Method for determining contents of heavy metals in sample

A determination method and technology for heavy metals, applied in the field of agricultural analytical chemistry, can solve the problems of excessive liquid foaming, incomplete sample digestion, affecting the accuracy of heavy metal detection data, etc., to simplify pretreatment steps, reduce detection costs, and improve detection efficiency. Effect

Active Publication Date: 2013-01-09
BEIJING ACADEMY OF AGRICULTURE & FORESTRY SCIENCES
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The aqua regia digestion method used in GB / T 23349-2009 and GB18877-2002 currently has many disadvantages in the process of use, such as excessive liquid foaming during digestion, incomplete digestion of samples, etc., which greatly affects the accuracy of heavy metal detection data in fertilizers. Accuracy, needs to be improved

Method used

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  • Method for determining contents of heavy metals in sample
  • Method for determining contents of heavy metals in sample
  • Method for determining contents of heavy metals in sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, the determination of the recovery rate of heavy metals in organic fertilizers

[0024] 1.1 Preparation of blank solution

[0025] Except that no sample is added, other steps are the same as step 1.3.

[0026] 1.2 Sample spiking

[0027] The laboratory selects organic fertilizers, weighs 2 parallel samples of each fertilizer, and adds chromium, cadmium, lead, mercury, and arsenic mixed standard solutions to one of them for determination, so as to obtain the recovery rate of heavy metal elements.

[0028] 1.3 Preparation of sample digestion solution

[0029] Weigh 4.0g of organic fertilizer sample, put it into a 400mL tall beaker, add 90mLHNO into the beaker in a fume hood 3 , 30mL HCl and 2mL HClO 4 , cover with a watch glass, shake the beaker slightly, and let stand for 12 hours. Put the beaker on the electric heating plate and heat it at 140°C for 4 hours, then raise the temperature of the electric heating plate to 170°C and continue heating. When th...

Embodiment 2

[0035] Embodiment 2, detection of heavy metals in contaminated soil reference material

[0036] The standard material of GBW08303 polluted farmland soil was selected to evaluate the accuracy of the method.

[0037] 2.1 Preparation of sample digestion solution

[0038] Weigh 2.0g of standard substance sample of GBW08303 polluted farmland soil, put it into a 400mL tall beaker, add 90mL HNO into the beaker in a fume hood 3 , 30mL HCl and 2mL HClO 4 , cover the watch glass, shake the beaker gently, and let it stand for 24 hours; put the beaker on the electric heating plate, first heat it at 140°C for 4 hours, then raise the temperature of the electric heating plate to 170°C and continue heating until the digestion solution is reduced When reaching 30% of the original volume, add 27mLHNO to the beaker 3 and 9mL HCl, continue heating until about 5mL of the digestion solution remains, slightly remove the watch glass and continue heating until the solution evaporates to almost dryn...

Embodiment 3

[0044] Embodiment 3, detection of heavy metals in spinach standard substance

[0045] GBW10015 spinach reference material was selected to evaluate the accuracy of the method.

[0046] 3.1 Preparation of sample digestion solution

[0047] Weigh 8.0g of GBW10015 spinach standard substance sample, put it into a 400mL tall beaker, add 90mL HNO into the beaker in a fume hood 3 , 30mL HCl and 2mL HClO 4 , cover the watch glass, shake the beaker gently, and let it stand for 12 hours; put the beaker on the electric heating plate, first heat it at a constant temperature of 140°C for 4 hours, then raise the temperature of the electric heating plate to 170°C and continue heating until the digestion solution is reduced When reaching 30% of the original volume, add 9mL HNO to the beaker 3 and 3mL HCl, continue to heat until about 5mL of the digestion solution remains, slightly remove the watch glass and continue heating until the solution evaporates to almost dryness to drive off the ni...

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Abstract

The invention discloses a method for determining the contents of heavy metals in a sample. The method comprises the steps that (1) a sample to be measured which is an organic fertilizer, an organic-inorganic mixed fertilizer, plant, soil or mud is immersed in a digestion solution a which is a mixed solution of HNO3, HCl an HClO4, and then is heated to 20-30 percent of the original volume, wherein the heavy metals include chromium, cadmium, lead, mercury and arsenic; (2) a digestion solution b which is a mixed solution of HNO3 and HCl is added into the digestion solution a till the volume of the digestion solution a is 50-100 percent of the original volume; and (3) the mixed solution treated by the second step is continuously heated till the solution is dried; and the hydrochloric acid solution is continuously added, then is made up to volume with water and subsequently measured to obtain the contents of the heavy metals in the sample to be measured. With the method, the problems during detecting fertilizers that the fore treatment methods are complicated, the digestion solutions for determining various elements are different and the like are better solved; the fore treatment steps are greatly simplified, the detection efficiency is improved, and the detection cost is reduced; and the method is worthy of popularization.

Description

technical field [0001] The invention relates to a method for determining heavy metals in samples, belonging to the field of agricultural analytical chemistry. Background technique [0002] At present, there are many fertilizer-related standards in my country. The more detailed national standards for the detection of heavy metals (cadmium, chromium, lead, mercury, and arsenic) in fertilizers are the ecological indicators of arsenic, cadmium, lead, chromium, and mercury in fertilizers (GB / T 23349-2009) and organic-inorganic compound fertilizer (GB18877-2002), in which the pretreatment of samples is relatively similar, both using aqua regia (HNO 3 :HCl=1:3) digestion. In the limit and content determination of mercury, arsenic, cadmium, lead, and chromium in water-soluble fertilizers (NY 1110-2006), the pretreatment methods of mercury, arsenic, and other three heavy metal elements cadmium, lead, and chromium are distinguished, and different pretreatment methods are used. method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/44
Inventor 刘善江田野孙昊马良
Owner BEIJING ACADEMY OF AGRICULTURE & FORESTRY SCIENCES
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