乳酸依沙吖啶一水物中水分含量的测定 应用资料

智能文字提取功能测试中

乳酸依沙吖啶一水物中水分含量的测定 应用资料根据药典规定，使用卡尔费休容量滴定法测量乳酸依沙吖啶一水物中的水分含量。本应用资料说明了根据药典测量该试样水分含量的示例。APKF-0153en Application Note Determination of moisture content in acrinol monohydrate IndustryPharmaceutical InstrumentKarl Fischer moisture titrator Measurement methodVolumetric titration/Direct method Standards The Japanese Pharmacopoeia, GB/T 6283 1. Scope Measuring the moisture content in acrinol monohydrate using the Karl Fischer volumetric titration method is stipulated in the Japanese Pharmacopoeia. This Application Note describes an example of measuring the moisture content of this solution in accordance with the Japanese Pharmacopoeia. 2. Precautions The method uses organic solvents, so place the Karl Fischer moisture titrator inside fume food. 3. Post-measurement procedure Drain the dehydrating agent, and then clean the titration flask and twin platinum electrode using methanol. If the burette is left filled with titrant, crystals will be deposited in the tip of the titration nozzle, clogging the discharge outlet. When the burette is not used for an extended period, drain the titrant from the burette, and clean the burette, titration nozzle, and the piping by flushing them with methanol. When not in use it for a short period, store the burette filled with titrant, and the titration nozzle immersed in methanol. This will prevent the discharge outlet from clogging. 4. Apparatus Main unit Karl Fischer moisture titrator(Volumetric titration) Electrodes Twin platinum electrode Sampler Finger shaped sampler(Available as an option) 5. Reagents Dehydrating agent KEM AQUA Solvent MET for general Titrant KEM AQUA Titrant TR-3 6. Procedure - Preparation- 1) Add approximately 50 mL of the dehydrating agent to a titration flask. 2) Perform pre-titration, and remove the water from within the titration cell. - Measurement- 1) Introduce approximately 0.2 g of the sample into the finger shaped sampler, and weigh it. 2) Open the side plug, and load the sample. 3) Attach the side plug, and start the measurement. 4) Weigh the finger shaped sampler. The difference in the weight of the sampler before and after the sample is loaded is the weight of the sample. 7. Calculation Moisture(%)=(( Data × TF – Drift × T – Blank)/( Wt1- Wt2)) × 0.1 Data Titer(mL) TF Factor of titrant(2.8187 mg/mL)* Drift Drift value(mg/s) T Measurement time(s) Blank Blank test value(0 mg) Wt1 Weight of the sampler before loading the sample(g) Wt2 Weight of the sampler after loading the sample(g) * To standardize the titrant, a standard substance(KEM AQUA Water Standard 10) with a known moisture concentration was used. This reagent contains approximately 10 mg of moisture per 1 gram. Using this rather than pure water has the advantage of reducing human error when measuring the mass and when adding the sample to the cell. 8. Example of measurement We were able to measure commercial beer in GV/ P+ AIR mode. ― Titration parameter ― ＜Titr.Para＞ ＜Ctrl.Para＞ Titration mode Normal End Time 30s t(stir) 0s Final vol. 0.01mL t(wait) 0s Titr. speed 3 t(max) 0s Detect. mode 1 t(interval) 0s Drift titr. On Max. Volume 10.0mL Start mode Manual Dose mode Off End level 75mV Data sampling time 5s 4 Stirrer speed (The above condition is an example. The setting condition depends on the model.) ― Example of Titration curve ― ― Measurement results ― Table1 Results of moisture measurement of acrinol monohydrate Sample (g) Titration (mL) Moisture (mg) Concentration of water content(%) 1 0.2052 3.780 10.6547 5.19 2 0.2058 3.785 10.6688 5.18 3 0.2029 3.760 10.5983 5.22 Mean - - - 5.20 SD - - - 0.02 RSD(%) - - - 0.40