镍电镀液中氯化镍检测方案(自动电位滴定)

KeM Application Note No.TIQ-05321 Platingsolution Concentration of Nickel chloride inNickel plating solution Precipitationtitration 1. Abstract The concentration of Nickel chloride is determined on the acidic mixed sample of Nickel chloride and Nickel sulfate which is prepared for Nickel plating solution.For ordinary Nickel plating solution， it is impossible to determine only Nickelchloride due to the coexistence of Nickel sulfate in the solution. Instead， it isdetermined by measuring the concentration of chloride ion in the sample. Theconcentration of chloride ion in the sample is determined by titrating the samplewith 0.1mol/L Silver nitrate solution to the equivalence point that corresponds tothe maximal inflection point on the titration curve. 2. Reference 3.Tips for measurement 1) In the case that the sample is taken out from Nickel plating bath， carry out anappropriate pretreatment such as filtration. 2) In the case that the sample may be contaminated by chloride ion from othercauses， this measuring method is not applicable. 3) Use the Mercury sulfate reference electrode or the conventional Silver chlorideelectrode the internal solution of which is replaced with 1mol/L Potassiumnitrate solution in order to prevent measurement error caused by the leakageof chloride ion. 4)) The tip of Silver electrode should be polished with special-purpose polishingpaper before the measurements. 5) In this application note， the convenient combined silver electrode is used； thesame measurement results will be obtained by using an ordinary silverelectrode plus the corresponding reference electrode. 上海市漕溪路222号航天大厦北楼902室网址： http：//www.kyoto-kem. net. cn 4.Equipment Main unit ： Automatic potentiometric titrator AT-510 Detector：： Standard preamplifier STD-510 Combination silver electrode C-372+ Cable #429-0012 (inner filling： 1mol/L Potassium nitrate) 5. Reagent Titration solution ：0.1mol/L Silver nitrate solution 6. Analysis Procedure 1) Place 5mL of sample in 200mL beaker. 2) Add pure water to make a total of 100mL solution. 3) Titrate with 0.1mol/L Silver nitrate solution to obtain concentration of Nickelchloride. 7. Calculation Concentration (g/L)=(EP1-BL1)xTFxC1xK1/SIZE EP1 ： titrated (mL) BL1 ： blank (mL)=0 ： titrant factor=0.9806 ： concentration conversion coefficient=6.48(1mL of 0.1mol/L AgNO3 corresponds to 6.48mg of NiCl2) K1 ： unit conversion coefficient=1 SIZE ： sample size=5 (mL) 8. Example of Measurement -Ambient condition- Room temperature： 22.5°℃ Humidity： 47% Weather： Cloudy Date：2005/06/18 11：49 Sample ID ： Method No.： 15 Method Name： NiCI2/NiSO4 Dose Reagent Name：0.1M-AgNO3 Titr Reagent Name：0.1M-AgNO3 Method Type ： Titration Form ： EP Stop APB No. ：1Unit No. ：1Detector No. ：1Unit ： mVMax Volume ：60.00 mLWait Time ： 0s Direction ： Auto Titr. Form：EP STOP End Point No..：：1 End Sense ： Auto End Point Area ： OffSeparation ： Off Auto Simulation ： NOOver Titr.Vol. ：0.0mLGain ：1 Data Samp.Pot. ：4.0mV Data Samp.Vol.： 0.5 mL Control Speed：Medium *** Result *** Sample No. 20-01 Date：2005/06/18 11：10Sample ID ： Method No. ：15 Method Name ： NiCI2/NiSO4 Titr. Time ：00：06：21 Size ： 5.0mL Conc-1 39.70g/L End Point-1Volume ：31.2425mLPotential ：292.1mV 100 [mU] 400 0.000T E 32.000[mL] Calc. Type： Sample Conc.1 ： Set CO1=(EP1-BL1)*TF*C1*K1/SIZE Unit ： g/L EP No. ：1 Level or EP： Level Conc.2 ： OffConc.3 ： OffConc.4 ： Off Conc.5 ： Off Temp. Comp： Off C1(mg/mL) ：： 6.48 K1 ： 1.0 Factor ： 0.9806Conc. 0.1 Blank 1 ： 0.0 上海市漕溪路222号航天大厦北楼902室网址： http：//www.kyoto-kem.net. cn -Results- Run Size(mL) Volume(mL) Conc.(g/L) 1 23 5.0 5.0 5.0 31.242531.2216 31.1905 39.7039.68 39.64 Statistics MeanSD RSD 39.675 g/L0.0333 g/L 0.0838% K-M KYOTO ELECTRONICSMANUFACTURING CO.，LTD. Overseas Division： 8-3，Niban-cho，Chiyoda-ku，TOKYO 102-0084 JAPAN FAX： +81-3-3237-0537，Phone： +81-3-3239-7333 E-mail： export@kem.co.jp URL：http：//www.kyoto-kem.com Factory： 56-2 Ninodan-cho，Shinden Kisshoin，Minami-ku，KYOTO601-8317，JAPAN FAX：+81-75-691-9961， Phone：+81-75-691-4122 E-mail： tech-english@kem.co.jp TIQ-05321 4/4 京都电子工业株式会社-可睦电子(上海)商贸有限公司上海市漕溪路222号航天大厦北楼902室电话：021-54488867 电邮： kemu-kem@163.com网址： http：//www.kyoto-kem. net. cn TIQ-都电子工业株式会社-可睦电子(上海)商贸有限公司电话： 电邮： kemu-kem@com