Phthalimide Potassium ntsev CAS 1074-82-4 Purity > 99.0% (HPLC)

3. Kev sim
3.1 Loss ntawm ziab (W / W)
3.1.1 Cov khoom siv thiab cov cuab yeej siv
Ib tshaj kaum txhiab ntawm hluav taws xob tshuav, hluav taws xob thermostatic ziab qhov cub, 40 * 25 lub raj mis hnyav, tshuab ziab khaub ncaws
Reagent: silica gel
3.1.2 Txoj kev
1. Ntxuav 3 40 * 25 lub raj mis hnyav.
2, muab tso rau hauv qhov cub ntawm 105 ℃ (± 2 ℃) qhuav rau 1 teev.
3. Tshem tawm lub raj mis hnyav 40 * 25 thiab muab tso rau hauv lub tshuab ziab khaub ncaws kom txias rau 30 feeb.
4, Qhov tseeb qhov hnyav 40 * 25 ntsuas lub raj mis khoob qhov hnyav W0.
5. Siv lub raj mis hnyav 40 * 25 los ntsuas qhov sib npaug sib npaug ntawm 3.0000g (W1), tag nrho ntawm 3.
6, Muab tso rau hauv qhov cub, tshem tawm lub hau lub raj mis, muab tso rau ntawm ib sab ntawm lub raj mis uas hnyav, lossis ib nrab qhib lub raj mis kom qhuav, tshem tawm, yuav tsum yog lub raj mis zoo, qhuav ntawm 105 ℃ (± 2 ℃) rau 3 hnu.
7. Tshem tawm lub raj mis uas hnyav 40 * 25 thiab muab tso rau hauv lub tshuab ziab kom txias rau 30 feeb.
8, Qhov tseeb qhov hnyav tom qab ziab 40 * 25 qhov hnyav ntawm lub raj mis W2.
Kev suav cov mis: poob ntawm ziab (%) = (W1-W2) / (W1-W0) × 100%
3. 4 Kev txiav txim siab txog cov ntsiab lus
3.4.1 Cov cuab yeej thiab cov cuab yeej siv
LC-UV100 Liquid Chromatograph (Shanghai Wufeng Scientific Instrument Co., LTD.)
10ml volumetric raj mis, stainless hlau kaum diav thiab lwm yam chaw
3.3.2 Cov txheej txheem
Txoj kev rau kev tsom xam Phthalimide Potassium ntsev
3.3.3 Ua kua chromatography
Chromatographic mob
Chromatographic kem: HypersilC6H5 (C8 kuj muaj) 4.6 * 250mm 5um
Ntsuas wavelength: 210nm
Kem kub: 30 ℃
Flow tus nqi: 1.0ml / min
Sample concentration: 0.05mg / ml (diluent yog theem mobile)
Reagents
Potassium Phosphate Dibasic (analytical ntshiab)
Phthalimide Potassium ntsev (tus qauv qauv)
Acetonitrile (kev tsom xam ntshiab)
Dej ntshiab
Mobile theem: acetonitrile: phosphate tsis (PH: 3.5) = 40:60
Qhov hnyav 1.63g Potassium Phosphate Dibasic thiab yaj hauv 600ml dej ntshiab, kho tus nqi PH rau 3.5 nrog phosphoric acid, ncuav rau hauv 1000ml beaker uas muaj 400ml acetonitrile, sib tov zoo, lim nrog 0.45um sib xyaw fiber ntau lim membrane, yaj nrog ultrasonic vibration, thiab standby daim ntawv thov.
3.3.4 Cov txheej txheem
1) Configuration test solution (0.05mg/ml)
Cov qauv 2.5mg tau raug ntsuas kom raug thiab muab tso rau hauv lub raj mis ntim 50ml.Lub sijhawm txawb tau ntxiv thiab diluted mus rau qhov ntsuas los ntawm ultrasonic dissolution.
2) Cov txheej txheem kev daws teeb meem (1.0mg / ml)
Tus qauv qauv 2.5mg tau raug ntsuas kom raug thiab muab tso rau hauv lub raj mis ntim 50ml.Lub sijhawm txawb tau ntxiv thiab diluted mus rau qhov ntsuas los ntawm ultrasonic dissolution.
3) System usability:
(1) Muab lub taub hau lim rau hauv 80% methanol thaum pib, qhib lub valve thiab ntws rau 3-5min, thiab kaw lub valve thiab yaug rau 10-15 feeb.Tom qab ntawd muab lub taub lim dej tso rau hauv 90% dej ntshiab, qhib lub valve thiab ntws rau 3-5min, kaw lub valve thiab yaug rau 10 feeb.
(2) Tom qab ntawd hloov lub sijhawm npaj txawb, tus nqi ntws yog 1.0ml / min, sab pem hauv ntej siab tsawg dua 1000Psi, qhib lub ntsuas, tos kom txog thaum lub hauv ntej siab ruaj khov, qhib lub computer workstation, thiab nkag mus hauv online
(3) Tom qab sab pem hauv ntej lub siab ruaj khov, qhib lub ntes.Ua ntej txhaj 1 koob ntawm lub sijhawm txawb, tom qab ntawd txhaj 1 koob ntawm tus qauv qauv, thiab thaum kawg txhaj cov qauv.
(4) Cov txiaj ntsig suav: thaj chaw normalization txoj kev
(5) Tom qab ua tiav txoj haujlwm tsom xam, kaw lub ntsuas ntsuas ua ntej, thiab tom qab ntawd yaug lub taub hau lim hauv dej ntshiab rau 10-15 feeb;Nyob rau tib lub sijhawm, qhov kev txhaj tshuaj valve tau yaug nrog dej thiab methanol.
(6) Thaum kawg, muab tso rau ntawm 80% methanol, yaug rau 30 feeb, thiab kaw.
4. Tom qab ua tiav kev tshuaj xyuas, sau rau hauv daim ntawv tshuaj ntsuam xyuas thiab kuaj cov ntawv kuaj.