17.2 Ukumiselwa koMgangatho wesitatshi kwiiPolymers eziNyibilikayo ngaManzi
17.2.1 Umgaqo
17.2.1.1 Injongo yolu vavanyo kukufumanisa ubukho besitatshi okanye izinto eziphuma kwistatshi kumgubo okanye iipolima ezinyibilikayo emanzini ezifana nePAC-LV.
17.2.1.2.Ukufunyanwa kwesisombululo sePAC-LV ngokudibanisa isisombululo seminerali/iodide*
Ukuba i-amylose ikhona, inikezelwa kwi-complex enemibala.
17.2.2 Ii-reagents kunye nemathiriyeli
a) Amanzi adiliweyo okanye adiyiliweyo
b) Isisombululo seNitrate, umz. Merck 1.09.089.1000 (i-CAS No. 7553-56-2) 7) 0.05.
c) Potassium iodide 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 Izixhobo
17.2.3.1 I-Stirrer 1ta Model 98 Multi-shaft Stirrers ixhotyiswe nge-9B29X i-impeller okanye iblade elinganayo nenye
sinusoidal waveform;blade ubukhulu malunga.25 mm (ilin, ubuso obubethelwe phezulu).
17.2.3.2 Ikomityi yokuzamazama inobungakanani obumalunga ne-180 mm (7.1 in) ubunzulu, 97 mm (3-5/6 in) ububanzi
umlomo ophezulu,kunye ne-70 mm (2.75 in) ububanzi besiseko esisezantsi (umz. M110-D uhlobo lweHamilton Beachikomityi eshukumisayo
okanye into efanayo).(Iglasi engama-600 ml nayo ingasetyenziswa njengebambela.)
17.2.3.3 Amacephe aseLabhoratri.
17.2.3.4 Isikrala.
17.2.3.5 Ibhalansi: Ukuchaneka ngu-0.01 g.
17.2.3.6 Iiflaski zeVolumetric 100ml
17.2.3.7 Iipayipi zePasteur okanye iiplastiki zedropper.
17.2.3.8 Ixesha: Oomatshini okanye i-elektroniki, ukuchaneka 0.1 min.17.2.3.9 pH yeemitha kunye ne-pH electrode:
umz. Thermo Russell uhlobo KDCW1 19)
17.2.3.10 Izixhobo zokutyisa zePolymeric (umz. Fann 10) okanye 0Fl uhlobo 11))
17.2.3.11 Iityhubhu zovavanyo.
17.2.4 Inkqubo - Ukulungiswa kwe-Iodine / Potassium Iodide Solution
17.2.4.1 Yongeza i-10 μl ± 0.1 ml ye-0.05 mol / l isisombululo se-iodine kwi-100 ml ± 0.1 ml ye-volumetric flask.
17.2.4.2 Yongeza 0.60 g±..01 g Potassium iodide (KI), vuthulula ngobunono iflask ukuyinyibilikisa.
17.2.4.3 Yongeza amanzi adibeneyo kwi-100 ml yamanqaku kwaye udibanise kakuhle.Bhala umhla wokulungiselela.
17.2.4.4 Umxube owenziweyo we-iodine/iodide ugcinwa kwisingxobo esivaliweyo kwaye ugcinwe kwindawo emnyama, epholileyo neyomileyo.
Umhla wokuphelelwa lixesha ukuya kwiinyanga ezintathu kwaye kufuneka ulahlwe kwaye uvuselelwe.
17.2.5 Inkqubo - ULungiselelo lweSisombululo sePAC-LV kunye nokufunyanwa kweStartshi
17.2.5.1 Lungiselela unyibiliko lwama-596 lwe-PAC-LV oluza kuvavanywa.
Yongeza i-380 g ± 0.1 g yamanzi adiyoni kwikomityi yokuxuba, yongeza i-2 g ± 0.1 g ye-PAC-LV ngesantya esifanayo.
ngelixa uvuselela i-stirler,kwaye ixesha lokongeza kufuneka liqhubeke kwi-60 ukuya kwi-120 s.
Isampulu kufuneka yongezwe kwisiphithiphithi kwikomityi yokuxuba, kwaye ugweme ukuvuselela i-shaft ukunciphisa uthuli.
Kukhethwa ukuba usebenzise isixhobo sokutshaja sepolymer kwi-17.2.3.10.
17.2.5.2 Emva kokuvuselela imizuzu emi-5 ± 0.1 imiz, susa ikomityi eshukumayo kwi-stirrer kwaye ukhuhle zonke ii-PAC-LVs ezincanyathiselwe.
udonga lwekomityi nge-spatula.Zonke ii-PAC-LVs ezinamathele kwi-scraper zixutywe kwisisombululo.
17.2.5.3 Ukulinganisa i-pH yesisombululo.Ukuba i-pH ingaphantsi kwe-10, yongeza isisombululo esixubileyo se-NaOH dropwise.
Nyusa i-pH ukuya kwi-10
17.2.5.4.Buyisela ikomityi evuselelayo kwi-stirmer kwaye uqhubeke uvuselela.Ixesha elipheleleyo lokuvuselela kufuneka libe yi-20 min ± 1 Min.
17.2.5.5 Beka i-2 ml yesisombululo sesampulu kwityhubhu yovavanyo kwaye wongeze amathontsi ama-3 esisombululo se-iodine / iodide,
ukuya kutsho kumathontsi angama-30.
17.2.5.6 Lungiselela iimvavanyo ezithathu ezingenanto ezinamanzi adiyiniweyo.Yongeza amathontsi ama-3, amathontsi angama-9, amathontsi angama-30 esisombululo se-iodine
imibhobho yovavanyo lothelekiso.
17.2.5.7 Emva kokongeza amaconsi ama-3 esisombululo ngexesha ngalinye, vuthulula kakuhle ityhubhu ukuthelekisa umbala wesisombululo sesampuli.
ngovavanyo olungenanto.Ukuthelekiswa kwemibala kufuneka kwenziwe ngokubhekiselele kwimvelaphi emhlophe.
17.2.6 Ukuzimisela - ukufunyanwa kwesitatshi sePAC-LV
17.2.6.1 Ukuba isisombululo sesampulu siza kuvavanywa sibonisa umbala otyheli ofanayo novavanyo olungenanto, isampuli ayifuni
ziqulathe naziphi na istatshi okanye izinto eziphuma kwistatshi.
17.2.6.2 Ukuba kukho nawuphi na omnye umbala, kuboniswa ngamandla ukuba kukho istatshi okanye
17.2.6.3 Ukuba umbala ubonakala unyamalala ngokukhawuleza, ebonisa ubukho be-arhente yokunciphisa, kule meko,
qhubeka ukongeza i-dropwise iodine / iodide Isisombululo, uthelekiso lombala kunye nolunye lweemvavanyo ezingenanto, bona i-17.2.61.
17.2.6.4 Ukuba kukho nakuphi na ukusabela kombala okwahlukileyo ku-17.2.6.1 kufunyenwe, akukho mfuneko yokuba kuqhutyekwe novavanyo olulandelayo.
17.3 Ukufuma
17.3.1 Izixhobo 17.3.1.1 I-oven: Ilawuleka kwi-105 ° C± 3 ° C (220±5>.
17.3.1.2 Ibhalansi: Ukuchaneka kwe-0.01 g.
17.3.1.3 Isitya sokuphunga: Umthamo 150 ml.
17.3.1.4 Isikrala.
17.3.1.5 I-Desiccant: Iqukethe i-desiccant (i-CAS No. 7778-18-9) i-desiccant, okanye ilingana
17.3.2 Inkqubo yoVavanyo
17.3.2.1 Ubunzima 10 g ± 0.1 g PAC-LV isampulu yokulinganisa Kwisitya esiphuphumayo, rekhoda ubunzima besampulu m
17.3.2.2 Yomisa isampuli kwi-oven i-4 h
17.3.2.3 Pholisa isampulu kwisithambiso ukuya kwiqondo lobushushu begumbi17.3.2.4 Phinda ulinganise isitya esiphuphumayo esiqulethe
i-PAC-LV eyomileyo, bhala umgangatho wesampula owomileyo m2.
17.3.3 Ukubala
17.4 Ilahleko yolwelo
17.4.1 Ii-reagents kunye nemathiriyeli
17.4.1.1 Ityuwa yolwandle: Vavanya umhlaba ngokwe-ASTM D 1141-98 (2003) 12
17.4.1.2 umgangatho we-API.
17.4.1.3 I-Potassium Chloride (i-CAS No. 7447-40-7)
17.4.1.4 I-Sodium Bicarbonate (i-CAS No. 144-55-8).
17.4.1.5 Amanzi adiliweyo okanye adiliweyo.
17.4.2 Izixhobo zokusebenza
17.4.2.1 Thermometer: Uluhlu lokulinganisa ngu-0 °C ~ 60 °C, ukuchaneka ngu-0.5 °C
(uluhlu lomlinganiselo yi 32 °F ~ 140 °F, ukuchaneka yi 1.0 °F)
17.4.2.2 Ibhalansi: Ukuchaneka ngu-0.01g.
17.4.2.3 I-Stirrer: Ukuba uhlobo lwe-9B lwe-multi-shaft stirrer luxhotyiswe nge-9B20x impeller,i-shaft kufuneka ifakwea
omnyei-sine wave blade enencakuba yedayamitha emalunga ne-25 mm (1 ngaphakathi) enobuso obunesitampu phezulu.
17.4.2.4 Ikomityi yokuzamazama inobungakanani obumalunga ne-180 mm (7.1 in) ubunzulu, 97 mm (3-5/6 in) ububanzi
umlomo ophezulu,kunye ne-70 mm (2.75 in) ububanzi besiseko esisezantsi (umz. i-M110-D uhlobo lwe-Hamilton Beach i-cutting cup).
17.4.2.5 isikrabhu.
17.4.2.6 Isikhongozelo: Iglasi okanye iplastiki, enesivalo okanye isiciko, esetyenziselwa amanzi anetyuwa.
17.4.2.7 Viscometers: Umbane, ukufunda ngokuthe ngqo, ngokuhambelana ne-ISO 10414-1
17.4.2.8 Izibali-xesha: Zimbini, oomatshini okanye i-elektroniki, ngokuchaneka kwe-0.1 min kwixesha elilinganisiweyo kolu vavanyo.
17.4.2.9 Izixhobo zoHluzo: Iqondo lobushushu eliphantsi kunye nodidi loxinzelelo, ngokuhambelana namalungiselelo eSahluko 7 se.
ISO 10414-1:2008.
17.4.2.10 Ukulinganisa iisilinda: ezimbini, ezinomthamo we-10 ml ± 0.1 ml kunye ne-500 ml ± 5 ml *
17.4.2.11 Isixhobo sokutyisa iPolymer (uhlobo lweFann okanye uhlobo lweOFI).
17.4.3 Inkqubo yoVavanyo - i-PAC-LV yokuLahleka kolwelo
17.4.3.1 Yongeza i-42 g ± 0.01 g yetyuwa yolwandle kwi-11 ± 2 ml yamanzi adiyoni.
17.4.3.2 Kwi-358 g yesisombululo setyuwa yolwandle, yongeza i-35.0 g ± 0.01 g ye-potassium chloride (KCl).
17.4.3.3 Emva kokuvuselela i-3 min ± 0.1 min, yongeza i-1.0 g ± 0.01 g ye-sodium bicarbonate.
17.4.3.4 Emva kokuvuselela i-3 min± 0.1 min, yongeza i-28.0 g± 0.01 g umgangatho we-API ukuvavanya
17.4.3.5 Emva kokuvuselela i-5 min± 0.1 min, susa ikomityi ephazamisayo kwi-stirter kwaye uyikhuphe eludongeni nge-scraper.
Yonke imigangatho ye-API ihlola umhlaba.Yonke imihlaba yokuvavanya umgangatho we-API enamathele kwi-scraper yaxutywa ekumisweni.
17.4.3.6 Buyisela indebe evuselelayo kwi-stirter kwaye uqhubeke uvuselela i-5 min ± 0.1 min.
17.4.3.7 Ubunzima 2.0 g±0.01 g PAC-L.
17.4.3.8 Kancinci ngelixa uvuselela kwi-stirrer, yongeza i-PAC-LV ngesantya esifanayo.
Ixesha lokudibanisa kufuneka lihlale malunga nemizuzwana engama-60.I-PAC-LV kufuneka yongezwe kwi-vortex kwikomityi yokuxuba
kwaye uphephe i-shaft eshukumisayo ukunciphisa uthuli.Kungcono ukusebenzisa isixhobo se-polymer feed kwi-17.4.2.11.
17.4.3.9 Emva kokuvuselela i-5 min ± 0.1 min, susa ikomityi yokugubha kwi-stirrer kwaye usebenzise i-spatula ukukrazula konke.
I-PAC-L ibambelele kudonga lwekomityi.Zonke ii-PAC-LVs ezinamathele kwi-scraper zaxutywa kwi-suspension.
17.4.3.10 Buyisela ingqayi kwisiqhumiso kwaye uqhubeke ushukumisa.Ukuba kuyimfuneko, emva kwemizuzu emi-5 kunye nemizuzu eyi-10, susa uchuku
ikomityi esuka kwi-stirrer kwaye ukhuhle yonke i-PAC-L enamathele eludongeni lwendebe.Ixesha elipheleleyo lokuvuselela ukusuka kwi
Ukuqala kokongezwa kwe-PAC-LV kufuneka ibe yi-20 min ± 1 min.
17.4.3.11 Kuma-25 °C ± 1 °C (77 °F ± 2 °F),gcina ukunqunyanyiswa kwisitya esivaliweyo okanye esivaliweyo kwi-16 h ± 0.5 h.
Rekhoda ubushushu bokunyanga kunye nexesha lokunyanga.
17.4.3.12 Emva kokunyanga, gxobhoza ukumiswa kwi-stirrer ye-5 min ± 0.1 min.
17.4.3.13 Galela ukumiswa kwe-PAC-LV kwikomityi yokucoca.Ngaphambi kokuthululela kwi-suspension,qiniseka ukubazonkeiinxalenye
Yendebe yokucoca yomile kwaye umsesane wokutywina awukhubekanga okanye unxitywe.Ubushushu bokumiswa kufuneka bube
25°C±1°C (77°F±2).Ukuya kwi-13 mm (0.5 phakathi) ukusuka phezulu kwekomityi.Hlanganisa ikomityi yokucoca, faka ikomityi yokucoca
umnini, vala i-valve yokunciphisa uxinzelelo, kwaye ubeke isitya phantsi kombhobho wokukhupha.
17.4.3.14 Misela isibali-xesha kwi-7.5 min kunye nenye iseti kwi-30 min.Kwangaxeshanye qalisa izibali-xesha ezibini kwaye ulungise uxinzelelo lwekomityi ukuya
690 kPa ± 35 kPa (100 psi ± 5 psi).Uxinzelelo kufuneka lunikezelwe ngomoya ocinezelweyo, i-nitrogen okanye i-helium.
Kufuneka igqitywe kwimizuzwana eyi-15.
17.4.3.15 ekuqaleni Ekupheleni kwesibali-xesha kuphela, susa isikhongozeli kwaye ususe naluphi na ulwelo olunamathela kumbhobho kwaye
yilahle.I-cylinder eyomileyo eyi-10 ml ifakwe phantsi kombhobho kwaye i-filtrate yaqokelelwa kude kube ngowesibini.
isibali-xesha siphelelwe lixesha.Susa i-cylinder kwaye urekhode umthamo we-filtrate eqokelelweyo.
17.4.4 Ukubala - Ilahleko yePAC-LV Isixa se-V esihluzwayo sibalwa ngokweequation (43) kwi ml;
v-2xVe (43) apho: 1⁄2_ umthamo wefiltrate eqokelelwe phakathi kwe-7.5 min kunye ne-30 min.Iyunithi yi ml.
17.5 I-Viscosity ebonakalayo yezisombululo
17.5.1 Inkqubo yoVavanyo-I-Viscosity ebonakalayo yesisombululo
17.5.1.1 Yongeza i-42 g ± 0.01 g yetyuwa yolwandle kwi-11 ± 2 ml yamanzi adibeneyo.
17.5.1.2 Kwi-358 g yesisombululo setyuwa yolwandle, yongeza i-35.0 g ± 0.01 g ye-potassium chloride (KCl).
17.5.1.3 Ubunzima 5.0 g ± 0.01 g PAC-Lv.Kancinci ngelixa uvuselela kwi-stirrer, yongeza i-PAC-LV kwizinga elifanayo.
Ixesha lokongeza kufuneka lihlale malunga nomzuzu omnye.I-PAC-LV kufuneka yongezwe kwi-vortex kwikomityi yokuxuba
kwaye uphephe i-shaft eshukumisayo ukunciphisa uthuli.
17.5.1.4 Emva kokuvuselela imizuzu emi-5 ± 0.1 imiz, susa ikomityi yokuvuselela kwi-stirrer, khuhla yonke i-PACw ebambelele eludongeni lwekomityi.
nge-spatula, kwaye udibanise yonke i-PAC-LV ibambelele kwi-spatula ukuya ekumisweni.
17.5.1.5 Buyisela ingqayi kwi-mixer kwaye uqhubeke udibanisa.Ukuba kuyimfuneko, susa ikomityi ye-stirrer kwi-mixer emva koko
Imizuzu emi-5 kunye ne-10 min, krazula zonke ii-PAC-Ws ezinamathele eludongeni lwendebe.Lilonke ixesha lokuvuselela ukususela ekuqaleni kodibaniso lwe
I-PAC-LV kufuneka ibe yi-20 min ± 1 min.
17.5.1.6 Kwi-25 °C ± 1 °C (777 ± 27), nqumamisa ukumiswa kwe-16 h ± 0.5 h kwisingxobo esivaliweyo okanye esifakwe isiciko.
Rekhoda ubushushu bokunyanga kunye nexesha lokunyanga ”
17.5.1.7 Gxuma ukumiswa kwi-stirrer kwi-5 min ± 0.1 min.
17.7.5.1.8 Galela isisombululo kwisampulu yekomityi exhotyiswe nge-viscometer yokufunda ngokuthe ngqo "kwi-25 °C ± 1 °C (77 Ngaphantsi
imeko ye °F ± 2), ukumiswa kwafundwa kwi-600 r / min.
17.5.2 Ukubala - I-viscosity ebonakalayo yesisombululo
Bala i-viscosity ebonakalayo yesisombululo ngokwefomula (44), kwi-mPas:
VA=R600/2 (44)
I-R600-viscometer yokufunda kwi-600 r / min.Rekhoda isiphumo sokubala
Ixesha lokuposa: Nov-12-2020