Chithunzi cha PAC-LVTEst Procedure

17.2 Kutsimikiza Kwabwino kwa Wowuma mu Ma polima Osungunuka M'madzi

17.2.1 Mfundo

17.2.1.1 Cholinga cha mayesowa ndikuzindikira kupezeka kwa wowuma kapena zotumphukira za wowuma mu ma polima osungunuka m'madzi aufa kapena granular monga PAC-LV.

17.2.1.2.Kuzindikira yankho la PAC-LV powonjezera yankho la mineral/iodide*

Ngati amylose alipo, amasinthidwa kukhala mtundu wamitundu.

17.2.2 Reagents ndi zipangizo

a) Madzi osungunuka kapena osungunuka

b) Nitrate solution, mwachitsanzo Merck 1.09.089.1000 (CAS No. 7553-56-2) 7) 0.05.

c) Iodide ya potaziyamu 1 Merck 1.0504 3.0250 PA (CAS No. 7681-11-0

d) Sodium hydroxide (NaOH) (CAS No. 1310-73-2): kuchepetsa njira, 0.1% -0.5%.

17.2.3 Zida

17.2.3.1 Stirrer 1ta Model 98 Multi-shaft Stirrers yokhala ndi chowongolera cha 9B29X kapena tsamba lofanana ndi limodzi

mawonekedwe a sinusoidal,blade diameter pafupifupi.25 mm (chingwe, chokhomerera nkhope).

17.2.3.2 Chikho chogwedeza chili ndi kukula pafupifupi 180 mm (7.1 mu) kuya, 97 mm (3-5/6 mu) m'mimba mwake.

kukamwa kwa pamwamba,ndi 70 mm (2.75 mu) m'mimba mwake m'munsi (monga M110-D mtundu wa Hamilton Beachoyambitsa chikho

kapena chinthu chofanana).(Galasi la 600 ml litha kugwiritsidwanso ntchito ngati cholowa m'malo.)

17.2.3.3 Laboratory spoons.

17.2.3.4 Chotupa.

17.2.3.5 Mlingo: Kulondola ndi 0.01 g.

17.2.3.6 Mabotolo a Volumetric 100ml

17.2.3.7 Pasteur pipette kapena dropper mapulasitiki.

17.2.3.8 Timer: Makina kapena zamagetsi, zolondola 0.1 min.17.2.3.9 pH mita ndi pH ma elekitirodi:

mwachitsanzo Thermo Russell lembani KDCW1 19)

17.2.3.10 Zida zodyetsera zapolymeric (monga Fann 10) kapena 0Fl mtundu 11))

17.2.3.11 Machubu oyesera.

17.2.4 Ndondomeko - Kukonzekera kwa Iodine / Potaziyamu Iodide Solution

17.2.4.1 Onjezani 10 μl ± 0.1 ml ya 0.05 mol / l yankho la ayodini mu botolo la voliyumu ya 100 ml ± 0.1 ml.

17.2.4.2 Onjezani 0,60 g±..01 g Potaziyamu iodide (KI), gwedezani botolo pang'onopang'ono kuti musungunuke.

17.2.4.3 Onjezani madzi osungunuka ku chizindikiro cha 100 ml ndikusakaniza bwino.Lembani tsiku lokonzekera.

17.2.4.4 Mankhwala opangidwa ndi ayodini/iodide amasungidwa mu chidebe chotsekedwa ndikusungidwa pamalo amdima, ozizira komanso owuma.

Tsiku lotha ntchito ndi miyezi itatu ndipo liyenera kutayidwa ndikukonzedwanso.

17.2.5 Ndondomeko - Kukonzekera Kwayankho kwa PAC-LV ndi Kuzindikira Wowuma

17.2.5.1 Konzani njira yamadzi 596 ya PAC-LV kuti iyesedwe.

Onjezani 380 g ± 0.1 g wa madzi opangidwa ndi deionized ku kapu yosakaniza, onjezerani 2 g ± 0.1 g wa PAC-LV pa liwiro lofanana.

pamene mukugwedeza pa mvuto,ndipo nthawi yowonjezera iyenera kupitilira kwa 60s mpaka 120 s.

Chitsanzocho chiyenera kuwonjezeredwa ku chipwirikiti mu kapu yosakaniza, ndipo pewani kugwedeza shaft kuti muchepetse fumbi.

Ndikwabwino kugwiritsa ntchito chipangizo chojambulira polima mu 17.2.3.10.

17.2.5.2 Mukakankhira kwa 5 min ± 0.1 min, chotsani kapu yosonkhezera kuchokera pa choyambitsa ndikukwapula ma PAC-LV onse omwe amamatira.

kapu khoma ndi spatula.Ma PAC-LV onse omwe amamatira ku scraper adasakanizidwa mu yankho.

17.2.5.3 Yezerani pH ya yankho.Ngati pH ili yotsika kuposa 10, onjezerani njira yochepetsera ya NaOH dropwise.

Kwezani pH mpaka 10

17.2.5.4.Bweretsani kapu yosonkhezera kwa oyambitsa ndikupitiriza kusonkhezera.Nthawi yonse yogwedeza iyenera kukhala 20 min ± 1 Min.

17.2.5.5 Ikani 2 ml ya yankho lachitsanzo mu chubu choyesera ndikuwonjezera madontho atatu a ayodini / ayodini,

mpaka 30 madontho.

17.2.5.6 Konzani zoyesera zitatu zopanda kanthu ndi madzi osapangidwanso.Onjezani madontho atatu, madontho 9, madontho 30 a ayodini / ayodini

machubu oyesa kufananiza.

17.2.5.7 Mukawonjezera madontho atatu a yankho nthawi iliyonse, gwedezani chubu pang'onopang'ono kuti mufananize mtundu wa yankho lachitsanzo.

ndi mayeso opanda kanthu.Kuyerekeza kwa mitundu kuyenera kupangidwa motsutsana ndi maziko oyera.

17.2.6 Kutsimikiza - Kuzindikira kwa Wowuma wa PAC-LV

17.2.6.1 Ngati yankho lachitsanzo loyesedwa likuwonetsa mtundu wachikasu womwewo ngati mayeso opanda kanthu, chitsanzocho

ali ndi zotumphukira zilizonse za wowuma kapena wowuma.

17.2.6.2 Ngati pali mtundu wina uliwonse, zikusonyezedwa kuti pali chotupitsa kapena chotupitsa.

17.2.6.3 Ngati mtunduwo ukuwoneka kuti ukutha mofulumira, kusonyeza kukhalapo kwa wothandizira kuchepetsa, pamenepa,

pitirizani kuwonjezera dropwise ayodini / ayodini Solution, kuyerekeza mtundu ndi chimodzi mwa mayesero opanda kanthu, onani 17.2.61.

17.2.6.4 Ngati mtundu uliwonse wamtundu womwe uli wosiyana ndi 17.2.6.1 wapezeka, sikoyenera kupitiliza mayeso ena.

17.3 Chinyezi

17.3.1 Zida 17.3.1.1 Ovuni: Yowongoka pa 105 ° C± 3 ° C (220±5>.

17.3.1.2 Kusamalitsa: Kulondola kwa 0.01 g.

17.3.1.3 Evaporation mbale: Mphamvu 150 ml.

17.3.1.4 Chikwapu.

17.3.1.5 Desiccator: Lili ndi desiccant (CAS No. 7778-18-9) desiccant, kapena zofanana

17.3.2 Njira Yoyesera

17.3.2.1 Yezerani 10 g ± 0.1 g Sampuli ya PAC-LV yoyezedwa M'mbale yomwe imatuluka nthunzi, lembani chitsanzo cha misa m

17.3.2.2 Yanikani chitsanzo mu uvuni kwa 4 h

17.3.2.3 Kuziziritsa chitsanzo mu desiccator mpaka kutentha kwa chipinda17.3.2.4 Wezaninso sikelo ya mbale yomwe ikutuluka nthunzi yomwe ili ndi

zouma PAC-LV, mbiri youma chitsanzo khalidwe m2.

17.3.3 Kuwerengera

17.4 Kutaya madzimadzi

17.4.1 Ma reagents ndi zida

17.4.1.1 Mchere wa m’nyanja: Unikani nthaka molingana ndi ASTM D 1141-98 (2003) 12

17.4.1.2 API muyezo.

17.4.1.3 Potaziyamu Chloride (CAS No. 7447-40-7)

17.4.1.4 Sodium Bicarbonate (CAS No. 144-55-8).

17.4.1.5 Madzi osungunuka kapena osungunuka.

17.4.2 Zida

17.4.2.1 Thermometer: Muyeso woyezera ndi 0 °C ~ 60 °C, kulondola ndi 0.5 °C

(kuyezera ndi 32 °F ~ 140 °F, kulondola kwake ndi 1.0 °F)

17.4.2.2 Chotsalira: Cholondola ndi 0.01g.

17.4.2.3 Stirrer: Ngati Type 9B multi-shaft stirrer ili ndi 9B20x impeller,shaft iyenera kuikidwaa

wosakwatiwatsamba la sine wave lomwe lili ndi mainchesi pafupifupi 25 mm (1 mkati) yokhala ndi nkhope yodinda m'mwamba.

17.4.2.4 Chikho chogwedeza chili ndi kukula pafupifupi 180 mm (7.1 mu) kuya, 97 mm (3-5/6 mu) m'mimba mwake

mlomo wapamwamba,ndi 70 mm (2.75 mu) m'mimba mwake wa m'munsi (monga M110-D mtundu wa Hamilton Beach yogwedeza chikho).

17.4.2.5 scraper.

17.4.2.6 Chidebe: Galasi kapena pulasitiki, yokhala ndi choyimilira kapena chivindikiro, yogwiritsidwa ntchito popanga madzi amchere.

17.4.2.7 Viscometers: Magetsi, kuwerenga molunjika, molingana ndi ISO 10414-1

17.4.2.8 Timers: Ziwiri, zamakina kapena zamagetsi, ndi zolondola za 0.1 min pa nthawi yoyesedwa muyeso ili.

17.4.2.9 Zida Zosefera: Kutentha kochepa ndi mtundu wa kuthamanga, molingana ndi zomwe zili mu Mutu 7 wa

ISO 10414-1: 2008.

17.4.2.10 Kuyeza masilinda: Awiri, okhala ndi mphamvu ya 10 ml ± 0.1 ml ndi 500 ml ± 5 ml *

17.4.2.11 Chida chodyera polima (mtundu wa Fann kapena mtundu wa OFI).

17.4.3 Njira Yoyesera - Kutayika kwa Madzi a PAC-LV

17.4.3.1 Onjezani 42 g ± 0.01 g ya mchere wa m'nyanja ku 11 ± 2 ml ya madzi a deionized.

17.4.3.2 Mu 358 g wa mchere wa m'nyanja, onjezerani 35.0 g ± 0.01 g wa potaziyamu chloride (KCl).

17.4.3.3 Pambuyo poyambitsa 3 min ± 0.1 min, onjezerani 1.0 g ± 0.01 g ya sodium bicarbonate.

17.4.3.4 Mutatha kusonkhezera kwa 3 min± 0.1 min, onjezani 28.0 g ± 0.01 g API muyezo kuti muwunikire

17.4.3.5 Mutatha kuyambitsa 5 min± 0.1 min, chotsani kapu yotsitsimutsa kuchokera ku choyambitsa ndikuchipukuta ku khoma ndi chopukutira.

Miyezo yonse ya API imawunika nthaka.Dothi lonse la API loyezetsa bwino lomwe limamatira ku scraper linasakanizidwa ndikuyimitsidwa.

17.4.3.6 Bweretsani chikho choyambitsa kugwedeza ndikupitiriza kuyambitsa 5 min ± 0.1 min.

17.4.3.7 Kulemera 2.0 g±0.01 g PAC-L.

17.4.3.8 Pang'onopang'ono pamene akuyambitsa pa stirrer, kuwonjezera PAC-LV pa mlingo yunifolomu.

Nthawi yowonjezera iyenera kukhala pafupifupi masekondi 60.PAC-LV iyenera kuwonjezeredwa ku vortex mu kapu yosakaniza

ndipo pewani shaft yogwedeza kuti muchepetse fumbi.Ndi bwino kugwiritsa ntchito polima chakudya chipangizo mu 17.4.2.11.

17.4.3.9 Mukakankhira kwa 5 min ± 0.1 min, chotsani kapu yosonkhezera kuchokera pa choyambitsa ndikugwiritsa ntchito spatula kuti muchotse zonse.

PAC-L idamamatira ku khoma la chikho.Ma PAC-LV onse omwe amamatira ku chopukusira adasakanizidwa ndikuyimitsidwa.

17.4.3.10 Bweretsani mtsukowo ku choyambitsa ndikupitiriza kusonkhezera.Ngati ndi kotheka, pakatha mphindi 5 ndi mphindi 10, chotsani chipwirikiti

kapu kuchokera pa chowombera ndikuchotsa zonse PAC-L zomata khoma la chikho.Nthawi yonse yolimbikitsa kuyambira pa

kuyamba kwa kuwonjezera kwa PAC-LV kuyenera kukhala 20 min ± 1 min.

17.4.3.11 Pa 25 °C ± 1 °C (77 °F ± 2 °F),sungani kuyimitsidwa mu chidebe chotsekedwa kapena chotsekedwa kwa 16 h ± 0.5 h.

Lembani kutentha kwa machiritso ndi nthawi yochiritsa.

17.4.3.12 Pambuyo kuchiritsa, yambitsani kuyimitsidwa pa choyambitsa 5 min ± 0.1 min.

17.4.3.13 Thirani kuyimitsidwa kwa PAC-LV mu kapu yosefera.Asanathire mu kuyimitsidwa,onetsetsani kutizonsemagawo

za kapu zosefera ndizouma ndipo mphete yosindikizirayo siili yopunduka kapena kuvala.Kutentha kwa kuyimitsidwa kuyenera kukhala

25°C±1°C (77°F±2).Kufikira mkati mwa 13 mm (0.5 mu) kuchokera pamwamba pa kapu.Sonkhanitsani chikho chosefera, ikani chikho chosefera

chogwirizira, kutseka valavu kuchepetsa kuthamanga, ndi kuika chidebe pansi pa chubu kukhetsa.

17.4.3.14 Khazikitsani chowerengera kukhala 7.5 min ndi chinanso 30 min.Nthawi yomweyo yambani zowerengera ziwiri ndikusintha kuthamanga kwa chikho kuti

690 kPa ± 35 kPa (100 psi ± 5 psi).Kupanikizika kuyenera kuperekedwa ndi mpweya wothinikizidwa, nayitrogeni kapena helium.

Iyenera kumalizidwa mkati mwa masekondi 15.

17.4.3.15 poyamba Pamapeto a chowerengera chokha, chotsani chidebe ndikuchotsa madzi aliwonse omwe amamatira kukhetsa ndi

kutaya.Silinda yowuma ya 10 ml idayikidwa pansi pa ngalande ndipo sefayo idasonkhanitsidwa mpaka yachiwiri.

chowerengera chatha.Chotsani silinda ndikulemba kuchuluka kwa filtrate yomwe yasonkhanitsidwa.

17.4.4 Kuwerengera - Kutayika kwa PAC-LV Kuchuluka kwa V yosefedwa kumawerengedwa molingana ndi equation (43) mu ml;

v-2xVe (43) pomwe: 1⁄2_ voliyumu ya kusefera yosonkhanitsidwa pakati pa 7.5 min ndi 30 min.Chigawo ndi ml.

17.5 Mawonekedwe a Viscosity of Solutions

17.5.1 Njira Yoyesera - Mawonekedwe a Viscosity Yankho

17.5.1.1 Onjezani 42 g ± 0.01 g ya mchere wa m'nyanja ku 11 ± 2 ml ya madzi a deionized.

17.5.1.2 Mu 358 g wa mchere wa m'nyanja, onjezerani 35.0 g ± 0.01 g wa potaziyamu chloride (KCl).

17.5.1.3 Kulemera 5.0 g ± 0.01 g PAC-Lv.Pang'onopang'ono pamene akuyambitsa pa stirrer, kuwonjezera PAC-LV pa yunifolomu mlingo.

Nthawi yowonjezera iyenera kukhala pafupifupi miniti imodzi.PAC-LV iyenera kuwonjezeredwa ku vortex mu kapu yosakaniza

ndipo pewani shaft yogwedeza kuti muchepetse fumbi.

17.5.1.4 Mukakankhira kwa 5 min ± 0.1 min, chotsani kapu yosonkhezera kuchokera pa choyambitsa, sukani PACw yonse yokanizidwa ku khoma la chikho.

ndi spatula, ndi kusakaniza onse PAC-LV munakhala pa spatula kuti kuyimitsidwa.

17.5.1.5 Bweretsani mtsuko kwa chosakanizira ndikupitiriza kusonkhezera.Ngati ndi kotheka, chotsani kapu yotsitsimutsa kuchokera ku chosakanizira pambuyo pake

5 min ndi 10 min, pezani ma PAC-W onse omwe adakakamira khoma la chikho.Okwana oyambitsa nthawi kuyambira chiyambi cha kuwonjezera

PAC-LV iyenera kukhala 20 min ± 1 min.

17.5.1.6 Pa 25 °C ± 1 °C (777 ± 27), kuyimitsa kuyimitsidwa kwa 16 h ± 0.5 h mu chidebe chotsekedwa kapena chotsekedwa.

Lembani kutentha kwa machiritso ndi nthawi yochiritsa ”

17.5.1.7 Limbikitsani kuyimitsidwa pa oyambitsa 5 min ± 0.1 min.

17.7.5.1.8 Thirani yankho mu chikho chachitsanzo chokhala ndi viscometer yowerengera molunjika" pa 25 °C ± 1 °C (77 Under

chikhalidwe cha ° F ± 2), kuyimitsidwa kunawerengedwa pa 600 r / min.

17.5.2 Kuwerengera - Kuwonekera kwa viscosity ya yankho

Kuwerengera kukhuthala kowonekera kwa yankho molingana ndi chilinganizo (44), mu mPas:

VA=R600/2 (44)

R600-viscometer kuwerenga pa 600 r / min.Lembani zotsatira za kuwerengera