CN107941976B - 一种2-甲氧基环己胺的含量测定方法 - Google Patents

一种2-甲氧基环己胺的含量测定方法 Download PDF

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CN107941976B
CN107941976B CN201710900841.1A CN201710900841A CN107941976B CN 107941976 B CN107941976 B CN 107941976B CN 201710900841 A CN201710900841 A CN 201710900841A CN 107941976 B CN107941976 B CN 107941976B
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methoxycyclohexyl amine
methoxycyclohexyl
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CN107941976A (zh
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段小刚
兰昭洪
方胜军
涂利根
黎晓华
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ZHEJIANG XINHUA CHEMICAL CO Ltd
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Abstract

本发明涉及通过气相色谱法测定分子化合物含量的测定方法，具体指是一种2‑甲氧基环己胺的含量测定方法。采用气相色谱法，检测条件为：载气为氢气，色谱柱的柱流量3ml/min，进样温度210‑230℃，初始柱温50‑70℃，最终温度190‑210℃，保持15分钟，检测温度230‑250℃，进样量0.8ul。本发明通过对特定测定条件的摸索，采用气相色谱法对2‑甲氧基环己胺进行含量测定，选用特定的色谱柱使2‑甲氧基环己胺和其他有机物杂质能更好的分离，方法重现性好，所测得的2‑甲氧基环己胺的含量值更加准确，精度更高。

Description

一种2-甲氧基环己胺的含量测定方法
技术领域
本发明涉及通过气相色谱法测定分子化合物含量的测定方法，具体指是一种2-甲氧基环己胺的含量测定方法。
背景技术
2-甲氧基环己胺，英文名称2-methoxycyclohexan-1-amine，分子式CH3OCH(CH2)4CHNH2,分子量129.00，是一种无色透明液体，与水混溶，溶于乙醇等大多数有机溶剂。有氨的气味。呈强碱性。相对密度(d20)0.9522。粘度低，沸点176-180℃。凝固点低于-18℃。折光率(n20D)1.4606。闪点(闭杯)64℃。可燃、有腐蚀性。2-甲氧基环己胺作为硬质聚氨酯泡沫塑料的催化剂，用途广泛。除此之外，他还可用于燃料油的稳定剂，主旨油炸形成，是150-480℃石油馏分的稳定添加剂；用于医药和农药的原料、用作杀菌剂、消毒剂、匀染剂和抗静电剂等。作为催化剂和稳定剂，如何精确测定2-甲氧基环己胺的含量就显得尤为重要。现阶段，2-甲氧基环己胺的含量测定方法目前文献还没有。
公告号为CN10169029B发明专利公开了一种通过气相色谱法进行无机磷分析的方法，具体包括：热解、分离、检测等步骤，对有机物中的无机磷进行检测分析。由于无机磷和本发明中的2-甲氧基环己胺的物理性状和化学特征具有较大不同，需要采用不同的测试步骤和测试条件。而现有技术中仅公开了分析方法中涉及的步骤以及相关的产品，不能解决可重复、准确测定2-甲氧基环己胺的含量的技术问题。
本发明通过对特定测定条件的摸索，采用气相色谱法对2-甲氧基环己胺进行含量测定，选用特定的色谱柱使2-甲氧基环己胺和其他有机物杂质能更好的分离，方法重现性好，所测得的2-甲氧基环己胺的含量值更加准确，精度更高。
发明内容
本发明提供如下的技术方案：
为解决上述技术问题，本发明的技术方案是：
一种2-甲氧基环己胺的含量测定方法，采用热导检测器进行检测，检测条件为：载气为氢气，色谱柱采用石英毛细管为材料的色谱柱，柱流量3ml/min，进样温度210-230℃，初始柱温50-70℃，采用程序升温，以6-15℃/min的速率升温，最终温度190-210℃，保持15分钟，检测温度230-250℃，进样量0.8ul。
优选的，上述2-甲氧基环己胺的含量测定方法，所述色谱柱为DB-1301石英毛细管色谱柱，长度60米，直径0.32mm，膜厚1.05um。
优选的，上述2-甲氧基环己胺的含量测定方法，所述进样温度220℃，初始柱温60℃，保持1分钟，采用程序升温，以10℃/min的速率升温，最终温度200℃，保持15分钟，检测温度250℃，进样量0.8ul。
本发明具有的优点是：
通过对特定测定条件的摸索，反复试验筛选，采用气相色谱法对2-甲氧基环己胺进行含量测定，采用毛细管柱死体积小，检测灵敏度高，选用特定的色谱柱使2-甲氧基环己胺和其他有机物杂质能更好的分离，方法重现性好，提高了测定方法的科学性，先进性，适用性，所测得的2-甲氧基环己胺的含量值精度方面更加准确，直接用于指导现场生产，将更快的指导现场生产工艺参数的调整，为生产提供准备客观的数据信息。
具体实施方式
下面结合实施例对本发明做进一步的详细说明，以下实施例是对本发明的解释而本发明并不局限于以下实施例。
实施例1
一种2-甲氧基环己胺的含量测定方法，采用气相色谱法，检测条件为：载气为氢气，色谱柱采用石英毛细管为材料的色谱柱，柱流量3ml/min，进样温度220℃，初始柱温60℃，升温至最终温度200℃，保持15分钟，检测温度250℃，进样量0.8ul。
采用气相色谱法测定2-甲氧基环己胺的含量，经过10次平行测定结果，样品1#X平均＝99.60％，相对标准偏差RSD＝0.04％,样品2#X平均＝99.62％相对标准偏差RSD＝0.04％两个样品测定结果符合规定要求。证明该测定方法“采用气相色谱法对2-甲氧基环己胺进行含量测定，选用特定的色谱柱使2-甲氧基环己胺和其他有机物杂质能更好的分离，方法重现性好，所测得的XX胺的含量值精度方面更加准确”。
实施例2
一种2-甲氧基环己胺的含量测定方法，检测条件为：载气为氢气，色谱柱采用石英毛细管为材料的色谱柱，柱流量3ml/min，进样温度210℃，初始柱温50℃，保持1分钟,采用程序升温，以10℃/min的速率升温，最终温度190℃，保持15分钟，检测温度230℃，进样量0.8ul。
实施例3
一种2-甲氧基环己胺的含量测定方法，采用热导检测器进行检测，检测条件为：载气为氢气，色谱柱采用石英毛细管为材料的色谱柱，柱流量3ml/min，进样温度215℃，初始柱温65℃，保持1分钟,采用程序升温，以15℃/min的速率升温，最终温度205℃，保持15分钟，检测温度245℃，进样量0.8ul。
实施例4
一种2-甲氧基环己胺的含量测定方法，采用热导检测器进行检测，检测条件为：载气为氢气，色谱柱采用石英毛细管为材料的色谱柱，柱流量3ml/min，进样温度215℃，初始柱温65℃，保持1分钟,采用程序升温，以10℃/min的速率升温，最终温度205℃，保持15分钟，检测温度240℃，进样量0.8ul。
实施例5
一种2-甲氧基环己胺的含量测定方法，采用热导检测器进行检测，检测条件为：载气为氢气，色谱柱采用石英毛细管为材料的色谱柱，柱流量3ml/min，进样温度230℃，初始柱温70℃，保持1分钟,采用程序升温，以6℃/min的速率升温，最终温度200℃，保持15分钟，检测温度235℃，进样量0.8ul。
实施例6
一种2-甲氧基环己胺的含量测定方法，采用热导检测器进行检测，检测条件为：载气为氢气，色谱柱采用石英毛细管为材料的色谱柱，柱流量3ml/min，进样温度230℃，初始柱温70℃，保持1分钟,采用程序升温，以10℃/min的速率升温，最终温度210℃，保持15分钟，检测温度245℃，进样量0.8ul。
上述实施例1-6所用色谱柱为DB-1301石英毛细管色谱柱，长度60米，直径0.32mm，膜厚1.05um。
上述参照实施例对该一种2-甲氧基环己胺的含量测定方法进行的详细描述，是说明性的而不是限定性的，可按照所限定范围列举出若干个实施例，因此在不脱离本发明总体构思下的变化和修改，应属本发明的保护范围之内。

Claims (3)

1.一种2-甲氧基环己胺的含量测定方法，其特征在于：采用气相色谱法，检测条件为：载气为氢气，色谱柱的柱流量3ml/min，进样温度210-230℃，初始柱温50-70℃，最终温度190-210℃，保持15分钟，检测温度230-250℃，进样量0.8ul；所用色谱柱为DB-1301石英毛细管色谱柱，长度60米，直径0.32mm，膜厚1.05um；
其中初始柱温保持1分钟，然后以6-15℃/min的速率升温至最终温度。
2.如权利要求1所述的2-甲氧基环己胺的含量测定方法，其特征在于：采用热导检测器进行检测。
3.如权利要求1所述的2-甲氧基环己胺的含量测定方法，其特征在于：所述进样温度220℃，初始柱温60℃，保持1分钟，采用程序升温，以10℃/min的速率升温，最终温度200℃，保持15分钟，检测温度250℃，进样量0.8ul。
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5051428A (en) * 1988-12-06 1991-09-24 Warner-Lambert Company 2-amino-4 or 5-methoxycyclohexyl amides useful as analgesics
CN106866431A (zh) * 2017-02-22 2017-06-20 浙江新化化工股份有限公司 一种n‑(2‑甲氧基环己基)‑1,3‑丙二胺的生产方法

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CA2873214C (en) * 2012-05-11 2021-02-16 Reset Therapeutics, Inc. Carbazole-containing sulfonamides as cryptochrome modulators

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5051428A (en) * 1988-12-06 1991-09-24 Warner-Lambert Company 2-amino-4 or 5-methoxycyclohexyl amides useful as analgesics
CN106866431A (zh) * 2017-02-22 2017-06-20 浙江新化化工股份有限公司 一种n‑(2‑甲氧基环己基)‑1,3‑丙二胺的生产方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Catalytic Hydrogenation of disubstitued benzenes and configruational isomerization of the correponding cyclohexanes 6 Configurational isomerization of substituted cyclohexylamines and cyclohexanols on Ru-Al2O3;L. Kh. Freidlin et al;《Bulletin of the Academy of Sciences of the USSR, Division of chemical science》;19790831;第28卷(第8期);1791-1795 *

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