1, ka ʻike ʻana o ke ʻano hydroxypropyl methyl cellulose
(1) E lawe i 1.0g o ka laʻana, ka wai wela (80 ~ 90 ℃) 100mL, e hoʻoulu mau, a hoʻomaʻalili i ka wai viscous i loko o ka ʻauʻau hau; E hookomo i 2mL o ka wai iloko o ka paipu hoao, e hookomo malie i 1mL sulfuric acid solution o 0.035% anthrone ma ka paia o ka paipu, a waiho no 5min. Hōʻike ʻia ke apo ʻōmaʻomaʻo ma ke kikowaena ma waena o nā wai ʻelua.
(2) E lawe i ka nui kūpono o ka slime i ʻōlelo ʻia ma luna no ka ʻike ʻana o (ⅰ) a ninini ma luna o ka pā aniani. Ma hope o ka haʻalele ʻana o ka wai, hana ʻia kahi kiʻi ductile.
2, hydroxypropyl methyl cellulose kānana o ka hoʻomākaukau hoʻonā maʻamau
(1) Sodium thiosulfate solution maʻamau (0.1mol/L, mana: hoʻokahi mahina)
Hoʻomākaukau: E hoʻolapalapa ma kahi o 1500mL wai i hoʻomaʻamaʻa ʻia a hoʻomaʻalili a mākaukau e hoʻohana. E kaupaona i 25g sodium thiosulfate (ʻo kona kaumaha mole he 248.17, a e ho'āʻo e pololei ma kahi o 24.817g i ke kaupaona ʻana) a i ʻole 16g anhydrous sodium thiosulfate, e hoʻoheheʻe i loko o 200mL o ka wai hoʻomaha ma luna, e hoʻoheheʻe i 1L, a waiho i loko o kahi ʻeleʻele. ʻōmole, waiho i ka ʻōmole i loko o ka pōʻeleʻele, a kānana no ka hoʻohana ʻana ma hope o ʻelua pule.
Kalibration: Kauona 0.15g o ka potassium dichromate i kālua ʻia i ke kaumaha mau, pololei i ka 0.0002g. E hoʻohui i 2g potassium iodide a me 20mL sulfuric acid (1 + 9), lulu maikaʻi, waiho i loko o ka pōʻeleʻele no 10min, hoʻohui i 150mL wai a me 3ml 0.5% starch solution indicator, titrate me 0.1mol/L sodium thiosulfate solution, huli ka hopena mai ka uliuli. i ka ʻōmaʻomaʻo ʻōmaʻomaʻo ma ka hopena. ʻAʻole i hoʻohui ʻia ka potassium chromate i ka hoʻokolohua blank. Ua hana hou ʻia ke kaʻina hana calibration 2 ~ 3 mau manawa a ua lawe ʻia ka waiwai awelika.
Ua helu ʻia ka ʻike molar C (mol/L) o ka solution maʻamau sodium thiosulfate penei:
Aia, M ka nuipa o ka potassium dichromate; ʻO V1 ka nui o ka sodium thiosulfate i hoʻopau ʻia, mL; ʻO V2 ka nui o ka sodium thiosulfate i hoʻopau ʻia i ka hoʻokolohua hakahaka, mL; ʻO 49.03 ka nuipaʻa o ka potassium dichromate e like me 1mol o ka sodium thiosulfate, g.
Ma hope o ka calibration, hoʻohui i kahi Na2CO3 liʻiliʻi e pale i ka decomposition microbial.
(2) NaOH hoʻonā maʻamau (0.1mol/L, mana: hoʻokahi mahina)
Hoʻomākaukau: Ma kahi o 4.0g o ka NaOH maʻemaʻe no ka nānā ʻana ua kaupaona ʻia i loko o ka beaker, a ua hoʻohui ʻia ka 100mL wai i hoʻoheheʻe ʻia e hoʻoheheʻe ʻia, a laila hoʻololi ʻia i loko o kahi pahu volumetric 1L, a hoʻohui ʻia ka wai distilled i ka unahi, a waiho ʻia no 7-10 mau lā a hiki i hoʻolālikelike.
Calibration: E hoʻokomo i ka 0.6 ~ 0.8g o ka potassium hydrogen phthalate maʻemaʻe i hoʻomaloʻo ʻia ma 120 ℃ (pololei i ka 0.0001g) i loko o kahi pahu conical 250mL, hoʻohui i 75mL wai distilled e hoʻoheheʻe ʻia, a laila hoʻohui i 2 ~ 3 kulu o 1% phenolphthalein hōʻailona, titrate ʻO ka hopena sodium hydroxide i hoʻomākaukau ʻia ma luna a hiki i ka ʻulaʻula iki, a ʻo ka hopena ʻaʻole e mae ke kala i loko o 30S. E kākau i ka nui o ka sodium hydroxide. Ua hana hou ʻia ke kaʻina hana calibration 2 ~ 3 mau manawa a ua lawe ʻia ka waiwai awelika. A hana i kahi hoʻokolohua hakahaka.
Ua helu ʻia ka ʻike o ka solution sodium hydroxide penei:
Kahi, ʻo C ka neʻe ʻana o ka solution sodium hydroxide, mol/L; Hōʻike ka M i ka nuipaʻa o ka potassium hydrogen phthalate, G; ʻO V1 ka nui o ka sodium hydroxide i hoʻopau ʻia, mL; Hōʻike ka V2 i ka nui o ka sodium hydroxide i hoʻopau ʻia i ka hoʻokolohua blank, mL; ʻO 204.2 ka nuipaʻa mola o ka pāhare hydrogen phthalate, g no ka mole.
(3) Dilute sulfuric acid (1+9) (Validity: 1 mahina)
Ma lalo o ka hoʻoulu ʻana, e hoʻohui pono i ka 100mL sulfuric acid concentrated i 900mL wai i hoʻoheheʻe ʻia, e hoʻohui mālie, me ka hoʻoulu ʻana.
(4) E hoʻoheheʻe i ka sulfuric acid (1+16.5) (Ka mana: 2 mahina)
Ma lalo o ka hoʻoulu ʻana, e hoʻohui pono i ka 100mL o ka sulfuric acid concentrated i ka 1650mL o ka wai i hoʻomaʻemaʻe ʻia, e hoʻohui mālie. E hoʻoulu i kou hele ʻana.
(5) Hōʻailona mākū (1%, mana: 30 lā)
E kaupaona i 1.0g soluble starch, e hoʻohui i 10mL wai, e hoʻoulu a hoʻokomo i loko o 100mL wai paila, e hoʻolapalapa iki no 2min, waiho, a lawe i ka supernatant no ka hoʻohana.
(6) Hōʻailona mākū
Loaʻa ka 0.5% starch indicator ma o ka lawe ʻana i 5mL o ka solution 1% starch i hoʻomākaukau ʻia a hoʻoheheʻe ʻia i 10mL me ka wai.
(7) 30% chromium trioxide solution (mana: 1 mahina)
E kaupaona i 60g o ka chromium trioxide a e hoʻoheheʻe i loko o 140mL o ka wai me ka ʻole o nā mea ola.
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Ua hoʻoheheʻe ʻia ka 10g o ka pāpaʻi acetate anhydrous i loko o kahi hopena 100mL o 90mL glacial acetic acid a me 10mL acetic anhydride.
(9) 25% sodium acetate solution (220g/L, mana: 2 mahina)
E hoʻoheheʻe i 220g o ka sodium acetate anhydrous i ka wai a hoʻoheheʻe i 1000mL.
(10) Hydrochloric acid (1:1, mana: 2 mahina)
E hoʻohui i ka waika hydrochloric concentrated me ka wai ma kahi ratio 1:1.
(11) Acetate buffer solution (pH=3.5, mana: 2 mahina)
E hoʻoheheʻe i 60mL acetic acid i 500mL wai, a laila hoʻohui i 100mL ammonium hydroxide a hoʻoheheʻe i 1000mL.
(12) Hoʻomākaukau hoʻomākaukau ʻana i ka nitrate alakaʻi
159.8mg o ke kēpau nitrate ua hoʻoheheʻe ʻia i loko o 100mL wai i loaʻa ka 1mL o ka waikawa nitric (density 1.42g/cm3), hoʻoheheʻe ʻia i 1000mL o ka wai a hui maikaʻi. E hana ʻia ka hoʻomākaukau ʻana a me ka mālama ʻana i kēia hopena i loko o ke aniani alakaʻi ʻole.
(13) Haʻina alakaʻi maʻamau (mana: 2 mahina)
Ua hoʻoheheʻe ʻia kahi ana kūpono o 10mL o ka hoʻomākaukau hoʻomākaukau ʻana o ke kēpau nitrate me ka wai i 100mL.
(14) 2% hydroxylamine hydrochloride solution (manawa o ka mana: 1 mahina)
E hoʻoheheʻe i 2g o ka hydroxylamine hydrochloride i 98mL o ka wai.
(15) Ammonia (5mol/L, mana: 2 mahina)
Ua hoʻoheheʻe ʻia ka 175.25g o ka amonia i ka wai a hoʻoheheʻe ʻia i 1000mL.
(16) Wai huikau (manawa mana: 2 mahina)
Hoʻohui i 100mL glycerol, 75mLNaOH solution (1mol/L), a me 25mL wai.
(17) Thioacetamide solution (4%, mana: 2 mahina)
Ua hoʻoheheʻe ʻia ka 4g thioacetamide i 96g wai.
(18) Phenanthroline (0.1%, mana: 1 mahina)
E hoʻoheheʻe i 0.1g o-phenanthroline i 100mL wai.
(19) Acid stannous chloride (mana: 1 mahina)
E hoʻoheheʻe i 20g stannous chloride i loko o 50mL hydrochloric acid concentrated.
(20) Potassium hydrogen phthalate solution buffer maʻamau (pH 4.0, mana: 2 mahina)
10.12g o ka potassium hydrogen phthalate (KHC8H4O4) i kaupaona pono a maloo ma (115±5) ℃ no 2~3h. E hoʻoheheʻe i ka 1000mL me ka wai.
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3.533g o anhydrous disodium hydrogen phosphate a me 3.387g o ka potassium dihydrogen phosphate i maloʻo ma (115±5) ℃ no 2 ~ 3h ua kaupaona pono a hoʻoheheʻe ʻia i 1000mL me ka wai.
3, hydroxypropyl methyl cellulose hui hoʻoholo maʻiʻo
(1) Ka hoʻoholo ʻana i ka ʻike methoxy
Hoʻoholo ʻia ka ʻike o ka methoxy ma muli o ka decomposition o ka waika hydroiodate ma ka hoʻomehana ʻana me kahi hoʻāʻo i loaʻa i ka methoxy e hana i ka methane iodide volatile (kahi paila 42.5 ° C). Hoʻopili ʻia ka methane iodide me ka nitrogen i loko o ka hopena autoreaction. Ma hope o ka holoi ʻana no ka wehe ʻana i nā mea keakea (HI, I2 a me H2S), hoʻomohu ʻia ka ʻea iodine methane e ka solution potassium acetate acetic acid me Br2 i lilo i IBr a laila oxidized i iodic acid. Ma hope o ka distillation, e hoʻoneʻe ʻia nā mea i loko o ka ʻae i nā hue iodine a hoʻoheheʻe ʻia me ka wai. Ma hope o ka hoʻohui ʻana i ka waika formic e wehe i ka Br2, ua hoʻohui ʻia ʻo KI a me H2SO4. Hiki ke helu ʻia ka ʻike methoxy ma ka titrating 12 me ka hopena o Na2S2O3. Hiki ke hōʻike ʻia ka hoʻohālikelike ʻana penei.
Hōʻike ʻia ka mea hana no ke ana ʻana i ka ʻike methoxy ma ke Kiʻi 7-6.
I ka 7-6 (a), A he 50mL poʻe lalo lalo i hoʻopili ʻia me kahi catheter. Hoʻolako ʻia ka bottleneck me kahi paipu hoʻoheheʻe ea pololei E, ma kahi o 25cm ka lōʻihi a me 9mm ka anawaena o loko. Hoʻopiʻi ʻia ka ʻaoʻao o luna o ka paipu i loko o kahi paipu capillary aniani me kahi puka i lalo a me 2mm ka anawaena o loko. Hōʻike ka 7-6 (b) i ka mea hana i hoʻomaikaʻi ʻia. ʻO 1 ka ipu hoʻonā, he 50mL poʻe lalo lalo, a aia ka paipu nitrogen ma ka hema. ʻO 2 ka paipu condensing vertical; ʻO 3 ka mea holoi holoi, kahi wai holoi; ʻO 4 ka paipu hoʻoheheʻe. ʻO ka ʻokoʻa nui loa ma waena o ka hāmeʻa a me ke ʻano pharmacopoeia, ʻo ia ka hui ʻana o nā mea hoʻoheheʻe ʻelua o ke ʻano pharmacopoeia i hoʻokahi, hiki ke hōʻemi i ka nalowale o ka hopena absorption hope. Eia kekahi, ʻokoʻa ka wai holoi i ka scrubber mai ke ʻano pharmacopoeia, ʻo ia ka wai distilled, a ʻo ka mea i hoʻomaikaʻi ʻia he hui ʻia o ka solution cadmium sulfate a me ka solution sodium thiosulfate, hiki ke maʻalahi i ka adsorb i nā haumia i loko o ke kinoea distilled.
Pipetta mea kani: 5mL (5), 10mL (1); Bureta: 50mL; ʻO ka ʻōmole ana iodine: 250mL; E noʻonoʻo i ke kaulike.
Reagent phenol (no ka mea he paʻa ia, no laila e hoʻohui ʻia ma mua o ka hānai ʻana); ʻO ka carbon dioxide a i ʻole ka nitrogen; ʻAkika Hydroiodate (45%); ʻIkepili o ka maʻemaʻe; ʻO ka hopena o ka potassium acetate (100g / L); Bromine: maʻemaʻe analytically; Formic acid: analytically pure; 25% sodium acetate solution (220g/L); KI: analytical pure; E hoʻoheheʻe i ka sulfuric acid (1+9); ʻO ka sodium thiosulfate solution maʻamau (0.1mol / L); Hōʻailona Phenolphthalein; 1% solution ethanol; Hōʻike ka starch: 0.5% starch i ka wai; E hoʻoheheʻe i ka sulfuric acid (1+16.5); 30% chromium trioxide solution; ʻO ka wai kūlohelohe ʻole: hoʻohui i 10mL dilute sulfuric acid (1 + 16.5) i 100mL wai, wela i ka paila, a hoʻohui i ka 0.1ml0.02mol /L potassium permanganate titer, hoʻolapalapa no 10min, pono e mālama i ka ʻulaʻula; 0.02mol/L sodium hydroxide titration solution: E like me ka Chinese Pharmacopoeia appendix method, 0.1mol/L sodium hydroxide titration solution i hoʻopaʻa ʻia a hoʻoheheʻe ʻia i ka 0.02mol/L me ka wai i hoʻolapalapa ʻia a maloʻo.
E hoʻohui ma kahi o 10mL o ka wai holoi holoi i loko o ka pahu holoi, hoʻohui i 31mL o ka mea hou i hoʻomākaukau ʻia i loko o ka pahu absorption, e hoʻokomo i ka mea hana, kaupaona ma kahi o 0.05g (pololei i 0.0001g) o ka hāpana maloʻo i hoʻomaloʻo ʻia i ke kaumaha mau ma 105 ℃ i loko o ka pahu pane, a hoʻohui i 5mL hydroiodate. Hoʻopili koke ʻia ka ʻōmole hopena i ka condenser hoʻihoʻi (ua hoʻomaʻemaʻe ʻia ka waha wili me ka hydroiodate), a hoʻomoʻi ʻia ka nitrogen i loko o ka pahu ma ka helu o 1 ~ 2 mau pahu i kēlā me kēia kekona. Hoʻomalu mālie ʻia ka mahana i piʻi ka mahu o ka wai paila i ka hapalua o ke kiʻekiʻe o ka condenser. Aia ka manawa pane i ke ʻano o ka hāpana, ma waena o 45min a me 3h. Wehe i ka paipu hoʻoheheʻe a hoʻoneʻe pono i ka wai hoʻoheheʻe i loko o kahi pahu iodine 500mL i loaʻa ka 10ml o 25% solution sodium acetate a hiki i ka nui o ka leo ma kahi o 125mL.
Ma lalo o ka lulu mau, e hoʻohui mālie i ka waika formic i kēlā me kēia kulu a nalowale ka melemele. E hoʻohui i kahi hāʻule o 0.1% methyl red indicator, a ʻaʻole e nalowale ka ʻulaʻula no 5 mau minuke. A laila hoʻohui i ʻekolu kulu o ka formic acid. E noho no kekahi manawa, a laila hoʻohui i 1g o ka potassium iodide a me 5mL o ka sulfuric acid dilute (1+9). Hoʻopili ʻia ka haʻina me ka 0.1mol/L sodium thiosulfate solution maʻamau, a ua hoʻohui ʻia nā kulu 3 ~ 4 o ka hōʻailona starch 0.5% kokoke i ka hopena, a ua hoʻomau ʻia ka titration a hiki i ka nalo ʻana o ke kala uliuli.
Ma ke kūlana like, ua hana ʻia kahi hoʻokolohua blank.
Heluhelu o ka huina methoxide:
Kahi, V1 hōʻike i ka leo (mL) o ka sodium thiosulfate solution maʻamau i hoʻopau ʻia e nā laʻana titration; ʻO V2 ka nui o ka hopena maʻamau sodium thiosulfate i hoʻopau ʻia i ka hoʻokolohua blank, mL; ʻO C ka paona o ka sodium thiosulfate solution maʻamau, mol/L; M pili i ka nuipa o ka hāpana maloʻo, g; ʻO 0.00517 ka 0.1mol/L sodium thiosulfate no 1ml like me 0.00517g o ka methoxy.
Hōʻike ka helu methoxy i ka nui o ka methoxy a me ka waiwai hydroxyproxy o ka helu methoxy, no laila pono e hoʻoponopono ʻia ka nui o ka alkoxy e ka hopena hydroxyproxy maʻiʻo e loaʻa ai ka ʻike methoxy pololei. E HOOPONOPONO MUA KA MAU HYDROXYPROPOXY NO PROPENE I HANAIA E KA HANA O HI ME HYDROXYPROPYL ME KA MAU K=0.93 (KE MEAN O KA HELU NUI O NA LA'ANA I HOOLOHE IA E KE METHOD Morgan). No laila:
Maʻiʻo methoxy i hoʻoponopono ʻia = maʻiʻo methoxy piha – (maʻiʻo hydroxypropoxy ×0.93×31/75)
ʻO nā helu 31 a me 75 ka nui o nā molar o nā hui methoxy a me hydroxypropoxy.
(2) Ka hoʻoholo ʻana o ka ʻike hydroxypropoxy
Hoʻopili ka pūʻulu hydropropoxy i ka hāpana me ka chromium trioxide e hana i ka ʻakika acetic. Ma hope o ka hoʻoheheʻe ʻia ʻana mai ka hopena autoreaction, hoʻoholo ʻia ka ʻike o ka chromic acid e ka titration me ka solution NaOH. Ma muli o ka lawe ʻia ʻana o ka waika chromic liʻiliʻi ma ke kaʻina distillation, e hoʻopau pū ʻia ka hopena NaOH, no laila e hoʻoholo hou ʻia ka ʻike o kēia waikawa chromic e ka iodimetry a unuhi ʻia mai ka helu ʻana. ʻO ka hoohalike pane:
Nā mea hana a me nā reagents He hui piha o nā mea hana no ka hoʻoholoʻana i nā hui hydroxypropoxy; ʻO ka'ōmole Volumetric: 1L, 500mL; Ke ana ana i ka cylinder: 50mL; Paipu: 10mL; ʻOmole ana iodine: 250mL. Burette kumu: 10mL; ʻO ka sodium thiosulfate solution maʻamau (0.1mol / L); E hoʻoheheʻe i ka sulfuric acid (1+16.5); E hoʻoheheʻe i ka sulfuric acid (1+9); Hōʻailona mākū (0.5%).
ʻO 7-7 kahi mea hana no ka hoʻoholo ʻana i ka ʻike hydroxypropoxy.
Ma 7-7 (a), D he 25mL pālua ʻāʻī distilling ipu, B he 25mm × 150mm pahu hoʻoheheʻe mahu, C he paipu pili kahe, A he ʻauʻau ʻaila hoʻomehana uila, E he kolamu shunt, G he ipu conical me ka ipu aniani, ʻo ke anawaena o loko he 0.25-1.25mm, hoʻokomo ʻia i loko o ka ipu hoʻoheheʻe; F he paipu condensing i hoohui ia me E. Ma ka mea hana i hooponoponoia i hoikeia ma FIG. ʻO 7-7 (b), ʻo 1 ka reactor, ʻo ia ka pahu hoʻoheheʻe 50mL; ʻO 2 ke poʻo distillation; ʻO 3 he 50mL aniani funnel e hoʻomalu i ka wikiwiki o ke kahe wai kūlohelohe; 4 he paipu nitrogen; 5 ka paipu condensing. ʻO ka ʻokoʻa koʻikoʻi ma waena o ka mea hana i hoʻololi ʻia a me ke ʻano pharmacopoeia, ʻo ia ka hoʻohui ʻana i kahi funnel aniani e hoʻomalu i ka kahe o ka wai, i hiki ke hoʻokele maʻalahi i ka wikiwiki o ka distillation.
ʻO nā ʻano hoʻāʻo i ka hāpana o ka 105 ℃ maloʻo i ke kaumaha mau ma kahi o 0.1 g (0.0002 g), pololei i ʻōlelo ʻia ma ka distillation omole, hoʻohui i 10 ml o 30% chromium trioxide solution, ka distillation flask i loko o ke kīʻaha ʻauʻau aila, pae wai wai ʻauʻau. e like me ka chromium trioxide wai wai, nā lako i hoʻokomo ʻia, ka wai hoʻoluʻu hāmama, ka nitrogen, o kā mākou hale hana e hoʻomalu i ka nui o ka nitrogen e pili ana i hoʻokahi pahu i kekona. I loko o 30min, ua wela ka ʻauʻau aila i 155 ℃ a mālama ʻia i kēia mahana a hiki i ka hopena i hōʻiliʻili ʻia i 50mL. Hoʻopau ʻia ka distillation e wehe i ka ʻauʻau ʻaila.
E holoi i ka paia o loko o ka mea hoʻomaʻamaʻa me ka wai hoʻomaʻemaʻe, e hui i ka wai holoi a me ka distillate i loko o kahi hue iodine 500mL, e hoʻohui i 2 kulu o 1% phenolphthalide indicator, titrate me 0.02mol / L sodium hydroxide solution i ka waiwai pH o 6.9 ~ 7.1 , a kakau iho i ka huina nui o ka sodium hydroxide i pau.
E hoʻohui i ka 0.5g sodium bicarbonate a me 10mL dilute sulfuric acid (1+16.5) i loko o ka ʻōmole iodine a waiho ʻia a kū ʻole a hana ʻia ke kalapona dioxide. A laila e hoʻohui i ka 1.0g potassium iodide, e hoʻopili paʻa, e lulu maikaʻi a waiho i loko o ka pōʻeleʻele no 5min. A laila e hoʻohui i 1mL 0.5% hōʻailona starch a e hoʻokaʻawale iā ia me 0.02mol/L sodium thiosulfate a hiki i ka hopena. E kākau i ka nui o ka sodium thiosulfate i ʻai ʻia.
Ma kahi hoʻokolohua ʻē aʻe, ua hoʻopaʻa ʻia nā helu leo o ka sodium hydroxide a me ka sodium thiosulfate titrators i hoʻopau ʻia.
Ka helu ʻana o ka maʻiʻo hydroxypropoxy:
ʻO K ke kiʻi helu hoʻoponopono o ka hoʻokolohua paʻa: ʻO V1 ka nui o ka titration sodium hydroxide i hoʻopau ʻia e ka hāpana, mL. ʻO C1 ka manaʻo o ka sodium hydroxide solution maʻamau, mol / L; ʻO V2 ka nui o ka sodium thiosulfate titration i hoʻopau ʻia e ka hāpana, mL; ʻO C2 ka paʻa o ka sodium thiosulfate solution maʻamau, mol / L; ʻO M ka nuipaʻa hāpana, g; ʻO Va ka leo o ka sodium hydroxide titration i hoʻopau ʻia ma ka hoʻokolohua blank, mL; ʻO Vb ka nui o ka sodium thiosulfate titration i hoʻopau ʻia ma ka hoʻokolohua paʻa, mL.
4. Ka hoʻoholoʻana i ka maʻamau
Ke kaulike analytical instrumental (pololei i ka 0.1mg); Ana omole: anawaena 60mm, kiekie 30mm; ʻO ka umu hoʻomaloʻo.
ʻO ke ala hoʻāʻo e kaupaona pololei i ka hāpana 2~ 4G (
Ka manawa hoʻouna: Sep-08-2022