CN107764617B - Digestion method for determining organic selenium in plants - Google Patents
Digestion method for determining organic selenium in plants Download PDFInfo
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- CN107764617B CN107764617B CN201711269000.1A CN201711269000A CN107764617B CN 107764617 B CN107764617 B CN 107764617B CN 201711269000 A CN201711269000 A CN 201711269000A CN 107764617 B CN107764617 B CN 107764617B
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 74
- 239000011669 selenium Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000029087 digestion Effects 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 61
- 238000001035 drying Methods 0.000 claims abstract description 24
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 22
- 238000002791 soaking Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000001546 nitrifying effect Effects 0.000 claims abstract description 10
- 239000012154 double-distilled water Substances 0.000 claims abstract description 9
- 238000010000 carbonizing Methods 0.000 claims abstract description 8
- 239000000779 smoke Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000004042 decolorization Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims 1
- 239000012085 test solution Substances 0.000 claims 1
- 238000003763 carbonization Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000004380 ashing Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to the technical field of organic selenium determination, and particularly discloses a digestion method for determining organic selenium in plants. Adding dried plant powder to be detected into double distilled water, soaking for 1-1.5 days, changing water every 8-10 h during soaking, removing inorganic selenium dissolved in water in the dried powder, drying the powder after soaking, and carbonizing until no smoke emerges to obtain carbonized powder; and (3) adding concentrated nitric acid to nitrify the carbonized powder, wherein the nitrifying temperature is 40-65 ℃, and the nitrifying time is 24-72 hours, so that all organic selenium is converted into inorganic selenium. The method adopts a digestion mode of carbonization and oxidation to convert all the organic selenium in the plants into inorganic selenium, thereby accurately and reliably measuring the organic selenium in the plants.
Description
Technical Field
The invention belongs to the technical field of organic selenium determination, and particularly relates to a digestion method for determining organic selenium in plants.
Background
The selenium in the plant is determined by oxidizing the organic selenium in the plant into inorganic selenium and determining the content of the selenium in the plant after constant volume. The conventional method for determining organic selenium comprises the following steps: drying plants, crushing, drying to constant weight, weighing, digesting (concentrated nitric acid, perchloric acid, concentrated ammonia water or microwave-assisted digesting), evaporating (removing acid), metering volume and measuring. Among them, the digestion of plants is generally performed by the following methods: oxidizing organic selenium in plants into inorganic selenium by using nitric acid, perchlorate and concentrated ammonia water or microwave auxiliary, nitric acid and ammonia water, and then fixing the volume for subsequent process measurement. However, tests prove that: because the organic selenium is connected with the plants in an organic chain mode, the organic selenium in the plants cannot be completely oxidized and dissolved out by ordinary digestion or microwave-assisted digestion, the plant powder is still the plant powder without being completely digested and dissolved, and the method cannot completely convert the organic selenium in the plants into inorganic selenium and cannot completely digest the plants. Therefore, the conventional determination method cannot achieve the purpose of accurately determining the organic selenium in the plants.
In order to solve the problem that organic selenium in plants cannot be completely digested, a concentrated sulfuric acid nitration method and a high-temperature (500-600 ℃) ashing method are adopted, because selenium oxide is sublimated at 309 ℃, the boiling point of concentrated sulfuric acid is 330.8 ℃, the boiling point exceeds the sublimation temperature of selenium oxide when concentrated sulfuric acid is nitrated, and selenium oxide is sublimated when being digested. The ashing method is carried out at a temperature higher than the sublimation point of selenium oxide, so that the two methods can influence the accurate determination of the organic selenium in the subsequent plants.
Disclosure of Invention
The invention aims to solve the technical problem of providing a digestion method for determining organic selenium in plants, which adopts a digestion mode of carbonization and oxidation to convert all the organic selenium in the plants into inorganic selenium, so that the subsequent determination of the organic selenium in the plants is more accurate and reliable.
In order to solve the technical problems, the invention adopts the technical scheme that: the digestion method for measuring the organic selenium in the plants specifically comprises the following steps:
(1) drying the plant to be detected, crushing the plant to be detected into powder, and continuously drying the powder to constant weight to obtain dry powder;
(2) adding the dried powder into double distilled water, soaking for 1-1.5 days, changing water every 8-10 h during soaking, removing inorganic selenium dissolved in water in the dried powder, drying the powder after soaking, and carbonizing until no smoke is emitted to obtain carbonized powder;
(3) after the step (2) is finished, adding concentrated nitric acid to nitrify the carbonized powder, wherein the nitrifying temperature is 40-65 ℃, and the nitrifying time is 24-72 hours;
(4) and (4) after the nitrification in the step (3) is finished, completely converting organic selenium into inorganic selenium, adding activated carbon for decolorization, performing suction filtration, distilling to remove concentrated nitric acid until the volume of the solution is 2-3 mL, and determining the selenium content after constant volume.
Wherein, the digestion method for measuring the organic selenium in the plants comprises the step (1) of drying at the temperature of 100-105 ℃.
The digestion method for determining the organic selenium in the plants comprises the step (2) that the mass ratio of the dry powder to the double distilled water is 1: 20-40.
Wherein, the digestion method for measuring the organic selenium in the plants comprises the step (2) of carbonizing at the temperature of 250-300 ℃.
The digestion method for determining the organic selenium in the plants comprises the step (3) that the mass-volume ratio of the carbonized powder to the concentrated nitric acid is 1: 4-6 g/mL.
Compared with the prior art, the invention has the beneficial effects that: the method adopts a digestion mode of carbonization and nitric acid oxidation to convert all organic selenium in plants into inorganic selenium; and before carbonization, the dry powder to be detected is soaked to remove the interference of inorganic selenium in the sample to be detected. The method can ensure that the subsequent determination of the organic selenium in the plants is more accurate and reliable.
Detailed Description
The invention provides a digestion method for determining organic selenium in plants, which specifically comprises the following steps:
(1) drying the plant to be detected, crushing the plant to be detected into powder, and continuously drying the powder to constant weight to obtain dry powder;
(2) adding the dried powder into double distilled water according to the mass ratio of 1: 20-40, soaking for 1-1.5 days, changing water every 8-10 h during soaking, removing inorganic selenium dissolved in water in the dried powder, drying the powder after soaking, and carbonizing at 250-300 ℃ until no smoke emerges, so as to obtain carbonized powder;
(3) after the step (2) is finished, adding concentrated nitric acid to nitrify the carbonized powder, wherein the mass-volume ratio of the carbonized powder to the concentrated nitric acid is 1: 4-6 g/mL, the nitrifying temperature is 40-65 ℃, and the nitrifying time is 24-72 hours;
(4) and (4) after the nitrification in the step (3) is finished, completely converting organic selenium into inorganic selenium, adding activated carbon for decolorization, performing suction filtration, distilling to remove concentrated nitric acid until the volume of the solution is 2-3 mL, and determining the selenium content after constant volume.
Wherein, the digestion method for measuring the organic selenium in the plants comprises the step (1) of drying at the temperature of 100-105 ℃.
The invention is further illustrated and described with reference to specific examples, which do not limit the scope of the invention.
Example 1
The digestion method for measuring the organic selenium in the plants specifically comprises the following steps:
(1) drying selenium-containing plant to be tested at 105 deg.C, pulverizing into powder, and continuously drying to constant weight to obtain dry powder;
(2) adding the dried powder into double distilled water according to the mass ratio of 1:20, soaking for 1 day, changing water every 8h during soaking, removing inorganic selenium dissolved in water in the dried powder, drying the powder after soaking, and carbonizing at 250 ℃ until no smoke emerges to obtain carbonized powder;
(3) after the step (2) is finished, adding concentrated nitric acid to nitrify the carbonized powder, wherein the mass-volume ratio of the carbonized powder to the concentrated nitric acid is 1:5g/mL, the nitrification temperature is 40 ℃, and the nitrification time is 72 hours;
(4) and (4) after the nitrification in the step (3) is finished, completely converting organic selenium into inorganic selenium, adding activated carbon for decolorization, performing suction filtration, distilling to remove concentrated nitric acid until the volume of the solution is 2mL, and determining the selenium content after constant volume.
Example 2
The digestion method for measuring the organic selenium in the plants specifically comprises the following steps:
(1) drying selenium-containing plant to be tested at 100 deg.C, pulverizing into powder, and continuously drying to constant weight to obtain dry powder;
(2) adding the dried powder into double distilled water according to the mass ratio of 1:30, soaking for 1.5 days, changing water every 10h during the soaking period, removing inorganic selenium dissolved in water in the dried powder, drying the powder after the soaking is finished, and carbonizing at 300 ℃ until no smoke emerges to obtain carbonized powder;
(3) after the step (2) is finished, adding concentrated nitric acid to nitrify the carbonized powder, wherein the mass-volume ratio of the carbonized powder to the concentrated nitric acid is 1:6g/mL, the nitrifying temperature is 55 ℃, and the nitrifying time is 50 hours;
(4) and (4) after the nitrification in the step (3) is finished, completely converting organic selenium into inorganic selenium, adding activated carbon for decolorization, performing suction filtration, distilling to remove concentrated nitric acid until the volume of the solution is 2mL, and determining the selenium content after constant volume.
Example 3
The digestion method for measuring the organic selenium in the plants specifically comprises the following steps:
(1) drying selenium-containing plant to be tested at 105 deg.C, pulverizing into powder, and continuously drying to constant weight to obtain dry powder;
(2) adding the dried powder into double distilled water according to the mass ratio of 1:40, soaking for 1 day, changing water every 8h during the soaking period, removing inorganic selenium dissolved in water in the dried powder, drying the powder after the soaking is finished, and carbonizing at 280 ℃ until no smoke emerges to obtain carbonized powder;
(3) after the step (2) is finished, adding concentrated nitric acid to nitrify the carbonized powder, wherein the mass-volume ratio of the carbonized powder to the concentrated nitric acid is 1:5g/mL, the nitrification temperature is 65 ℃, and the nitrification time is 30 hours;
(4) and (4) after the nitrification in the step (3) is finished, completely converting organic selenium into inorganic selenium, adding activated carbon for decolorization, performing suction filtration, distilling to remove concentrated nitric acid until the volume of the solution is 3mL, and determining the selenium content after constant volume.
The foregoing is a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various changes and modifications without departing from the spirit of the present invention, and these should be construed as the scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicability of the present invention.
Claims (3)
1. A digestion method for measuring organic selenium in plants is characterized by comprising the following steps:
(1) drying the plant to be detected, crushing the plant into powder, and continuously drying the powder to constant weight to obtain dry powder;
(2) adding the dried powder into double distilled water, soaking for 1-1.5 days, changing water every 8-10 h during soaking, removing inorganic selenium dissolved in water in the dried powder, drying the powder after soaking, and carbonizing at the temperature of 250-300 ℃ until no smoke emerges to obtain carbonized powder;
(3) after the step (2) is finished, adding concentrated nitric acid to nitrify the carbonized powder, wherein the mass-volume ratio of the carbonized powder to the concentrated nitric acid is 1: 4-6 g/mL, the nitrifying temperature is 40-65 ℃, and the nitrifying time is 24-72 hours;
(4) and (4) after the nitrification in the step (3) is finished, completely converting organic selenium into inorganic selenium, adding activated carbon for decolorization, carrying out suction filtration, distilling to remove concentrated sulfuric acid until the volume of the solution is 2-3 mL, and measuring the selenium content after constant volume.
2. The digestion method for detecting organic selenium in plants according to claim 1, wherein the drying temperature in step (1) is 100-105 ℃.
3. The method for digesting plant-derived organic selenium in a test solution according to claim 1, wherein the mass ratio of the dry powder to the double distilled water in step (2) is 1: 20-40.
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| CN201711269000.1A CN107764617B (en) | 2017-12-05 | 2017-12-05 | Digestion method for determining organic selenium in plants |
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| CN201711269000.1A CN107764617B (en) | 2017-12-05 | 2017-12-05 | Digestion method for determining organic selenium in plants |
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| CN107764617B true CN107764617B (en) | 2020-05-08 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101419174A (en) * | 2007-10-24 | 2009-04-29 | 中国科学院沈阳应用生态研究所 | Method for detecting whole copper in soil |
| CN101458181A (en) * | 2007-12-11 | 2009-06-17 | 张可萌 | Heavy metal content rapid measuring method in vivo of fish and prawn |
| CN103335991A (en) * | 2013-06-19 | 2013-10-02 | 新疆师范大学 | Method for separating and detecting complicated mixed state arsenic in coal |
| CN105044078A (en) * | 2015-05-25 | 2015-11-11 | 中华人民共和国东莞出入境检验检疫局 | Method for determining lead, cadmium, chromium and mercury in plastic through EDTA-2Na complexation digestion |
| CN106324075A (en) * | 2016-10-20 | 2017-01-11 | 黄河三角洲京博化工研究院有限公司 | Method for determining content of organic selenium in selenium-rich vegetables by virtue of inductively coupled plasma mass-spectrometry |
-
2017
- 2017-12-05 CN CN201711269000.1A patent/CN107764617B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101419174A (en) * | 2007-10-24 | 2009-04-29 | 中国科学院沈阳应用生态研究所 | Method for detecting whole copper in soil |
| CN101458181A (en) * | 2007-12-11 | 2009-06-17 | 张可萌 | Heavy metal content rapid measuring method in vivo of fish and prawn |
| CN103335991A (en) * | 2013-06-19 | 2013-10-02 | 新疆师范大学 | Method for separating and detecting complicated mixed state arsenic in coal |
| CN105044078A (en) * | 2015-05-25 | 2015-11-11 | 中华人民共和国东莞出入境检验检疫局 | Method for determining lead, cadmium, chromium and mercury in plastic through EDTA-2Na complexation digestion |
| CN106324075A (en) * | 2016-10-20 | 2017-01-11 | 黄河三角洲京博化工研究院有限公司 | Method for determining content of organic selenium in selenium-rich vegetables by virtue of inductively coupled plasma mass-spectrometry |
Non-Patent Citations (1)
| Title |
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| 食品中无机砷和有机砷的分离和测定;金阳，李薇雅;《食品工业科技》;20031231;第92-93页 * |
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