CN106018362A - 一种检测苦味酸的测定器 - Google Patents
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Abstract
本发明公开一种检测苦味酸的测定器，包括针筒状的柱形筒、锥形头和推杆，所述锥形头上设有控制锥形头开闭的第一开关，所述推杆包括依次连接的推杆头、推杆柱和推托，所述推杆头通过密封圈与柱形筒内壁滑动连接，柱形筒的侧壁固定有研磨机构，研磨机构包括贯穿柱形筒侧壁的连通管、与连通管连接的研磨室，连通管上设有控制连通管开闭的第二开关，研磨室包括入料腔、出料漏斗腔和研磨腔，研磨腔内设置有砂轮，砂轮套装在转轴上，砂轮与转轴固定连接，转轴与研磨腔壁转动连接。本发明提供一种检测苦味酸的测定器，可以实现对苦味酸吸附前后荧光强度的变化对苦味酸分子进行选择性定性及定量检测，灵敏度高，具有很好的应用前景。
Description
技术领域
本发明涉及环保检测领域，特别是关于一种检测苦味酸的测定器。
背景技术
2,4,6-三硝基苯酚是一种硝基芳香族化合物，又称作苦味酸，常被用来制作烈性炸药，同时也是一种环境污染物。因此不仅涉及公共安全问题，也是一类高毒性的环境污染物，存在于空气、海水、土壤和石油中。由于其毒性，2,4,6-三硝基苯酚的存在会对人类健康产生极大的危害，尤其是对于人的循环系统、肝、脾和免疫系统造成严重的伤害。并且，2,4,6-三硝基苯酚和它的生物降解产物具有诱变性和致癌性，对水生物和陆生物也有很大的危害。目前很多仪器分析技术方法，包括气相色谱分析法、气质联用分析法以及表面增强拉曼光谱分析法等，均可对2, 4, 6- 三硝基苯酚进行高灵敏度检测，但不足之处在于检测过程往往需要庞大的仪器设备和复杂的操作流程，需要耗费大量的时间，不适宜当今社会快速检测的需求。相比较而言，荧光化学检测方法则是一类更加便捷、经济的检测手段。因此，开发出一种快速，具有单一性检测2,4,6-三硝基苯酚的荧光化学传感器具有重要意义。
发明内容
有鉴于此，本发明为解决上述技术问题，提供一种检测苦味酸的测定器。
本发明的目的通过以下技术方案实现：
一种检测苦味酸的测定器，包括针筒状的柱形筒、锥形头和推杆，所述锥形头上设有控制锥形头开闭的第一开关，所述推杆包括依次连接的推杆头、推杆柱和推托，所述推杆头通过密封圈与柱形筒内壁滑动连接，柱形筒的侧壁固定有研磨机构，研磨机构包括贯穿柱形筒侧壁的连通管、与连通管连接的研磨室，连通管上设有控制连通管开闭的第二开关，研磨室包括入料腔、出料漏斗腔和研磨腔，研磨腔内设置有砂轮，砂轮套装在转轴上，砂轮与转轴固定连接，转轴与研磨腔壁转动连接，转轴的端部与手摇臂固定连接，手摇臂位于研磨腔外，入料腔壁上设有开口，开口上设有开闭门，开口旁设有磁体一，开闭门上设有与磁体一相互磁吸的磁体二，出料漏斗腔位于入料腔旁，入料腔、出料漏斗腔和研磨腔相互连通；所述柱形筒内含有乙腈溶剂，所述研磨机构内含有化学式为(C14H8N8S)2Zn的荧光传感器，其中，C14H8N8S为二(4-(1H-四唑-5-基)苯基)硫烷根；所述荧光传感器为单斜晶系，P21/m空间群，晶胞参数为a =10.163(3) Å，b =9.353(5) Å，c =12.845(3) Å，α =γ=90 º，β =103.673(1) º，V=1220.97 (1) Å3。
所述荧光传感器的制备方法是，将有机化合物4,4'-硫代二苯甲腈、叠氮化钠和氯化锌溶于水和乙醇的混合溶剂当中，其中水和乙醇体积比为1:1，在室温下搅拌形成混合液A，然后将所述混合液A在水热条件下反应36小时后得到所述荧光传感器。
优选的，所述4,4'-硫代二苯甲腈、叠氮化钠和氯化锌的摩尔比为2:6:1。
优选的，所述的水热温度为140℃。
其中，4,4'-硫代二苯甲腈英文为4,4'-thiodibenzonitrile，在水热条件下，利用锌离子和叠氮化钠的作用下能够生成二(4-(1H-四唑-5-基)苯基)硫烷，而二(4-(1H-四唑-5-基)苯基)硫烷质子化后能够原位与锌离子形成一种配合物。而二(4-(1H-四唑-5-基)苯基)硫烷中四唑环具有丰富的氮原子，能够提供孤对电子与2,4,6-三硝基苯酚通过质子转移相互作用。
所述检测苦味酸的测定器的使用方式是，使用时，将便携式检测器以锥形头朝上、推杆朝下的状态放置，开启开闭门，将荧光传感器由开口置入研磨室，荧光传感器经过入料腔到达研磨腔，转动手摇臂带动砂轮转动，转动的砂轮将荧光传感器研磨呈粉末状，此后开启第一开关，并将柱形筒内装有乙腈溶剂的便携式检测器以锥形头朝下、推杆朝上的方式靠近乙腈溶剂，将乙腈溶剂吸入柱形筒内，关闭第一开关并开启第二开关，粉末状荧光传感器进入柱形筒内与乙腈溶剂混合，此后关闭第二开关并开启第一开关，将柱形筒内装有乙腈溶剂的便携式检测器以倾斜的方式靠近待测水体，当锥形头伸入待测水体水面下方后，拉动推杆，将部分待测水体吸入柱形筒内，此后旋转便携式的铅离子测定器至锥形头朝上、推杆朝下的状态，当便携式的铅离子测定器处于锥形头朝上、推杆朝下的状态时，对柱形筒内混合液进行荧光光谱测试，利用荧光强度的变化对2,4,6-三硝基苯酚分子进行选择性定性及定量检测。
本发明相较于现有技术的有益效果是：
本发明的检测苦味酸的测定器，往研磨机构内置入荧光传感器，并将置入研磨机构的荧光传感器研磨成粉末，粉末状的荧光传感器沿着连通管进入到柱形筒内与乙腈溶剂混合，混合液与待测物质进行荧光光谱测试即可根据荧光强度判断苦味酸含量，方便实用，且荧光传感器易于制备，而且在水热情况下能够发生原位反应，合成出来的荧光传感器化学稳定性好。本发明的荧光传感器具有良好的荧光特性，四唑环结构中富含具有孤对电子的氮原子，通过质子转移相互作用，可以实现对苦味酸吸附前后荧光强度的变化对苦味酸分子进行选择性定性及定量检测，灵敏度高，具有很好的应用前景。
附图说明
利用附图对本发明作进一步说明，但附图中的实施例不构成对本发明的任何限制。
图1是本发明的检测苦味酸的测定器的整体结构图。
图2为本发明的荧光传感器化学结构图。
图3为本发明的荧光传感器吸附苦味酸分子的荧光光谱图。
具体实施方式
为了便于本领域技术人员理解，下面将结合附图以及实施例对本发明作进一步详细描述。
请参照图1-3，本发明实施例如下
一种检测苦味酸的测定器，包括针筒状的柱形筒1、锥形头2和推杆3，所述锥形头2上设有控制锥形头开闭的第一开关4，所述推杆3包括依次连接的推杆头5、推杆柱6和推托7，所述推杆头5通过密封圈8与柱形筒1内壁滑动连接，柱形筒1的侧壁固定有研磨机构，研磨机构包括贯穿柱形筒1侧壁的连通管9、与连通管9连接的研磨室，连通管9上设有控制连通管9开闭的第二开关10，研磨室包括入料腔11、出料漏斗腔12和研磨腔13，研磨腔13内设置有砂轮14，砂轮14套装在转轴15上，砂轮14与转轴15固定连接，转轴14与研磨腔13壁转动连接，转轴15的端部与手摇臂16固定连接，手摇臂16位于研磨腔13外，入料腔11壁上设有开口17，开口17上设有开闭门18，开口17旁设有磁体一19，开闭门18上设有与磁体一19相互磁吸的磁体二20，出料漏斗腔12位于入料腔11旁，入料腔11、出料漏斗腔12和研磨腔13相互连通；所述柱形筒1内含有乙腈溶剂，所述研磨机构内含有化学式为(C14H8N8S)2Zn的荧光传感器。
将1mmol4,4'-硫代二苯甲腈、3mmol叠氮化钠与0.5mmol氯化锌溶解于10mL水和10mL乙醇的混合溶液中，常温搅拌30分钟，随后转移到聚四氟乙烯高压反应釜中，将其放在140℃烘箱中反应36小时，之后以5℃/小时降至室温过滤得到荧光传感器，产率50.2%（基于锌）。
然后将所得的荧光传感器进行单晶表征。
该化合物的X射线衍射数据是在Bruker Smart Apex CCD面探衍射仪上，用MoKα辐射(λ = 0.71073 Å)，以ω扫描方式收集并进行Lp因子校正，吸收校正使用SADABS程序。用直接法解结构，然后用差值傅立叶法求出全部非氢原子坐标，并用理论加氢法得到氢原子位置(C−H 1.083 Å)，用最小二乘法对结构进行修正。计算工作在PC机上用SHELXTL程序包完成。化学结构图如图1所示。
经测试解析可知，该荧光传感器化学式为(C14H8N8S)2Zn；其中，C14H8N8S为二(4-(1H-四唑-5-基)苯基)硫烷根，单斜晶系，P21/m空间群，晶胞参数为a =10.163(3) Å，b =9.353(5) Å，c =12.845(3) Å，α =γ=90 º，β =103.673(1) º，V=1220.97 (1) Å3，Z=2。其化学结构图如图1所示，其中，4,4'-硫代二苯甲腈在叠氮化钠和锌离子的作用下原位生成二(4-(1H-四唑-5-基)苯基)硫烷，而二(4-(1H-四唑-5-基)苯基)硫烷质子化后有与锌离子配位，锌离子采取4配位4面体的模式与4个二(4-(1H-四唑-5-基)苯基)硫烷上四唑环上的N原子配位，而二(4-(1H-四唑-5-基)苯基)硫烷两头的四唑环也分别与锌离子配位。
将0.001g实施例1中所得的荧光传感器研磨成粉末后分散至10mL乙腈溶剂中，然后添加不同浓度的2,4,6-三硝基苯酚进行荧光光谱测试，激发波长为338nm。荧光光谱图如图2所示，从图中我们可以看出，随着2,4,6-三硝基苯酚的浓度从0增加到10mM，荧光强度逐渐降低，而且，如果添加的是2,4,6-三硝基甲苯、二硝基甲苯、1,3-二硝基苯、硝基苯这类物质的话不影响本发明的荧光传感器荧光强度，基本和浓度为0mM时类似，因此可以利用荧光强度的变化对2,4,6-三硝基苯酚分子进行选择性定性及定量检测。
本发明的检测苦味酸的测定器，往研磨机构内置入荧光传感器，并将置入研磨机构的荧光传感器研磨成粉末，粉末状的荧光传感器沿着连通管进入到柱形筒内与乙腈溶剂混合，混合液与待测物质进行荧光光谱测试即可根据荧光强度判断苦味酸含量，方便实用。
最后应当说明的是，以上实施例说明本发明的技术方案，而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细地说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。
Claims (4)
1.一种检测苦味酸的测定器，其特征在于，包括针筒状的柱形筒（1）、锥形头（2）和推杆（3），所述锥形头（2）上设有控制锥形头开闭的第一开关（4），所述推杆（3）包括依次连接的推杆头（5）、推杆柱（6）和推托（7），所述推杆头（5）通过密封圈（8）与柱形筒（1）内壁滑动连接，柱形筒（1）的侧壁固定有研磨机构，研磨机构包括贯穿柱形筒（1）侧壁的连通管（9）、与连通管（9）连接的研磨室，连通管（9）上设有控制连通管（9）开闭的第二开关（10），研磨室包括入料腔（11）、出料漏斗腔（12）和研磨腔（13），研磨腔（13）内设置有砂轮（14），砂轮（14）套装在转轴（15）上，砂轮（14）与转轴（15）固定连接，转轴（14）与研磨腔（13）壁转动连接，转轴（15）的端部与手摇臂（16）固定连接，手摇臂（16）位于研磨腔（13）外，入料腔（11）壁上设有开口（17），开口（17）上设有开闭门（18），开口（17）旁设有磁体一（19），开闭门（18）上设有与磁体一（19）相互磁吸的磁体二（20），出料漏斗腔（12）位于入料腔（11）旁，入料腔（11）、出料漏斗腔（12）和研磨腔（13）相互连通；所述柱形筒（2）内含有乙腈溶剂，所述研磨机构内含有化学式为(C14H8N8S)2Zn的荧光传感器，其中，C14H8N8S为二(4-(1H-四唑-5-基)苯基)硫烷根；所述荧光传感器为单斜晶系，P21/m空间群，晶胞参数为a =10.163(3) Å，b =9.353(5) Å，c=12.845(3) Å，α =γ=90 º，β =103.673(1) º，V=1220.97 (1) Å3。
2.根据权利要求1所述的检测苦味酸的测定器，其特征在于，所述荧光传感器的方法是，将有机化合物4,4'-硫代二苯甲腈、叠氮化钠和氯化锌溶于水和乙醇的混合溶剂当中，其中水和乙醇体积比为1:1，在室温下搅拌形成混合液A，然后将所述混合液A在水热条件下反应36小时后得到所述荧光传感器。
3.根据权利要求1所述的检测苦味酸的测定器，其特征在于，所述4,4'-硫代二苯甲腈、叠氮化钠和氯化锌的摩尔比为2:6:1。
4.根据权利要求1所述的检测苦味酸的测定器，其特征在于：所述的水热温度为140℃。
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| CN104730262A (zh) * | 2013-12-24 | 2015-06-24 | 广州万孚生物技术股份有限公司 | 一种液体检测装置 |
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| JPH11183372A (ja) * | 1997-12-19 | 1999-07-09 | Toto Ltd | Ｓｐｒセンサ装置および分析システムとこれを用いた検出方法 |
| WO2006007180A2 (en) * | 2004-06-07 | 2006-01-19 | The Charlotte-Mecklenburg Hospital Authority | Utilizing lipopolysaccharide in exhaled breath condensate to diagnose gram negative pneumonia |
| WO2010036352A1 (en) * | 2008-09-23 | 2010-04-01 | Quantalife, Inc | Droplet-based assay system |
| CN103534575A (zh) * | 2011-02-04 | 2014-01-22 | 环球生物研究株式会社 | 自动反应/光测定装置及其方法 |
| JP2013113953A (ja) * | 2011-11-28 | 2013-06-10 | Ricoh Co Ltd | 光学センサ及びそれを有する画像形成装置 |
| CN104730262A (zh) * | 2013-12-24 | 2015-06-24 | 广州万孚生物技术股份有限公司 | 一种液体检测装置 |
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