В предыдущей части мы кратко рассмотрели испытательное оборудование, которое применяют в лабораториях органического синтеза. В этой статье речь пойдет о хроматографическом оборудовании. Мы не будем перечислять всевозможные виды хроматографии, речь пойдёт о приборах, которые используются в синтетических лабораториях.
Итак, начнём.
1. Газовая хроматография, или сокращенно ГХ. Принцип – сорбция/десорбция из газовой фазы. Чем более летучее вещество, тем скорее оно пройдёт путь через колонку и выйдет в детектор. Детектором может быть любой прибор, который даёт количественный отклик на изменения состава газовой фазы.
Самые ходовые из детекторов:
- Пламенно-ионизационный. Достоинства: хороший диапазон линейности, дешевый, простой в использовании. Недостатки: отсутствие селективности.
- Катарометрический. Измеряет теплопроводность. Достоинства: дешевый, простой. Недостатки: низкая чувствительность, неселективен.
- Детектор электронного захвата. Принцип работы – равновесная ионизация образца свободными электронами. Достоинства: большая чувствительность и линейность. Недостатки: сложный, не универсальный.
-Масс-спектрометрический. Достоинства: высокая чувствительность, предоставление информации о молекулярной массе, строении вещества. Недостатки: дорогой, невысокий диапазон линейности, необходима особая квалификация.
ГХ чаще всего является аналитическим методом. Применяется для исследования каталитических процессов, для изучения кинетики реакций, определяем состав и примеси в растворителях. Газовый хроматограф удобен для потокового анализа и HTS.
По цене сориентировать сложно, так как цены очень разнятся. Например, ГХ с ПИД и катарометром можно купить около 1 миллиона. С МС-детектором – раза в два дороже. Разброс цен будет зависеть от многих факторов.
2. Высокоэффективная жидкостная хроматография, ВЭЖХ. Принцип разделения – сорбция/реабсорбция из жидкого состояния в твердое. Главное отличие от других жидкостных хоматографов – высокое давление в магистрали. Детекторов в ВЭЖХ тоже достаточно. Рассмотрим некоторые из них:
- Фотометрический детектор. Представляет из себя маленький и сильно упрощенный проточный сепктрофотометр. Плюсы - дешевизна, универсальность, линейность. Минусы - относительно невысокая чувствительность, видит не всё. Требования к элюенту - чтобы не поглощал на измеряемой длине волны. Один из самых популярных детекторов для ВЭЖХ.
- Флуориметрический детектор. Тоже небольшой, упрощенный спектрофлуориметр. Плюсы - чувствительность. Минусы - многое не видит, на интенсивность люминесценции может влиять куча факторов вплоть до микропримесей.
- Рефрактометрический детектор. Отслеживает изменение показателя преломления. Плюсы - дешевизна, универсальность. Минусы - очень низкая чувствительность, особенно если вещество не содержит тяжелых атомов.
- Масс-спектрометрический детектор. Плюсы - видит почти всё, высокая чувствительность, дает информацию о составе и даже строении. Обычно по стоимостит подобные детекторы стоят намного больше самого хроматографа.
Стоимость ВЭЖХ так же, как и ГХ очень сильно разнится. В зависимости от комплектации, состояния (новое оборудование или бывшее в употреблении), за прибор можно отдать от нескольких сотен тысяч до нескольких миллионов.
3. Колоночная хроматография низкого давления. Принцип разделения тот же, что и у ВЭЖХ, но давление ниже.
В целом, схема работы похожа на ВЭЖХ, но с некоторыми различиями: - Низкие давления. Фитинги из полипропилена и фторопласта. - Колонки не термостатируют.
- Высокая производительность насоса.
- Ввод образца не через Rheodyne, а шприцом прямо в колонку. Ещё включена опция сухого нанесения.
В среднем стоимость подобного прибора от 1 до 5 миллионов рублей (если состояние прибора отличное). Но есть и высокопроизводительные системы, которые могут достигать по стоимости и 10 миллионов.
Итак, в данной статье мы рассмотрели приборы, необходимые для органического синтеза. По цене они обойдутся лабораториям в достаточно большую сумму, однако, при желании, можно сэкономить и приобрести не новое оборудование, а поддержанное. Среди Б/У приборов можно найти в отличном состоянии, при этом сэкономить. В дальнейшем будем рассматривать дорогие и объемные приборы (в основном спектрометрия), а также поговорим о стекле для органического синтеза. В этих темах составим более точную смету.
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