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高級色譜法 2020：水環境中氯苯胺的色譜分析 - Abdullayeva Nabat- Sumgait 州立大學

Abdullayeva Nabat-蘇姆蓋特州立大學

水環境中苯胺及其氯衍生物的分析是一個複雜的過程：以低靈敏度（0.01-0.1 mg/dm3）測定微量濃度。從水中分離苯胺和氯苯胺是很困難的，這些化合物的分離方法並不完全通用。大多數液體萃取物用於苯胺及其衍生物。用於液體抽取的挖土機必須符合以下要求：

萃取苯胺的有效溶劑如下： 飽和kh

借助高效能毛細管柱和現代濃度選擇性檢測器（ECD、NPD）方法，通常可以直接根據所需的靈敏度等級（0.05 μg/dm3 和 0.5-5 μg/dm3）測定氯苯胺。

靈敏度不令人滿意的原因是氯苯胺中胺基的存在會幹擾樣品並導致各個色譜峰的侵蝕和不對稱。另一方面，NH2 基對苯胺改質具有很高的反應活性。利用這一點，胺基的去除將對苯胺的萃取濃度及其色譜測定產生同樣積極的影響。

獲得用於氣相層析測定此類化合物的氮衍生物的反應如下。它們可以分為兩種類型：纖毛和同化反應。矽質有機化合物也是極性官能基失活最通用的方法之一。使用以下試劑製備單胺和雙胺的二氧化矽衍生物。

MSTFA：N-甲基-N（三甲基）-三氟乙醯胺

BSTFA：N,O-雙（三甲基）-三氟乙醯胺

Trimethylchlorosilane (TMCS) or trimethylillyl-imidazole (TMSIM) is used as the catalyst. Trimethylsilyl chloride, also known as chlorotrimethylsilane. It is an unstable fluid that is steady without water. It is generally utilized in natural science. 1-(Trimethylsilyl)imidazole (TMSI) was utilized for derivatization of sugars into trimethylsilyl ethers. It was additionally used to integrate polysubstituted chiral spirotetrahydropyrans and as silylating reagent for the assurance of hydroxyl bunches within the sight of amine functionalities.

Silylating reagent for the protection of hydroxyl groups in the presence of amine functionalities It should be noted that the activity of different classes of organic compounds in cilia reactions varies and decreases as follows: alcohols> phenols> carboxylic acids> single amines> double amines> amides.

The reaction is carried out only between organic solvents, because both reagents and reaction products are easily hydrolyzed even in small amounts of water. It has been found that tetrabutyldimethylylyl derivatives (TBDMS) are more resistant to hydrolysis than trimethylcyl derivatives (TMS), and that MTBSTFA, which is reactive for their preparation, can be stored for a long time. Another problem with silage is the replacement of both H atoms with a mixture of mono and di-TMS derivatives. MTBSTFA also has advantages here, as di-TBDMS derivatives are practically not formed due to steric barriers created by mass TBDMS groups.

Oxidation reactions are more efficient than cilification because some derivatives show hydrolytic and thermal resistance to N-silicon derivatives, respectively, and this requires more stringent conditions for gas chromatographic analysis. The acidification reactions are carried out in organic solvents, using pridine, trimethyl or triethylamine as catalysts and solvents for by-products.

Although acetyl amine products are more resistant to hydrolysis than sillic derivatives, acidification occurs after extraction in the liquid and solid phases. The combination of acidification with solid-phase extraction to increase the rate of removal of amines from water is described using various reagents. Derivatives of anhydrides and acylides containing F and Cl atoms significantly increase the sensitivity of their determination when using ECD or GC in the chemical ionization mode with the combination of ions.  In this case, the detection sensitivity of DEZ increases in the order F

氣相層析 (GC) 是診斷科學中使用的典型色譜，用於分離和剖析可分解而不腐爛的強化物。 GC 的常規應用包括測試特定物質的純淨度，或分離混合物的各個部分（同樣可以解析這些部分的總體測量）。在某些情況下，GC 可能有助於區分化合物。在製備色譜中，GC 可用於從混合物中規劃出純混合物。在任何情況下，多鹵化試劑（PFPA、HFBA、TCA-Cl、HFB-Cl、HFB-Cl）。與 ECD 一起使用需要排除過量的試劑和結果（多鹵碳酸）。因為這些混合物會幹擾氣相層析的研究。