润滑油中碱值检测方案

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KEM Application Note No.TIA-06311 Petroleumproducts Base number of lubricant Acid-Basetitration (Non-aqueous) 1. Abstract The Base Number (BN) of petroleum products and lubricants can be determinedby potentiometric titration method with 0.1mol/L Perchloric acid standard aceticacid solution according to “JIS K2501 Petroleum products and lubricants -determination of neutralization number”，“ASTM D2896 Standard Test Method forBase Number of Petroleum Products by Potentiometric Perchloric Acid Titration”，“ISO 3771 Petroleum products -Determination of base number -Perchloric acidpotentiometric titration method”or the like. The end point is the inflection pointon the titration curve. In the case where inflection points are not definitive， apply the back titrationmethod with Sodium acetate standard acetic acid solution. Then calculate theBase Number (BN) of petroleum products and lubricants from the volume ofPerchloric acid standard acetic acid solution required for titration until the endpoint. The sample is usually dissolved in a mixture of Chlorobenzene and Acetic acid.Therefore， the possible basic constituents in petroleum products and lubricantsinclude organic bases， inorganic bases， amino compounds， weak acid salts(soap)， and basic salts of polyacidic bases. 2... Reference 1) JIS K2501 Petroleum products and lubricants -determination of neutralizationnumber 2) ASTM D2896 Standard Test Method for Base Number of Petroleum Productsby Potentiometric Perchloric Acid Titration 3) ISO 3771 Petroleum products-Determination of base number-Perchloric acidpotentiometric titration method 1/4 3. Tips for measurement 1) After each measurement， immerse electrodes in distilled water for a fewminutes to one hour to recover the sensitivity of them. 2) The oils containing perbasic additives or polymers having nitrogen are likely toshow rather higher test results， 3) Acetic acid， Acetic anhydride acid and Chlorobenzene are toxic and irritative.Whole operations of these chemicals shall be carried out in a well ventilatedplace or in a draft. 4) Because of the relatively large coefficient of cubic expansion of organicsolvents， the difference between temperatures of standardization and in use ofPerchloric acid standard acetic acid solution shall be within 5°C. 5) Standardize repeatedly the Perchloric acid standard acetic solution at leastonce a week. 4. Equipment Main unit ： Automatic potentiometric titrator AT-510 Detector ： Standard preamplifier STD-510 Combination glass electrode C-173+Cable #429-0012 (Replace the inner filling of reference electrode with saturatedPerchloric acid standard acetic acid solution.) 5. Reagent Titration solution ：0.1mol/L Perchloric acid standard acetic acid solution Additive ： Acetic acid ： Chlorobenzene=1 ： 2 6. Analysis Procedure 1) Place 0.6g of sample in 200mL beaker. 2) Add 120mL of solvent and dissolve the sample. 3) Titrate with 0.1mol/L Perchloric acid standard acetic acid solution to determinethe total base number oflubricant. 7. Calculation Total base number (mg/g)：(EP1-BL1)xTFxC1xK1/SIZE EP1 ： volume (mL) BL1 ： blank (mL)=0 ： titrant factor=0.934 ： concentration conversion coefficient=5.611 (1mL of 0.1mol/L HCIO4 corresponds to 5.611mg of Potassium hydroxide) K1 ： unit conversion coefficient=1 SIZE ： sample size (g) Http：//www.shxf17. com 8. Example of Measurement -Ambient condition- Room temperature： 22.5℃ Humidity：47% Weather： Cloudy -Titration parameter- -Titration curve- [Titration Parameterl Date：2006/07/15 09：18Sample ID： Method No.： 12 Method Name： Base Value Dose Reagent Name：HCIO4/CH3COOH Titr Reagent Name：HCIO4/CH3COQH Method Type ： Dose&Titr. Mode ：Volume StopAPB No. ：1Unit No. ：1Volume ： 3.5 mLCut-Off Time 0sDispense Speed ： 1 s/mLDose Wait ： 0s Form ： EP STOPAPB No. ：1Unit No. ：1 Detector No.：：1Unit ： mVMax Volume ： 20.00 mLWait Time ：60 s Direction ： Auto Titr. Form：： EP STOP End Point No. ：1 End Sense ： AutoEnd Point Area ： Off Separation ： Off Over Titr.Vol. ：0.0 mLGain ：1Data Samp.Pot. ：4.0 mVData Samp.Vol. ：0.05 mLIntegral Time ： 60 sStart Lim.Time ： OsLimit Time 0s1st Volume ： 0.1 mL2nd Volume ： 0.05mLStability ：5mV/mindE(1st-2nd) ： 30 mV Calc. Type ： Sample Conc.1 ： Set CO1=(EP1-BL1)*TF*C1*K1/SIZE Unit ：mg/gEP No. ：1Conc.2 ： OffConc.3 ： OffConc.4 ： OffConc.5 ： Off Temp. Comp ： Off C1(mg/mL) ：5.611 Factor ：0.934Conc. ：0.100 Factor ： 0.934Conc. ：0.100 Blank 1 ： 0.0 ***Result *** Sample No. 22-03 Date：2006/07/15 09：09Sample ID ： Method No. ：12 Method Name： Acid Value Titr. Time ： 00：43：31 Size ： 0.6347g Conc-1 49.967mg/g End Point-1 Volume ： 6.0526mLPotential ：390.4mV 150 [mV] 556 0，必00 8.000 CmL3 Http：//www.shxf17. com Run Size(g) Vol.(mL) Total base number(mg/g) 123 0.63470.63470.6363 6.05266.02226.0570 49.96749.716 49.878 Statistics MeanSD RSD 49.854 mg/g0.1273 mg/g0.2553% 【AT-610】 【AT-510】 【AT-500N-1】 Awarded Supreme Technology fromKyoto City ·Compact andd 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. r· GLP/GMP conformed model · Simultaneous titration in parallel · Both potentiometric and KarlFischer moisture titration(coulometric·volumetric)can beperformed at a time. KM KYOTO ELECTRONICSMANUFACTURINGCO.，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： 56-2Ninodan-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 Http：//www.shxf17.com TIA-海旭风科学仪器有限公司 上海市闸北区荣路 Http：//www.shxfcomTel： Fax： 周峰 zhou-fengcom