Digestion method
A digestion solution and sample technology, applied in sampling, measuring devices, instruments, etc., can solve the problems of low recovery rate of low-temperature elements, environmental pollution, and high background value, and achieve the effect of protecting the environment, improving experimental efficiency, and avoiding excess.
Inactive Publication Date: 2017-06-13
朱山
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Problems solved by technology
Dry ashing is facing elimination in trace and ultra-trace analysis due to the low recovery rate and high background value of some low-temperature elements; both wet digestion and microwave digestion require a long time for pre-digestion and acid removal (Volatilize excess acid by heating) process, the efficiency is very low; nitrogen oxides and acid gas generated in the digestion and acid removal process are discharged into the air, which will also cause environmental pollution
Method used
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Embodiment 1
[0021] Sample source: Standard Material for Analysis of Lead, Chromium and Cadmium in Wheat Flour (GBW10035).
[0022] 1. Pretreatment: Accurately weigh 5 samples (about 2g each) into glass conical flasks, heat on a heating plate to 140°C, and add concentrated nitric acid (65%) continuously at a rate of 0.3mL / min; After 40 minutes, the large yellow foam decreased significantly. Raise the temperature of the electric heating plate to 200°C, and adjust the adding rate of concentrated nitric acid to 0.8mL / min; Remove the bottle from the heating plate, cool it to room temperature, transfer it to a 25mL colorimetric tube with deionized water, dilute to volume, and shake well to obtain the sample treatment solution. At the same time, make a reagent blank.
[0023] 2. Determination: Measure the concentration of lead, chromium and cadmium in the reagent blank and sample treatment solution by ICP-MS, calculate the content of lead, chromium and cadmium in the sample, and compare with th...
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The invention relates to the field of pretreatment of metal element analysis, in particular to a sample digestion method. The method comprises the following steps: step I, weighing and putting a to-be-digested sample into a container, and heating the to-be-digested sample in heating equipment; step II, after the temperature of the sample in the step I is stable, slowly adding a digestion solution; step III, after the sample in the step I does not fiercely react, rising a digestion temperature and increasing adding speed of the digestion solution; and step IV, after the sample in the step I is completely digested, stopping heating, stopping adding the digestion solution, transferring and keeping volume constant after cooling, thereby completing digestion. The digestion method can greatly improve working efficiency, and reduces environmental pollution.
Description
technical field [0001] The invention relates to the field of pretreatment of metal element analysis, especially the sample digestion method. Background technique [0002] In samples, metal elements are often combined with organic substances such as proteins, carbohydrates, and lipids, or mixed with other inorganic components, and need to be converted into ions in solution through pretreatment for analysis. [0003] At present, the commonly used pretreatment technologies mainly include dry ashing, wet digestion, and microwave digestion. Dry ashing is facing elimination in trace and ultra-trace analysis due to the low recovery rate and high background value of some low-temperature elements; both wet digestion and microwave digestion require a long time for pre-digestion and acid removal (Volatilization of excess acid by heating) process, the efficiency is very low; the discharge of nitrogen oxides and acid gas produced in the process of digestion and acid removal into the air...
Claims
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IPC IPC(8): G01N1/40
CPCG01N1/4044
Inventor 朱山卢蕊曾庆真
Owner 朱山