.61.
17.2.6.4 Uma kutholwa noma yikuphi ukusabela kombala okwehlukile ku-17.2.6.1, akudingekile ukuqhubeka nokuhlola okulandelayo.
17.3 Umswakama
17.3.1 I-Apparatus 17.3.1.1 I-Oven: Ilawuleka ku-105°C±3°C (220±5>.
17.3.1.2 Ibhalansi: Ukunemba kwe-0.01 g.
17.3.1.3 Isitsha sokuhwamuka: Umthamo 150 ml.
17.3.1.4 I-Scraper.
17.3.1.5 I-Desiccant: Iqukethe i-desiccant (CAS No. 7778-18-9) i-desiccant, noma okulinganayo
17.3.2 Inqubo Yokuhlola
17.3.2.1 Isisindo esingu-10 g ± 0.1 g Isampula le-PAC-LV elizokalwa Esitsheni esihwamukayo, rekhoda isisindo sesampula m
17.3.2.2 Yomisa isampula kuhhavini amahora ama-4
17.3.2.3 Pholisa isampula emshinini wokukhipha i-desika ekamelweni lokushisa17.3.2.4 Kala kabusha isitsha esihwamukayo esiqukethe
i-PAC-LV eyomile, rekhoda ikhwalithi yesampula eyomile m2.
17.3.3 Ukubala
17.4 Ukulahlekelwa uketshezi
17.4.1 Ama-reagents nezinto zokwakha
17.4.1.1 Usawoti wasolwandle: Hlola umhlabathi ngokwe-ASTM D 1141-98 (2003) 12
17.4.1.2 API indinganiso.
17.4.1.3 I-Potassium Chloride (CAS No. 7447-40-7)
17.4.1.4 I-Sodium Bicarbonate (i-CAS No. 144-55-8).
17.4.1.5 Amanzi akhishiwe noma acwecwe.
17.4.2 Izinsimbi
17.4.2.1 I-thermometer: Ibanga lokulinganisa lingu-0 °C ~ 60 °C, ukunemba kungu-0.5 °C
(ibanga lokulinganisa lingu-32 °F ~ 140 °F, ukunemba kungu-1.0 °F)
17.4.2.2 Ibhalansi: Ukunemba ngu-0.01g.
17.4.2.3 I-Stirrer: Uma i-Type 9B multi-shaft stirrer ifakwe i-9B20x impeller,i-shaft kufanele ifakwea
ongashadilei-sine wave blade enobubanzi bensingo obungaba ngu-25 mm (1 in) enobuso obugxivizwe phezulu.
17.4.2.4 Inkomishi enyakazayo inosayizi ocishe ube ngu-180 mm (7.1 in) ukujula, 97 mm (3-5/6 in) ububanzi
umlomo ongenhla,kanye no-70 mm (2.75 in) ububanzi besisekelo esingezansi (isb. Inkomishi yohlobo lwe-M110-D i-Hamilton Beach).
17.4.2.5 isikhihli.
17.4.2.6 Isitsha: Ingilazi noma ipulasitiki, enesivalo noma isivalo, esetshenziselwa amanzi anosawoti.
17.4.2.7 Viscometers: Ugesi, ukufunda okuqondile, ngokuhambisana ne-ISO 10414-1
17.4.2.8 Izibali-sikhathi: Okubili, okomshini noma nge-elekthronikhi, nokunemba okungu-0.1 min ngesikhathi esikalwe kulokhu kuhlolwa.
17.4.2.9 Izinsiza Zokuhlunga: Izinga lokushisa eliphansi kanye nohlobo lomfutho, ngokuhambisana nezinhlinzeko zeSahluko 7
ISO 10414-1:2008.
17.4.2.10 Amasilinda okulinganisa: Amabili, anamandla angu-10 ml ± 0.1 ml no-500 ml ± 5 ml *
17.4.2.11 Idivayisi yokuphakela i-polymer (uhlobo lwe-Fann noma uhlobo lwe-OFI).
17.4.3 Inqubo Yokuhlola - Ukulahleka Koketshezi Lwe-PAC-LV
17.4.3.1 Engeza u-42 g ± 0.01 g kasawoti wasolwandle ku-11 ± 2 ml wamanzi angcolile.
17.4.3.2 Ku-358 g wesixazululo sikasawoti wasolwandle, engeza u-35.0 g ± 0.01 g we-potassium chloride (KCl).
17.4.3.3 Ngemva kokushukumisa imizuzu emi-3 ± 0.1 iminithi, engeza u-1.0 g ± 0.01 g we-sodium bicarbonate.
17.4.3.4 Ngemva kokushukumisa amaminithi angu-3±0.1 amaminithi, engeza izinga le-API elingu-28.0 g±0.01 g ukuze ulihlole.
17.4.3.5 Ngemva kokugqugquzela imizuzu emi-5±0.1, susa inkomishi enyakazayo ku-stirrer bese uyinwaya odongeni nge-scraper.
Wonke amazinga e-API ahlola inhlabathi.Yonke inhlabathi yokuhlola ejwayelekile ye-API enamathele ku-scraper ixutshwe ekumisweni.
17.4.3.6 Buyisela inkomishi enyakazayo ku-stirrer futhi uqhubeke ugoqa imizuzu emi-5 ± 0.1 imiz.
17.4.3.7 Isisindo esingu-2.0 g±0.01 g PAC-L.
17.4.3.8 Kancane kancane ngenkathi ushukumisa isivusi, engeza i-PAC-LV ngesilinganiso esifanayo.
Isikhathi sokwengeza kufanele sithathe cishe imizuzwana engama-60.I-PAC-LV kufanele yengezwe ku-vortex enkomishini yokuxuba
futhi ugweme i-shaft eshukumisayo ukuze unciphise uthuli.Kungcono ukusebenzisa idivayisi ye-polymer feed ku-17.4.2.11.
17.4.3.9 Ngemva kokugqugquzela imizuzu emi-5 ± 0.1 iminithi, susa inkomishi enyakazayo kwisivusi bese usebenzisa isikhafu ukuze usule konke.
I-PAC-L inamathele odongeni lwenkomishi.Wonke ama-PAC-LV anamathele ku-scraper ahlanganiswe nokumiswa.
17.4.3.10 Buyisela imbiza kusivusi bese uqhubeke uguqisa.Uma kunesidingo, ngemuva kwemizuzu emi-5 nemizuzu eyi-10, susa ukugoqa
inkomishi kusukela ku-stirrer bese usula yonke i-PAC-L enamathele odongeni lwenkomishi.Isikhathi esiphelele sokuvuselela kusukela ku-
ukuqala kokwengezwa kwe-PAC-LV kufanele kube amaminithi angu-20 ± 1 iminithi.
17.4.3.11 Ku-25 °C ± 1 °C (77 °F ± 2 °F),gcina ukumiswa esitsheni esivaliwe noma esivalekile amahora angu-16 ± 0.5 h.
Qopha izinga lokushisa lokuphulukisa kanye nesikhathi sokuphulukisa.
17.4.3.12 Ngemva kokuphulukisa, gubha ukumiswa ku-stirrer imizuzu engu-5 ± 0.1 min.
17.4.3.13 Thela ukumiswa kwe-PAC-LV enkomishini yokuhlunga.Ngaphambi kokuthululela ekumisweni,qiniseka ukuthikonkeizingxenye
enkomishini yokuhlunga yomile futhi iringi yophawu ayikhubazekile noma ayigugi.Izinga lokushisa lokumiswa kufanele libe
25°C±1°C (77°F±2).Ukufika phakathi kuka-13 mm (0.5 in) ukusuka phezulu kwenkomishi.Hlanganisa inkomishi yokuhlunga, faka inkomishi yokuhlunga
umbambi, vala i-valve yokusiza ukucindezela, bese ubeka isitsha ngaphansi kweshubhu lokudonsa.
17.4.3.14 Misa isibali sikhathi sibe yimizuzu engu-7.5 futhi enye isethwe kumaminithi angu-30.Ngesikhathi esifanayo qala izibali sikhathi ezimbili futhi ulungise ukucindezela kwenkomishi ukuze
690 kPa ± 35 kPa (100 psi ± 5 psi).Ukucindezela kufanele kuhlinzekwe ngomoya ocindezelweyo, i-nitrogen noma i-helium.
Kufanele iqedwe phakathi kwamasekhondi angu-15.
17.4.3.15 ekuqaleni Ekupheleni kwesibali sikhathi kuphela, khipha isiqukathi bese ukhipha noma yiluphi uketshezi olunamathela emseleni futhi
yilahle.Isilinda esomile esingu-10 ml safakwa ngaphansi komsele futhi isihlungi saqoqwa kuze kube ngowesibili.
isibali sikhathi siphelelwe yisikhathi.Susa isilinda bese urekhoda umthamo we-filtrate eqoqwe.
17.4.4 Ukubala - Ukulahleka kwe-PAC-LV Inani lika-V elihlungiwe libalwa ngokwezibalo (43) ku-ml;
I-v-2xVe (43) lapho: 1⁄2_ ivolumu yokuhlunga eqoqwe phakathi kwamaminithi angu-7.5 nama-30 amaminithi.Iyunithi ingu-ml.
17.5 I-Viscosity ebonakalayo Yezixazululo
17.5.1 Inqubo Yokuhlola - I-Viscosity ebonakalayo Yesixazululo
17.5.1.1 Engeza u-42 g ± 0.01 g kasawoti wasolwandle ku-11 ± 2 ml wamanzi angcolile.
17.5.1.2 Ku-358 g wesixazululo sikasawoti wasolwandle, engeza u-35.0 g ± 0.01 g we-potassium chloride (KCl).
17.5.1.3 Isisindo 5.0 g ± 0.01 g PAC-Lv.Kancane kancane ngenkathi uvuselela ku-stirrer, engeza i-PAC-LV ngesilinganiso esifanayo.
Isikhathi sokwengeza kufanele sithathe cishe iminithi elingu-1.I-PAC-LV kufanele yengezwe ku-vortex enkomishini yokuxuba
futhi ugweme i-shaft eshukumisayo ukuze unciphise uthuli.
17.5.1.4 Ngemva kokunyakazisa imizuzu emi-5 ± 0.1 iminithi, susa inkomishi enyakazayo kusivusi, khuhla yonke i-PACw enamathiselwe odongeni lwenkomishi.
nge-spatula, bese uxuba yonke i-PAC-LV enamathele ku-spatula kuya ekumisweni.
17.5.1.5 Buyisela imbiza emshinini wokuhlanganisa bese uqhubeka uguqisa.Uma kunesidingo, susa inkomishi yesiqhumiso ku-mixer ngemva kwalokho
Imizuzu emi-5 nemizuzu eyi-10, khuhla wonke ama-PAC-W anamathele odongeni lwenkomishi.Isikhathi esiphelele sokunyakazisa kusukela ekuqaleni kokwengezwa kwe
I-PAC-LV kufanele ibe yimizuzu engu-20 ± 1 iminithi.
17.5.1.6 Ku-25 °C ± 1 °C (777 ± 27), misa ukumiswa amahora angu-16 ± 0.5 h esitsheni esivaliwe noma esivalekile.
Qopha izinga lokushisa lokuphulukisa kanye nesikhathi sokuphulukisa ”
17.5.1.7 Gcoba ukumiswa ku-stirrer imizuzu emi-5 ± 0.1 min.
17.7.5.1.8 Thela ikhambi enkomishini yesampula efakwe i-viscometer yokufunda eqondile” ku-25 °C ± 1 °C (77 Ngaphansi
isimo sika ° F ± 2), ukumiswa kwafundwa ku-600 r / min.
17.5.2 Ukubala - I-viscosity ebonakalayo yesixazululo
Bala i-viscosity ebonakalayo yesixazululo ngokuya ngefomula (44), kuma-mPas:
VA=R600/2 (44)
I-R600-viscometer yokufunda ku-600 r / min.Rekhoda umphumela wokubala
Isikhathi sokuthumela: Nov-12-2020