CN106124467A - A kind of soil activation state arsenic, bismuth, the detection method of antimony - Google Patents
A kind of soil activation state arsenic, bismuth, the detection method of antimony Download PDFInfo
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- CN106124467A CN106124467A CN201610443975.0A CN201610443975A CN106124467A CN 106124467 A CN106124467 A CN 106124467A CN 201610443975 A CN201610443975 A CN 201610443975A CN 106124467 A CN106124467 A CN 106124467A
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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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- 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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Abstract
Heavy metal-polluted soil arsenic, bismuth, antimony produce toxic action to plant, and are threatened health by food chain；Being now to measure heavy metal-polluted soil full dose by detection method, detection process is complicated, and in measurement result, arsenic, bismuth, antimony do not possess biologically effective activity greatly.Arsenic in soil that soil activation state arsenic, bismuth, antimony detection method analyze, bismuth, antimony, can reflect to greatest extent heavy metal-polluted soil arsenic, bismuth, antimony and root system of plant absorb between relation, characterize heavy metal pollution of soil state.The detection of soil activation state arsenic, bismuth, antimony uses super large soil sample amount, and diethylenetriamine pentaacetic acid is chelating agen, and in calcium chloride, calcium ion extracts out soil activated state arsenic, bismuth, antimony for chelating extraction poising agent, triethanolamine as buffer agent, chelating；With atomic fluorescence spectrometry, use ultralow mass concentration standard curve, it is ensured that ultramicron soil activation state arsenic, bismuth, the detection of antimony in soil.Soil activation state arsenic, bismuth, the representation unit of antimony content are 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 soil activation state arsenic of agricultural product quality, bismuth, the analyzing detecting method of antimony.
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.
In soil, exchangeable species heavy metal and combination state heavy metal have great activeness and bioavailable
Property, heavy metal can produce toxic action to plant, causes a series of physiological features such as plant height degree, main root length, leaf area
Change, thus have influence on plant physio-ecological processes, yield and quality；They can be put aside in vivo, causes crops
Poisoning, the underproduction, until death, affect the safety of ecosystem；Human body is entered, directly to health finally by food chain
Threaten；The homergy of the arsenic meeting interference cell of excess in human body, impact is breathed and oxidizing process, makes cell that disease to occur
Become, arsenic also can coup injury small artery and capillary wall, and vasoactive relaxes contracting maincenter, causes vascular permeability to increase,
Cause blood volume to reduce, increase the weight of organ injury；Bismuth can accumulate the kidney at human body, and causes chronic poisoning；Antimony is to human body and ring
Border biology has toxic action, is even suspect to be carcinogen, antimony and compound thereof and is classified as emphasis pollution by many countries
Thing, acute stibialism can cause the infringement of multiple histoorgans such as skin mucosa, heart, liver, lung and nervous system.
The inorganic arsenic of trivalent and pentavalent is mainly had at Arsenic in Soil；The chemical form of antimony has inorganic and organic form, nothing
Machine form quantivalence is for for+3 and+5, and organic form mainly quantivalence is the trimethylantimony compound of+5；GB5749-2006 is raw
Sanitary standard for drinking water of living specifies, arsenic concentration must not exceed 0.01mg/L, and antimony concentration must not exceed 0.005 mg/L；GB3838-
2002 Environmental Quality Standard of Surface Water arsenic full dose I classes～III class≤0.05mg/L, IV～V class water 0.05～0.10mg/L；
GB15618-2008 standard of soil environment quality farmland total arsenic secondary standard value is 20～45mg/kg, and total antimony secondary standard value is
10mg/kg。
It is now the full dose measuring heavy metal in soil with heavy metal-polluted soil arsenic, bismuth, antimony analyzing detecting method, marks according to country
Standard, soil sample is after nitric acid-hydrochloric acid-perchloric acid is cleared up, and in acid medium, in sample, arsenic, bismuth, antimony are by potassium borohydride (KBH4) or
Sodium borohydride (NaBH4) be reduced into atomic state arsenic, bismuth, antimony, carrier gas (argon) bring in atomizer, at special arsenic, bismuth, antimony
Under hollow cathode light irradiation, ground state arsenic, bismuth, antimony atoms are excited to upper state, deactivate return to ground state time, launch feature
The fluorescence of wavelength, its fluorescence intensity is directly proportional to arsenic, bismuth, antimony content, compares quantitative with standard series；But assay method at present
The full arsenic of soil, full bismuth, only some can be entered in plant full antimony content by root system of plant, remainder is integrally fixed at
Being combined into indissoluble state in soil crystal or with other material in soil, do not possess biologically effective activity, therefore measurement result is not
Soil activation state arsenic, bismuth, antimony can be represented plant absorption affected state.
This patent is to the Bashan Mountain, Qinling Mountains regional soil heavy metal arsenic, bismuth, antimony full dose, soil activation state arsenic, bismuth, antimony and agriculture
On the basis of product heavy metal arsenic, bismuth, antimony full dose are analyzed, research heavy metal-polluted soil full dose, activated state content produce with agricultural
Heavy metal arsenic, bismuth, the dependency of antimony full dose in product, create " a kind of soil activation state arsenic, bismuth, the detection method of antimony ", should
The soil activation state arsenic of analysis method detection, bismuth, antimony content can reflect heavy metal-polluted soil arsenic, bismuth, antimony and plant to greatest extent
Relation between absorption, characterizes heavy metal pollution of soil state；Through retrieving domestic and international pertinent literature, find no and " a kind of soil
Earth activated state arsenic, bismuth, the detection method of antimony " report of identical content.
Summary of the invention
Soil activation state arsenic, bismuth, the detection of antimony are analyzed and are used diethylenetriamine pentaacetic acid extraction atomic fluorescence spectrometer inspection
Survey method；Diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine buffer solution is used to extract out soil activation as digestion agent, chelating
State arsenic, bismuth, antimony, measure by atomic fluorescence spectrometer method；The most appropriate diethylenetriamine pentaacetic acid is chelating agen, appropriate chlorination
In calcium, calcium ion is chelating extraction poising agent, and chloride ion prevents the dissolving of free calcium carbonate in calacareous soil, it is to avoid because of carbonic acid
Calcium wrapped cover arsenic, bismuth, antimony element release and the impact that produces；Appropriate triethanolamine, as buffer agent, can make pH value of solution protect
Holding about 7.3, triethanolamine also has supression effect to dissolution of calcium carbonate simultaneously.
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
Activated state arsenic, bismuth, the detection of antimony；Weigh the air-dried sample 20.00g by 2mm aperture nylon mesh in 200mL plastic bottle, add
Enter the diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent 40mL of 25 DEG C ± 2 DEG C, build bottle cap, shake up, 25 DEG C ± 2
Under conditions of DEG C, 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 content is the lowest in soil soil activation state arsenic, bismuth, the detection of antimony；Concrete grammar is to use 100.0 μ in general measure
G/L arsenic, bismuth, antimony standard solution concentration 1/10 as the arsenic in the present invention, bismuth, antimony titer concentration, i.e. 10.0 μ g/
L；Standard curve uses ultralow mass concentration standard curve, and arsenic, bismuth, antimony standard curve maximum upper limit take 2.0 μ g/L, on zero point
First concentration value use conventional criteria to measure in arsenic, bismuth, the 1/5 of antimony concentration of standard solution 1.0 μ g/L, i.e. 0.2 μ g/L arsenic,
Bismuth, antimony are as on zero point in the present invention first standard curve concentration value.
Soil activation state arsenic, bismuth, the representation unit of antimony content are the micrograms of activated state arsenic, bismuth, antimony in every kilogram of soil
Or milligram number, representation unit is: μ g/kg or A × 10-3mg/kg；Soil activation state arsenic, bismuth, antimony content are the lowest, about exist
Between 0.0001mg/kg～0.01mg/kg, i.e. 0.1 μ g/kg～10 μ g/kg, during with normal international standard mg/kg representation unit
There is statement unit defect, convenient, with μ g/kg or A × 10 for reading and recording-3Mg/kg represents soil activation state arsenic, bismuth, antimony
Unit more gears to actual circumstances.
Detailed description of the invention
Soil activation state arsenic, bismuth, antimony one detection method: chelating extraction atomic fluorescence spectrometer method；Use diethyl three
Triamine pentaacetic acid-calcium chloride-triethanolamine buffer solution is as digestion agent, and wherein diethylenetriamine pentaacetic acid is chelating agen, calcium chloride
For 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
Arsenic, bismuth, antimony, use atomic fluorescence spectrometer method, uses ultralow mass concentration standard curve, measures soil activation state arsenic, bismuth, antimony.
Key instrument equipment: 1, analytical balance: precision is 0.0001g；2, atomic fluorescence spectrophotometer；3, arsenic, bismuth, antimony element
Hollow cathode lamp；4, acidometer；5, constant temperature (temperature control 25 DEG C ± 2 DEG C) reciprocating or rotary vibrating machine, or it is placed on thermostatic chamber
Interior common vibrating machine, meets the frequency of oscillation of 180r min-1 ± 20r min-1 or reaches same effect；6, water bath with thermostatic control
Device；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=1.19 g/mL；5, potassium hydroxide (KOH): top grade is pure；6, potassium borohydride
(KBH4): top grade is pure；7, thiourea (CH4N2S): analytical pure；8, ascorbic acid (C6H8O6): analytical pure；9, arsenic trioxide
(As2O3) top grade is pure；10, high pure metal bismuth；11, antimony oxide (Sb2O3)；12, 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 5.0g potassium hydroxide to put into and fill
In the beaker of 100mL experimental water, Glass rod stirring adds 2.5g 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；
13.8,5.0% potassium hydroxide solution: weigh after 25g potassium hydroxide dissolves and be diluted to 500mL with experimental water；
13.7,5.0% thiourea and ascorbic acid mixed solution: weigh thiourea, each 50g of ascorbic acid, dissolves with experimental water, fixed
It is dissolved in 1000mL volumetric flask；Mixing, uses preparation on the same day.
Arsenic (As), bismuth (Bi), antimony (Sb) standard solution:
14,1, arsenic (As) standard solution
14.1.1, arsenic Standard Reserving Solution: ρ=100.0mg/L；Buy commercially available certified reference material/have card standard sample, or weigh
0.1320g is through the top grade pure arsenic trioxide (As of 105 DEG C of dry 2h2O3) be dissolved in 5mL5.0% potassium hydroxide solution, use
The hydrochloric acid solution of 5.0% is neutralized to phenolphthalein redness and takes off, and experimental water is settled to 1000ml, mixing；
14.1.2 arsenic standard intermediate liquid: ρ=1.00mg/L；Pipette arsenic Standard Reserving Solution 5.00ml, be placed in the volumetric flask of 500mL,
Add 200mL50% hydrochloric acid solution, be settled to graticule with experimental water, mixing；
14.2, bismuth (Bi) standard solution
14.2.1, bismuth Standard Reserving Solution: ρ=100.0mg/L；Buy commercially available certified reference material/have card standard sample, or weigh
High pure metal bismuth 0.1000g, is placed in 100mL beaker, adds 20mL nitric acid, and low-temperature heat, to dissolving completely, cools down, and moves into
In 1000mL volumetric flask, it is settled to graticule with experimental water, mixing；
14.2.2, bismuth standard intermediate liquid: ρ=1.00mg/L；Pipette bismuth Standard Reserving Solution 5.00ml, be placed in the volumetric flask of 500mL
In, add 200mL50% hydrochloric acid solution, be settled to graticule with experimental water, mixing；
14.3, antimony (Sb) standard solution
14.3.1, antimony Standard Reserving Solution: ρ=100.0mg/L；Buy commercially available certified reference material/have card standard sample, or weigh
0.1197g is through the antimony oxide (Sb of 105 DEG C of dry 2h2O3) be dissolved in 80mL hydrochloric acid, proceed in 1000mL volumetric flask,
Add 120mL hydrochloric acid, be settled to graticule with experimental water, mixing；
14.3.2, antimony standard intermediate liquid: ρ=1.00mg/L；Pipette antimony Standard Reserving Solution 5.00ml, be placed in the volumetric flask of 500mL
In, add 200mL50% hydrochloric acid solution, be settled to graticule with experimental water, mixing；
14.4, arsenic, bismuth, antimony hybrid standard use liquid: arsenic, bismuth, antimony ρ=10.0 μ g/L；Pipette arsenic, bismuth, antimony standard intermediate liquid each
5.00ml, is placed in 500mL capacity, is settled to graticule with chelating digestion agent, 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, vibration liquid centrifuge filters after 5 minutes immediately；Retain filtrate,
Point taking 25.0mL filtrate is placed in 50mL volumetric flask, adds concentrated hydrochloric acid 10mL50% hydrochloric acid solution, 5.0% thiourea and ascorbic acid and mixes
Closing solution 10mL, be settled to graticule mixing with diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent, room temperature is placed
30min；When room temperature is less than 15 DEG C, it is placed in 30 DEG C of water-baths insulation 20min；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, according to instrument operation instructions set lamp
The running parameters such as electric current, negative high voltage, carrier gas flux, shield gas flow amount, preheating prepares arsenic or the bismuth element hollow cathode lamp of detection
20 minutes；Reference conditions are shown in Table 1；
The running parameter of table 1 atomic fluorescence spectrophotometer
The preparation of 16.2, calibration series: arsenic (As), bismuth (Bi), the calibration series of antimony (Sb)；
Pipette ρ=10.0 μ g/L arsenic (As), bismuth (Bi), antimony (Sb) standard mixed liquor 0.00,1.00,2.00,3.00,5.00,
7.00,10.00mL is in 50mL volumetric flask, adds 50% hydrochloric acid solution 10mL, 5.0% thiourea and ascorbic acid mixed solution
10mL, is settled to graticule with diethylenetriamine pentaacetic acid-calcium chloride-triethanolamine digestion agent, mixing；Room temperature places 30min；Room
When temperature is less than 15 DEG C, it is placed in 30 DEG C of water-baths insulation 20min.Arsenic, bismuth, the calibration serial solution concentration of antimony are shown in Table 2；
Table 2 arsenic (As), bismuth (Bi), antimony (Sb) element alignment serial solution concentration unit: g/L
16.3, draw calibration curve: with solution of potassium borohydride as reducing agent, 5% hydrochloric acid solution as current-carrying, by low concentration to highly concentrated
Degree sequentially measures the atomic fluorescence intensity of calibration series standard solution.The calibration series atomic fluorescence blank with deduction zero-dose is strong
Degree is vertical coordinate, and concentration of element (μ g/L) corresponding in solution is abscissa, draws calibration curve；And according to identical reagent
Blank assay is carried out with 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 arsenic, bismuth, antimony；
In formula: the content of activated state arsenic, bismuth, antimony 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 arsenic, bismuth, antimony content representation unit be: 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
Significant digits.
Claims (8)
1. soil activation state arsenic, bismuth, antimony detection use chelating digestion agent to extract out soil activated state arsenic, bismuth, antimony, and it chelates extraction
The complete formula of agent is: diethylenetriamine pentaacetic acid 1.967g, is dissolved in 14.92g (about 13.3mL) triethanolamine and a small amount of water；Again will
After 1.47g calcium chloride is dissolved in water, proceed in the lump, in 1000mL volumetric flask, add water to about 950mL；Acidometer is used 1:1 hydrochloric acid
Solution or 1:1 ammonia regulation pH to 7.3, be settled to 1000mL with water.
2. chelating digestion agent in calcium chloride calcium ion be soil activation state arsenic, bismuth, antimony detection chelating extraction poising agent.
3. soil activation state arsenic, bismuth, the detection of antimony increase pedotheque quantity as far as possible to ensure the soil that in soil, content is the lowest
Earth activated state arsenic, bismuth, the detection of antimony, weigh sample 20.00g, adds chelating digestion agent 40mL.
4., on soil activation state arsenic, bismuth, antimony lixiviating solution before machine testing, soil extraction refilters after 5 minutes with centrifuge.
5. soil activation state arsenic, bismuth, antimony are detected as ensureing soil activation state arsenic that in soil, content is the lowest, bismuth, the detection of antimony；
Arsenic, bismuth, antimony standard solution concentration are 10 μ g/L.
6. soil activation state arsenic, bismuth, antimony examination criteria curve use ultralow mass concentration standard curve, first on zero point
Minimum uses the arsenic of 0.2 μ g/L, bismuth, antimony standard curve concentration.
7. soil activation state arsenic, bismuth, the representation unit of antimony content are μ g/kg.
8. soil activation state arsenic, bismuth, the representation unit of antimony content are 10-3mg/kg。
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| CN108362545A (en) * | 2018-03-21 | 2018-08-03 | 江苏实朴检测服务有限公司 | The method for measuring soil available arsenic |
| CN110632054A (en) * | 2019-10-30 | 2019-12-31 | 扬州杰嘉检测技术有限公司 | Atomic fluorescence detection method for antimony content in soil and sediment |
| CN110749583A (en) * | 2019-11-08 | 2020-02-04 | 广东优策检验检测技术有限公司 | Detection method for measuring arsenic in soil and sediment by using atomic fluorescence |
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