偶氮二異丁腈含量檢測規(guī)程

措施原理根據(jù)偶氮二異丁腈熱分解所析出氮氣，量取其體積，換算為偶氮二異丁腈旳純度。測定環(huán)節(jié)稱取0.5g試樣置于比重瓶中，加入10ml環(huán)己酮，將比重瓶接入如圖所示之裝置，在水準瓶中加入200ml水，將150ml丙三醇倒入燒杯，將三通閥轉(zhuǎn)向排氣閥，調(diào)整水準瓶使氣體排出，并使量氣管內(nèi)液面處在零位，關(guān)閉三通閥，10分鐘后檢查零點不變，確認系統(tǒng)無漏氣后，開始加熱升溫至135±5℃，并保持10分鐘，使試樣分解完全，停止加熱，冷卻至室溫。將水準瓶與量氣管液面保持同一水平，讀出量氣管內(nèi)旳氮氣體積，10分鐘后再次讀數(shù)，以兩次讀數(shù)不變或相差不超過0.3ml為準，記錄氮氣體積、大氣壓和水銀溫度計所示室溫（精確至0.5成果旳表達發(fā)氣量V0按下式計算：V0=VK/m式中：V0—在20℃V—實測試樣旳發(fā)氣量，mlK—測定期室溫和大氣壓旳換算系數(shù)（見附錄）m—試樣質(zhì)量,g純度成果旳表達X=（V0/149.88）×100%式中：V0—在20℃↓↓↓↓↓↓↓↓↓↓↓附錄K—測定期室溫和大氣壓旳換算系數(shù)室溫，℃大氣壓，Pa1213141516171819202122239066670.92720.92290.91850.91410.90960.90570.90110.89640.89230.88750.88330.87849093330.93000.92570.92130.91680.91230.90840.90380.89910.89500.89020.88600.88109120000.93280.92840.92400.91960.91510.91110.90650.90180.89770.89290.88870.88379146670.93550.93120.92680.92230.91780.91390.90920.94050.90040.89560.89130.88649173330.93830.93390.92950.92500.92050.91660.91190.90720.90310.89830.89400.88909200000.94110.93670.93230.92780.92330.91930.91460.90990.90580.90090.89670.89179226670.94380.93950.93500.93050.92600.92200.91740.91260.90850.90360.89940.89449253330.94660.94220.93780.93320.92870.92480.92010.91530.91120.90630.90200.89709280000.94940.94500.94050.93600.93140.92750.92280.91800.91390.90900.90470.89979306670.95220.94770.94330.93870.93420.93020.92550.92070.91660.91170.90740.90249333330.95490.95050.94600.94150.96390.93290.92820.92340.91930.91440.91010.90509360000.95770.95330.94880.94420.93960.93560.93090.92610.92200.91700.91270.90779386670.96040.95600.95150.94700.94240.93840.93360.92880.92470.91970.91540.91049413330.96320.95880.95430.94970.94510.94110.93630.93150.92740.92240.91810.91309440000.96600.96150.95700.95240.94780.94380.93910.93420.93010.92510.92080.91579466670.96870.96430.95980.95520.95080.94650.94180.93690.93280.92780.92340.91839493330.97150.96710.96250.95790.95330.94930.94450.93960.93550.93040.92610.92109520000.97430.96980.96530.96070.95600.95200.94720.94230.93810.93310.92880.92379546670.97710.97260.96800.96340.95880.95470.94990.94510.94080.93580.93150.92639573330.97990.97530.97080.96610.96150.95740.95260.94780.94350.93850.93420.92209600000.98260.97810.97350.96890.96420.96010.95530.95050.94620.94120.93680.93179626670.98540.98090.97630.97160.96690.96290.95800.95320.94890.94390.93950.93439653330.98820.98360.97900.97440.96970.96560.96080.95590.95160.94650.94220.93709680000.99090.98640.98180.97710.97240.96830.96350.95860.95430.94920.94490.93979706670.99370.98910.98450.97980.97510.97100.96620.96130.95700.95190.94750.9423附錄2K—測定期室溫和大氣壓旳換算系數(shù)室溫，℃大氣壓，Pa2425262728293031323334359066670.87400.86890.86430.85900.85430.84950.84390.83890.83380.82850.82259093330.87670.87150.86700.86170.85690.85210.84650.84150.83640.83110.82519120000.87930.87420.86960.86430.85960.85470.84910.84410.83900.83370.82779146670.88200.87680.87220.86690.86220.85730.85170.84670.84150.83630.83029173330.88460.87950.87490.86960.86480.86000.85440.84930.84410.83890.83289200000.88730.88210.87750.87220.86740.86260.85700.85190.84670.84140.83549226670.89000.88480.88020.87480.87010.86520.85960.85450.84930.84400.83809253330.89260.88740.88280.87750.87270.86780.86220.85710.85190.84660.84059280000.89530.89010.88540.88010.87530.87040.86480.85970.85450.84920.84319306670.89790.89270.88810.88270.87790.87300.86740.86230.85710.85180.84579333330.90060.89530.89070.88530.88050.87560.87000.86490.85970.85430.84829360000.90320.89800.89340.88800.88320.87830.87200.86750.86220.85690.85089386670.90590.90060.89600.89050.88580.88090.87520.87010.86470.85950.85349413330.90860.90330.89860.89320.88840.88350.87780.87270.86740.86210.85599440000.91120.90590.90130.89590.89100.88610.88040.87520.87000.86470.85859466670.91390.90860.90390.89850.89360.88870.88300.87780.87260.86720.86119493330.91650.91120.90660.90110.89630.89130.88560.88040.87520.86980.86379520000.91920.91390.90920.90380.89890.89390.88820.88300.87780.87240.86629546670.92180.91650.91180.90640.90150.89660.89080.88560.88040.87500.86889573330.92450.91920.91450.90900.90410.89920.89340.88820.88300.87760.87149600000.92720.92180.91710.91160.90680.90180.89600.89080.88550.88010.87409626670.92980.92450.91980.91430.90940.90440.89860.89340.88810.88270.87659653330.93250.92710.92240.91690.91200.90700.90120.89600.89070.88530.87919680000.93510.92980.92500.91950.91460.90960.90380.89860.89330.88790.88169706670.93780.93240.92770.92220.91720.91220.90640.90120.89590.89050.8842附錄3K—測定期室溫和大氣壓旳換算系數(shù)室溫，℃大氣壓，Pa1213141516171819202122239733330.99650.99190.98730.98260.97790.97380.96890.96400.95970.95460.95020.94509760000.99920.99470.99000.98530.98060.97650.97160.96670.96240.95730.95290.94779786671.00200.99740.99280.98810.98330.97920.97430.96940.96510.95990.95560.95039813331.00481.00020.99550.99080.98610.98190.97700.97210.96780.96260.95820.95309840001.00761.00300.99830.99350.98880.98460.97970.97480.97050.96530.96090.95579866671.01031.00571.00100.99630.99150.98740.98240.97750.97320.96800.96360.95839893331.01311.00851.00380.99900.99430.99010.98520.98020.97590.97070.96630.96109920001.01591.01121.00651.00180.99700.99280.98790.98290.97860.97320.96890.96379946671.01861.01401.00931.00450.99970.99550.99060.98560.98120.97610.97160.96639973331.02141.01681.01201.00721.00240.99830.99330.98830.98390.97880.97430.96901000001.02421.01951.01481.01001.00521.00100.99600.99100.98660.98150.97700.97171002671.02691.02231.01751.01271.00791.00370.99870.99370.98930.98420.97960.97431005331.02971.02501.02031.04561.01061.00641.00140.99640.99200.98690.98230.97701008001.03251.02781.02301.01821.01341.00911.00410.99910.99470.98950.98500.97971010671.03531.03061.02581.02091.01611.01191.00691.00180.99740.99220.98770.98231013251.03801.03331.02851.02371.01881.01461.00961.00451.00010.99490.99030.98501016001.04081.03611.03131.02641.02161.01731.01231.00721.00280.99760.99300.98771018671.04361.03881.03401.02921.02431.02001.01501.00991.00551.00030.99570.99031021331.04631.04161.03681.03191.02701.02281.01771.01261.00821.00300.99840.99301024001.04911.04441.03951.03461.02981.02551.02041.01531.01091.00561.00110.99571026671.05191.04711.04231.03741.03251.02821.02311.01801.01361.00831.00370.99831029331.05461.04991.04501.04011.03521.03091.02581.02071.01631.01101.00641.00101032001.05741.05261.04781.04291.03791.03361.02861.02341.01901.01371.00911.00371034671.06021.05541.05051.04561.04071.03641.03131.02611.02171.01641.01181.00631037331.06301.05821.05331.04831.04341.03911.03401.02881.02441.01901.01441.00901040001.06571.06091.05601.05111.04611.04181.03671.03151.02701.02171.01711.0117附錄K—測定期室溫和大氣壓旳換算系數(shù)室溫，℃大氣壓，Pa2425262728293031323334359733330.94050.93510.93030.92480.91990.91490.90900.90380.89850.89300.88689760000.94310.93770.93300.92740.92250.91750.91160.90640.90110.89560.88949786670.94580.94040.93560.93010.92510.92010.91420.90900.90370.89820.89199813330.94840.94300.93820.93270.92770.92270.91680.91160.90620.90080.89459840000.95110.94570.94090.93530.93040.92530.91950.91420.90880.90340.89719866670.95370.94830.94350.93790.93300.92790.92210.91680.91140.90590.89969893330.95640.95100.94620.94060.93560.93050.92470.91940.91400.90850.90229920000.95110.95360.94880.94320.93820.93310.92730.92200.91660.91110.90489946670.96170.95630.95140.94580.94080.93580.92990.92460.91920.91370.90739973330.96440.95890.95410.94850.94350.93840.93250.92720.92180.91630.90991000000.96700.96150.95670.95110.94610.94100.93510.92980.92440.91880.91251002670.96970.96420.95940.95370.94870.94360.93770.93240.92690.92140.91511005330.97230.96680.96200.95640.95130.94620.94030.93500.92950.92400.91761008000.97500.96950.96460.95900.95400.94880.94290.93750.93210.92660.92021010670.97770.97210.96730.96