{"id":3260,"date":"2024-03-04T06:25:08","date_gmt":"2024-03-04T06:25:08","guid":{"rendered":"https:\/\/longchangextracts.com\/?p=2966"},"modified":"2024-03-04T06:25:08","modified_gmt":"2024-03-04T06:25:08","slug":"what-do-you-know-about-recrystallisation-experience-and-methods","status":"publish","type":"post","link":"https:\/\/longchangextracts.com\/tr\/yeniden-kristallestirme-deneyimi-ve-yontemleri-hakkinda-ne-biliyorsunuz\/","title":{"rendered":"Yeniden kristalle\u015ftirme deneyimi ve y\u00f6ntemleri hakk\u0131nda ne biliyorsunuz?"},"content":{"rendered":"

Yeniden kristalle\u015ftirme deneyimi ve y\u00f6ntemleri hakk\u0131nda ne biliyorsunuz?<\/strong><\/h1>\n

Kristalizasyon s\u00fcreci kontrol\u00fc ve \u00fcr\u00fcn \u00f6zelliklerinin d\u00fczenlenmesi<\/p>\n

Yeniden kristalle\u015ftirme bir \u00f6\u011frenme s\u00fcrecidir. \u00c7\u00f6z\u00fcc\u00fc se\u00e7imi (tekli veya birle\u015fik), kristalle\u015fme s\u0131cakl\u0131\u011f\u0131, kar\u0131\u015ft\u0131rma h\u0131z\u0131, kar\u0131\u015ft\u0131rma y\u00f6ntemi, a\u015f\u0131r\u0131 doygunluk se\u00e7imi, kristalleri y\u00fckseltme s\u00fcresi, \u00e7\u00f6z\u00fcc\u00fc ekleme \u015fekli ve oran\u0131 vb. kristallerin safl\u0131\u011f\u0131n\u0131 ve kristal \u015feklini etkileyecektir.<\/p>\n

Yeniden Kristalle\u015ftirme Safla\u015ft\u0131rma Prensipleri<\/p>\n

Yeniden kristalle\u015ftirme y\u00f6ntemi, kat\u0131 bir kar\u0131\u015f\u0131m\u0131n bile\u015fenlerinin belirli bir \u00e7\u00f6z\u00fcc\u00fcdeki farkl\u0131 \u00e7\u00f6z\u00fcn\u00fcrl\u00fckleri ile birbirlerinden ayr\u0131lmas\u0131 ger\u00e7e\u011finden yararlan\u0131r. Yeniden kristalle\u015ftirme i\u00e7in basit prosed\u00fcr, saf olmayan kat\u0131 maddeyi uygun bir s\u0131cak \u00e7\u00f6z\u00fcc\u00fcde \u00e7\u00f6zerek neredeyse doymu\u015f bir \u00e7\u00f6zelti olu\u015fturmak, \u00e7\u00f6z\u00fcnmeyen safs\u0131zl\u0131klar\u0131 gidermek i\u00e7in hala s\u0131cakken s\u00fczmek, s\u00fcz\u00fcnt\u00fcy\u00fc so\u011futmak, b\u00f6ylece kristallerin a\u015f\u0131r\u0131 doymu\u015f \u00e7\u00f6zeltiden \u00e7\u00f6kelmesini ve \u00e7\u00f6z\u00fcnen safs\u0131zl\u0131klar\u0131n ana lik\u00f6rde kalmas\u0131n\u0131 sa\u011flamakt\u0131r, ana s\u0131v\u0131dan kristalleri pompalay\u0131n ve filtreleyin, kurutun ve ard\u0131ndan erime noktas\u0131n\u0131 belirleyin, \u00f6rne\u011fin \u00fcr\u00fcn\u00fcn safl\u0131\u011f\u0131 hala gereksinimlere uygun de\u011filse, \u00fcr\u00fcn\u00fcn safl\u0131\u011f\u0131 gereksinimleri kar\u015f\u0131layana kadar yeniden kristalle\u015ftirilebilir. Safl\u0131k hala gereksinimleri kar\u015f\u0131lam\u0131yorsa, gereksinimleri kar\u015f\u0131layana kadar yeniden kristalle\u015ftirme tekrar yap\u0131labilir.<\/p>\n

 <\/p>\n

Kristalizasyon ve yeniden kristalizasyon detayl\u0131 i\u015fletim prosed\u00fcrleri<\/p>\n

1. Safla\u015ft\u0131r\u0131lacak kimyasal reaktifi kaynayan veya kaynayacak olan uygun bir \u00e7\u00f6z\u00fcc\u00fcde \u00e7\u00f6z\u00fcn;
\n2. \u00c7\u00f6z\u00fcnmeyen safs\u0131zl\u0131klar\u0131 gidermek i\u00e7in s\u0131cak \u00e7\u00f6zeltiyi hala s\u0131cakken s\u00fcz\u00fcn;
\n3. Kristallerin \u00e7\u00f6kelmesi i\u00e7in s\u00fcz\u00fcnt\u00fcn\u00fcn so\u011futulmas\u0131;
\n4. Gerekirse kristalleri y\u0131kamak i\u00e7in uygun bir \u00e7\u00f6z\u00fcc\u00fc ile kristalleri s\u00fcz\u00fcn<\/p>\n

 <\/p>\n

1, eleme \u00e7\u00f6z\u00fcc\u00fcs\u00fc: kristalize edilecek bir test t\u00fcp\u00fcne (bu\u011fday taneleri b\u00fcy\u00fckl\u00fc\u011f\u00fcnde) az miktarda ekleyin, yukar\u0131daki kurallara g\u00f6re se\u00e7ilen \u00e7\u00f6z\u00fcc\u00fcden 0,5 mL ekleyin, \u00e7\u00f6z\u00fcnenin \u00e7\u00f6z\u00fcn\u00fcp \u00e7\u00f6z\u00fcnmedi\u011fini g\u00f6rmek i\u00e7in birka\u00e7 dakika \u0131s\u0131t\u0131n ve kaynat\u0131n. \u00c7\u00f6z\u00fcnm\u00fc\u015fse, kristallerin \u00e7\u00f6k\u00fcp \u00e7\u00f6kmedi\u011fini g\u00f6rmek i\u00e7in test t\u00fcp\u00fcn\u00fc testin d\u0131\u015f\u0131na y\u0131kamak i\u00e7in musluk suyu kullan\u0131n. Yeni ba\u015flayanlar genellikle \u00e7\u00f6z\u00fcnmeyen safs\u0131zl\u0131klar\u0131 kristalle\u015fmi\u015f olarak kabul eder! Uzun s\u00fcreli \u0131s\u0131tmadan sonra bile hala \u00e7\u00f6z\u00fcnmeyen maddeler varsa, test t\u00fcp\u00fcn\u00fc birka\u00e7 dakika b\u0131rakabilir ve test t\u00fcp\u00fcn\u00fc so\u011fuk suyla so\u011futabilirsiniz (\u00e7alkalamay\u0131n). E\u011fer madde berrak s\u0131v\u0131n\u0131n \u00fcst katman\u0131nda \u00e7\u00f6kelirse, bu biraz daha \u00e7\u00f6z\u00fcnebilece\u011fi anlam\u0131na gelir. Hafif bulan\u0131ksa, \u00e7\u00f6z\u00fcc\u00fc \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fc \u00e7ok azd\u0131r; de\u011fi\u015fiklik yoksa, \u00e7\u00f6z\u00fcnmeyen kat\u0131lar bir \u015feydir, \u00e7\u00f6z\u00fcnebilir maddeler olmu\u015ftur ve \u00e7ok \u00e7\u00f6z\u00fcn\u00fcr, \u00e7\u00f6kelmesi kolay de\u011fildir.<\/p>\n

2, rutin i\u015flem: konik bir \u015fi\u015fede veya yuvarlak tabanl\u0131 \u015fi\u015fede 52A0 \u00e7\u00f6z\u00fcnen maddeye ve belirli bir \u00e7\u00f6z\u00fcc\u00fcye, topun \u00fczerine monte edilmi\u015f so\u011fuk, 10 dakika \u0131s\u0131t\u0131lm\u0131\u015f, hala \u00e7\u00f6z\u00fcnmeyen malzeme varsa, \u00e7\u00f6z\u00fcnmeyi tamamlamak i\u00e7in \u00e7\u00f6z\u00fcc\u00fcn\u00fcn a\u011fz\u0131ndaki kondansat\u00f6r t\u00fcp\u00fcnden telafi etmeye devam edin ve ard\u0131ndan fazla 30% \u00e7\u00f6z\u00fcc\u00fc ekleyin. Katlanm\u0131\u015f filtre ka\u011f\u0131d\u0131 (katlanm\u0131\u015f filtre ka\u011f\u0131d\u0131 ve \u00fc\u00e7gen huni \u00f6nceden \u0131s\u0131t\u0131lacak) s\u0131cak iken konik bir \u015fi\u015feye s\u00fcz\u00fcl\u00fcr. S\u00fcz\u00fcnt\u00fc do\u011fal olarak so\u011fur ve bir B\u00fcchner hunisinden \u00e7ekilir (konik \u015fi\u015feyi s\u00fcz\u00fcnt\u00fc ile tersten durulay\u0131n!). . Maddenin oda s\u0131cakl\u0131\u011f\u0131nda \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fc azsa, filtre keki az miktarda so\u011fuk \u00e7\u00f6z\u00fcc\u00fc ile y\u0131kanabilir (\u00f6nce azalt\u0131lm\u0131\u015f bas\u0131nc\u0131 geri \u00e7ekin, filtre kekini \u0131slatmak i\u00e7in az miktarda \u00e7\u00f6z\u00fcc\u00fc ekleyin ve ard\u0131ndan azalt\u0131lm\u0131\u015f bas\u0131n\u00e7 alt\u0131nda kurutun. (Not: filtre kekinin bir cam t\u0131pa ile s\u0131k\u0131\u015ft\u0131r\u0131lmas\u0131 daha fazla \u00e7\u00f6z\u00fcc\u00fcden kurtulmaya yard\u0131mc\u0131 olur! Kullan\u0131lan \u00e7\u00f6z\u00fcc\u00fc u\u00e7ucu de\u011filse, kek atmosferik bas\u0131n\u00e7ta az miktarda u\u00e7ucu \u00e7\u00f6z\u00fcc\u00fc ile \u0131slat\u0131labilir, \u00f6rne\u011fin DMF etanol ile y\u0131kanabilir, diklorobenzen, klorobenzen, ksilen, siklohekzanon toluen ile y\u0131kanabilir. Yeni ba\u015flayanlar genellikle sorunlarla kar\u015f\u0131la\u015f\u0131r: filtre ka\u011f\u0131d\u0131nda \u00e7ok say\u0131da kristal \u00e7\u00f6kelir, bunun nedeni huni ve filtre ka\u011f\u0131d\u0131 \u00f6n \u0131s\u0131tmas\u0131n\u0131n iyi olmamas\u0131, \u00e7ok az \u00e7\u00f6z\u00fcc\u00fc doz a\u015f\u0131m\u0131, filtrasyon s\u00fcresinin \u00e7ok uzun olmas\u0131d\u0131r. \u00dcr\u00fcn de\u011ferliyse, \u00fc\u00e7gen huni ve filtre ka\u011f\u0131d\u0131 buhar \u00f6n \u0131s\u0131tmal\u0131 konik bir \u015fi\u015feye yerle\u015ftirilebilir, filtrat ile filtreleme s\u0131ras\u0131nda buhar yal\u0131t\u0131m\u0131 filtrelenmi\u015ftir, ancak yukar\u0131daki i\u015flem daha tehlikelidir, toluen, eter, petrol eteri, sikloheksan ve di\u011fer yan\u0131c\u0131 \u00e7\u00f6z\u00fcc\u00fcler bu y\u00f6ntemi kullanmak i\u00e7in dikkatli olmal\u0131d\u0131r. Not: Filtre ka\u011f\u0131d\u0131n\u0131 y\u0131kamak i\u00e7in s\u0131cak yeniden kristalle\u015ftirme ana lik\u00f6r\u00fc ve t\u00fcm yap\u0131\u015f\u0131k \u00e7\u00f6z\u00fcnen aparatlar ve so\u011futma kristal kayb\u0131n\u0131 azaltabilir.<\/p>\n

3, s\u0131cak filtrasyonun paradoksal \u00e7al\u0131\u015fmas\u0131: emi\u015f filtresi \u015fi\u015fesi \u00f6nceden \u0131s\u0131t\u0131lamaz, Brinell'in hunisi ve filtre ka\u011f\u0131d\u0131, y\u00fckselen buhar \u0131slatmas\u0131n\u0131 kullanmak i\u00e7in konik \u015fi\u015fenin \u00fcst\u00fcndeki \u00e7\u00f6zeltide, emi\u015f filtresi \u015fi\u015fesine koyun ve hemen s\u0131cak filtrasyon s\u0131ras\u0131nda. Emme filtresi \u015fi\u015fesindeki ana lik\u00f6r\u00fcn kaynamas\u0131n\u0131 \u00f6nlemek i\u00e7in pompalama bas\u0131nc\u0131n\u0131n \u00e7ok b\u00fcy\u00fck olamayaca\u011f\u0131n\u0131 unutmay\u0131n! Yeni ba\u015flayanlar taraf\u0131ndan yap\u0131lan yayg\u0131n hatalar: filtre ka\u011f\u0131d\u0131 s\u0131k\u0131ca lamine edilmemi\u015ftir (\u00e7ift katmanl\u0131 ka\u011f\u0131t kullan\u0131labilir), yava\u015f hareketler B\u00fcchner hunisinde kristallerin \u00e7\u00f6kelmesine neden olur, \u00e7ok y\u00fcksek pompalama bas\u0131nc\u0131 filtrat\u0131n pompaya emilmesine neden olur ve filtrasyon tamamland\u0131ktan hemen sonra bas\u0131n\u00e7 kald\u0131r\u0131lmad\u0131\u011f\u0131 i\u00e7in pompaya b\u00fcy\u00fck miktarda \u00e7\u00f6z\u00fcc\u00fc pompalan\u0131r.<\/p>\n

K\u0131sacas\u0131, \"benzer \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fcn\" aksine, b\u00fcy\u00fck polariteli \u015feyleri kristalize etmek i\u00e7in orta polariteli \u00e7\u00f6z\u00fcc\u00fcler ve k\u00fc\u00e7\u00fck polariteli \u015feyleri kristalize etmek i\u00e7in b\u00fcy\u00fck polariteli \u00e7\u00f6z\u00fcc\u00fcler kullanmak do\u011frudur. Bu \u015fekilde, vakalar\u0131n yar\u0131s\u0131ndan fazlas\u0131 uygundur.<\/p>\n

 <\/p>\n

1. \u00d6nce petrol eteri (hekzan), eter, etil asetat, etanol, su ve ard\u0131ndan aseton, metanol, asetonitril, benzen, kloroform, asetik asit, piridin ve benzerlerini deneyin. Bu i\u015fe yaramazsa, bunlar\u0131 kar\u0131\u015ft\u0131rman\u0131z gerekecektir. Eter (1) u\u00e7uculu\u011fu ve (2) cam\u0131 yukar\u0131 do\u011fru uzatarak kat\u0131lar\u0131 \u00e7\u00f6keltme \u00f6zelli\u011fi i\u00e7in kullan\u0131labilir. Aseton, su ile de\u011filse, kurutulmal\u0131d\u0131r.<\/p>\n

2. Kar\u0131\u015f\u0131k \u00e7\u00f6z\u00fcc\u00fc y\u00f6ntemi: fazla s\u0131cak iyi \u00e7\u00f6z\u00fcc\u00fc ile \u00e7\u00f6z\u00fcn, s\u00fcz\u00fcn, \u0131s\u0131t\u0131n, bulan\u0131kla\u015fana kadar yava\u015f\u00e7a k\u00f6t\u00fc \u00e7\u00f6z\u00fcc\u00fc ekleyin, berrakla\u015fana kadar \u0131s\u0131t\u0131n. Beklemeye b\u0131rak\u0131n ve bekleyin.<\/p>\n

3. Kademeli kristalizasyon y\u00f6ntemi ile. Kolon \u00fczerinde biriken ana s\u0131v\u0131.
\n1) kolon \u00fczerinde \u00f6n safla\u015ft\u0131rma, ham ay\u0131rma ve ard\u0131ndan kristalle\u015ftirme; 2) petrol eteri s\u0131cak ekstraksiyon - so\u011fuk \u00e7\u00f6keltme y\u00f6ntemi; 3) eter gibi d\u00fc\u015f\u00fck kaynama noktal\u0131 bir \u00e7\u00f6z\u00fcc\u00fc se\u00e7in; 4) kristalin t\u00fcrlerin elde edilmesi, bir damla \u00e7\u00f6zeltiyi dald\u0131rmak i\u00e7in bir cam \u00e7ubukla, u\u00e7ucu hale getirilmi\u015f kuru. 5) \u00e7\u00f6z\u00fcc\u00fcn\u00fcn do\u011fal olarak buharla\u015fmas\u0131na izin verme y\u00f6ntemi ile kolayca donmaz.<\/p>\n

Eter ile kristallendirme \u00fczerine. Eteri geri ak\u0131t\u0131rken bir kondansat\u00f6r t\u00fcp\u00fc ekleyin. Bulan\u0131kl\u0131k kaybolana kadar \u00fcst porttan eter eklemeye devam edin, bazen bunun nedeni \u00e7\u00f6z\u00fcnmenin yava\u015f olmas\u0131, \u00e7\u00f6z\u00fcnmemesi de\u011fildir, bu nedenle sab\u0131rl\u0131 olun. \u00c7ok fazla eter eklenirse ve hala \u00e7\u00f6z\u00fcnmeyen az miktarda \u00e7\u00f6kelti varsa, s\u00fcz\u00fcl\u00fcr ve s\u00fcz\u00fcnt\u00fc kat\u0131 bir \u00e7\u00f6kelti olu\u015fana kadar konsantre edilir, daha sonra tekrar \u0131s\u0131t\u0131l\u0131r ve berrakla\u015ft\u0131rmak i\u00e7in az miktarda eter eklenir. Do\u011fal olarak so\u011fumaya b\u0131rak\u0131n ve iyi kristal formda kristaller elde edilebilir. Filtre edin. Kristalleri az miktarda eter ile y\u0131kay\u0131n. Y\u0131kamalar ana lik\u00f6rle birle\u015ftirilir ve ana lik\u00f6r\u00fc i\u00e7eren \u015fi\u015fenin a\u011fz\u0131 bir filtre ka\u011f\u0131d\u0131 tabakas\u0131yla kapat\u0131l\u0131r veya eterin toz haline gelmeden do\u011fal olarak buharla\u015fmas\u0131n\u0131 sa\u011flamak i\u00e7in bir top ka\u011f\u0131t mendille doldurulur. Tatmin edici say\u0131da kristal \u00e7\u0131kana kadar her sabah bak\u0131n ve \u00e7ok a\u00e7g\u00f6zl\u00fc olmay\u0131n, buharla\u015f\u0131r ve kurursa her \u015feye yeniden ba\u015flamak zorunda kal\u0131rs\u0131n\u0131z \ud83d\ude42 Bu y\u00f6ntemi hem levo- hem de dekstro-alkaloidleri ba\u015far\u0131l\u0131 bir \u015fekilde ay\u0131rmak i\u00e7in kulland\u0131m. \"Petrol eteri s\u0131cak ekstraksiyon - so\u011futma y\u00f6ntemi\" de ya\u011fla ba\u015fa \u00e7\u0131kmak i\u00e7in kulland\u0131\u011f\u0131m y\u00f6ntemdir, petrol eteri ekleyin, kaynat\u0131n, s\u00fcpernatant\u0131 d\u00f6k\u00fcn, alttaki ya\u011fa petrol eteri eklemeye devam edin s\u0131cak ekstraksiyon, petrol eteri tabakas\u0131 renksiz olana kadar, o zaman ekstraksiyon temelde tamamlanm\u0131\u015ft\u0131r. Kristaller genellikle so\u011fuduktan sonra \u00e7\u00f6kelir.
\nYa\u011f haline gelmenin bir di\u011fer nedeni de \u00e7ok h\u0131zl\u0131 so\u011fumakt\u0131r.<\/p>\n

 <\/p>\n

 <\/p>\n

Dikkat edilmesi gereken birka\u00e7 sorun<\/p>\n

1. \u00d6nceden safla\u015ft\u0131r\u0131lm\u0131\u015f kimyasal reaktifleri \u00e7\u00f6zerken, laboratuvar g\u00fcvenlik y\u00f6netmeliklerine kesinlikle uymal\u0131 ve yan\u0131c\u0131 ve patlay\u0131c\u0131 \u00e7\u00f6z\u00fcc\u00fcleri \u0131s\u0131t\u0131rken, a\u00e7\u0131k alev olmayan bir ortamda \u00e7al\u0131\u015fmal\u0131 ve do\u011frudan \u0131s\u0131tmadan ka\u00e7\u0131nmal\u0131y\u0131z. \u00c7\u00f6z\u00fcn\u00fcrl\u00fck e\u011frisi normal \u015fartlar alt\u0131nda \u00e7\u00f6z\u00fcc\u00fcn\u00fcn kaynama noktas\u0131 yak\u0131n\u0131nda dik bir \u015fekilde y\u00fckseldi\u011finden, kristalizasyon ve yeniden kristalizasyon s\u0131ras\u0131nda \u00e7\u00f6z\u00fcc\u00fc kaynama noktas\u0131na kadar \u0131s\u0131t\u0131lmal\u0131d\u0131r. Kristalizasyon ve yeniden kristalizasyon veriminin y\u00fcksek olmas\u0131 i\u00e7in \u00e7\u00f6z\u00fcc\u00fc miktar\u0131 m\u00fcmk\u00fcn oldu\u011funca azd\u0131r, bu nedenle ba\u015flang\u0131\u00e7ta eklenen \u00e7\u00f6z\u00fcc\u00fc miktar\u0131 safla\u015ft\u0131r\u0131lmak istenen t\u00fcm kimyasal reaktifleri \u00e7\u00f6zmek i\u00e7in yeterli de\u011fildir, \u0131s\u0131tma s\u00fcrecinde kat\u0131 maddenin kaynamas\u0131 tamamen \u00e7\u00f6z\u00fclene kadar dikkatlice \u00e7\u00f6z\u00fcc\u00fc eklenebilir. \u00c7\u00f6z\u00fcc\u00fc eklerken dikkatli olun, \u00e7\u00f6zelti kaynama noktas\u0131n\u0131n alt\u0131na so\u011futulur, patlamaya dayan\u0131kl\u0131 zeolit etkili de\u011fildir, yeni bir zeolit eklemeniz gerekir.<\/p>\n

2. Kristalle\u015fme ve yeniden kristalle\u015fme i\u015flemlerini niceliksel olarak de\u011ferlendirmek ve tekrarlamay\u0131 kolayla\u015ft\u0131rmak i\u00e7in kat\u0131lar ve \u00e7\u00f6z\u00fcc\u00fcler tart\u0131lmal\u0131 ve \u00f6l\u00e7\u00fclmelidir.<\/p>\n

3. Kristalizasyon ve yeniden kristalizasyon i\u00e7in kar\u0131\u0122\u0131k \u00e7\u00f6z\u00fcc\u00fclerin kullan\u0131m\u0131nda, en iyisi safla\u0122t\u0131r\u0131lacak kimyasal\u0131 az miktarda daha fazla \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011fe sahip bir \u00e7\u00f6z\u00fcc\u00fcde \u00e7\u00f6zmek ve ard\u0131ndan daha az \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011fe sahip ikinci \u00e7\u00f6z\u00fcc\u00fcy\u00fc hen\u00fcz s\u0131cakken \u00e7\u00f6zeltinin \u00e7\u00f6kelti olu\u0122an k\u0131sm\u0131na de\u011fip hemen \u00e7\u00f6z\u00fcnene kadar k\u00fc\u00e7\u00fck porsiyonlar halinde yava\u0122\u00e7a eklemektir. \u00c7\u00f6zeltinin toplam hacmi \u00e7ok k\u00fc\u00e7\u00fckse, daha fazla \u00e7\u00f6z\u00fcnen \u00e7\u00f6z\u00fcc\u00fcden daha fazla ekleyin ve prosed\u00fcr\u00fc tekrarlay\u0131n. Bazen tersi bir prosed\u00fcr de kullan\u0131labilir, safla\u015ft\u0131r\u0131lacak kimyasal reaktif k\u00fc\u00e7\u00fck \u00e7\u00f6z\u00fcn\u00fcrl\u00fckl\u00fc \u00e7\u00f6z\u00fcc\u00fcde s\u00fcspanse edilir, \u00e7\u00f6z\u00fcnene kadar yava\u015f\u00e7a b\u00fcy\u00fck \u00e7\u00f6z\u00fcn\u00fcrl\u00fckl\u00fc \u00e7\u00f6z\u00fcc\u00fc eklenir ve ard\u0131ndan so\u011futulacak k\u00fc\u00e7\u00fck \u00e7\u00f6z\u00fcn\u00fcrl\u00fckl\u00fc k\u00fc\u00e7\u00fck bir \u00e7\u00f6z\u00fcc\u00fcye b\u0131rak\u0131l\u0131r.<\/p>\n

4. Gerekirse, safla\u015ft\u0131r\u0131lacak kimyasal reaktif \u00e7\u00f6z\u00fcld\u00fckten sonra renk giderme i\u00e7in aktif karbon ekleyebilir (dozaj, safla\u015ft\u0131r\u0131lacak maddenin a\u011f\u0131rl\u0131\u011f\u0131n\u0131n yakla\u015f\u0131k 1\/50~1\/20'sine e\u015fittir) veya \u00e7\u00f6zeltiyi berrakla\u015ft\u0131rmak i\u00e7in filtre ka\u011f\u0131d\u0131 hamuru, diyatomlu toprak vb. ekleyebilirsiniz. Renk giderici madde eklenmeden \u00f6nce \u00e7\u00f6z\u00fcc\u00fc hafif\u00e7e so\u011futulmal\u0131d\u0131r, \u00e7\u00fcnk\u00fc renk giderici maddenin eklenmesi \u00f6nceden engellenmi\u015f bir kaynamay\u0131 otomatik olarak tetikleyerek \u015fiddetli ve patlay\u0131c\u0131 bir ani kaynamaya neden olabilir. Aktif karbon b\u00fcy\u00fck miktarda hava i\u00e7erir ve bu nedenle k\u00f6p\u00fcrebilir. Aktif karbon ilave edildikten sonra 5-10 dakika kaynat\u0131labilir ve ard\u0131ndan aktif karbon hala s\u0131cakken filtreleme yoluyla \u00e7\u0131kar\u0131labilir. Benzen, petrol eteri gibi polar olmayan \u00e7\u00f6z\u00fcc\u00fclerde aktif karbon renk giderme etkisi iyi de\u011fildir, al\u00fcmina renk giderme ile adsorpsiyon gibi di\u011fer y\u00f6ntemleri deneyebilirsiniz.<\/p>\n

5. Organik reaktifler i\u00e7in kimyasal reaktifleri safla\u015ft\u0131rmak istiyorsan\u0131z, a\u015f\u0131r\u0131 doymu\u015f \u00e7\u00f6zelti olu\u015fumu e\u011filimi \u00e7ok b\u00fcy\u00fckt\u00fcr, bu fenomeni \u00f6nlemek i\u00e7in ayn\u0131 t\u00fcr reaktif veya homojen homokristal kristal t\u00fcrlerine eklenebilir. Duvar\u0131 bir cam \u00e7ubukla ovmak da bir \u00e7ekirdek olu\u015fturabilir, ard\u0131ndan kristaller bu \u00e7ekirdek boyunca b\u00fcy\u00fcyecektir.<\/p>\n

6. Kristalle\u015fme h\u0131z\u0131 bazen \u00e7ok yava\u015ft\u0131r ve so\u011fuk \u00e7\u00f6zeltilerin kristalle\u015fmesinin tamamlanmas\u0131 bazen birka\u00e7 saat s\u00fcrer. Baz\u0131 durumlarda, kristaller haftalar veya aylar sonra \u00e7\u00f6kelmeye devam edecektir, bu nedenle ana lik\u00f6r \u00e7ok erken at\u0131lmamal\u0131d\u0131r.<\/p>\n

7. Safla\u015ft\u0131r\u0131lacak reaktifin \u00e7\u00f6zeltideki \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fcn\u00fc azaltmak, b\u00f6ylece daha fazla kristal \u00e7\u00f6keltmek ve verimi art\u0131rmak i\u00e7in \u00e7\u00f6zelti genellikle dondurulur. Buzdolab\u0131na yerle\u015ftirilebilir veya buz, kar\u0131\u015f\u0131k so\u011futucu ak\u0131\u015fkanlarla so\u011futulabilir.<\/p>\n

8. Haz\u0131rlanan s\u0131cak \u00e7\u00f6zelti, \u00e7\u00f6z\u00fcnmeyen safs\u0131zl\u0131klar\u0131 gidermek i\u00e7in filtrelenmeli ve filtreleme s\u0131ras\u0131nda filtre \u00fczerinde kristalle\u015fmesi \u00f6nlenmelidir. T\u00fcm i\u015flemler d\u00fczenli ise, ger\u00e7ekten reaktifin kristalleri \u00e7\u00f6keltmesi ve filtrasyonu engellemesi \u00e7ok kolay oldu\u011fundan, \u00e7\u00f6zelti biraz seyreltik olarak haz\u0131rlanabilir veya yal\u0131t\u0131m veya \u0131s\u0131t\u0131lm\u0131\u015f filtrasyon cihaz\u0131 (yal\u0131t\u0131ml\u0131 huni gibi) filtrasyonu kullan\u0131labilir.<\/p>\n

9. \u00c7\u00f6kelmi\u015f kristalleri ana s\u0131v\u0131dan etkili bir \u015fekilde ay\u0131rmak i\u00e7in, filtreleme genellikle bir Brinell hunisi kullan\u0131larak ger\u00e7ekle\u015ftirilir. Kristalleri ana s\u0131v\u0131dan daha iyi ay\u0131rmak i\u00e7in, kristalleri temiz bir cam t\u0131pa ile Brinell hunisinden s\u0131kmak ve ana s\u0131v\u0131n\u0131n m\u00fcmk\u00fcn oldu\u011funca \u00e7o\u011funu pompalayarak \u00e7\u0131karmak en iyisidir. Kristallerin y\u00fczeyindeki ana s\u0131v\u0131 m\u00fcmk\u00fcn oldu\u011funca az \u00e7\u00f6z\u00fcc\u00fc ile y\u0131kanabilir. Bu durumda, pompalama ge\u00e7ici olarak durdurulmal\u0131 ve preslenmi\u015f kristalleri gev\u015fetmek i\u00e7in bir cam \u00e7ubuk veya paslanmaz \u00e7elik b\u0131\u00e7ak kullan\u0131lmal\u0131, nemlendirmek i\u00e7in az miktarda \u00e7\u00f6z\u00fcc\u00fc eklenmeli ve kristallerin d\u00fczg\u00fcn bir \u015fekilde emprenye edilebilmesi i\u00e7in birka\u00e7 dakika beklenmeli ve ard\u0131ndan tekrar kuru olarak pompalanmal\u0131 ve bu bir veya iki kez tekrarlanmal\u0131d\u0131r, b\u00f6ylece emprenye edilmi\u015f y\u00fczeylere ba\u011fl\u0131 ana lik\u00f6r\u00fcn tamam\u0131 \u00e7\u0131kar\u0131l\u0131ncaya kadar \u00e7\u0131kar\u0131lmal\u0131d\u0131r.<\/p>\n

10. E\u011fer kristaller \u0131s\u0131ya maruz kald\u0131\u011f\u0131nda ayr\u0131\u015fm\u0131yorsa, f\u0131r\u0131nda \u0131s\u0131t\u0131larak kurutulabilir. Kristallerin \u0131s\u0131 ile ayr\u0131\u015fmas\u0131 kolaysa, f\u0131r\u0131n\u0131n s\u0131cakl\u0131\u011f\u0131n\u0131n \u00e7ok y\u00fcksek olmamas\u0131na dikkat edilmeli veya oda s\u0131cakl\u0131\u011f\u0131nda kurutmak i\u00e7in vakumlu kurutucuya konulmal\u0131d\u0131r. Yeniden kristalle\u015ftirme y\u00fcksek kaynama noktas\u0131na sahip \u00e7\u00f6z\u00fcc\u00fclerle ger\u00e7ekle\u015ftiriliyorsa, kristaller kurumay\u0131 kolayla\u015ft\u0131rmak i\u00e7in d\u00fc\u015f\u00fck kaynama noktas\u0131na ve az \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011fe sahip \u00e7\u00f6z\u00fcc\u00fclerle y\u0131kanmal\u0131d\u0131r. Kolay eriyebilen kristaller \u00f6nce f\u0131r\u0131nda belirli bir s\u0131cakl\u0131\u011fa kadar \u0131s\u0131t\u0131lmal\u0131 ve ard\u0131ndan kristaller f\u0131r\u0131na konulmal\u0131d\u0131r; ancak \u00e7ok kolay eriyebilen kristaller f\u0131r\u0131nda pi\u015firilemez ve h\u0131zl\u0131 bir \u015fekilde kurumalar\u0131 i\u00e7in vakum desikat\u00f6r\u00fcne konulmal\u0131d\u0131r. Yan\u0131c\u0131 organik \u00e7\u00f6z\u00fcc\u00fclerle yeniden kristalle\u015ftirilen kristaller g\u00f6nderilmeden \u00f6nce f\u0131r\u0131nda kurutulmal\u0131d\u0131r, aksi takdirde \u00e7\u00f6z\u00fcc\u00fcn\u00fcn yanmas\u0131na veya patlamas\u0131na neden olabilir.<\/p>\n

11. Yeniden kristalize edilen k\u00fc\u00e7\u00fck ve eser miktardaki maddeler: Yukar\u0131da belirtilen temel gerekliliklerle kristalize edilen veya yeniden kristalize edilen k\u00fc\u00e7\u00fck miktardaki maddeler, ancak k\u00fc\u00e7\u00fck kaba uygun madde miktar\u0131 ile kullan\u0131l\u0131r. Eser maddelerin kristalizasyonu ve yeniden kristalizasyonu k\u00fc\u00e7\u00fck santrif\u00fcj t\u00fcplerinde ger\u00e7ekle\u015ftirilebilir. S\u0131cak \u00e7\u00f6zelti haz\u0131rland\u0131ktan hemen sonra santrif\u00fcjlenir, b\u00f6ylece kabul edilemez safs\u0131zl\u0131klar t\u00fcp\u00fcn dibine \u00e7\u00f6ker ve \u00fcst tabaka kristalle\u015fmek \u00fczere ba\u015fka bir k\u00fc\u00e7\u00fck santrif\u00fcj t\u00fcp\u00fcne pipetlenir. Kristalizasyondan sonra kristaller santrif\u00fcjleme yoluyla ana s\u0131v\u0131dan ayr\u0131l\u0131r. Kristaller ayr\u0131ca santrif\u00fcj t\u00fcp\u00fcnde az miktarda \u00e7\u00f6z\u00fcc\u00fc ile y\u0131kanabilir ve \u00e7\u00f6z\u00fcc\u00fc santrif\u00fcjleme ile kristallerden ayr\u0131labilir.<\/p>\n

12. Ana lik\u00f6r genellikle istenen maddenin belirli bir miktar\u0131n\u0131 i\u00e7erir ve bu madde dikkatle geri kazan\u0131lmal\u0131d\u0131r. \u00c7\u00f6z\u00fcc\u00fc k\u0131smen \u00e7\u0131kar\u0131l\u0131r ve ard\u0131ndan kristallerin \u00e7\u00f6kmesi i\u00e7in so\u011fumaya b\u0131rak\u0131l\u0131rsa, genellikle ilk kez \u00e7\u00f6keltilen kristaller kadar saf olmazlar. Safl\u0131k kontrol\u00fc gereksinimleri kar\u015f\u0131lam\u0131yorsa, safl\u0131k gereksinimlerini kar\u015f\u0131layana kadar taze \u00e7\u00f6z\u00fcc\u00fc kristalleri kullan\u0131labilir.<\/p>\n

 <\/p>\n

\u00c7\u00f6z\u00fcc\u00fc se\u00e7imi<\/p>\n

Yeniden kristalle\u015ftirme i\u015fleminin ba\u015far\u0131s\u0131 i\u00e7in uygun \u00e7\u00f6z\u00fcc\u00fcn\u00fcn se\u00e7ilmesi b\u00fcy\u00fck \u00f6nem ta\u015f\u0131r, iyi bir \u00e7\u00f6z\u00fcc\u00fc a\u015fa\u011f\u0131daki ko\u015fullar\u0131 kar\u015f\u0131lamal\u0131d\u0131r:
\n1, safla\u015ft\u0131r\u0131lm\u0131\u015f malzeme ile kimyasal reaksiyon yok
\n2, y\u00fcksek s\u0131cakl\u0131kta safla\u015ft\u0131r\u0131lm\u0131\u015f malzemenin b\u00fcy\u00fck bir miktar\u0131n\u0131 \u00e7\u00f6zebilir ve oda s\u0131cakl\u0131\u011f\u0131nda veya daha d\u00fc\u015f\u00fck s\u0131cakl\u0131kta sadece k\u00fc\u00e7\u00fck bir miktar\u0131n\u0131 \u00e7\u00f6zebilir;
\n3. Safs\u0131zl\u0131klar\u0131n \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fc \u00e7ok b\u00fcy\u00fck veya \u00e7ok k\u00fc\u00e7\u00fckt\u00fcr, ilk durumda safs\u0131zl\u0131klar ana lik\u00f6rde kal\u0131r, ikinci durumda ise safs\u0131zl\u0131klar s\u0131cakken filtrelenir;
\n4. \u00c7\u00f6z\u00fcc\u00fcn\u00fcn kaynama noktas\u0131 ne \u00e7ok d\u00fc\u015f\u00fck ne de \u00e7ok y\u00fcksek olmal\u0131d\u0131r. Bir \u00e7\u00f6zelti haline getirildi\u011finde \u00e7\u00f6z\u00fcc\u00fcn\u00fcn kaynama noktas\u0131 \u00e7ok d\u00fc\u015f\u00fckt\u00fcr ve s\u0131cakl\u0131k fark\u0131n\u0131n iki a\u015famal\u0131 i\u015fleminin so\u011futma kristalizasyonu k\u00fc\u00e7\u00fckt\u00fcr, grup malzemesinin \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fc \u00e7ok fazla de\u011fi\u015fmez, verimi etkiler ve d\u00fc\u015f\u00fck kaynama noktal\u0131 \u00e7\u00f6z\u00fcc\u00fc i\u015flemi uygun de\u011fildir, \u00f6rne\u011fin eter kullan\u0131lmamal\u0131d\u0131r. \u00c7\u00f6z\u00fcc\u00fc kaynama noktas\u0131 \u00e7ok y\u00fcksektir, kristalin y\u00fczeyine yap\u0131\u015fan \u00e7\u00f6z\u00fcc\u00fcn\u00fcn \u00e7\u0131kar\u0131lmas\u0131 kolay de\u011fildir.<\/p>\n

5. Daha iyi kristalle\u015fme sa\u011flayabilir.<\/p>\n

\u00c7e\u015fitli \u00e7\u00f6z\u00fcc\u00fclerde uygulanabilir, geri kazan\u0131m oran\u0131n\u0131n kristalle\u015fmesine, kullan\u0131m kolayl\u0131\u011f\u0131na, \u00e7\u00f6z\u00fcc\u00fcn\u00fcn toksisitesinin boyutuna ve yan\u0131c\u0131 olup olmad\u0131\u011f\u0131na, fiyat\u0131n y\u00fcksek veya d\u00fc\u015f\u00fck olmas\u0131na ve b\u00f6ylece en iyisinin se\u00e7imine dayanmal\u0131d\u0131r.<\/p>\n

 <\/p>\n

1\u3001Yayg\u0131n olarak kullan\u0131lan \u00e7\u00f6z\u00fcc\u00fcler: DMF, klorobenzen, ksilen, toluen, asetonitril, etanol, THF, kloroform, etil asetat, siklohekzan, b\u00fctanon, aseton, petrol eteri.<\/p>\n

2, daha yayg\u0131n olarak kullan\u0131lan \u00e7\u00f6z\u00fcc\u00fcler: DMSO, hekzametilfosforamid, N-metilpirolidon, benzen, siklohekzanon, b\u00fctanon, siklohekzanon, diklorobenzen, piridin, asetik asit, dioksan, etilen glikol monometil eter, 1,2-dikloroetan, etil eter, n-oktan.<\/p>\n

3, kristalin malzemeyi i\u015flemek i\u00e7in kaynama noktas\u0131na yak\u0131n iyi bir \u00e7\u00f6z\u00fcc\u00fc \u00e7\u00f6z\u00fcn\u00fcrl\u00fck y\u00fcksektir ve d\u00fc\u015f\u00fck s\u0131cakl\u0131klarda \u00e7\u00f6z\u00fcn\u00fcrl\u00fck \u00e7ok azd\u0131r. DMF, benzen, dioksan, siklohekzan donma noktas\u0131na yak\u0131n d\u00fc\u015f\u00fck s\u0131cakl\u0131klarda \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fc \u00e7ok zay\u0131f olan ideal \u00e7\u00f6z\u00fcc\u00fclerdir. Asetonitril, klorobenzen, ksilen, toluen, b\u00fctanon, etanol de ideal \u00e7\u00f6z\u00fcc\u00fclerdir.<\/p>\n

4, \u00e7\u00f6z\u00fcc\u00fcn\u00fcn kaynama noktas\u0131, kristal malzemenin erime noktas\u0131n\u0131n 50 \u2103'den d\u00fc\u015f\u00fck olmas\u0131ndan daha iyidir. Aksi takdirde, \u00e7\u00f6z\u00fcnen s\u0131v\u0131la\u015fma tabakala\u015fma fenomeni \u00fcretmek kolayd\u0131r.<\/p>\n

5, \u00e7\u00f6z\u00fcc\u00fcn\u00fcn kaynama noktas\u0131 ne kadar y\u00fcksekse, kaynarken \u00e7\u00f6z\u00fcc\u00fcl\u00fck o kadar g\u00fc\u00e7l\u00fcd\u00fcr, y\u00fcksek erime noktal\u0131 maddeler i\u00e7in, y\u00fcksek kaynama noktal\u0131 bir \u00e7\u00f6z\u00fcc\u00fc se\u00e7mek en iyisidir.<\/p>\n

6, hidroksil, amino i\u00e7eren ve erime noktas\u0131 \u00e7ok y\u00fcksek olmayan oksijenli \u00e7\u00f6z\u00fcc\u00fcleri m\u00fcmk\u00fcn oldu\u011funca tercih etmeyin. \u00c7\u00fcnk\u00fc \u00e7\u00f6z\u00fcnen ve \u00e7\u00f6z\u00fcc\u00fc molek\u00fcller aras\u0131 hidrojen ba\u011f\u0131 olu\u015fturdu\u011fundan \u00e7\u00f6kelmesi zordur.<\/p>\n

7, oksijen, nitrojen i\u00e7eren maddeler ayn\u0131 nedenden dolay\u0131 \u00e7\u00f6z\u00fcc\u00fc olarak alkol\u00fc se\u00e7memeye \u00e7al\u0131\u015f\u0131n.<\/p>\n

8, \u00e7\u00f6z\u00fcnen ve \u00e7\u00f6z\u00fcc\u00fc polaritesi \u00e7ok farkl\u0131 olmamal\u0131d\u0131r. Su>Formik asit>Metanol>Asetik asit>Etanol>\u0130zopropanol>Asetonitril>DMSO>DMF>Aseton>HMPA>CH2Cl2>Piridin>Kloroform>Klorobenzen>THF>Dioksan>Eter>Benzen>Toluen>CCl4>Oktan>Siklohekzan>Petrol eteri.<\/p>\n

 <\/p>\n

 <\/p>\n

 <\/p>\n

Kristallerin \u00e7\u00f6kelmesi hakk\u0131nda<\/p>\n

Kristalle\u015fme ko\u015fullar\u0131: temel olarak s\u0131cakl\u0131k, bas\u0131n\u00e7, kar\u0131\u015ft\u0131rma veya kar\u0131\u015ft\u0131rmama. S\u0131cakl\u0131k \u00e7ok \u00f6nemlidir, genellikle d\u00fc\u015f\u00fck s\u0131cakl\u0131kta so\u011futma yap\u0131yoruz, asl\u0131nda bazen y\u00fcksek s\u0131cakl\u0131kta izolasyona ihtiya\u00e7 duyuyoruz! Bunun esas olarak kristalle\u015fme s\u0131cakl\u0131\u011f\u0131n\u0131 belirlemede \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fc aras\u0131ndaki ili\u015fkiyi bulmas\u0131 gerekir. Kar\u0131\u015ft\u0131rma da etkili bir fakt\u00f6rd\u00fcr, kristal formun kristalle\u015fmesi, kristalle\u015fme h\u0131z\u0131 \u00fczerinde bir etkisi vard\u0131r.<\/p>\n

 <\/p>\n

Kristal form ve verim \u00fczerinde gradyan so\u011futma ko\u015fullar\u0131n\u0131n se\u00e7imi de daha b\u00fcy\u00fck bir etkiye sahiptir.<\/p>\n

Kristal \u00e7ekirde\u011fi ilavesinin zamanlamas\u0131 da s\u00f6z konusudur: \u00e7ok erken eklenen kristal \u00e7ekirde\u011fi, kristal form taraf\u0131ndan \u00e7\u00f6z\u00fclen veya \u00fcretilen kristal \u00e7ekirde\u011fi genellikle iyidir; ge\u00e7 eklendi\u011finde, \u00e7\u00f6zelti \u00e7ekirde\u011fi \u00fcretmi\u015f olabilir ve kristalle\u015fme safs\u0131zl\u0131klarla sar\u0131lm\u0131\u015f olabilir<\/p>\n

 <\/p>\n

Filtrasyon ile elde edilen s\u00fcz\u00fcnt\u00fc so\u011futuldu\u011funda kristaller \u00e7\u00f6kelecektir. So\u011fuk su veya buzlu su ile h\u0131zl\u0131 so\u011futma ve \u00e7\u00f6zeltiyi kuvvetlice kar\u0131\u015ft\u0131rarak, \u00e7ok k\u00fc\u00e7\u00fck kristaller elde edebilirsiniz, hava s\u0131cakl\u0131\u011f\u0131nda s\u0131cak bir \u00e7\u00f6zelti olacak ko\u015fullarda yava\u015f so\u011futma yaparak, d\u00fczg\u00fcn ve daha b\u00fcy\u00fck bir g\u00f6vde elde edebilirsiniz.<\/p>\n

 <\/p>\n

\u00c7\u00f6zelti so\u011futulursa ve kristaller hala \u00e7\u00f6kelmemi\u015fse, cam silme Mo s\u0131v\u0131 seviyesinin alt\u0131ndaki kap duvar\u0131n\u0131 kontrol etmek i\u00e7in kullan\u0131labilir, ayr\u0131ca t\u00fcrlere eklenebilir veya \u00e7\u00f6zeltinin s\u0131cakl\u0131\u011f\u0131n\u0131 daha da d\u00fc\u015f\u00fcrmek i\u00e7in kullan\u0131labilir (buzlu su veya di\u011fer donmu\u015f \u00e7\u00f6zelti ile so\u011futulur).<\/p>\n

 <\/p>\n

\u00dcr\u00fcn so\u011futulduktan ve ya\u011f elde edildikten sonra \u00e7\u00f6zelti \u00e7\u00f6kelmezse, berrakla\u015ft\u0131r\u0131lm\u0131\u015f s\u0131cak bir \u00e7\u00f6zelti olu\u015fturmak i\u00e7in yeniden \u0131s\u0131t\u0131labilir, kendi kendine so\u011fumaya b\u0131rak\u0131labilir ve \u00fcr\u00fcn\u00fcn \u00e7\u00f6kelmesini h\u0131zland\u0131rmak i\u00e7in \u00e7\u00f6zeltiyi bir cam \u00e7ubukla s\u00fcrekli kar\u0131\u015ft\u0131rarak, kab\u0131n duvarlar\u0131na veya d\u00f6k\u00fcm \u00e7e\u015fitlerine s\u00fcrt\u00fcnebilir. Hala ya\u011fl\u0131 bir madde d\u0131\u015far\u0131 \u00e7\u0131kmaya ba\u015flarsa, ya\u011f damlac\u0131klar\u0131n\u0131n da\u011f\u0131lmas\u0131n\u0131 sa\u011flamak i\u00e7in hemen kuvvetlice kar\u0131\u015ft\u0131r\u0131lmal\u0131d\u0131r.<\/p>\n

 <\/p>\n

 <\/p>\n

Kristal y\u00f6nteminin safl\u0131\u011f\u0131n\u0131 belirleyin<\/p>\n

Fiziksel ve kimyasal \u00f6zellikler tek tiptir; kat\u0131 bile\u015fik erime mesafesi \u2264 2 \u2103; TLC veya PC a\u00e7\u0131l\u0131m\u0131 tek bir noktad\u0131r; HPLC veya GC analizi tek bir piktir, NMR spektrumunda \u00e7apak yoktur.<\/p>\n

 <\/p>\n

Daha fazla yap\u0131lan baz\u0131 \u00fcr\u00fcnler, tekrarlanan yeniden kristalle\u015ftirmeden sonra numune gibi deneyime dayanabilir, \u00f6nceki test sonu\u00e7lar\u0131na g\u00f6re kristal t\u00fcr\u00fcn\u00fcn nas\u0131l g\u00f6r\u00fcnmesi gerekti\u011fine bak\u0131n, safl\u0131\u011f\u0131 yakla\u015f\u0131k sekiz veya dokuz olmal\u0131d\u0131r.<\/p>\n

 <\/p>\n

 <\/p>\n

Kristalle\u015fme ipu\u00e7lar\u0131<\/p>\n

 <\/p>\n

1. Kristallerin haz\u0131rlanmas\u0131nda, uygun \u00e7\u00f6z\u00fcc\u00fclerin se\u00e7ilmesine ve do\u011fru miktarda \u00e7\u00f6z\u00fcc\u00fc uygulanmas\u0131na dikkat edilmelidir. Uygun \u00e7\u00f6z\u00fcc\u00fcler, tercihen \u00e7\u00f6z\u00fcn\u00fcrl\u00fc\u011f\u00fcn gerekli bile\u015fenleri \u00fczerinde so\u011fukta k\u00fc\u00e7\u00fck, \u00e7\u00f6z\u00fcn\u00fcrl\u00fck b\u00fcy\u00fck oldu\u011funda ise \u0131s\u0131d\u0131r. \u00c7\u00f6z\u00fcc\u00fcn\u00fcn kaynama noktas\u0131 \u00e7ok y\u00fcksek olmamal\u0131d\u0131r. Genellikle metanol, aseton, kloroform, etanol, etil asetat sirke vb. kullan\u0131l\u0131r. Ancak baz\u0131 bile\u015fiklerin genel \u00e7\u00f6z\u00fcc\u00fclerde kristal olu\u015fturmas\u0131 kolay de\u011filken, baz\u0131 \u00e7\u00f6z\u00fcc\u00fclerde kristal olu\u015fturmas\u0131 kolayd\u0131r.<\/p>\n

2. Kristal \u00e7\u00f6zeltinin haz\u0131rlanmas\u0131, a\u015f\u0131r\u0131 doymu\u015f \u00e7\u00f6zelti haline gelmesi gerekir. Genel olarak, bile\u015fi\u011fi \u0131s\u0131tma ko\u015fulu alt\u0131nda \u00e7\u00f6zmek i\u00e7in uygun miktarda \u00e7\u00f6z\u00fcc\u00fc uygulanmal\u0131 ve daha sonra so\u011fuk bir yere yerle\u015ftirilmelidir. Kristaller oda s\u0131cakl\u0131\u011f\u0131nda \u00e7\u00f6kt\u00fcr\u00fclebiliyorsa, kristallerle birlikte daha fazla safs\u0131zl\u0131\u011f\u0131n \u00e7\u00f6kelmesini \u00f6nlemek i\u00e7in bunlar\u0131 buzdolab\u0131na yerle\u015ftirmek gerekli de\u011fildir. \"Yeni ekolojik\" maddeler, yani yeni serbest maddeler veya amorf toz halindeki maddeler, kristal halindeki maddelerden \u00e7ok daha fazla \u00e7\u00f6z\u00fcn\u00fcr ve kolayca a\u015f\u0131r\u0131 doymu\u015f \u00e7\u00f6zeltiler olu\u015fturabilir. Genel olarak rafine edilmi\u015f bile\u015fikler, amorf toz i\u00e7in \u00e7\u00f6z\u00fcc\u00fc ekstraksiyonunun buharla\u015ft\u0131r\u0131lmas\u0131nda, bazen az miktarda \u00e7\u00f6z\u00fcc\u00fc eklendi\u011fi s\u00fcrece, genellikle hemen \u00e7\u00f6z\u00fclebilir, kristalleri \u00e7\u00f6keltmek i\u00e7in biraz zaman gerekir.<\/p>\n

3. Kristal \u00e7\u00f6zeltinin haz\u0131rlanmas\u0131, tek bir \u00e7\u00f6z\u00fcc\u00fc se\u00e7imine ek olarak, ayn\u0131 zamanda s\u0131kl\u0131kla bir \u00e7\u00f6z\u00fcc\u00fc kar\u0131\u015f\u0131m\u0131 kullan\u0131r. Genellikle ilk bile\u015fik \u00e7\u00f6z\u00fcn\u00fcr \u00e7\u00f6z\u00fcc\u00fclerde \u00e7\u00f6z\u00fcl\u00fcr ve daha sonra \u00e7\u00f6zelti hafif bulan\u0131k olana kadar oda s\u0131cakl\u0131\u011f\u0131nda damla damla uygun miktarda \u00e7\u00f6z\u00fcnmeyen \u00e7\u00f6z\u00fcc\u00fc eklenir ve bu \u00e7\u00f6zelti hafif\u00e7e \u0131s\u0131t\u0131l\u0131r, b\u00f6ylece \u00e7\u00f6zelti tamamen berrakla\u015ft\u0131r\u0131l\u0131r ve yerle\u015ftirilir.<\/p>\n

4. Kristalizasyon s\u00fcreci, genellikle y\u00fcksek konsantrasyonda \u00e7\u00f6zelti, so\u011futma becerisi, kristallerin daha h\u0131zl\u0131 \u00e7\u00f6kelmesi. Ancak kristal partik\u00fcller daha k\u00fc\u00e7\u00fckt\u00fcr, safs\u0131zl\u0131klar da daha fazla olabilir. Bazen \u00e7\u00f6zeltiden \u00e7\u00f6kelme oran\u0131 \u00e7ok h\u0131zl\u0131d\u0131r, bile\u015fik \u00e7ekirdeklerin olu\u015fumundan daha fazlas\u0131 molek\u00fcler oryantasyon h\u0131z\u0131n\u0131 ikna eder, genellikle sadece amorf toz elde edilir. Bazen \u00e7\u00f6zelti \u00e7ok kal\u0131nd\u0131r, viskozitenin kristalle\u015fmesi kolay de\u011fildir. \u00c7\u00f6zeltinin konsantrasyonu uygunsa, s\u0131cakl\u0131k yava\u015f\u00e7a d\u00fc\u015f\u00fcr\u00fcl\u00fcr, daha b\u00fcy\u00fck kristalleri ve daha y\u00fcksek safl\u0131kta kristalleri \u00e7\u00f6keltmek m\u00fcmk\u00fcnd\u00fcr. Baz\u0131 bile\u015fiklerin kristallerinin olu\u015fmas\u0131 i\u00e7in daha uzun bir s\u00fcre gerekir.<\/p>\n

5. Kristallerin haz\u0131rlanmas\u0131na ek olarak, yukar\u0131daki noktalara dikkat etmelidir, yerle\u015ftirme s\u00fcrecinde, s\u0131v\u0131 y\u00fczeyinin ilk \u00f6nce kristallerin ortaya \u00e7\u0131kmas\u0131n\u0131 \u00f6nlemek i\u00e7in \u015fi\u015feyi s\u0131k\u0131ca t\u0131kamak en iyisidir, bu da kristallerin daha d\u00fc\u015f\u00fck safl\u0131\u011f\u0131na neden olur. Bir s\u00fcre sonra kristal \u00e7\u00f6kelmezse, \u00e7ok az miktarda tohum kristali, yani ayn\u0131 bile\u015fik kristalize k\u00fc\u00e7\u00fck par\u00e7ac\u0131klar ekleyebilirsiniz. Tohum kristallerinin eklenmesi, kristal \u00e7ekirdeklerinin olu\u015fumunu te\u015fvik etmenin yayg\u0131n ve etkili bir yoludur. Genel olarak, kristalle\u015fme s\u00fcreci olduk\u00e7a se\u00e7icidir ve ayn\u0131 molek\u00fcl veya iyon eklendi\u011finde, kristaller hemen b\u00fcy\u00fcme e\u011filimindedir. Dahas\u0131, e\u011fer \u00e7\u00f6zelti optik izomerlerin bir kar\u0131\u015f\u0131m\u0131 ise, ayn\u0131 optik izomer tohum kristalinin do\u011fas\u0131na g\u00f6re tercihli olarak \u00e7\u00f6kelebilir. Tohum kristali yoksa, bir damla doymu\u015f \u00e7\u00f6zelti \u00fczerine bir cam \u00e7ubuk bat\u0131r\u0131labilir, havada bekletilebilir ve \u00e7\u00f6z\u00fcc\u00fcn\u00fcn buharla\u015fmas\u0131na izin verilebilir ve ard\u0131ndan kristal olu\u015fumunu te\u015fvik etmek i\u00e7in kab\u0131n i\u00e7 duvar\u0131n\u0131 \u00e7\u00f6zeltinin kenar\u0131na s\u00fcrtmek i\u00e7in kullan\u0131labilir. Hala kristallerin \u00e7\u00f6kelmesi yoksa, \u00e7\u00f6zeltinin yava\u015f yava\u015f da\u011f\u0131lmas\u0131na izin vermek i\u00e7in \u015fi\u015fe t\u0131pas\u0131n\u0131 a\u00e7abilir, kristalleri yava\u015f\u00e7a \u00e7\u00f6keltebilirsiniz. Veya kristalizasyondan sonra t\u00fcm safs\u0131zl\u0131klar\u0131 gidermek i\u00e7in m\u00fcmk\u00fcn oldu\u011funca ba\u015fka bir uygun \u00e7\u00f6z\u00fcc\u00fc i\u015flemi se\u00e7in veya bir kez daha rafine edin.<\/p>\n

6. Kristallerin haz\u0131rlanmas\u0131nda, \u00fcst \u00e7\u00f6zelti tabakas\u0131n\u0131n olu\u0122umundan hemen sonra bir parti kristal olu\u0122turmak ve daha sonra ikinci bir parti kristal elde etmek i\u00e7in b\u0131rakmak en iyisidir. Kristal malzeme bir \u00e7\u00f6z\u00fcc\u00fc i\u00e7inde \u00e7\u00f6z\u00fclerek tekrar kristalize edilebilir ve rafine edilebilir. Bu y\u00f6nteme yeniden kristalle\u015ftirme denir. \u00c7e\u015fitli par\u00e7alardan elde edilen ana lik\u00f6r\u00fcn yeniden kristalle\u015ftirilmesinden sonra kristalle\u015ftirme ve ard\u0131ndan s\u0131ras\u0131yla ikinci ve \u00fc\u00e7\u00fcnc\u00fc parti kristalleri elde etmek i\u00e7in i\u015flenir. Bu y\u00f6ntem ad\u0131m ad\u0131m kristalizasyon veya kademeli kristalizasyon olarak bilinir. Tekrarlanan kristalizasyon s\u00fcrecinde kristal maddeler, kristallerin \u00e7\u00f6kelmesi her zaman daha h\u0131zl\u0131 ve daha h\u0131zl\u0131d\u0131r, safl\u0131k da daha y\u00fcksek ve daha y\u00fcksektir. Elde edilen par\u00e7alar\u0131n kristalizasyonunun ad\u0131m ad\u0131m kristalizasyon y\u00f6ntemi, safl\u0131\u011f\u0131 genellikle b\u00fcy\u00fck farkl\u0131l\u0131klar g\u00f6sterir, ancak genellikle birden fazla kristal bile\u015fen elde edilebilir, kontrol yoklu\u011funda aceleyle birbirine kar\u0131\u015ft\u0131r\u0131lmaz.<\/p>\n

7. Bile\u015fiklerin kristalle\u015fmesi belirli bir kristal \u015fekline, rengine, erime noktas\u0131na ve erime mesafesine sahiptir, biri tan\u0131mlama i\u00e7in bir \u00f6n temel olarak kullan\u0131labilir. Bu kristal olmayan bir madde fiziksel \u00f6zelliklere sahip de\u011fildir. Bile\u015fik kristallerin \u015fekli ve erime noktas\u0131 genellikle kullan\u0131lan \u00e7\u00f6z\u00fcc\u00fcye ba\u011fl\u0131 olarak de\u011fi\u015fir. Prizmatik kristaller olu\u015fturmak i\u00e7in kloroformda protopin baz\u0131, erime noktas\u0131 207 \u2103; asetonda, yar\u0131m k\u00fcre kristallerin olu\u015fumu, erime noktas\u0131 203 \u2103; kloroform ve aseton kar\u0131\u015f\u0131k \u00e7\u00f6z\u00fcc\u00fcde, kristallerin yukar\u0131daki iki kristal \u015feklinin olu\u015fumudur. Bu nedenle, literat\u00fcrde genellikle bile\u015fi\u011fin kristal \u015fekli, erime noktas\u0131 ve ard\u0131ndan kullan\u0131lan \u00e7\u00f6z\u00fcc\u00fcn\u00fcn belirtisi yer almaktad\u0131r. Erime mesafesinin genel monomer saf bile\u015fik kristalizasyonu daha dard\u0131r, bazen 0.5 \u2103 veya daha fazla gereklidir, erime mesafesi daha uzunsa, bile\u015fi\u011fin saf olmad\u0131\u011f\u0131 anlam\u0131na gelir!<\/p>\n

 <\/p>\n

 <\/p>\n

Modern kristalografinin ana dallar\u0131<\/p>\n

 <\/p>\n

(1) kristal \u00fcretimi (kristalojen): do\u011fal ve yapay kristallerin incelenmesi, b\u00fcy\u00fcme ve de\u011fi\u015fim s\u00fcreci ve mekanizmas\u0131n\u0131n yan\u0131 s\u0131ra bunlar\u0131 kontrol eden ve etkileyen fakt\u00f6rler.
\n(2) Geometrik kristalografi: Kristallerin d\u0131\u015f y\u00fczeyindeki geometrik \u00e7ok y\u00fczl\u00fclerin \u015feklinin ve bunlar aras\u0131ndaki d\u00fczenlili\u011fin incelenmesi.
\n(3) Kristalografi: Kristallerin i\u00e7 yap\u0131s\u0131ndaki plazmalar\u0131n d\u00fczeninin ve kristal yap\u0131n\u0131n kusurlar\u0131n\u0131n incelenmesi.
\n(4) kristalokimya: kristallerin kimyasal bile\u015fimi ve yap\u0131lar\u0131n\u0131n yan\u0131 s\u0131ra kristallerin fiziksel ve kimyasal \u00f6zellikleri aras\u0131ndaki ili\u015fkinin d\u00fczenlili\u011finin incelenmesi.
\n(5) Kristalofizik: Kristallerin fiziksel \u00f6zelliklerinin ve bunlar\u0131 \u00fcreten mekanizmalar\u0131n incelenmesi.<\/p>","protected":false},"excerpt":{"rendered":"

Yeniden kristalle\u015ftirme deneyimi ve y\u00f6ntemleri hakk\u0131nda ne biliyorsunuz? Kristalle\u015fme s\u00fcreci kontrol\u00fc ve \u00fcr\u00fcn \u00f6zelliklerinin d\u00fczenlenmesi Yeniden kristalle\u015fme bir \u00f6\u011frenme s\u00fcrecidir. \u00c7\u00f6z\u00fcc\u00fc se\u00e7imi (tekli veya kombine), kristalle\u015fme s\u0131cakl\u0131\u011f\u0131, kar\u0131\u015ft\u0131rma h\u0131z\u0131, kar\u0131\u015ft\u0131rma y\u00f6ntemi, a\u015f\u0131r\u0131 doygunluk se\u00e7imi, kristalleri y\u00fckseltme s\u00fcresi, \u00e7\u00f6z\u00fcc\u00fc ekleme \u015fekli ve oran\u0131 vb. safl\u0131\u011f\u0131 etkileyecektir [...]<\/p>","protected":false},"author":1,"featured_media":0,"comment_status":"closed","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"footnotes":""},"categories":[20],"tags":[],"yoast_head":"\nWhat do you know about recrystallisation experience and methods? - China Chemical Manufacturer<\/title>\n<meta name=\"robots\" content=\"index, follow, max-snippet:-1, max-image-preview:large, max-video-preview:-1\" \/>\n<link rel=\"canonical\" href=\"https:\/\/longchangextracts.com\/tr\/yeniden-kristallestirme-deneyimi-ve-yontemleri-hakkinda-ne-biliyorsunuz\/\" \/>\n<meta property=\"og:locale\" content=\"tr_TR\" \/>\n<meta property=\"og:type\" content=\"article\" \/>\n<meta property=\"og:title\" content=\"What do you know about recrystallisation experience and methods? - China Chemical Manufacturer\" \/>\n<meta property=\"og:description\" content=\"What do you know about recrystallisation experience and methods? 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