發(fā)泡劑偶氮二甲酰胺（ADC）

1本標(biāo)準(zhǔn)規(guī)定了發(fā)泡劑偶氮二甲酰胺(簡稱發(fā)泡劑ADC)的技術(shù)要求、試驗(yàn)方法、檢驗(yàn)規(guī)則、標(biāo)相對分子質(zhì)量：116.06(按2016年國際相對原子質(zhì)量)件。凡是不注日期的引用文件，其最新版本(包括所有的修改單)適用于本文件。發(fā)泡劑ADC的技術(shù)要求和相應(yīng)的試驗(yàn)方法應(yīng)符合表1的規(guī)定。2表1發(fā)泡劑ADC的技術(shù)要求和試驗(yàn)方法試驗(yàn)方法優(yōu)等品一等品合格品淡黃色粉末(2)發(fā)氣量(20℃,101325Pa)/(mL/g)≥(3)篩余物(75μm)/%≤(4)中值粒徑(以D?o表示)/μm用戶協(xié)商指標(biāo)(5)分解溫度/℃≥6.5～7.5除非另有說明，在分析中所用標(biāo)準(zhǔn)滴定溶液、制劑和制品，均按GB/T601、GB/T603的規(guī)定分析中僅使用確認(rèn)為分析純的試劑和GB/T6682中規(guī)定的三級水。標(biāo)準(zhǔn)中檢驗(yàn)結(jié)果的判定按GB/T8170—2008中4.3.3修約值比較法進(jìn)行。樣品在一定溫度下加熱分解產(chǎn)生氣體，以排水集氣法測出發(fā)氣量。4.3.2試劑4.3.2.1鄰苯二甲酸二辛酯[117-84-0]。4.3.2.2丙三醇[56-81-5]傳熱液。4.3.3.1發(fā)氣量測定裝置(見圖1)。32——水準(zhǔn)瓶(250mL);6——水銀溫度計(jì)(0℃~250℃);7——燒杯(500mL);8——調(diào)壓器(1kV·A);9——電爐(300W);4.3.3.2水銀溫度計(jì)：分度值為1℃。4.3.3.4氣壓表。稱取0.3g樣品(精確至0.0001g),置于25mL密度瓶中，加入2mL鄰苯二甲酸二辛酯，按圖1裝好儀器，將三通活塞通大氣。提高水準(zhǔn)瓶，調(diào)整量氣管零點(diǎn)(在室溫下),關(guān)三通活塞，檢查零浸入傳熱液中，其深度以由密度瓶底部至傳熱液面15mm～20mm為宜。待傳熱液升溫至180℃時(shí)，調(diào)整熱源再以4℃/min～5℃/min的升溫速率加熱至220℃±2℃,保持2min,使其分解完全。停止加熱，移去傳熱液，使其冷至室溫(約需30min)。提高水準(zhǔn)瓶使液面和量氣管液面保持同一水平，進(jìn)行讀數(shù)，等待5min后再次讀數(shù)。兩次讀數(shù)相差不超過0.2mL時(shí)，以最后一次讀數(shù)值為準(zhǔn)，讀數(shù)值為V?。44.3.5結(jié)果計(jì)算發(fā)氣量以發(fā)泡劑ADC的質(zhì)量體積Vo計(jì)，數(shù)值以毫升每克(mL/g)表示，按公式(1)計(jì)算：V?——實(shí)測樣品的發(fā)氣量的數(shù)值，單位為毫升(mL);p?——測定時(shí)的大氣壓的數(shù)值，單位為帕斯卡(Pa);m?——樣品的質(zhì)量的數(shù)值，單位為克(g);t?——測定時(shí)的溫度的數(shù)值，單位為攝氏度(℃);po——20℃時(shí)水的飽和蒸氣壓的數(shù)值，單位為帕斯卡(Pa);k——測定時(shí)室溫和大氣壓的換算系數(shù)(見附錄A);101325——標(biāo)準(zhǔn)大氣壓的數(shù)值，單位為帕斯卡(Pa)。4.3.6允許差平行測定兩個(gè)結(jié)果的絕對差值不大于5.0mL/g,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定4.4.1干法(仲裁法)按GB/T11409—2008中3.5.2的規(guī)定進(jìn)行測定。稱量約20.0g樣品(精確至0.1g)。試驗(yàn)篩孔4.4.2機(jī)械篩干法按GB/T11409—2008中3.5.2的規(guī)定進(jìn)行測定。稱量約100.0g樣品(精確至0.1g),放入帶發(fā)泡劑ADC的篩余物以質(zhì)量分?jǐn)?shù)w?計(jì)，數(shù)值以%表示，按公式(2)計(jì)算：……m?——過篩后的不能通過篩網(wǎng)樣品的質(zhì)量的數(shù)值，單位為克(g);m?——樣品的質(zhì)量的數(shù)值，單位為克(g)。4.5中值粒徑的測定4.5.1原理顆粒在激光束的照射下，其散射光的角度與顆粒的直徑成反比關(guān)系，散射光強(qiáng)度隨角度的增加呈對數(shù)規(guī)律衰減。5激光粒度儀：要求儀器重復(fù)性≤3%(以D?0計(jì)算)。4.5.4試驗(yàn)步驟按儀器說明規(guī)定的程序開啟儀器，預(yù)熱待儀器穩(wěn)定，然后將一定濃度的分散介質(zhì)加入樣品池中，再加入適當(dāng)?shù)臉悠罚瑪嚢璨⑹箻悠吩诜稚⒁褐谐浞址稚?，按儀器操作步驟進(jìn)行測量，連續(xù)測量兩次。計(jì)算結(jié)果以中值粒徑(D?0)表示。平行測定兩個(gè)結(jié)果的絕對差值不大于0.5μm,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定結(jié)果。4.6分解溫度的測定4.6.1毛細(xì)管測定法(仲裁法)將裝有樣品的毛細(xì)管在油浴中加熱，樣品液化崩裂或分解變白的瞬間的溫度即為樣品的分解4.6.1.2試劑4.6.1.3.1分解溫度測定裝置(見圖2)。6單位為毫米5—-輔助溫度計(jì)；圖2分解溫度測定裝置4.6.1.3.4毛細(xì)管：用中性硬度玻璃制成的毛細(xì)管，內(nèi)徑為0.9mm～1.1mm,管壁厚度為0.10mm～0.15mm,長度為100mm。4.6.1.3.6輔助溫度計(jì)：0℃~100℃,分度值為1℃。露出液面的兩端可套上孔徑適宜的玻璃管和白瓷接頭相連接。向燒杯中注入約3/4高度的傳熱液。將上7若使用全浸式溫度計(jì)，則測得分解溫度按公式(3)計(jì)算：T=t?+0.00016h(t?—to)………………(3)t?——測量溫度計(jì)指示的溫度的數(shù)值，單位為℃;h——露出液面的水銀高度的數(shù)值(以溫度表示);to——輔助溫度計(jì)指示的溫度的數(shù)值，單位為℃;平行測定兩個(gè)結(jié)果的絕對差值不大于0.5℃,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定結(jié)果。4.6.2.2.1熔點(diǎn)儀：帶有觀測鏡的熔點(diǎn)儀，溫度范圍為20℃~400℃,測量精度為±0.5℃。熔點(diǎn)儀開機(jī)預(yù)熱，儀器不同預(yù)熱要求會有差異。設(shè)定起始溫度為190℃,最高溫度為215℃,升溫速率為3℃/min。按4.6.1.5的規(guī)定把樣品裝入毛細(xì)管內(nèi)，待熔點(diǎn)儀溫度達(dá)到起始溫度時(shí)將毛細(xì)管平行測定兩個(gè)結(jié)果的絕對差值不大于0.5℃,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定結(jié)果。按GB/T11409—2008中3.4的規(guī)定進(jìn)行測定。稱取約2g樣品(精確至0.0001g),在105℃±2℃干平行測定兩個(gè)結(jié)果的絕對差值不大于0.005%,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定84.8灰分的測定按GB/T11409—2008中3.7的規(guī)定進(jìn)行測定。稱取約5g樣品(精確至0.0001g),在800℃±20℃平行測定兩個(gè)結(jié)果的絕對差值不大于0.005%,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定結(jié)果。4.9pH值的測定4.9.1儀器和材料4.9.1.1pH計(jì)：精度值為0.01pH單位的帶有溫度校正功能的pH計(jì)。4.9.1.2濾紙：定性濾紙。4.9.2試驗(yàn)步驟稱取約2g樣品(精確至0.1g),加入裝有100mL蒸餾水的200mL燒杯中，攪拌后用濾紙過濾，用酸度計(jì)測濾液的pH值，以pH?表示；同時(shí)測蒸餾水的pH值，以pH?表示。4.9.3結(jié)果計(jì)算pH=pH?+(7.00—pH?)……………(4)式中：pH?——樣品在蒸餾水中的pH值；pH?——蒸餾水的pH值。4.9.4允許差平行測定兩個(gè)結(jié)果的絕對差值不大于0.10,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定結(jié)果。4.10純度的測定4.10.1方法原理用定量水合聯(lián)氨和發(fā)泡劑ADC反應(yīng)生成聯(lián)二脲，余量的肼用碘標(biāo)準(zhǔn)滴定溶液滴定，從而計(jì)算出發(fā)泡劑ADC的含量。4.10.2試劑和溶液4.10.2.1碳酸氫鈉[144-55-8]。4.10.2.2碘標(biāo)準(zhǔn)滴定溶液：4.10.2.3水合聯(lián)氨[7803-57-8]:1+99溶液。4.10.2.4淀粉指示液：10g/L。4.10.3試驗(yàn)步驟稱取0.15g樣品(精確至0.0001g),置于100mL碘量瓶中，加入10mL水，再用移液管加入95.0mL水合聯(lián)氨溶液，加塞水封，在60℃±2℃水浴中加熱20min,待樣品完全呈白色后，冷卻至15℃~20℃。將1g碳酸氫鈉加入其中，用碘標(biāo)準(zhǔn)滴定溶液滴定，近終點(diǎn)時(shí)加入1mL淀粉指示液，繼續(xù)滴定至呈紫紅色30s不褪色為終點(diǎn)。同時(shí)進(jìn)行空白試驗(yàn)。4.10.4結(jié)果計(jì)算發(fā)泡劑ADC的純度以質(zhì)量分?jǐn)?shù)wz計(jì)，數(shù)值以%表示，按公式(5)計(jì)算：式中：………………V?——空白試驗(yàn)消耗碘標(biāo)準(zhǔn)滴定溶液的體積的數(shù)值，單位為毫升(mL);V?——樣品消耗碘標(biāo)準(zhǔn)滴定溶液的體積的數(shù)值，單位為毫升(mL);c——碘標(biāo)準(zhǔn)滴定溶液的濃度的數(shù)值，單位為摩爾每升(mol/L);m?——樣品的質(zhì)量的數(shù)值，單位為克(g);M——發(fā)泡劑ADC的摩爾質(zhì)量的數(shù)值，單位為克每摩爾(g/mol)(M=116.06)。4.10.5允許差平行測定兩個(gè)結(jié)果的絕對差值不大于0.50%,取平行測定兩個(gè)結(jié)果的算術(shù)平均值作為測定結(jié)果。5檢驗(yàn)規(guī)則5.1檢驗(yàn)分類檢驗(yàn)包括出廠檢驗(yàn)和型式檢驗(yàn)兩類。表1中(1)～(8)項(xiàng)為出廠檢驗(yàn)項(xiàng)目。5.1.2型式檢驗(yàn)表1中全部檢驗(yàn)項(xiàng)目為型式檢驗(yàn)項(xiàng)目。正常生產(chǎn)的情況下，每月應(yīng)至少進(jìn)行一次型式檢驗(yàn)。在有下列情況之一時(shí)，也應(yīng)進(jìn)行型式檢驗(yàn)：a)更新關(guān)鍵生產(chǎn)工藝；c)停產(chǎn)后重新恢復(fù)生產(chǎn)；d)出廠檢驗(yàn)結(jié)果與上次型式檢驗(yàn)結(jié)果有較大差異。本產(chǎn)品以同一班組的均勻產(chǎn)品進(jìn)行組批。5.3采樣按GB/T6679的規(guī)定，以批為單位采樣(以一次混合均勻的產(chǎn)品為一批)。采樣量不得少于500g。分裝于兩個(gè)清潔、干燥、密封良好的磨口瓶(塑料袋)中，密封。瓶(袋)上粘貼標(biāo)簽，注明生產(chǎn)廠名稱、產(chǎn)品名稱、批號、采樣日期、采樣人等。一瓶(袋)供檢驗(yàn)部門檢驗(yàn)，另一瓶(袋)保存?zhèn)洳?。本產(chǎn)品的外包裝件上應(yīng)有清晰、牢固的標(biāo)志，內(nèi)容包括：產(chǎn)品名稱、標(biāo)準(zhǔn)號、生產(chǎn)廠名稱、地址、生產(chǎn)日期、批號、凈含量和符合GB190—2009規(guī)定的“易燃固體”標(biāo)志以及按GB/T191—每桶凈含量40kg。也可以根據(jù)用戶要求采用其他包裝形式。產(chǎn)品的包裝應(yīng)符合GB12463的有關(guān)根據(jù)GB12268—2012的規(guī)定，本產(chǎn)品屬于第4類4.1項(xiàng)易燃固體；吸入可能導(dǎo)致過敏或哮喘癥劇烈分解或爆炸，熔點(diǎn)180℃~200℃,在120℃以上易分解，放出大量氮?dú)夂鸵谎趸迹诿荛]容器中易造成爆炸事故，如含尿素、縮二脲等雜質(zhì)則分解溫度大大降低。與堿或酸接觸引起危險(xiǎn)性分氣體體積換算系數(shù)附表A.1氣體體積換算系數(shù)(氣體體積換算成20℃、101325Pa狀態(tài)下的系數(shù))室溫大氣壓/Pa906670.92720.92290.91850.91410.96060.90570.90110.89640.89230.88750.88330.87840.87400.86890.86430.85900.85430.84950.84390.83890.83380.82850.8225909330.93000.92570.92130.91680.91230.90840.90380.89910.89500.89020.88600.88100.87670.87150.86700.86170.85690.85210.84650.84150.83640.83110.8251912000.93280.92840.924.00.91960.91510.91110.90650.90180.89770.89290.88870.88370.87930.87420.86960.86430.85960.85470.84910.84410.83900.83370.8277914670.93550.93120.92680.92230.91780.91390.90920.90450.90040.89560.89130.88640.88200.87680.87220.86690.86220.85730.85170.84670.84150.83630.8302917330.93830.93390.92950.92500.92050.91660.91190.90720.90310.89830.89400.88900.88460.87950.87490.86960.86480.86000.85440.84930.84410.83890.8328920000.94110.93670.93230.92780.92330.91930.91460.90990.90580.90090.89670.89170.88730.88210.87750.87220.86740.86260.85700.85190.84670.84140.8354922670.94380.93950.93500.93050.92600.92200.91740.91260.90850.90360.89940.89440.89000.88480.08020.87480.87010.86520.85960.85450.84930.84400.8380925330.94660.94220.93780.93320.92870.92480.92010.91530.91120.90630.90200.89700.89290.88740.88200.87750.87270.86780.86220.85710.85190.84660.8405928000.94940.94500.94050.93600.93140.92750.92280.91800.91390.90900.90470.89970.89530.89010.88540.88010.87530.87040.86480.85970.85450.84920.8431930670.95220.94770.94330.93870.93420.93020.92550.92070.91660.91170.90740.90240.89790.89270.88810.88270.87790.87300.86740.86230.85710.85180.8457933330.95490.95050.94600.94150.93690.93290.92820.92340.91930.914.40.91010.90500.90060.89530.89070.88530.88050.87560.87000.86490.85970.85430.8482936000.95770.95330.94880.94420.939.60.93560.93090.92610.92200.91700.91270.90770.90320.89800.89340.88800.88320.87830.87260.86750.86220.85690.8508938670.96040.95600.95150.94700.94240.93840.93360.928.80.92470.91970.91540.91040.90590.90060.89600.89050.88580.88090.87520.87010.86470.85950.8534941330.96320.95880.95430.94490.94510.94110.93630.93150.92740.92240.91810.91300.90860.90030.89860.89320.88840.88350.87780.87270.86740.86210.8559944000.96600.96150.95700.95240.94780.94380.93910.93420.93010.92510.92080.91570.91120.90590.90130.89590.89100.88610.88040.87520.87000.86470.8585946670.96870.96430.95980.95520.95080.94650.94180.93690.93280.92780.92340.91830.91390.90860.90390.89850.89360.88870.88300.87780.87260.86720.8611949330.97150.96710.96260.95790.95330.94930.94450.93960.93550.93040.92610.92100.91650.91120.90660.90110.89630.89130.88560.88040.87520.86980.8637952000.97430.96980.96530.96070.95600.95200.94720.94230.93810.93310.92280.92370.91920.91390.90920.90380.89890.89390.88820.88300.87780.87240.8662954670.97710.97260.96800.96340.95880.95470.94990.94510.94080.93580.93150.92630.92180.91650.91180.90640.90150.89660.89080.88560.88040.87500.8688957330.97990.97530.97080.96610.96150.95740.95260.94780.94350.93850.93420.92900.92450.91920.91450.90900.90410.89920.89340.88820.88300.87760.8714960000.98260.97810.97350.96890.96420.96010.95530.95050.94620.94120.93680.93170.92720.92180.91710.91160.90680.90180.89600.89080.88550.88010.8740962670.98540.98090.97630.97160.96690.96290.95800.95320.94890.94390.93950.93430.92980.92450.91980.91430.90940.90440.89860.89340.88810.88270.8765965330.98820.98360.97900.97440.96970.96560.96080.95590.95160.94650.94220.93700.93250.92710.92240.91690.91200.90700.90120.89600.89070.88530.8791968000.99090.98640.98180.97710.97240.96830.96350.95860.95430.94920.94490.93970.93510.92980.92500.91950.91460.90960.90380.89860.89330.88790.8816室溫大氣壓/Pa970670.99370.98910.98450.97980.97510.97100.96620.96130.95700.95190.94750.94230.93780.93240.92770.92220.91720.91220.90640.90120.89590.89050.8842973330.88650.99190.98730.98260.97790.97380.96890.96400.95970.95460.95020.94500.94050.93510.93030.92480.91990.91490.90900.90380.89850.89300.8868976000.99920.99470.99000.98530.98060.97650.97160.96670.96240.95730.95290.94770.94310.93770.93300.92740.92250.91750.91160.90640.90110.89560.8894978670.99740.99280.98810.98330.97920.97430.96940.96510.95990.95560.95030.94580.94040.93560.93010.92510.92010.91420.90900.90370.89820.8919981330.99550.99080.98610.98190.97700.97210.96780.96260.95820.95300.94840.94300.93820.93270.92770.92270.91680.91160.90620.90080.8945984000.99830.99350.98880.98460.97970.97480.97050.96530.96090.95570.95110.94570.94090.93530.93040.92530.91950.91420.90880.90340.8971986670.99630.99150.98740.98240.97750.97320.96800.96360.95830.95370.94830.94350.93790.93300.92790.92210.91680.91140.90590.8996989330.99900.99430.99010.98520.98020.97590.97070.96630.96100.95640.95100.94620.94060.93560.93050.92470.91940.914.00.90850.9022992000.99700.99280.98790.98290.97860.97320.96890.96370.95910.95360.94880.94320.93820.93310.92730.92200.916.60.91110.9048994670.99970.99550.99060.98560.98120.97610.97160.96630.96170.95630.95140.94580.94080.93580.92990.92460.91920.91370.9073997330.99830.99330.98830.98390.97880.97430.96900.96440.95890.95410.94850.94350.93840.93250.92720.92180.91630.90990.99600.99100.98660.98150.97700.97170.96700.96150.95670.95110.94610.94100.93510.92980.92440.91880.91250.99870.99370.98930.98420.97960.97430.96970.96420.95940.95370.94870.9436