化学药中理化常数检测方案

9.Example of measurement NeTIC-99326 kMApplication NotePharmaceuticalBenzalkonium Chloride in BactericidelRedox titration byAutomatic Potentiometric Titrator Japanesepharmacopoeia Standard codex 15 1.Abstract Benzalkonium chloride (Ammonium salt， class 4) is a bactericide. Here， its content(quantified as C22H40ClN=354.02) in a sample from commercially sold bactericide ismeasured according to Japanese pharmacopoeia codex 15 by potentiometric titrationwith 0.02mol/L sodium tetraphenylboron solution. The endpoint is determined by themaximum inflexion point on titration curve. R in below formula stands for alkyl， allyl group. [C6H5CH2N(CH3)2R]Cl + Na[B(C6H5)4] =[C6H5CH2N(CH3)2R[B(C6H5)4]+NaCl assuming R=C：H17~C18H37 2.Reference 1) Japanese pharmacopoeia codex 15 Quantitative determination of Benzalkonium chloride B.Cautions in measurement 1))The sample liquid may cause irritation on the skin. Handle with care. 2)Be careful the liquid is flammable and explosive. 4.Post-measurement care The electrode after rinsed with pure water must be kept in pure water in a beaker sothat its tip may not dry up. Http：//www.shxf17.com Tel： 021-66581985，63172460 Fax： 021-66581986 周峰13916388882 zhou-feng1027@163. com 5.Test equipment Main unit ： Automatic potentiometric titrator (Standard preamplifier： STD-)Electrode ： Combination platinum electrode C-272 [No 98100C272] optional 6.Reagent Reagent ：0.02mo1/L Sodium tetraphenylboron solution Additive ：Hydrochloric acid (1+2) (Commercially sold HCl diluted by ratio 1：2) 7.Measurement procedure -Measurement- 1Prepare approximately 0.15g sample in a 200m beaker. 2)Add 75mL pure water， and Add HCl(1+2) to make pH adjusted to 2.6~3.4. 3))Titrate with 0.02mol/L sodium tetraphenylboron to obtain the content. 8.Formula Content (%)=(EP1 - BL1)×TF×C1×K1/SIZE EP1 ：Titration volume(mL) BL1 ： Blank level (mL)=0 TF ： Factor = 1.05 C1 ：CConcentration conversion coefficient=7.080 (Benzalkonium chloride (mg) equivalent to 1mL of 0.02M-NaB(C6H5)41mL) K1 ： Unit conversion coefficient =0.1 SIZE ：Sample size (g) -Ambient condition-一 Room temperature ： 22.5℃ Humidity ：447% Weather：(Cloudy Sample No. ：73-01 Date ：1999/08/23 11：10Sample ID ：C22H4OClN Method No. ： 13 Method Name ： Benzal konium Cl Titr. Time ：00：14：40 Size ：0.1589g Conc-1 ：95.507% End point-1Volume ：20.4143mLPotential： ：-187.6mV-300 [mU] 1000.000 32.000 [mL] -Titration parameter- Model ： AT-510 Method No.： 13 Form ： EP Stop Calc. Type ：Sample APB No. ：1 Conc.1 ：Set Unit No. ：1 CO1= Detector No. ：1 (EP1-BL1)*TF*K1*C1/SIZ Unit ：nmV E Max.Volume ：40.0mL Wait Time 0s Unit ：% Direction ：Auto EP No. ：1 Temp.Comp.： Off C1(mg/mL) ： 7.080 End Point No. ：1 JK1 ：0.1 End sense ： Auto End Point Area ：Off Separation ：(Off Factor ： 1.05 Over Titr.Vol. ：C0mL Gain ： 2 Data samp.Pot. ：4.0mV Blank1 ：0.00 Data samp.Vol.： 0.5mL Stability ： 10mV/s Delay Time ： 1s Limit Time ：30s Meaning of printout data： -Measurement resultsS二 Statistics Sample (g) Titrate (mL) 20.4143 Content (%) Mean SD RSD 95.408% 0.2614% 0.2739% 19.6518 95.507 95.112 19.2010 95.606 * The above results were obtained by 3 tests of the same sample. *Red underline shows the data from page 3/4. 10. Summary Benzalkonium chloride is cationic surfactant (invert soap) having reverse charge，and is usually used as bactericide. The sample this time as bactericide showed high 95% concentration with a goodrepeatability of less than 0.3% relative standard deviation. Precise and reliable measurement is assured by the automated potentiometry. The analysis of Benzalkonium chloride as bactericide can be perfectly made by anyof the following titration systems manufactured by Kyoto Electronics (KEM). 【AT-610】 【AT-510】【AT-500N-1】 AwardedProduct of SupremeTechnology from Kyoto City · Compact and cost performancemodel ·Low cost and high performance·Easy view with back light LCD ·Easy key entry by touch panel oflarge color LCD (8-inch wide) · PC card expands data memory forconvenience and versatility. ( · GLP/GMP conformed mode ) ·Simultaneous titration in parallel · Bothpotentiometric aand KarlFischer moisture titration(coulometricvolumetric)) can beperformed at a time. K-MKYOTO ELECTRONICSMANUFACTURING CO.，LTD. Overseas Division： Yamawaki Bldg 9F，4-8-21 Kudan-minami，Chiyoda-ku， Tokyo 102-0074 JAPAN Phone：+81-3-3239-7333， Fax： +81-3-3237-0537 Head Office： 56-2 Ninodan-cho，Shinden，Kisshoin，Minami-ku， Kyoto 601-8317 JAPAN Phone： +81-75-691-4122， Fax： +81-75-691-9961 URL： http：//www.kyoto-kem.com 上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 200072 Tel： 021-66581985，63172460 Fax： 021-66581986 周峰 13916388882 zhou-feng1027@163.com 上海旭风科学仪器有限公司 上海市闸北区荣路 IC-Ver. Tel： Fax： 周峰 zhou-feng comTIC-Ver.