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各位大侠谁做过二(对硝基)苯基碳酸酯的色谱分析,能不能告诉在下操作的条件?小弟是新手,第一次摸条件,总是出错啊![em09512]
事件回放:“丈夫没有了,两个孩子也还在医院里,这两天我都不知道怎么过来的。”刘从兰用手擦去眼角的眼泪,静静地望着刚做完血透的小女儿琳琳(化名)。她说,现在一点都不敢想象今后的生活该怎么过下去,怕自己会承受不了。 9月13日,东阳市画水镇发生一起因废塑中毒事件,目前已造成3人死亡、17人住院治疗的严重后果。[font=黑体][size=4]何谓二硝基苯酚?[/size][/font][color=#00008B]分子式2,4-(NO2)2C6H3F。 2,4-二硝基氟苯为淡黄色晶体; 熔点25.8℃,沸点 296℃,密度1.4718克/厘米3(84℃); 溶于乙醇、苯、丙二醇等。 2,4-二硝基氟苯主要由2,4-二硝基氯苯与氟化钾在硝基苯中反应制得 2,4-二硝基氟苯是一种重要的分析试剂,用来鉴定有机化合物中的氨基,尤其是用于蛋白质或多肽的N-端残基分析。鉴定时,2,4-二硝基氟苯与肽链的游离氨基作用,生成2,4-二硝基衍生物。将其水解后,末端氨基酸的N-(2,4-二硝基苯基)衍生物常为亮黄色结晶,易与其他氨基酸分离。该方法结合其他方法,可确定蛋白质或多肽氨基端碳链的结构。由F.桑格于1945年提出,故称桑格法 此外,它在碳酸氢钠溶液中与醛糖的肟反应时可发生降解,生成次级醛糖、2,4-二硝基苯酚和氢氰酸,故可用于醛糖的分析。2,4-二硝基氟苯能使皮肤糜烂,使用时应注意。[/color]&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&77[color=#DC143C]1)作为一名专业的分析工作者,如果从自己的专业角度去分析。我们使用什么方法和仪器可以检测出二硝基苯酚?2)遇到这样的事情如何加强自我预防?3)在我们平时的分析工作中,我们会遇到那些有毒的化学试剂或者样品,我们如何做好自我防备。欢迎大家讨论。。。。[/color]
粗精硝基苯纯度及杂质分析方法整合探究崔华宝 叶冬芸 邓颖良(万华化学(宁波)有限公司,浙江省 宁波市 315812) 摘要:本方法的开发致力于解决硝苯装置样品粗精硝基苯纯度及杂质的分析。本方法利用安捷伦气相色谱技术,使用一根HP-5色谱柱让组分进行分离,粗精硝基苯纯度及杂质,分别通过FID检测器进行归一化和面积百分比法定量。将归一化和面积百分比法组分含量之间的关系,进行线性模型的拟合,利用拟合方程,预测面积百分比法组分含量所对应的归一化法组分含量。本方案实现了粗精硝基苯纯度及杂质,分析方法整合运用,降低了分析成本,提高了工作效率。 关键词:硝苯装置 硝基苯 线性模型 1.%2.%3. 背景介绍 硝基苯装置是以原料苯和硝酸制造硝基苯的生产装置,装置包括:硝化反应单元、产品汽提单元等。硝化反应单元以苯和硝酸为原料,硫酸为催化剂,采用绝热硝化方式制得粗硝基苯;产品汽提单元是通过汽提塔,采用蒸汽直接汽提法,除去粗硝基苯中的苯。得到精制的硝基苯,作为下游装置原料。 硝化反应过程中需严格控制硝基酚、二硝基苯等硝化副产物的生成,在反应加入过量的苯约5-8%的条件下进行操作。其主要反应式如下: 1.1整合前方法 由于粗硝基苯和精硝基苯在苯组分含量上相差6%,[/font]且苯和其它各组分响应差异较大,所以面积百分比法并不能完全适用于二者纯度及杂质的分析。 处理方法: 1、粗硝基苯归一化法校正因子制作 使用精密天平分别称取10.0000g苯、0.0200g邻硝基甲苯、间硝基甲苯、对硝基甲苯、硝基二甲苯、对二硝基苯、间二硝基苯、邻二硝基苯、正庚烷、90.00g硝基苯于100mL容量瓶中,该溶液中杂质各组分的浓度分别为苯:9.98%,其他含量为0.02%、硝基苯含量为89.86%,此溶液为标准溶液A。 将标准溶液A按照本方法的操作步骤进行气相色谱分析。根据标准溶液各组分含量与色谱峰面积计算各组分的校正因子(见图1),精硝基苯无校正因子(见图2)。 在HP-5色谱柱上,粗硝基苯各组分色谱图(见图3),精硝基苯各组分色谱图(见图4)。 https://ng1.17img.cn/bbsfiles/images/2024/10/202410011351303952_3510_2367669_3.png图1 粗硝基苯校正表https://ng1.17img.cn/bbsfiles/images/2024/10/202410011351306386_9342_2367669_3.png图2精硝基苯化合物表https://ng1.17img.cn/bbsfiles/images/2024/10/202410011351308647_1379_2367669_3.png图3 粗硝基各组分色谱图https://ng1.17img.cn/bbsfiles/images/2024/10/202410011351309948_8131_2367669_3.png图4精硝基各组分色谱图 1.2 线性模型的原理 1、线性方程如下直线方程属于线性方程:y=kx+b图像可表示为:https://ng1.17img.cn/bbsfiles/images/2024/10/202410011351311198_5917_2367669_3.jpeg图5 线性方程图2、线性拟合线性拟合是曲线拟合的一种形式,通过一组观测数据来寻求最佳的理论曲线,使得观测数据与理论曲线之间的误差最小。在实际应用中,具体来说,线性拟合是通过找到一条最佳拟合直线,这条直线能够最好地匹配给定的数据点。如下图所示:https://ng1.17img.cn/bbsfiles/images/2024/10/202410011351312166_2994_2367669_3.jpeg图6 拟合线图线性拟合就是根据一组x, y的值,来寻求最佳k,b的值,这个过程也可称为线性回归。 1.3探究方向 此方法利用安捷伦气相色谱技术,使用一根HP-5色谱柱让组分进行分离,粗精硝基苯纯度及杂质,分别通过FID检测器进行归一化和面积百分比法定量。将归一化和面积百分比法组分含量之间的关系,进行线性模型的拟合,利用拟合方程,预测面积百分比法组分含量所对应的归一化法组分含量。[/size] 1.4降本增效 本方案实现了粗精硝基苯纯度及杂质,分析方法整合运用;降低了人员和有毒有害试剂的使用,可以快速搭建分析方法,出具分析数据,提高了工作效率。对硝苯装置的生产具有重要的指导意义。 2.具体开展工作 2.1方法开发 利用CDS操作系统,随机选取2024年5-8月份粗硝基苯样品序列,分别使用归一化和面积百分比法,测定各组分含量,录入表单,制成基础数据表。色谱图如下:https://ng1.17img.cn/bbsfiles/images/2024/10/202410011351312673_1690_2367669_3.jpeg图7 各组分归一化和面积百分比法含量色谱图表1苯基础数据:数量样品归一化苯%面积百分比苯%12211B 24-5-46.496010.129122221B 24-5-46.551110.21343[/font]2211B 24-5-76.31419.842042221B 24-5-76.560910.228152211B 24-5-76.31339.85762211B 24-5-96.41609.999172211B 24-5-116.631810.30882221B 24-5-116.708410.422992211B 24-5-146.544010.1838102221B 24-5-146.28239.7961112211B 24-5-166.31779.8382122221B 24-5-166.32219.8468132211B 24-5-186.22559.6862142221B 24-5-186.34059.8612152211B 24-5-216.41309.9781162221B 24-5-216.503710.1172172211B 24-5-236.894910.7144182221B 24-5-236.763410.5216192211B 24-5-256.946010.7991202221B 24-5-256.865110.68212211B 24-5-28[td]7.056110.9576222221B 24-5-286.867410.6797232211B 24-5-306.419910.01242221B 24-5-306.19459.6722252211B 24-6-016.843210.6376262221B 24-6-016.769910.5311272211B 24-6-066.512810.1252282221B 24-6-066.552210.1853292211B 24-6-086.15689.5895302221B 24-6-086.3137[align=center]9.8241312211B 24-6-136.38619.9479322221B 24-6-136.442510.0345332211B 24-6-156.14329.5826342221B 24-6-155.99259.3564352211B 24-6-206.25659.7563362221B 24-6-206.34659.8964372211B 24-6-226.592510.2676382221B 24-6-226.656210.3664392211B 24-6-256.550510.189640[/align]2221B 24-6-256.531710.1664412211B 24-6-276.650710.3532422221B 24-6-276.973110.8357432211B 24-6-296.29719.8167442221B 24-6-296.454310.0553452211B 24-7-026.578710.2292462221B 24-7-026.544010.1811472211B 24-7-046.531810.1581482221B 24-7-046.520310.143492211B 24-7-066.887210.6905502221B 24-7-066.820010.5942512211B 24-7-096.439710.0182522221B 24-7-096.33199.8601532211B 24-7-115.88189.2542221B 24-7-115.84099.1368552211B 24-7-166.616210.2957562221B 24-7-166.495710.1173572211B 24-7-186.18039.6382582221B 24-7-186.02789.409592211B 24-7-206.04289.4217602221B 24-7-205.97119.3155612211B 24-7-236.05659.4544622221B 24-7-236.08099.4929632211B 24-7-256.25019.7429642221B 24-7-256.21199.6872652211B 24-7-276.42379.9947662221B 24-7-276.35029.8881672211B 24-7-306.583410.2525682221B 24-7-306.489610.1129692211B 24-8-16.466210.0774702221B 24-8-16.417210.0057712211B 24-8-37.013510.8917722221B 24-8-37.494311.602732211B 24-8-66.34569.8863742221B 24-8-66.38109.9419752211B 24-8-85.93189.2817762221B 24-8-86.02949.428777[align=center]2211B 24-8-106.40859.9907782221B 24-8-106.36999.9325792211B 24-8-136.32399.8566802221B 24-8-136.19519.6641812211B 24-8-156.576510.24822221B 24-8-156.40839.9879832211B 24-8-176.477610.0762842221B 24-8-176.29399.8025852211B 24-8-206.32659.8392862221B 24-8-20[font='楷体']6.03619.4056872211B 24-8-226.594810.2563882221B 24-8-226.40989.9802892211B 24-8-246.663510.3508902221B 24-8-246.497610.1034912211B 24-8-276.37089.919922221B 24-8-276.30359.82932211B 24-8-296.799410.5755942221B 24-8-296.786110.5548952211B 24-8-316.795810.5671[/tr]962221B 24-8-316.684010.3998表2硝基苯基础数据:数量样品归一化硝基苯%面积百分比硝基苯%12211B 24-5-493.458689.569422221B 24-5-493.410189.508732211B 24-5-792.841588.946242221B 24-5-793.392489.486852211B 24-5-793.640189.859362211B 24-5-993.546889.6066[/align]72211B 24-5-1193.319889.151282221B 24-5-1193.244289.044492211B 24-5-1493.404389.3408102221B 24-5-1493.667389.7708112211B 24-5-1693.632489.6181122221B 24-5-1693.629389.6304132211B 24-5-1893.729689.6332142221B 24-5-1893.616289.4891152211B 24-5-21[/td]93.549489.4629162221B 24-5-2193.459889.3597172211B 24-5-2393.068688.8913182221B 24-5-2393.200589.1149192211B 24-5-2593.023488.8901202221B 24-5-2593.105789.0248212211B 24-5-2892.907388.6780222221B 24-5-2893.095588.9839232211B 24-5-3093.539989.6438[/td]242221B 24-5-3093.763589.9834252211B 24-6-0193.115988.9659262221B 24-6-0193.191289.1001272211B 24-6-0693.447989.2929282221B 24-6-0693.408089.2450292211B 24-6-0893.801389.7978302221B 24-6-0893.645789.5600312211B 24-6-1393.574389.590832[align=center]2221B 24-6-1393.518389.5262332211B 24-6-1593.815989.9464342221B 24-6-1593.966690.1753352211B 24-6-2093.705989.8117362221B 24-6-2093.614889.7218372211B 24-6-2293.372489.3814382221B 24-6-2293.306889.3150392211B 24-6-2593.406189.3038402221B 24-6-2593.4251[td]89.3747412211B 24-6-2793.303989.2727422221B 24-6-2792.983488.8075432211B 24-6-2993.663189.7443442221B 24-6-2993.505189.5358452211B 24-7-0293.386289.2480462221B 24-7-0293.421289.3327472211B 24-7-0493.435689.3113482221B 24-7-0493.447389.346449[/td]2211B 24-7-0693.069588.7920502221B 24-7-0693.136788.9235512211B 24-7-0993.522689.4243522221B 24-7-0993.630689.6146532211B 24-7-1194.071890.4374542221B 24-7-1194.112590.4852552211B 24-7-1693.349689.2834562221B 24-7-1693.469389.4797572211B 24-7-1893.7831[/align]89.8923582221B 24-7-1893.934890.1203592211B 24-7-2093.918490.0024602221B 24-7-2093.991390.1270612211B 24-7-2393.906790.0988622221B 24-7-2393.884490.0825632211B 24-7-2593.713089.7871642221B 24-7-2593.753589.8625652211B 24-7-2793.544589.4584[align=center]662221B 24-7-2793.621289.6015672211B 24-7-3093.375289.3768682221B 24-7-3093.469689.5246692211B 24-8-193.489789.5522702221B 24-8-193.540089.6423712211B 24-8-392.946488.7177722221B 24-8-392.466187.9825732211B 24-8-693.615189.6438742221B 24-8-6[font='楷体']93.579889.6136752211B 24-8-894.017590.4205762221B 24-8-893.926690.2767772211B 24-8-1093.551189.6404782221B 24-8-1093.590889.6958792211B 24-8-1393.629489.6944802221B 24-8-1393.757889.8946812211B 24-8-1593.386889.3723822221B 24-8-1593.556289.6220[align=center]832211B 24-8-1793.488789.3836842221B 24-8-1793.671689.6686852211B 24-8-2093.633489.5038862221B 24-8-2093.925189.9552872211B 24-8-2293.371189.2509882221B 24-8-2293.556389.5318892211B 24-8-2493.304489.0823902221B 24-8-2493.470689.3307912211B 24-8-27[font='楷体']93.587289.5583922221B 24-8-2793.655189.6757932211B 24-8-2993.170889.0684942221B 24-8-2993.183989.0807952211B 24-8-3193.166589.0414962221B 24-8-3193.278589.2034表3对二硝基苯基础数据:数量样品归一化对二硝基苯%面积百分比对二硝基苯%12211B 24-5-40.00400.00252[td]2221B 24-5-40.00210.001332211B 24-5-70.06300.040142221B 24-5-70.00590.003752211B 24-5-70.00350.002262211B 24-5-90.00160.001072211B 24-5-110.00110.000782221B 24-5-110.00110.000792211B 24-5-140.00110.0007102221B 24-5-140.00120.0007112211B 24-5-160.00120.0008122221B 24-5-160.00120.0008132211B24-5-180.00120.0008142221B 24-5-180.00120.0007152211B 24-5-210.00110.0007162221B 24-5-210.00110.0007172211B 24-5-230.00100.0007182221B 24-5-230.00100.000619[/td]2211B 24-5-250.00100.0006202221B 24-5-250.00090.0006212211B 24-5-280.00100.0007222221B 24-5-280.00110.0007232211B 24-5-300.00120.0008242221B 24-5-300.00130.0008252211B 24-6-010.00110.0007262221B 24-6-010.00100.0006272211B 24-6-06[font='楷体']0.00110.0007282221B 24-6-060.00100.0007292211B 24-6-080.00120.0007302221B 24-6-080.00110.0007312211B 24-6-130.00110.0007322221B 24-6-130.00100.0007332211B 24-6-150.00120.0008342221B 24-6-150.00120.0007352211B 24-6-200.00120.0007[align=center]362221B 24-6-200.00120.0007372211B 24-6-220.00100.0007382221B 24-6-220.00110.0007392211B 24-6-250.00110.0007402221B 24-6-250.00110.0007412211B 24-6-270.00100.0007422221B 24-6-270.00100.0006432211B 24-6-290.00110.0007442221B 24-6-29[/align]0.00120.0008452211B 24-7-020.00110.0007462221B 24-7-020.00110.0007472211B 24-7-040.00100.0007482221B 24-7-040.00100.0007492211B 24-7-060.00100.0006502221B 24-7-060.00100.0006512211B 24-7-090.00110.0007522221B 24-7-090.0011[align=center]0.0007532211B 24-7-110.00150.0009542221B 24-7-110.00140.0009552211B 24-7-160.00100.0006562221B 24-7-160.00100.0006572211B 24-7-180.00110.0007582221B 24-7-180.00110.0007592211B 24-7-200.00110.0007602221B 24-7-200.00100.000761[/font]2211B 24-7-230.00120.0007622221B 24-7-230.00110.0007632211B 24-7-250.00100.0006642221B 24-7-250.00090.0006652211B 24-7-270.00100.0006662221B 24-7-270.00090.0006672211B 24-7-300.00090.0006682221B 24-7-300.00090.0006692211B 24-8-10.00100.0006702221B 24-8-10.00100.0006712211B 24-8-30.00080.0005722221B 24-8-30.00080.0005732211B 24-8-60.00110.0007742221B 24-8-60.00110.0007752211B 24-8-80.00170.0011762221B 24-8-80.00140.0009772211B 24-8-100.00110.0007[font='楷ign=center]检测器温度260℃进样口温度260℃进样量0.2uL载气高纯氮气色谱柱1模式:恒定流量柱流量:2.3mL/min分流比15:1隔垫吹扫流量3mL/min尾吹气流量30mL/min程序升温60℃保持1min,以20℃/min的速率升温到230℃保持5min,总运行时间12 min助燃气燃气[/