CN105954249A - Method for detecting soil active selenium - Google Patents
Method for detecting soil active selenium Download PDFInfo
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- CN105954249A CN105954249A CN201610443955.3A CN201610443955A CN105954249A CN 105954249 A CN105954249 A CN 105954249A CN 201610443955 A CN201610443955 A CN 201610443955A CN 105954249 A CN105954249 A CN 105954249A
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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
- G01N21/6404—Atomic fluorescence
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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
- G01N2021/6417—Spectrofluorimetric devices
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Abstract
A proper amount of heavy metal selenium in soil is beneficial to plants and the human body, while excessive selenium has a toxic effect on plants and threats the health of human body through a food chain. According to an existing method for detecting heavy metal selenium in soil, the full amount of heavy metal selenium in soil is detected, a detection process is complex, and a large part of selenium in a detection result does not have biological effective activity. Soil active selenium analyzed through a method for detecting soil active selenium can reflect the relation between heavy metal selenium in soil and absorption of the root systems of plants to the maximum, and represent the effective state of heavy metal selenium in soil. According to the method for detecting soil active selenium, an extra large soil sampling amount is adopted, diethylenetriamine pentaacetic acid serves as a chelating agent, calcium ions in calcium chloride serve as a chelating and extracting balance agent, triethanolamine serves as a buffering agent, and soil active selenium is extracted through chelating; an atomic fluorescence spectrometry and an ultralow mass concentration standard curve are adopted, and thus it is ensured that ultramicro-amount of soil active selenium is detected. The expression unit of the content of soil active selenium is microgram/kg or 10<-3> mg/kg.
Description
Technical field
The invention belongs to agriculture field, proprietary code is A99；It is specifically related in soil easily be absorbed by root system of plant, and energy
Enter in agricultural production results product, affect the analyzing detecting method of the soil activation state selenium of agricultural product quality.
Background technology
Heavy metal-polluted soil mainly includes cadmium (Cd), hydrargyrum (Hg), arsenic (As), lead (Pb), chromium (Cr), copper (Cu), zinc (Zn), nickel
(Ni), the heavy metal element such as selenium (Se), antimony (Sb), bismuth (Bi)；Heavy metal existing forms in soil can be divided into five classes, and first
It is present in the clay lattice such as silicate, primary and secondary mineral, is the result of nature geology efflorescence, at nature just
Release it is difficult under the conditions of Chang, can be steady in a long-term in deposit, it is difficult to as plant absorption；Next to that iron and manganese oxides combined state weight
Metal, is the external capsule thing with mineral and the existence of fine powder scattered seed, and the iron and manganese oxides specific surface area of activity is big, adsorbs or is co-precipitated
Anion forms；3rd is carbonate combined state heavy metal, is being total to of being formed on carbonate mineral of heavy metals in soil
Precipitation combined state；It is fixed in soil crystal, or is combined into the heavy metal of indissoluble state with other material in soil and does not possess life
Thing effective active, it is impossible to be absorbed by plants and enter food chain；4th is to organically combine state heavy metal, and it is various in soil to have
The integuments of machine thing and mineral grain etc. and heavy metal in soil chelate, chelating degree determines whether this heavy metal can be planted
Thing absorbs；5th class is exchangeable species heavy metal in soil, and it is absorption gold on surface of clay, humus and other composition
Belong to, sensitive to environmental change, it is easy to Transport And Transformation, can be absorbed by plants, can reflect that geobiont toxicity and the mankind arrange in the recent period
Dirty state.
Exchangeable species heavy metal and combination state heavy metal have great activeness and bioavailability, soil
In heavy metal on plants produce toxic action time, a series of physiological features such as plant height degree, main root length, leaf area can be caused
Change, thus affect plant physio-ecological processes, plant products and quality；They can be put aside in vivo, causes farming
Thing poisoning, the underproduction, until death, affect the safety of ecosystem；Enter human body finally by food chain, directly human body is good for
Health threatens；Appropriate selenium is useful to plant and human body, but as other effect of fertilizers, human body is persistently taken in containing selenium
High food and water may occur in which selenosis；The symptom of acute selenium poisoning has vomiting, stomachache, hair and loss of finger-nail, erythra, surrounding
Neuritis, can occur disordered breathing, respiratory failure time serious, belong to severe toxicity level according to acute toxicity classification selenium.
Selenium exists with variform in soil, including native selenium, mineral state selenium, water soluble speciation, Organic Selenium etc., changes
Conjunction valency has+2 ,+4 ,+6；GB5749-2006 drinking water sanitary standard specifies, selenium concentration must not exceed 0.01mg/L；
GB3838-2002 Environmental Quality Standard of Surface Water selenium full dose I class～III class≤0.01mg/L, IV～V class water 0.02mg/L；
GB15618-2008 standard of soil environment quality farmland total selenium secondary standard value is 3.0mg/kg.
It is now the full dose of mensuration Selenium in Soils with heavy metal-polluted soil selenium analyzing detecting method, according to national standard, soil sample warp
After nitric acid-hydrochloric acid-perchloric acid is cleared up, in acid medium, in sample, selenium is by potassium borohydride (KBH4) or sodium borohydride (NaBH4)
It is reduced into atomic state selenium, by carrier gas (argon) band people's atomizer, under special selenium hollow cathode light irradiation, ground state selenium atom
Be excited to upper state, deactivate return to ground state time, launch the fluorescence of characteristic wavelength, its fluorescence intensity just becomes with Se content
Ratio, compares quantitative with standard series；During detection, pedotheque will be through strong acid, strong oxidizer by a large amount of fixing in soil
Out, operational approach is complicated for heavy metal release；During cold-vapour atomic absorption method measures, only focus on the full selenium of soil of high level
And ignore the detection of the soil activation state selenium of low content；And the full Se content of soil of current assay method only some can pass through
Root system of plant enters in plant, and other parts are integrally fixed in soil crystal or are combined into indissoluble with other material in soil
State, does not possess biologically effective activity, and therefore measurement result can not represent soil activation state selenium affects state to plant absorption.
This patent is to the Bashan Mountain, Qinling Mountains regional soil heavy metal selenium full dose, soil activation state selenium and weight in Agricultural Output product
On the basis of metallic selenium full dose is analyzed, research heavy metal-polluted soil full dose, activated state content and heavy metal in Agricultural Output product
The dependency of selenium full dose, creates " detection method of a kind of soil activation state selenium ", the soil activation state of this analysis method detection
Se content can reflect the relation between heavy metal-polluted soil selenium and plant absorption to greatest extent, really reflects heavy metal pollution of soil
State；Through retrieving domestic and international pertinent literature, find no the report with " detection method of a kind of soil activation state selenium " identical content
Road.
Summary of the invention
The detection of soil activation state selenium is analyzed and is used diethylenetriamine pentaacetic acid extraction atomic fluorescence spectrometer detection；Use
Diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine buffer solution extracts out soil activated state selenium, with cold as digestion agent, chelating
Atom atomic fluorescence spectrometer method measures；The most appropriate diethylenetriamine pentaacetic acid is chelating agen, in appropriate calcium chloride calcium from
Son is chelating extraction poising agent, and chloride ion prevents the dissolving of free calcium carbonate in calacareous soil, it is to avoid covered because calcium carbonate wraps
Selenium Element release and the impact that produces；Appropriate triethanolamine, as buffer agent, can make pH value of solution holding about 7.3, simultaneously
Triethanolamine also has supression effect to dissolution of calcium carbonate.
Under the soil ratio premise of 2:1, increase pedotheque quantity as far as possible to ensure the soil that in soil, content is the lowest
The detection of activated state selenium, weighs the air-dried sample 20.00g by 2mm aperture nylon mesh in 200mL plastic bottle, adds 25 DEG C
Diethylenetriamine pentaacetic acid-the calcium chloride of ± 2 DEG C-triethanolamine digestion agent 40mL, builds bottle cap, shakes up, at the bar of 25 DEG C ± 2 DEG C
Under part, with 180r min-1±20r•min-1Hunting of frequency 2h, vibration liquid centrifuge filter immediately after 5 minutes, protect
Reserved filtrate also completes to measure in 48h, does blank assay simultaneously.
Use ultralow mass concentration standard curve, play atomic fluorescence spectrometer ultramicro-element detection function as far as possible,
To ensure the detection of the soil activation state selenium that content is the lowest in soil；Concrete grammar is to use 100.0 μ g/L selenium in general measure
The 1/10 of standard solution concentration is as the selenium standard solution concentration in the present invention, i.e. 10.0 μ g/L；Standard curve uses super
Low quality concentration standard curve, selenium standard curve maximum upper limit takes 2.0 μ g/L, and on zero point, first concentration value uses routine to survey
In amount, the 1/5 of selenium concentration of standard solution 1.0 μ g/L, i.e. 0.2 μ g/L selenium is dense as on zero point in the present invention first standard curve
Angle value.
The representation unit of soil activation state heavy metal Se content is micrograms or the milligram of activated state selenium in every kilogram of soil
Number, representation unit is: μ g/kg or A × 10-3Mg/kg, soil activation state Se content is the lowest, about at 0.0001mg/kg-
0.01mg/kg, between i.e. 0.1 μ g/kg-10 μ g/kg, scarce there is statement unit during normal international standard mg/kg representation unit
Fall into, convenient, with μ g/kg or A × 10 for reading and recording-3Mg/kg represents that soil activation state selenium unit more gears to actual circumstances.
Detailed description of the invention
Soil activation state selenium one detection method: chelating extraction atomic fluorescence spectrometer method；Use Diethylenetriamine five second
Acid-calcium chloride-triethanolamine buffer solution is as digestion agent, and wherein diethylenetriamine pentaacetic acid is chelating agen, and calcium chloride is chelating
Extraction poising agent, triethanolamine is buffer agent, and pH value of solution can be made to keep about 7.3, and chelating extracts out soil activated state selenium, with former
Sub-fluorescence spectrophotometer method, uses ultralow mass concentration standard curve, measures soil activation state selenium.
Key instrument equipment: 1, analytical balance: precision is 0.0001g；2, atomic fluorescence spectrophotometer；3, selenium element is hollow
Cathode modulation；4, acidometer；5, constant temperature (temperature control 25 DEG C ± 2 DEG C) reciprocating or rotary vibrating machine, or be placed in thermostatic chamber
Common vibrating machine, meets the frequency of oscillation of 180r min-1 ± 20r min-1 or reaches same effect；6, centrifuge；7、
200mL plastic bottle with cover or 250mL triangular flask.
Reagent and preparation of reagents:
13.1, reagent: 1, diethylenetriamine pentaacetic acid: top grade is pure；2, triethanolamine: top grade is pure；3, calcium chloride (CaCl2·
2H2O): top grade is pure；4, hydrochloric acid (HCl): top grade is pure, ρ=1.19 g/mL；5, potassium hydroxide (KOH): top grade is pure；6, potassium borohydride
(KBH4): top grade is pure；7, high-purity selenium powder；8, ammonia；
13.2,50% hydrochloric acid solution: pipette 500mL hydrochloric acid, be diluted to 1000mL with experimental water；
13.3,50% ammonia spirit: pipette 500mL ammonia, be diluted to 1000mL with experimental water；
13.4, chelating digestion agent preparation: weigh 1.967g diethylenetriamine pentaacetic acid, be dissolved in 14.92g (about 13.3mL) triethanolamine
With in a small amount of water；Again by 1.47g calcium chloride (CaCl2·2H2O), after being dissolved in water, proceed in the lump, in 1L volumetric flask, add water to about
950mL；Regulate pH to 7.3 at acidometer 50% hydrochloric acid solution or 50% ammonia, use water constant volume, store in plastic bottle stand-by；
13.5, reducing agent preparation: 1.0% potassium borohydride+0.5% potassium hydroxide solution；Weigh 2.5g potassium hydroxide to put into and fill
In the beaker of 100mL experimental water, Glass rod stirring adds 5.0g potassium borohydride, stirring and dissolving, constant volume until completely dissolved
To 500mL；This solution preparation on the same day；
13.6, current-carrying preparation: 5% hydrochloric acid solution: pipette 25mL hydrochloric acid experimental water and be diluted to 500mL.
Selenium (Se) standard solution:
14.1, selenium Standard Reserving Solution: ρ=100.0mg/L；Buy commercially available certified reference material-have card standard sample, or weigh
The high-purity selenium powder of 0.1000g, is placed in 100mL beaker, adds after 20mL nitric acid low-temperature heat is dissolved and is cooled to greenhouse, moves into 1000mL
In volumetric flask, it is settled to graticule with experimental water, mixing；
14.2, selenium standard intermediate liquid: ρ=1.00mg/L；Pipette selenium Standard Reserving Solution 5.00ml, be placed in the volumetric flask of 500mL,
It is settled to graticule, mixing with diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent；
14.3, selenium standard solution: ρ=10.0 μ g/L；Pipette selenium standard intermediate liquid 5.00ml, be placed in 500mL volumetric flask, use
Diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent is settled to graticule, mixing.Used time now joins.
Extract liquid to be measured to prepare:
Weigh the air-dried sample 20.00g by 2mm aperture nylon mesh in 200mL plastic bottle, add the diethyl of 25 DEG C ± 2 DEG C
Pentaacetic acid-calcium chloride-triethanolamine digestion agent 40mL, builds bottle cap, shakes up, under conditions of 25 DEG C ± 2 DEG C, with
The hunting of frequency 2h of 180r min-1 ± 20r min-1, filters immediately；Retain filtrate, point take 25.0mL test solution and be placed in 50mL and hold
In measuring bottle, add concentrated hydrochloric acid 10mL, be settled to graticule mixing, room with diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent
Temperature places 30min；Complete to measure in 48h, do blank assay simultaneously.
Analyze and measure:
16.1, the debugging of atomic fluorescence spectrophotometer: atomic fluorescence spectrophotometer start preheating, sets lamp according to instrument operation instructions
The running parameters such as electric current, negative high voltage, carrier gas flux, shield gas flow amount, preheating selenium element hollow cathode lamp 20 minutes；Instrument reference
Condition is shown in Table 1；
The running parameter of table 1 atomic fluorescence spectrophotometer
16.2, the preparation of selenium (Se) calibration series:
Pipette respectively ρ=10.0 μ g/L selenium (Se) titer 0.00,1.00,2.00,3.00,5.00,7.00,10.00mL selenium standard
Use liquid in 50mL volumetric flask, be separately added into 50% hydrochloric acid solution 5mL, with diethylenetriamine pentaacetic acid-calcium chloride-three ethanol
Amine digestion agent is settled to graticule, mixing；The calibration serial solution concentration of selenium is shown in Table 2；
Table 2 mercury element calibration serial solution concentration unit: g/L
16.3, draw calibration curve: with 1.0% potassium borohydride+0.5% potassium hydroxide solution as reducing agent, 5% hydrochloric acid solution be carry
Stream, is sequentially measured the atomic fluorescence intensity of calibration series standard solution by low concentration to high concentration.By deduction zero-dose blank
Calibration series atomic fluorescence intensity is vertical coordinate, and concentration of element (μ g/L) corresponding in solution is abscissa, draws calibration song
Line；And carry out blank assay according to identical reagent and step；
16.4, measure: the test portion that prepare is imported in atomic fluorescence spectrophotometer, according to draw calibration curve same instruments work
It is measured as condition；If tested concentration of element exceedes calibration curve concentration range, mensuration should be re-started after diluting；Simultaneously
The blank test portion prepared is imported in atomic fluorescence spectrophotometer, carries out according to drafting calibration curve same instruments working condition
Measure.
Result calculates and represents:
17.1, result calculates: soil activation state selenium；
In formula: the content of activated state selenium element in ω soil, 10-3mg/kg；
ρ is checked in by calibration curve and measures the concentration of element, g/L in test solution；
ρ0The mensuration concentration of element, g/L in blank solution；
V0Add diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent volume；
V1Divide the volume taking digestion agent test solution, mL；
V2Divide the constant volume measuring test solution after taking, mL；
M weighs the quality of sample, g；
17.2, result represents: soil activation state Se content representation unit is: 10-3mg/kg；When measurement result is less than 1 × 10- 3During mg/kg, after arithmetic point, numeral at most retains to three；When measurement result is more than 1 × 10-3During mg/kg, retain three effectively
Numeral.
Claims (8)
1. the detection of soil activation state selenium uses chelating digestion agent to extract out soil activated state selenium, and it chelates the complete formula of digestion agent
It is: diethylenetriamine pentaacetic acid 1.967g to be dissolved in 14.92g (about 13.3mL) triethanolamine and a small amount of water；Again by 1.47g chlorination
After calcium is dissolved in water, proceed in the lump, in 1000mL volumetric flask, add water to about 950mL；With 50% hydrochloric acid solution or 50% on acidometer
Ammonia regulation pH to 7.3, is settled to 1000mL with water.
2. with calcium chloride calcium ion for soil activation state selenium detection chelating extraction poising agent in chelating digestion agent.
3. the detection of soil activation state selenium increases pedotheque quantity as far as possible to ensure the soil activation that in soil, content is the lowest
The detection of state selenium, weighs sample 20.00g, adds chelating digestion agent 40mL.
4., on soil activation state selenium lixiviating solution before machine testing, mixed liquor refilters after 5 minutes with centrifuge.
5. soil activation state selenium is detected as ensureing the detection of the soil activation state selenium that content is the lowest in soil；Selenium standard solution is dense
Degree is 10 μ g/L.
6. soil activation state selenium is detected as ensureing the detection of the soil activation state selenium that content is the lowest in soil, and examination criteria curve is adopted
Using low quality concentration standard curve, first minimum on zero uses the selenium standard curve concentration of 0.2 μ g/L.
7. the representation unit of soil activation state Se content is μ g/kg.
8. the representation unit of soil activation state Se content is 10-3mg/kg。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109975101A (en) * | 2019-03-30 | 2019-07-05 | 青岛东方标牌有限公司 | A kind of Soil K+adsorption method |
| CN110333209A (en) * | 2019-07-11 | 2019-10-15 | 恩施土家族苗族自治州农业科学院(恩施土家族苗族自治州硒应用技术与产品开发研究院) | A kind of detection method of soil available Se |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109975101A (en) * | 2019-03-30 | 2019-07-05 | 青岛东方标牌有限公司 | A kind of Soil K+adsorption method |
| CN110333209A (en) * | 2019-07-11 | 2019-10-15 | 恩施土家族苗族自治州农业科学院(恩施土家族苗族自治州硒应用技术与产品开发研究院) | A kind of detection method of soil available Se |
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