CN109490453A - 一种三乙烯四胺的分离鉴定方法 - Google Patents
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Abstract
本发明实施例提供一种三乙烯四胺的分离鉴定方法,该方法包括如下步骤:采用红外分光光度计对样品进行检测得到光谱图;采用气相色谱‑质谱联用仪对所述样品进行分离检测,得到色谱图和质谱图;根据所述质谱图和光谱图确定所述样品中的三乙烯四胺。采用上述分离鉴定方法能够准确、快速的检测样品中的三乙烯四胺,并且耗时短、成本较低。
Description
技术领域
本发明涉及分析化学技术领域,具体涉及一种三乙烯四胺的分离鉴定方法。
背景技术
三乙烯四胺又名三亚乙基四胺,分子式为C6H18N4,浅黄色或橙黄色液体;有氨气味,相对密度0.9818(20/20℃),易溶于水和乙醇,不溶于乙醚;有碱性,在空气中易吸水分和二氧化碳;与酸作用生成相应的盐;三乙烯四胺是一种化工原料,除作溶剂外,还用于制造环氧树脂固化剂、金属螯合剂以及合成聚酰胺树脂和离子交换树脂等;具体地,可以用于合成聚酰胺树脂、乳化剂、橡胶硫化促进剂和稳定剂、润滑油添加剂、织物整理剂等;也可用作环氧树脂固化剂、金属螯合剂等。
由于三乙烯四胺具有易燃性,接触明火和高热有发生燃烧的危险,具有一定的危险性,三乙烯四胺被列入危险化学品目录中;目前,对三乙烯四胺的检测方法比较复杂,用时较多,而且存在一定的假阳性;因此,对于快速准确分离鉴定三乙烯四胺有着重要意义。
发明内容
本发明实施例的目的在于提供一种三乙烯四胺的分离鉴定方法,该方法能够准确、快速的检测样品中的三乙烯四胺,并且耗时短、成本较低。
为了实现本发明的上述目的,特采用以下技术方案:
本发明实施例提供一种三乙烯四胺的分离鉴定方法,该方法包括如下步骤:
采用红外分光光度计对样品进行检测得到光谱图;
采用气相色谱-质谱联用仪对所述样品进行分离检测,得到色谱图和质谱图;
根据所述质谱图和光谱图确定所述样品中的三乙烯四胺。
本发明分离鉴定方法先通过红外分光光度计对样品进行检测得到光谱图,初步判断样品中是否含有三乙烯四胺;再通过气相色谱-质谱联用仪对样品进行快速、准确分离检测得到色谱图以及各分离峰出样本的质谱图,随后通过样本质谱图实现对三乙烯四胺的准确鉴定;本发明通过红外分光光度计和气相色谱-质谱联用仪实现双重检测,提高了三乙烯四胺鉴定的可靠性,避免假阳性的出现;进一步地,本发明通过外标法准确确定三乙烯四胺的含量。本发明的上述方法通过光谱和质谱的双重检测可实现对三乙烯四胺的同步定性和定量的有效检测,且耗时短、成本低。
进一步地,所述气相色谱采用的色谱柱为DB-5MS,所述色谱柱的柱长为15-30m、内径为0.1-0.25mm、液膜厚度为0.1-0.25um;优选地,所述色谱柱的柱长为30m、内径为0.25mm、液膜厚度为0.25um。
进一步地,所述气相色谱中柱温为50℃保持1min,以10℃/min升至100℃保持7min,以30℃/min升至310℃保持5min。
进一步地,所述气相色谱的载气为氦气;载气流速为0.8-1.2ml/min;进样口温度为140-160℃;压力为53-55Kpa;分流动比(90-110):1;优选地,载气流速为1.0ml/min;压力为53.5Kpa;分流动比100:1。
本发明实施例中对质谱条件不作严格限制,优选地,所述质谱中离子源温度为250-280℃;接口温度为260-300℃;检测器电压为0.6-0.8KV;质量扫描范围为m/z=50-500;采集方式为SCAN;更优选地,所述质谱中离子源温度为260℃;接口温度为280℃;检测器电压为0.7KV。
进一步地,所述红外分光光度计为傅立叶红外分光光度计。
本发明实施例中对检测样品不作严格限制,例如,可以为含有三乙烯四胺的固化剂或化工原料,也可以为三乙烯四胺试剂,亦或是未知样品鉴定是否含有三乙烯四胺。
进一步地,本发明气相色谱采用顶空气相色谱法进行分离检测。
与现有技术相比,本发明实施例的有益效果至少包括:
本发明提供一种三乙烯四胺的分离鉴定方法,该方法先通过红外分光光度计对样品进行检测得到光谱图,初步判断样品中是否含有三乙烯四胺;再通过气相色谱-质谱联用仪对样品进行快速、准确分离检测得到色谱图以及各分离峰出样本的质谱图,随后通过样本质谱图实现对三乙烯四胺的准确鉴定;;本发明的上述方法通过光谱和质谱的双重检测可实现对三乙烯四胺的同步定性和定量的有效检测,提高了三乙烯四胺鉴定的可靠性,避免假阳性的出现,且耗时短、成本低;此外,该方法操作简单,高效,准确,稳定。
附图说明
图1为本发明实施例1中提供的待测样品的红外光谱图;
图2本发明实施例1中提供的待测样品的色谱图;
图3本发明实施例1中提供的色谱保留时间Rt=16.485min处样本的质谱图;
图4本发明实施例1中提供的待测样品红外光谱图与谱库中的Tetraethylenepentamine CP物质的匹配图;
图5本发明实施例2中提供的三乙烯四胺标准品的色谱图;
图6本发明实施例2中提供的色谱保留时间Rt=16.485min处三乙烯四胺标准品的质谱图。
具体实施方式
下面将结合实施例对本发明的实施方案进行详细描述,但是本领域技术人员将会理解,下列实施例仅用于说明本发明,而不应视为限制本发明的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购买获得的常规产品。
本发明各实施例中采用的设备和试剂如下:
气相色谱-质谱联用仪型号为岛津GC-MS QP 2010 Plus;
傅立叶红外分光光度计的型号为WQF-510A FTIR;
标准品为GCS 5ml,纯度>99.5%。
实施例1
本实施例为一种液态待测样品中三乙烯四胺的分离鉴定方法,包括如下步骤:
一、采用傅立叶红外分光光度计对上述待测样品进行检测得到光谱图;
傅里叶红外分光光度计对待测样品的检测方法具体为:
(1)先将无待测样品的溴化钾镜片插在样品架上进行本底测试;
(2)再将待测样品在溴化钾镜片上涂抹一薄层,随后,将涂抹待测样品的溴化钾镜片插在样品架上,并将盖盖上,采用傅立叶红外分光光度计采集透过率光谱;
(3)将步骤(2)中得到的光谱减去步骤(1)得到的光谱得到待测样品的红外光谱图(如图1所示)。
二、按照气相色谱-质谱联用仪条件,对待测样品进行分离检测,得到色谱图和质谱图;
气相色谱-质谱联用仪对待测样品的检测方法具体为:将待测样品采用乙醇稀释500倍后进样,进样量为1.0μL;气象色谱条件:色谱柱为DB-5MS;色谱柱的柱长为30m、内径为0.25mm、液膜厚度为0.25um;柱温为50℃保持1min,以10℃/min升至100℃保持7min,以30℃/min升至310℃保持5min;载气为氦气;载气流速为1.0ml/min;压力为53.5Kpa;分流动比100:1;
质谱条件为:离子源温度为260℃;接口温度为280℃;检测器电压为0.7KV;质量扫描范围为m/z=50-500;采集方式为SCAN;
按照上述气相色谱条件得到待测样品的色谱图(如图2所示),并分离得到保留时间Rt=16.485min处的样本;按照上述质谱条件得到保留时间Rt=16.485min处的样本的质谱图(如图3所示);
将得到的红外光谱图在谱库中解析,并与谱库中的物质进行匹配(如图4所示),匹配结果如表1所示:
表1
再根据质谱图中碎片离子与气相色谱-质谱联用仪的谱库中进行匹配,匹配结果如表2所示:
表2
由表1、表2可知,本实施例液态待测样品中含有三乙烯四胺;通过傅立叶红外分光光度计和气相色谱-质谱联用仪能够快速准确鉴定该待测样品中是否含有三乙烯四胺;并且通过两者结合提高了鉴定的可靠性,避免假阳性的出现。
实施例2
本实施例为一种样品中三乙烯四胺含量的检测方法,具体包括:
采用实施例1的方法对上述样品进行检测,得到色谱图和质谱图;
按照实施例1中的气相色谱-质谱联用仪的条件对标准品(三乙烯四胺)进行检测得到三乙烯四胺标准品的色谱图(如图5所示)和保留时间Rt=16.485min处样本的质谱图(如图6所示),通过上述方法得到不同浓度标准品(三乙烯四胺)特征离子M/Z=44的标准曲线;
再将样品中得到的特征离子M/Z=44代入标准曲线得到样品中三乙烯四胺的含量。
最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,但本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (10)
1.一种三乙烯四胺的分离鉴定方法,其特征在于,包括如下步骤:
采用红外分光光度计对样品进行检测得到光谱图;
采用气相色谱-质谱联用仪对所述样品进行分离检测,得到色谱图和质谱图;
根据所述质谱图和光谱图确定所述样品中的三乙烯四胺。
2.根据权利要求1所述的分离鉴定方法,其特征在于,所述分离鉴定方法还包括采用外标法对三乙烯四胺进行定量。
3.根据权利要求1或2所述的分离鉴定方法,其特征在于,所述气相色谱采用的色谱柱为DB-5MS,所述色谱柱的柱长为15-30m、内径为0.1-0.25mm、液膜厚度为0.1-0.25um。
4.根据权利要求3所述的分离鉴定方法,其特征在于,所述色谱柱的柱长为30m、内径为0.25mm、液膜厚度为0.25um。
5.根据权利要求1或2所述的分离鉴定方法,其特征在于,所述气相色谱中柱温为50℃保持1min,以10℃/min升至100℃保持7min,以30℃/min升至310℃保持5min。
6.根据权利要求1或2所述的分离鉴定方法,其特征在于,所述气相色谱的载气为氦气;载气流速为0.8-1.2ml/min;进样口温度为140-160℃;压力为53-55Kpa;分流动比(90-110):1。
7.根据权利要求6所述的分离鉴定方法,其特征在于,载气流速为1.0ml/min;压力为53.5Kpa;分流动比100:1。
8.根据权利要求1或2所述的分离鉴定方法,其特征在于,所述质谱中离子源温度为250-280℃;接口温度为260-300℃;检测器电压为0.6-0.8KV;质量扫描范围为m/z=50-500;采集方式为SCAN。
9.根据权利要求8所述的分离鉴定方法,其特征在于,所述质谱中离子源温度为260℃;接口温度为280℃;检测器电压为0.7KV。
10.根据权利要求1或2所述的分离鉴定方法,其特征在于,所述红外分光光度计为傅立叶红外分光光度计。
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