CN110286111A - The detection method of Se content in soil - Google Patents
The detection method of Se content in soil Download PDFInfo
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- CN110286111A CN110286111A CN201910700101.2A CN201910700101A CN110286111A CN 110286111 A CN110286111 A CN 110286111A CN 201910700101 A CN201910700101 A CN 201910700101A CN 110286111 A CN110286111 A CN 110286111A
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The present invention discloses a kind of detection method of Se content in soil, includes the following steps that (1) samples: determining that the area in the sample of being acquired plot, each point sampling quantity are consistent, soil collection depth need to be consistent；(2) sample preparation: the pedotheque of acquisition is dried, and is ground up, sieved to obtain pedotheque after dry;(3) preparation of sample solution: being added nitric acid-perchloric acid mixed acid into pedotheque and cleared up, and digestion condition is 160 DEG C, and then carry out digestion solution catches up with sour processing；6 mol/L hydrochloric acid are added in pedotheque after resolution to be restored, sample solution is obtained to reducing solution constant volume；(4) blank sample and sample solution are measured respectively with fluorescence method to determine the Se content in sample solution.
Description
Technical field
The present invention relates to the technical field of Determination of Selenium in soil, the detection method of Se content in soil is referred specifically to.
Background technique
Selenium is microelement and the nutrient beneficial to plant necessary to people and animal, constitutes Selenonic protein in human body
It is the component part of glutathione peroxidase with selenoenzyme ingredient；It is that one kind has anti-oxidant, anti-aging, antitumor, guarantor
Shield and repair cell, the multi-functional life nutritional such as to improve the immunity of the human body, releases heavy metallic poison plain.Vegetable active selenium is selenium
Be combined by bioconversion and amino acid, generally in the form of selenomethionine exist, be human and animal allow using
Selenium source.
The Se content in soil is detected, is the important topic of selenium-enriched crop plantation research, currently, Selenium In Some Selenium-rich Biological Samples content
Detection method has: atomic absorption spectrography (AAS), inductively coupled plasma mass spectrometry, Neutron activation analysiss.But existing method is surveyed
Try is suddenly more, complicated for operation, and detection cycle is long, and testing result deviation is larger, and detection limit is not low enough.
Summary of the invention
Present invention seek to address that the defect of the prior art, a kind of detection method of Se content in soil is provided.
Technical scheme is as follows:
The detection method of Se content in soil, comprising the following steps:
(1) it samples: determining the area in the sample of being acquired plot, route, Mei Gedian to determine sampled point and are acquired with this
Position sampling quantity is consistent, and soil collection depth need to be consistent, can be first by re-sampling after surface layer chaff interferent or pollutant removal；
(2) sample preparation:
A. it dries: the stone adulterated in the pedotheque of acquisition, broken rubble, plant and animal residues etc. being chosen and are removed, Sheng is placed in
It in the vessel of sample, uniformly spreads out, is placed in hurricane drier, when pedotheque is in leather hard, soil sample is pulverized with mallet, is placed in
Shady and cool ground natural air drying；
B. it grinds: dry pedotheque being placed on hard plank in grinding chamber, pedotheque is pulverized with mallet, is gone
Except plant fibrous root and other impurities；All samples are all powdered hammer out, nylon mesh is crossed, unsifted larger soil particle needs anti-
It grinds and is sieved again, pass through until all, to mix well obtained pedotheque after sample sieving；
(3) preparation of sample solution:
Nitric acid-perchloric acid mixed acid is added into pedotheque to be cleared up, digestion condition is 160 DEG C, is then disappeared
Solution solution catches up with sour processing；6mol/L hydrochloric acid is added in pedotheque after resolution to be restored, sample is obtained to reducing solution constant volume
Product solution；
(4) blank sample and sample solution are measured respectively with fluorescence method, sample solution is calculated according to formula
In Se content:
In formula: m is the mass figures of selenium in the sample solution checked in from working curve, and unit is nanogram (ng)；m1For
The mass figures of selenium measured by blank test solution, unit are nanogram (ng)；v1The sample solution volumetric quantities drawn when for measurement,
Unit is milliliter (mL)；M is the numerical value of the quality of sample, and unit is gram (g)；50 be sample solution constant volume numerical value, unit
For milliliter (mL)；10-3Mass figures as unit of nanogram are scaled the mass figures conversion coefficient as unit of microgram.
The continuous mode of step (4) described sample solution is as follows: hydroxylamine hydrochloride-ethylenediamine tetra-acetic acid is added to sample solution
Two sodium solutions, it is anti-that 2, the 3- diaminonaphthalene solution that then addition density is 0.778~0.80g/mL heats 5min in boiling water bath
4,5- BaP selenium brain should be generated, after being cooled to room temperature, is extracted with hexamethylene, water layer is removed after layering, on fluophotometer
The fluorescence intensity of hexamethylene layer is measured, measurement result obtains the mass number of selenium in sample solution compared with the standard curve of drafting
Value.
The method for drafting of the standard curve is as follows: by ρ(Se)Preparation is diluted step by step for the selenium standard solution of 0.05mg/L
At ρ(Se)The standard solution of respectively 0.00 μ g/L, 1.00 μ g/L, 2.00 μ g/L, 4.00 μ g/L, 8.00 μ g/L；It is each to inhale
20.00mL, making its Se content is respectively 0.00ng, 20.00ng, 40.00ng, 80.00ng, 160.00ng, is put into 100mL tool plug
In conical flask, carried out simultaneously by sample solution determination step.
The configuration method of the hydroxylamine hydrochloride-disodium ethylene diamine tetra-acetic acid solution is as follows: it is molten to weigh 10g ethylenediamine tetra-acetic acid
In 500mL water, 25g hydroxylamine hydrochloride is added, makes it dissolve, is diluted with water to 1000mL and obtains.
The determination principle of step (1) described sampled point are as follows: 0.33hm2Below to take at 9~11 points, area is greater than 0.3hm2When,
Every increase 667m2Increase sampled point 1~2.
0.15mm~2mm is in the nylon mesh aperture used in step (2) process of lapping.
The beneficial effects of the present invention are:
1. the present invention carries out the measurement of Se content in soil using fluorescence method, hydroxylamine hydrochloride-ethylenediamine tetraacetic is added when detection
Two sodium solution of acetic acid can eliminate the interference that copper in sample liquid, iron, molybdenum and a large amount of oxidizing substances measure full selenium, make testing result
It is more acurrate.
2. the detection method of Se content of the present invention, easy to operate, accuracy is high, and detection limit is low.
Detailed description of the invention
Fig. 1 is the preparation principle figure of pedotheque of the present invention.
Specific embodiment
The present invention will be further described below with reference to the drawings.
Embodiment 1
The detection method of Se content in soil, comprising the following steps:
(1) it samples: according to the difference condition of soil, soil being divided into several sampling units, different soil types must
It must be divided into different sampling units, make the soil uniformity as far as possible of each sampling unit, with determining the sample of being acquired
The area of block to determine sampled point and acquires route with this, and each point sampling quantity is consistent, and soil collection depth needs to keep
It unanimously, can be first by re-sampling after surface layer chaff interferent or pollutant removal；The determination principle of sampled point are as follows: 0.33hm2It is below to take 9
~11 points, area is greater than 0.3hm2When, every increase 667m2Increase sampled point 1~2.
(2) sample preparation:
A. it dries: the stone adulterated in the pedotheque of acquisition, broken rubble, plant and animal residues etc. being chosen and are removed, Sheng is placed in
It in the vessel of sample, uniformly spreads out, is placed in hurricane drier, when pedotheque is in leather hard, soil sample is pulverized with mallet, is placed in
Shady and cool ground natural air drying；If being influenced by uncontrollable factors such as weather, pedotheque can also be put into drying box and be dried,
Temperature controls between 30~40 DEG C；
B. it grinds: dry pedotheque being placed on hard plank in grinding chamber, pedotheque is pulverized with mallet, is gone
Except plant fibrous root and other impurities；All samples are all powdered hammer out, cross the nylon mesh that aperture is 0.15mm~2mm, non-mistake
The larger soil particle of sieve need to grind and be sieved repeatedly, pass through until all, mix well obtained soil-like after sample sieving
Product；
The preparation process schematic diagram of pedotheque is as shown in Figure 1.
(3) preparation of sample solution:
Pedotheque 2g to be measured is weighed in 100mL conical flask, nitric acid-perchloric acid 10~15mL of mixed acid is added, covers
Small funnel, stands overnight；Next day, digestion to soil sample was in canescence on 160 DEG C of temperature automatically controlled digestings, continued digestion to Mao Bai
Removed after cigarette, in 1~2min it is slightly cold, into conical flask be added 10mL hydrochloric acid solution, be placed in boiling water bath and heat 10min, remove
Conical flask is cooled to room temperature, and digestive juice is transferred in 50mL volumetric flask with deionized water, is settled to scale, is shaken up up to sample
Solution；
(4) blank sample and sample solution are measured respectively with fluorescence method, sample solution is calculated according to formula
In Se content:
In formula: m is the mass figures of selenium in the sample solution checked in from working curve, and unit is nanogram (ng)；m1For
The mass figures of selenium measured by blank test solution, unit are nanogram (ng)；v1The sample solution volumetric quantities drawn when for measurement,
Unit is milliliter (mL)；M is the numerical value of the quality of sample, and unit is gram (g)；50 be sample solution constant volume numerical value, unit
For milliliter (mL)；10-3Mass figures as unit of nanogram are scaled the mass figures conversion coefficient as unit of microgram.
The continuous mode of the sample solution is as follows: draw 10.00~20.00mL reduction constant volume after prepare liquid in
In 100mL stuffed conical flask bottle, add 10mL hydroxylamine hydrochloride-disodium ethylene diamine tetra-acetic acid solution, mix, 2 drop cresol reds is added to indicate
Agent, solution are added dropwise ammonia spirit to there is yellow, continuously add in pink, then with hydrochloric acid solution and be adjusted to orange in pink
Yellow, that is, pH is 1.5~2.0.Following steps carry out in darkroom: adding 2mL density is the 2,3- diamino of 0.778~0.80g/mL
Naphthalene solution mixes, and sets and boils 5min reaction generation 4,5- BaP selenium brain in boiling water bath, and taking-up is cooled to room temperature；It is accurate that 5mL is added
Hexamethylene is extracted, and bottle stopper is covered, and is moved into separatory funnel solution after 10min is vibrated on vibrating machine, is abandoned after being layered
Water layer is removed, hexamethylene layer is transferred in test tube with cover, 4,5- BaP is measured at excitation wavelength 376nm, launch wavelength 525nm
The fluorescence intensity of selenium brain, looks into standard working curve, obtains the mass figures of selenium in sample solution.
The configuration method of the hydroxylamine hydrochloride-disodium ethylene diamine tetra-acetic acid solution is as follows: it is molten to weigh 10g ethylenediamine tetra-acetic acid
In 500mL water, 25g hydroxylamine hydrochloride is added, makes it dissolve, is diluted with water to 1000mL and obtains.
The method for drafting of the standard curve is as follows: by ρ(Se)Preparation is diluted step by step for the selenium standard solution of 0.05mg/L
At ρ(Se)The standard solution of respectively 0.00 μ g/L, 1.00 μ g/L, 2.00 μ g/L, 4.00 μ g/L, 8.00 μ g/L；It is each to inhale
20.00mL, making its Se content is respectively 0.00ng, 20.00ng, 40.00ng, 80.00ng, 160.00ng, is put into 100mL tool plug
In conical flask, carried out simultaneously by sample solution determination step.Use the detection limit of this method for 3ng.
The present invention carries out the measurement of Se content in soil using fluorescence method, and hydroxylamine hydrochloride-ethylenediamine tetrem is added when detection
Acid disodium solution can eliminate the interference that copper in sample liquid, iron, molybdenum and a large amount of oxidizing substances measure full selenium, make testing result more
Accurately.
The detection method of Se content of the present invention, easy to operate, accuracy is high, and detection limit is low.
Claims (6)
1. the detection method of Se content in soil, which comprises the following steps:
(1) it samples: determining the area in the sample of being acquired plot, route to determine sampled point and is acquired with this, each point is adopted
Sample amount is consistent, and soil collection depth need to be consistent, can be first by re-sampling after surface layer chaff interferent or pollutant removal；
(2) sample preparation:
A. it dries: the stone adulterated in the pedotheque of acquisition, broken rubble, plant and animal residues etc. being chosen and are removed, be placed in and contain sample
It in vessel, uniformly spreads out, is placed in hurricane drier, when pedotheque is in leather hard, soil sample is pulverized with mallet, is placed in cool place
Ground natural air drying；
B. it grinds: dry pedotheque being placed on hard plank in grinding chamber, is pulverized pedotheque with mallet, removal is planted
Object fibrous root and other impurities；All samples are all powdered hammer out, nylon mesh is crossed, unsifted larger soil particle need to be ground repeatedly
It grinds and is sieved, pass through until all, to mix well obtained pedotheque after sample sieving；
(3) preparation of sample solution:
Nitric acid-perchloric acid mixed acid is added into pedotheque to be cleared up, digestion condition is 160 DEG C, then carries out clearing up molten
Liquid catches up with sour processing；6mol/L hydrochloric acid is added in pedotheque after resolution to be restored, it is molten to obtain sample to reducing solution constant volume
Liquid；
(4) blank sample and sample solution are measured respectively with fluorescence method, are calculated in sample solution according to formula
Se content:
In formula: m is the mass figures of selenium in the sample solution checked in from working curve, and unit is nanogram (ng)；m1For blank examination
The mass figures of selenium measured by liquid, unit are nanogram (ng)；v1For the sample solution volumetric quantities drawn when measurement, unit is
Milliliter (mL)；M is the numerical value of the quality of sample, and unit is gram (g)；50 be sample solution constant volume numerical value, and unit is milliliter
(mL)；10-3Mass figures as unit of nanogram are scaled the mass figures conversion coefficient as unit of microgram.
2. the detection method of Se content in soil as described in claim 1, which is characterized in that step (4) described sample solution
Continuous mode is as follows: hydroxylamine hydrochloride-disodium ethylene diamine tetra-acetic acid solution is added to sample solution, it is 0.778 that density, which is then added,
2, the 3- diaminonaphthalene solution of~0.80g/mL heats 5min reaction in boiling water bath and generates 4,5- BaP selenium brain, is cooled to room
Wen Hou is extracted with hexamethylene, and water layer is removed after layering, and the fluorescence intensity of hexamethylene layer, measurement knot are measured on fluophotometer
Fruit obtains the mass figures of selenium in sample solution compared with the standard curve of drafting.
3. the detection method of Se content in soil as claimed in claim 2, which is characterized in that the method for drafting of the standard curve
It is as follows: by ρ(Se)It dilutes be configured to ρ step by step for the selenium standard solution of 0.05mg/L(Se)Respectively 0.00 μ g/L, 1.00 μ g/L,
The standard solution of 2.00 μ g/L, 4.00 μ g/L, 8.00 μ g/L；It is each to inhale 20.00mL, make its Se content be respectively 0.00ng,
20.00ng, 40.00ng, 80.00ng, 160.00ng are put into 100mL stuffed conical flask, simultaneously by sample solution determination step
It carries out.
4. the detection method of Se content in soil as claimed in claim 2, which is characterized in that the hydroxylamine hydrochloride-ethylenediamine tetraacetic
The configuration method of two sodium solution of acetic acid is as follows: it weighs 10g ethylenediamine tetra-acetic acid and is dissolved in 500mL water, 25g hydroxylamine hydrochloride is added,
It makes it dissolve, is diluted with water to 1000mL and obtains.
5. the detection method of Se content in soil as described in claim 1, which is characterized in that step (1) described sampled point is really
Determine principle are as follows: 0.33hm2Below to take at 9~11 points, area is greater than 0.3hm2When, every increase 667m2Increase sampled point 1~2.
6. the detection method of Se content in soil as described in claim 1, which is characterized in that in step (2) process of lapping
0.15mm~2mm is in the nylon mesh aperture used.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110940544A (en) * | 2019-11-13 | 2020-03-31 | 西安重光明宸检测技术有限公司 | Soil pollution detection method |
| CN111157306A (en) * | 2019-11-14 | 2020-05-15 | 西安重光明宸检测技术有限公司 | Soil analysis and detection method |
| CN112504735A (en) * | 2020-12-17 | 2021-03-16 | 青岛康环检测科技有限公司 | Soil detection method |
| CN112683579A (en) * | 2020-12-31 | 2021-04-20 | 山东泰诺检测科技有限公司 | Soil pollution detection method |
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| CN102519931A (en) * | 2011-12-20 | 2012-06-27 | 苏州硒谷科技有限公司 | Method for rapid determination of content of selenium in soil sample |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110940544A (en) * | 2019-11-13 | 2020-03-31 | 西安重光明宸检测技术有限公司 | Soil pollution detection method |
| CN111157306A (en) * | 2019-11-14 | 2020-05-15 | 西安重光明宸检测技术有限公司 | Soil analysis and detection method |
| CN112504735A (en) * | 2020-12-17 | 2021-03-16 | 青岛康环检测科技有限公司 | Soil detection method |
| CN112683579A (en) * | 2020-12-31 | 2021-04-20 | 山东泰诺检测科技有限公司 | Soil pollution detection method |
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