主题：【资料】 植物和动物组织消解处理过程---样品消解资料之一

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DESTRUCTION OF ORGANIC MATTER IN PLANT AND ANIMAL TISSUE WITH PERCHLORIC ACID-NITRIC ACID MIXTURES

Publication:  Handbook of  INDUCTIVELY COUPLED PLASMA SPECTROMETRY
Authors: M. Thompson and J N Walsh
Field:  Biology, Animal, Agriculture, plant


Reagents

(i)    Nitric acid, ~ 70 % m/m
(ii)    Perchloric acid  ~ 60 % m/m.
(iii)    Hydrochloric acid ( 6 M). Dilute hydrochloric acid ( 36 % m/m, 534 ml) to 1l.
(iv)    Calibration blank – hydrochloric acid ( 1 M).

Procedure

(i)    Weigh each sample (2.00 g, dried at 105 °C and ground *) into a clean, dry, numbered conical flask.
(ii)    Add nitric acid (40 ml) to each flask, cover with a watch glass, and set aside in the fume cupboard
Overnight.
(iii)           Place the flask on the hotplate and warm gently until frothing ceases and the solutions are almost clear. The nitric acid should be boiling gently ( but without major loss of volume) at the end of this stage.
(iv)    Allow the flasks to cool, and check that there are no fat globules floating in the liquid.
(v)    Add perchloric acid ( 3 ml), replace the flasks on the hotplace without cover glasses, and very gently heat until the contents have just reached dryness. Do not overheat.
(vi)    Allow the flasks to cool, and add water (2-3 ml) and hydrochloric acid (2.0 ml, 6 M) to each. Warm to dissolve the residues.
(vii)    Transfer the cooled solutions either to graduated test-tubes or to graduated flasks, and dilute to volume with water.

* Samples which are difficult to dry by heating (e.g soft fruits) can be freeze-dried, or homogenized and weighed wet. Moisture content can be determined separately.





















植物和动物组织使用高氯酸和硝酸混合物消解

发表:  ICP 手册
作者: M. Thompson and J N Walsh
应用领域:  生物学，动物学，农业，植物研究


试剂：

1.    70 % m/m 硝酸
2.    60 %  m/m 高氯酸
3.    稀释盐酸36% m/m 534ml 至 1 L
4.    标准空白 盐酸（1M）

过程：

1.    每个样品称重（2.00g ,在105 °C 下干燥并研碎 *）置于干净、干燥、带刻度的几个锥形烧瓶中
2.    在每个瓶中添加硝酸 (40 ml), 用玻璃覆盖, 放置在通风橱内，过夜.
3.    将烧瓶放置在电炉加热盘上，缓慢加热至起泡并溶液几乎是清亮的. 在本步骤最后硝酸应该缓慢沸腾（但主要体积没有损耗）
4.    让烧瓶冷却并检查溶液中没有漂浮的脂肪球.
5.    添加高氯酸 ( 3 ml), 再次将烧瓶放置在电炉加热盘上不用盖盖，然后非常缓慢的加热至内部刚好干燥，不要过热 .
6.    让烧瓶冷却并且添加水 (2-3 ml) 和盐酸 (2.0 ml, 6 M) 到每个烧瓶. 加热并溶解瓶中的剩余物质
7.    将冷却后的溶液移到最后的试管或测试的容量瓶中，然后用水稀释定容.

* 难于加热干燥的样品(如软的水果)可以冷冻干燥,或者结构均匀可以称量湿重,水份可以分开测量.