检测有机溶剂中水分含量

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Julabo.VIscOAnalysis And Testing TechnologyApplication Application Use This method is a general description how to determine the water content in organic liquids such as methanol，isopropyl alcohol， glycol and other similar liquids. Appliances Titrator： TL 7500 KF (TL 7500 KF 05/10/20) or TL 7750 with KF accessories ul syringe or one-way insulin syringe with needle (> 0.8 mm) 4 digit balance ● KF 1100 with fixed cable Reagents Titration agent： 1 component titrant or 2 component Titrant with 2 or 5 mg/ml concentration Solvent： dry methanol， combi solvent or a two component solvent/solvent E Description The setup of the instrument is described in the operating manual. Determination of the titrant concentration The determination of the titrant concentration (titer determination， standardization) is necessary before thesample titration and we recommend a weekly titer determination. Fill the titrant in the exchange unit and the solvent in the titration vessel as described in the manual. Do notforget to enter the concentration of the titrant (e.g. 2 or 5) into the WA unit. Otherwise the drift determinationis wrong. Load the standard method (default method) Titer 1-Comp. (liq. std.) or Titer 2-Comp. (liq. std.) asuser method and start the method. The KF titrator starts automatically the conditioning routine. The solvent and also the titration vessel contentsalso water which has to be titrated before. When the conditioning is ready you see“Conditioning ready” onthe screen. The conditioning remains active until the actual titration is started by pressing . Open the glass ampoule with the water standard (10 mg/g) and rinse the 10 ml syringe 1-2 timeswith 0.5- 1 ml of the standard. Fill the complete content of the liquid standard then into the syringe and wipe then the needle with atissue. Place the syringe with needle on a 4 digit balance. Maybe use a beaker， place this beaker on thebalance and put the syringe then into the beaker during the weighing process. Press the tara button. e Press Start/F1 to interrupt the conditioning. You are prompted immediately to add the sample. Please add between 0.5 and 1 g standard for a 2 mg/ml titrant and 1.5-2 g for a 5 mg/ml titrantthrough the septum， Place the syringe again on the balance and read the absolute weight form the balance (ignore theminus) ●Enter the sample ID (optional)●Enter the sample weight and confirm with ENTER/F1 Application The titrator starts then automatically the titration. The result will appear on the screen at the end of thetitration. Repeat the titer determination two times (total 3 times). The average value of the titrantconcentration in mg/ml will be stored automatically in the exchange unit and used for the calculation of thesample water concentration. GLP documentation Titration graph mm1l/s Method data Method name： Titer 2-Comp. (liq. st.) Titration duration： 1 m 43 s End date： 27.05.13 End time： 16：03：32 Titration data Sample ID： 10.0 merck Weight： 0.90070 g Stait uA： -0.052 pA End pA： 22.873 pA Start drift： 59 pg/min End drift： 43 pg/min Consumption： 4.624 ml Drift correction： Off Titer： 1.9479 mg/ml Mean value： RSD： Calculation formula Titer：(W*F2)/((EP-B)*M*F1)-> WAMol (M)：1.00000Weight (W)：0.90070g (m)Factor2 (F2)：10.0000Blank value (B)：0.0000 mlFactor 1(F1)：1.0000Statistics：1 from 3 Application Method data overall view Dosing parameterDosing speed：60.00 %Filling speed：30 sMaximum dosing volume：50.00 mlUnit valuesUnit size：10mlUnit ID：10035454 Reagent： Composite 2 Batch ID： no entry Concentration [mg/ml]： 1.94360Determined at： 05/14/13 23：46：49Expire date： Opened/compounded： Test according ISO 8655： 08/21/12 Last modification： 05/27/13 15：56：13 Application Sample Titration The procedure for organic liquid samples is the sample as for the liquid standard. The only difference is theused method. Please load the default method"Sample 1 Comp."or"Sample 2 Comp."for the sampletitration. Use also a suitable syringe (1， 2， 5 or 10 ml) with needle for the liquid sample. Rinse syringe 1-2 times with 0.5-1 ml of the sample. Use between 0.2-10 g of the sampledepending on the expected water concentration (Please refer to the enclosed table) Place the syringe with needle on a 4 digit balance. Maybe use a beaker， place this beaker on thebalance and put the syringe then into the beaker during the weighing process. Press the tara button. Press Start/F1 to interrupt the conditioning. You are prompted immediately to add the sample. Add the sample trough the septum Place the syringe again on the balance and read the absolute weight form the balance (ignore theminus Enter the sample ID (optional) Enter the sample weight and confirm with ENTER/F1 The titrator starts then automatically the titration. The result will appear on the screen at the end of thetitration. Recommended sample amounts： expected water amount Titre 2 mg/ml Titre 5 mg/ml 10 ppm- 100 ppm >10 g 100-500 ppm 2-10g -- -- 500 ppm-1000 ppm (0.1%) 1-5g 5-10g 0.1%-10% 0.5-1g 1-2g 1%-10% 0.1-2g 10%-100% --- max. 0.1 g Application Methods Sample titration (page 1) GLP documentation Titration graph Calculation formula result： (EP-B)*T*M*F1/(W*F2) Mol (M)： 1.00000 Blank value (B)：0.0000 mlTitre (T)：5.17870000 (a)Factor 1 (F1)：0.1000Weight (W)：manFactor 2 (F2)：1.0000Statistics：Off Application sample titration (page 2)： Dosing parameter Dosing speed： 60 % Filling speed： 30 s Maximum dosing volume： 50.00 ml Unit values Unit size： 10ml Unit ID： 10035463 Reagent： Batch ID： no entry Concentration [mg/ml]： 5.17870 Determined at： Expire date： Opened/compounded： 一一 Test according ISO 8655： 08/27/12 Last modification： 09/06/1216：15：24 Application Hints lf you have any questions concerning the application， you are welcome to contact us. Literature JULABO TECHNOLOGY(Beijing)Co.，LTD地址：北京市朝阳区酒仙桥东路1号院M8号楼C厅3层301室 Add ： Room 301，C hall，M8 office building，No.1 jiuxianqiao east road ，Chaoyang District，Beijing，China Tel.：4008092068 Fax： +86 (0)10 64390585 ③Web： www.julabo.cn， www.julabo-visco.com 优莱博技术(北京)有限公司 Page of Date： Page of Date：