CN106153587A - A kind of detection method of soil activation state cadmium - Google Patents
A kind of detection method of soil activation state cadmium Download PDFInfo
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- G—PHYSICS
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- 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
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
Soil heavy metal cadmium produces toxic action to plant, and is threatened health by food chain；Being now to measure soil heavy metal cadmium full dose by soil heavy metal cadmium detection method, detection process is complicated, and in measurement result, cadmium does not possess biological effectiveness greatly.The soil activation state cadmium that soil activation state heavy metal cadmium detection method detects, can reflect relation between soil heavy metal cadmium and root system of plant absorption, real reflection heavy metal pollution of soil state to greatest extent.The detection of soil activation state cadmium uses diethylenetriamine pentaacetic acid to be chelating agen, and in calcium chloride, calcium ion extracts out soil activated state cadmium for chelating extraction poising agent, triethanolamine as buffer agent, chelating；Use atomic fluorescence spectrometer method, use super amount Soil K+adsorption sampling amount, ultralow mass concentration standard curve, it is ensured that the detection of ultramicron soil activation state cadmium in soil.The representation unit of soil activation state heavy metal cadmium content is μ g/kg or 10‑3mg/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 heavy metal cadmium 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 kind of form is exchangeable species heavy metal in soil, and it is that absorption is on surface of clay, humus and other composition
Metal, it is sensitive to environmental change, it is easy to Transport And Transformation, can be absorbed by plants, and can reflect geobiont toxicity.
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；After cadmium is absorbed by the body, forms cadmium sulfoprotein in vivo, be optionally accumulated in liver, kidney；Cadmium is from digestive tract
Enter human body, then there will be the symptoms such as vomiting, gastrointestinal convulsion, abdomen pain, diarrhoea, even can be dead because of hepatorenal syndrome；In human body
Being enriched with too much cadmium can make the metabolism of skeleton be obstructed, and causes the series of symptoms such as osteoporosis, atrophy, deformation.
In nature, the many character with compound of cadmium exists, and cadmium quantivalence is+1 and+2；GB5749-2006 life is drunk
Water hygiene standard regulation cadmium concentration must not exceed 0.005mg/L；GB3838-2002 cadmium Environmental Quality Standard of Surface Water I class water≤
0.001mg/L, II class～IV class water 0.0011～0.005mg/L, V class water 0.0051～0.01mg/L；GB15618-1995 cadmium
Full dose standard of soil environment quality one-level≤0.20mg/kg, two grade 0.21～0.60mg/kg, three grade 0.61～1.00mg/kg；
The difficulty of prevention and cure of Cadmium Pollution in Soils is big, and producing the widest method of upper employing at present is with Calx i.e. Ca(OH)2Administer, logical
The activity crossing the suppression soil activation state cadmium of the Ca ionic equilibrium in Calx has better effects；Biological restoration utilize super accumulation plant
The enrichment of thing, it is possible to reduce the content of heavy metal in soil cadmium；But chemical repair method is not means of repairing thoroughly,
Heavy metal-polluted soil easy reactivation harm plant, there is secondary pollution equivalent risk in biological restoration.
It is now the full dose of mensuration heavy metal in soil with soil heavy metal cadmium analyzing detecting method, according to national standard, entirely
Amount cadmium be soil sample after hydrochloric acid-nitric acid-perchloric acid (or hydrochloric acid-nitrate acid and hydrofluoric acid-perchloric acid) is cleared up, thoroughly destroy soil
Mineral lattice, makes the element to be measured in sample all enter people's test solution；Then, test solution is noted in people's graphite furnace, through presetting
Be dried, the matrix composition evaporation that makes to coexist of ashing, the heating schedule such as atomization removes, while under the high temperature of atomized stage cadmium
Compound dissociates into ground state atom steam, and the characteristic spectral line launching hollow cathode lamp produces selective absorbing；Select
Under optimum determining condition, by background deduction, measure the absorbance of cadmium in test solution, and compare with standard series quantitative；Adopt at present
The full cadmium content of soil measured by the method only has fraction can enter in plant by root system of plant, and remainder is then solid
It is scheduled in soil crystal or is combined into indissoluble state with other material in soil, not possessing biologically effective activity, therefore measure knot
Fruit can not represent the soil activation state cadmium in soil affects state to plant absorption.
This patent is to the Bashan Mountain, Qinling Mountains regional soil heavy metal cadmium full dose, soil activation state cadmium content and weight in agricultural product
On the basis of cadmium metal full dose carries out detection analysis, research heavy metal-polluted soil full dose, activated state content and agricultural product heavy metal cadmium
The dependency of full dose, creates " detection method of a kind of soil activation state cadmium ", the soil activation state that this analytical goes out
Cadmium content can reflect the relation between soil heavy metal cadmium 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 cadmium " identical content
Road.
Summary of the invention
The detection of soil activation state heavy metal cadmium is analyzed and is used diethylenetriamine pentaacetic acid extraction atomic fluorescence spectrometer method；
Diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine buffer solution is used to extract out soil activated state cadmium as digestion agent, chelating,
Measure by atomic fluorescence spectrometer method；The most appropriate diethylenetriamine pentaacetic acid is chelating agen, calcium ion in appropriate calcium chloride
For chelating extraction poising agent, chloride ion prevents in calacareous soil the dissolving of free calcium carbonate, it is to avoid covered because calcium carbonate wraps
The impact that cadmium element discharges and produces；Appropriate triethanolamine, as buffer agent, can make pH value of solution keep about 7.3, simultaneously three
Ethanolamine also 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 heavy metal cadmium, weighs air-dried soil sample 20.0g by 2mm aperture nylon mesh in 200mL plastic bottle, adds
Diethylenetriamine pentaacetic acid-the calcium chloride of 25 DEG C ± 2 DEG C-triethanolamine digestion agent 40mL, builds bottle cap, shakes up, at 25 DEG C ± 2 DEG C
Under conditions of, with 180r min-1±20r•min-1Hunting of frequency 2h, vibration liquid mistake immediately after centrifuge 5 minutes
Filter, retains filtrate and completes to measure in 48h, doing 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 cadmium that content is the lowest in soil；Concrete grammar is to use 50.0 μ g/L cadmium marks in general measure
The 1/50 of quasi-use liquid concentration is as the cadmium standard solution concentration in the present invention, i.e. 1.0 μ g/L；Standard curve uses ultralow matter
Amount concentration standard curve, cadmium standard curve maximum upper limit takes 0.20 μ g/L, and on zero point, first concentration value uses general measure
1/5, the i.e. 0.02 μ g/L cadmium of middle cadmium concentration of standard solution 0.1 μ g/L is as on zero point in the present invention first standard curve concentration
Value.
The representation unit of soil activation state heavy metal cadmium content is micrograms or the milligram of activated state cadmium in every kilogram of soil
Number, representation unit is: μ g/kg or A × 10-3Mg/kg, in soil, the content of activated state heavy metal cadmium is about at 0.00001mg/kg
～between 0.01mg/kg, i.e. 0.01 μ g/kg～10 μ g/kg, single there is statement during normal international standard mg/kg representation unit
Position defect, convenient, with μ g/kg or A × 10 for reading and recording-3Mg/kg represents that soil activation state cadmium unit more gears to actual circumstances.
Detailed description of the invention
Soil activation state heavy metal cadmium detection method: chelating extraction atomic fluorescence spectrometer method；Use Diethylenetriamine five
Acetic acid-calcium chloride-triethanolamine buffer solution is as digestion agent, and wherein diethylenetriamine pentaacetic acid is chelating agen, and calcium chloride is chela
Closing 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 cadmium, uses
Atomic fluorescence spectrometer method, uses ultralow mass concentration standard curve, measures soil activation state cadmium.
Key instrument equipment: 1, analytical balance: precision is 0.0001g；2, atomic fluorescence spectrophotometer；3, hollow the moon of cadmium element
Pole lamp；4, acidometer；5, constant temperature (temperature control 25 DEG C ± 2 DEG C) reciprocating or rotary vibrating machine, or be placed in thermostatic chamber general
Logical vibrating machine, meets 180r min-1±20r·min-1Frequency of oscillation or reach same effect；6, constant temperature water bath apparatus；7、
Centrifuge；8,200mL 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=1.19g/mL；5, potassium hydroxide (KOH): top grade is pure；6, potassium borohydride
(KBH4): top grade is pure；7, ammonia: 8, Caddy (Cleary) (Hg Cl2): top grade is pure；9, cobaltous chloride (CoCl2.6H2O): top grade is pure；10、8-
Hydroxyquinoline: top grade is pure；11, nitric acid: top grade is pure；
13.2,50% hydrochloric acid solution: pipette 500mL hydrochloric acid experimental water and be diluted to 1000mL；
13.3,50% ammonia spirit: pipette 500mL ammonia experimental water and be diluted to 1000mL；
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: 2% potassium borohydride+0.5% potassium hydroxide solution；Weigh 2.5g potassium hydroxide to put into and fill 100mL
In the beaker of experimental water, Glass rod stirring adds until completely dissolved and weighs up 10.0g potassium borohydride, and stirring and dissolving is settled to
500mL；This solution preparation on the same day, is used for measuring cadmium；
13.6, current-carrying preparation: 2% hydrochloric acid solution: pipette 10mL hydrochloric acid experimental water and be diluted to 500mL；
13.7, sensitizer preparation: 250mg/L8-hydroxyquinoline and 200mg/L cobaltous chloride mixed liquor；0.25g8-hydroxyquinoline, adds
After entering 50% hydrochloric acid solution 10mL dissolving, add about 20mL experimental water, add 0.2g cobaltous chloride (CoCl2·6H2O), mixing,
It is settled to 1000mL with experiment water.
Cadmium (Cd) standard solution:
14.1, cadmium Standard Reserving Solution ρ=100.0mg/L；Buy commercially available certified reference material/have card standard sample, or accurately weigh
0.1000g(is accurate to 0.0002g) high pure metal spectrum cadmium in 50mL beaker, add people's 10mL salpeter solution, slight fever is dissolved, cold
It is transferred to the most afterwards in 1000mL volumetric flask, is settled to graticule with water, shakes up；
14.2, cadmium standard intermediate liquid: ρ=1.00mg/L；Pipette cadmium Standard Reserving Solution 5.00ml, be placed in the volumetric flask of 500mL,
Add 50% hydrochloric acid solution 200mL experimental water and be settled to graticule, mixing；
14.3, cadmium standard solution ρ=1.0 μ g/L；Pipette 1.00mg/L cadmium standard intermediate liquid 5.00ml, be placed in 500mL volumetric flask
In, it is settled to graticule with lixiviating solution, then from 500ml volumetric flask, pipettes 5ml constant volume liquid, be placed in 50ml volumetric flask, with chelating
Digestion agent is settled to graticule；Used time now joins.
Extract liquid to be measured to prepare:
Weigh air-dried soil sample 20.0g by 2mm aperture nylon mesh in 200mL plastic bottle, add the diethyl three of 25 DEG C ± 2 DEG C
Triamine pentaacetic acid-calcium chloride-triethanolamine digestion agent 40mL, builds bottle cap, shakes up, under conditions of 25 DEG C ± 2 DEG C, with 180r
min-1±20r•min-1Hunting of frequency 2h, filter immediately；Point taking 25.0mL filtrate is placed in 50mL volumetric flask, adds 50% salt
Acid solution 5mL, 250mg/L8-hydroxyquinoline and 200mg/L cobaltous chloride sensitizer mixed liquor 1.0ml, with diethylenetriamine pentaacetic acid-
Calcium chloride-triethanolamine digestion agent is settled to graticule mixing, and room temperature places 30min；When room temperature is less than 15 DEG C, it is placed in 30 DEG C of water
Bath is incubated 20min, completes 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, reference conditions are shown in Table 1；
The running parameter of table 1 atomic fluorescence spectrophotometer
16.2, the preparation of cadmium calibration series:
Pipette respectively ρ=1.0 μ g/L cadmium standard solution 0.00,1.00,2.00,3.00,5.00,7.00,10.00mL is in 50mL
In volumetric flask, it is separately added into 50% hydrochloric acid solution 5mL, 250mg/L8-hydroxyquinoline and 200mg/L cobaltous chloride synergist mixed liquor
1.0mg, is settled to graticule with diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent, mixing；The calibration serial solution of cadmium
Concentration is shown in Table 2；
Table 2 cadmium element calibration serial solution concentration unit: g/L
16.3, draw calibration curve: with 2% potassium borohydride+0.5% potassium hydroxide solution as reducing agent, 2% hydrochloric acid solution as current-carrying,
The atomic fluorescence intensity of calibration series standard solution is sequentially measured by low concentration to high concentration；With the calibration that deduction zero-dose is blank
Series atomic fluorescence intensity is vertical coordinate, and concentration of element (μ g/L) corresponding in solution is abscissa, draws calibration curve；And
Blank assay is carried out 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 cadmium (Cd)；
In formula: the content of activated state cadmium 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 heavy metal cadmium (Cd) content representation unit is: g/kg or 10-3mg/kg；Work as survey
Determine result less than g/kg or 1 × 10-3During mg/kg, after arithmetic point, numeral at most retains to three；When measurement result is more than g/kg
Or 1 × 10-3During mg/kg, retain three position effective digitals.
Claims (8)
1. the detection of soil activation state cadmium uses chelating digestion agent to extract out soil activated state cadmium, 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 1:1 hydrochloric acid solution or 1:1 on acidometer
Ammonia regulation pH to 7.3, is settled to 1000mL with water.
2. with calcium chloride calcium ion for soil activation state cadmium detection chelating extraction poising agent in chelating digestion agent.
3. the detection of soil activation state heavy metal cadmium increases pedotheque quantity as far as possible to ensure the soil that in soil, content is the lowest
The detection of earth activated state cadmium, weighs sample 20.00g, adds chelating digestion agent 40mL.
4., on soil activation state cadmium lixiviating solution before machine testing, mixed liquor refilters after 5 minutes with centrifuge.
5. in the detection of soil activation state cadmium, cadmium standard solution concentration is 1.0 μ g/L.
6. soil activation state heavy metal cadmium examination criteria curve uses low quality concentration standard curve, first mark on zero point
Directrix curve minimum uses 0.02 μ g/L cadmium standard curve concentration.
7. the representation unit of soil activation state heavy metal cadmium content is μ g/kg.
8. the representation unit of soil activation state heavy metal cadmium content is 10-3mg/kg。
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| CN112345622A (en) * | 2020-10-09 | 2021-02-09 | 广电计量检测（湖南）有限公司 | Method for testing soil available cadmium |
| CN113640236A (en) * | 2021-08-11 | 2021-11-12 | 哈尔滨蔚蓝环境检测有限公司 | Method for detecting heavy metal cadmium in farmland soil |
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