CN106680461A - Method for determining lead content of red soil in Guizhou province and correcting factor thereof - Google Patents
Method for determining lead content of red soil in Guizhou province and correcting factor thereof Download PDFInfo
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Abstract
The invention discloses a method for determining lead content of red soil in Guizhou province and a correcting factor thereof. The method comprises the following steps of: taking a ratio of a determining value of the lead content in a soil sample acquired on the basis of the flame atomic absorption spectrometry to the determining value acquired on the basis of a 1:1 chloroazotic acid water-bath digestion-ICP-MS preliminary screening method as a correcting coefficient; taking an average value of the correcting coefficients of all the samples as the correcting factor; utilizing the correcting factor to quickly determine the lead content of the red soil in Guizhou province according to the 1:1 chloroazotic acid water-bath digestion-ICP-MS preliminary screening method. Through the method and the correcting factor, the determining time can be greatly shortened. The 1:1 chloroazotic acid water-bath digestion-ICP-MS preliminary screening method is adopted for correcting the determining value of the lead element in the soil, so that the application requirement in the practical work can be met.
Description
Technical field
The invention belongs to heavy metal-polluted soil detection technique field, and in particular to a kind of 1:At the beginning of 1 chloroazotic acid Water bath-ICP-MS
Sieve method determines the method and its correction factor of Guizhou Province's red soil lead content.
Background technology
Heavy metal pollution of soil (heavy metal pollution of the soil) is referred to due to mankind's activity, soil
Content of the minor metallic element in earth in soil exceedes background value, excess deposition and the too high levels that cause, is referred to as soil
Earth heavy metal pollution.Heavy metal-polluted soil referred to because mankind's activity is added to metal in soil, causes heavy metal in soil bright
The aobvious phenomenon for being higher than primary content and causing eco-environmental quality to deteriorate.
The heavy metal of contaminated soil mainly includes that hydrargyrum (Hg), cadmium (Cd), lead (Pb), chromium (Cr) and metalloid arsenic (As) etc. are raw
The significant element of thing toxicity, and have the elements such as zinc (Zn), copper (Cu), the nickel (Ni) of certain toxicity.Essentially from pesticide, give up
Water, sludge and atmospheric sedimentation etc., such as hydrargyrum are discharged and automobile exhaust gas essentially from mercury-containing waste water, cadmium, lead contamination essentially from smelting
Sedimentation, arsenic is then widely used as insecticide, antibacterial, rat poison and herbicide.Excessive heavy metal can cause physiological function of plants
Element concentration coefficients in crop grain such as disorderly, nutritional disorder, cadmium, hydrargyrum are higher, even more than food hygienic standard, also not shadow
Plant growth, development and yield are rung, in addition hydrargyrum, arsenic can weaken and suppress nitrification in soil, Ammonifying bacteria activity, affect nitrogen to supply
Should.Heavy metal contaminants mobility very little in soil, is difficult with water leaching, is not microbial degradation, is entered by food chain
After human body, potential hazard is very big, it should be specifically noted that preventing heavy metal to soil pollution.Stone is not yet set up in some mines in exploitation
Grand style and Tailings Dam, barren rock and mine tailing are arbitrarily stacked, and cause in mine tailing and enter soil rich in the heavy metal being difficult to resolve, and in addition Ore adds
Remaining metal waste residue enters ground water regime with rainwater after work, causes serious heavy metal pollution of soil.Therefore, soil is determined
The content of middle heavy metal, is the premise for preventing and treating heavy metal pollution of soil.And different regions, in soil type, heavy metal contains
The assay method of amount is had any different again, therefore, distinguish area and soil types heavy metal in soil content is measured is that have must
Want.
In heavy metal-polluted soil detection field, chloroazotic acid Water bath method completely can be leached out Arsenic in Soil, mercury element,
Suitable for all soil types.Detected with the use of atomic fluorescence spectrophotometer, short with digestion time, speed is fast, step
Simply, acid adding amount is few, and reagent interference is little, and preci-sion and accuracy is high, many merits such as favorable reproducibility.Ministry of Agriculture's environmental conservation
Scientific research monitoring is based on the method above advantage, develops GB/T22105.1-2008《Soil quality total mercury, total arsenic, total lead
Determine atomic fluorescence method part 1：The measure of Mercury In Soil》With GB/T 22105.2-2008《Soil quality total mercury, total arsenic,
The measure atomic fluorescence method part 2 of total lead：The measure of total Arsenic In Soil》Two national standards, drastically increase China pair
The detection level of Mercury In Soil and total arsenic.
Chloroazotic acid resolution method also has many applications, such as ISO 11466, Europe DIN in the detection application aspect of other elements
38414-S7 chloroazotic acid methods, U.S.'s USEPA SW846-3050 acid pasting and Taiwan NIEA S321.63B are chloroazotic acid
Resolution method.
But, using the method when Lead In Soil element is detected, due to being added without Fluohydric acid., therefore soil cannot be broken
Middle silicate mineral lattice, it is impossible to extract Lead In Soil element completely, causes detected value substantially low compared with it totally disappeared solution, because
This China does not recommend the method and goes to detect Lead In Soil element.
Inductivity coupled plasma mass spectrometry (ICP-MS) detection technique is a kind of by ICP thermal ionizations characteristic and quadrupole rod matter
A kind of new Element and isotope analytical technology that the advantage of the sensitive quick scanning of spectrometer combines and formed.It is provided
Extremely low detection limit, very wide dynamic linear response range, interference is less, precision is high, analyze speed is fast, is widely used in recent years
Various analysis fields.
At present, chloroazotic acid Water bath method determines heavy metal in soil content has substantial amounts of research and report in China.
Yang Yanfang such as Ministry of Agriculture's environment protection and monitoring institute exists《Determining heavy metals are cleared up in the chloroazotic acid backflow of pedotheque
The research of method》Middle finger goes out to use the method, and the measured value of chromium and lead element in standard sample is substantially lower than standard value, can
Seeing the chromium and lead of pedotheque can not be extracted with chloroazotic acid, and extraction ratio because different soil property difference it is larger.
The Qi Wenqi of China Environmental Monitoring General Station exists《With different acid dissolution methods to Pb in three class soil, Cr, Ni, Cd, Mn,
The dissolution of Cu, Zn is compared》In point out in addition to Fluohydric acid., the dissolution of lead, chromium is all than relatively low in various great soil groups.Because chromium and lead
Mainly contain in the mineral lattice of soil, and stable lattice.
The model of Guizhou Institute of Soil ＆ Fertilizer it is luxuriant and bdautiful in January, 2016 in Jiangsu's agriculture science volume 44 the 1st interim
Table《The ICP-MS methods of different pre-treatments mode determine 7 Heavy Metallic Elements in Guizhou Province's typical soil》.Article compared for resistance to
Hot glass long tube resolution method, Microwave Digestion and immersion method these three pre-treating methods, by many experiments immersion method energy is shown
Analysis application requirement is enough reached, is the pretreatment mode of a fast, economical for carrying out heavy metal-polluted soil screening.
But, in visible having been reported that, temporarily without method and its school that Guizhou Province's red soil lead element is cleared up for chloroazotic acid
Positive divisor, therefore the application demand in real work cannot be solved.
The content of the invention
It is an object of the invention to provide a kind of 1:Just sieve method measure Guizhou Province's red soil lead contains 1 chloroazotic acid Water bath-ICP-MS
The method and its correction factor of amount, to overcome existing chloroazotic acid resolution method to meet in real work to Lead In Soil element primary dcreening operation
Detection work application demand problem, to meet real work in high-volume Content of Pb in Soil primary dcreening operation work, so as to reach
Reduce reagent to use, reduce detecting step, reduce detection time, improve work efficiency, shorten the environmental accident emergency reaction time
Purpose.
Technical scheme is as follows：
The method of this measure Guizhou Province red soil lead content of the present invention is first to choose Guizhou Province's red soil pedotheque, each
Pedotheque makees parallel pair of sample；Atomic absorption spectrophotometry and 1 is used respectively:The first sieve methods of 1 chloroazotic acid Water bath-ICP-MS
Lead content in pedotheque is detected；Contain by the pedotheque lead of the measured value of atomic absorption spectrophotometry
The true value of amount, with 1:The measured value of the first sieve methods of 1 chloroazotic acid Water bath-ICP-MS is the non-correction value of the pedotheque lead content；
Using the ratio of the true value of the pedotheque lead and non-correction value as a correction coefficient；The correction coefficient of all samples it is average
Value is 1:The first sieve methods of 1 chloroazotic acid Water bath-ICP-MS determine the correction factor of Guizhou Province's red soil lead content；Use the correction factor
By 1:Lead content in the first sieve method quick detection Guizhou Province red soil soil of 1 chloroazotic acid Water bath-ICP-MS, i.e., by 1:1 chloroazotic acid
The value of lead content, is multiplied by correction factor, you can obtain Guizhou in Water bath-ICP-MS just sieve method detection Guizhou Province's red soil soil
Save the exact value of lead content in red soil soil.
Proposed by the present invention 1:1 chloroazotic acid Water bath-ICP-MS just sieve method determine the correction of Guizhou Province's red soil lead content because
Son, refers to the measured value and 1 of the atomic absorption spectrophotometry of be intended to pedotheque lead element content:1 chloroazotic acid water-bath disappears
The meansigma methodss of the ratio of the measured value of the first sieve methods of solution-ICP-MS.Wherein, the 1 of Guizhou Province's red soil lead content:1 chloroazotic acid Water bath-
The correction factor of the first sieve methods of ICP-MS is 1.24.
Further investigation and lot of experimental data discovery that the present invention passes through the principle to chloroazotic acid resolution method, chloroazotic acid resolution method
It is relevant with soil types and its parent rock lithology to the extracting efficiency of Lead In Soil element.Therefore, the present invention is according to different soils class
Type determines the correction factor of the soil types lead, detection of the method to soil lead element can be made to be worth to amendment, so as to full
Application demand in sufficient real work.
The present invention beneficial outcomes be：(1)《GB/T 17141-1997 soil quality lead, Cadmium detrmination sampling Graphite Furnace Atomic
Absorptiometry》The method for determining Lead In Soil, general time for sample pretreatment needs 5-6 hour, using the correction
The factor coordinates 1:Just sieve method is detected that time for sample pretreatment only needs to 2 hours, significantly to 1 chloroazotic acid Water bath-ICP-MS
Shorten detection time.(2) common chloroazotic acid Water bath method, due to the correction factor without lead, it is impossible in real work
It is applied.The present invention sums up 1 by lot of experimental data:Just sieve method determines Guizhou Province to 1 chloroazotic acid Water bath-ICP-MS
The correction factor of red soil lead content, makes detection of the method to Red Soil In Guizhou lead element be worth to amendment, so as to meet reality
Application demand in work.
Description of the drawings
Fig. 1 is that Guizhou Province's red soil lead element detects two kinds of pre-treating method dependency diagrams.
Specific embodiment
In order to deepen to present invention understanding, with reference to the accompanying drawings and examples the present invention is described in further detail.
The present invention from Inst. of Soils and Fertilizers, Guizhou Academy of Agricultural Sciences's sample library by choosing what 80 types determined
Guizhou Province's red soil pedotheque.Use respectively《GB/T 17141-1997 soil quality lead, Cadmium detrmination sampling Graphite Furnace Atomic Absorption point
Light photometry》(hereinafter referred to as standard technique) and 1:1 chloroazotic acid Water bath-ICP-MS just examined by sieve method (hereinafter referred to as immersion method)
Survey.Standard technique measured value is the true value of the pedotheque lead content, and immersion method measured value is not repairing for the pedotheque lead content
On the occasion of.Each pedotheque must make parallel pair of sample.The true value of the pedotheque lead is then the soil-like with the ratio of non-correction value
The correction coefficient of product lead element.The meansigma methodss of all correction coefficients are 1:Just sieve method determines expensive to 1 chloroazotic acid Water bath-ICP-MS
The correction factor of state province red soil lead content.
Presented below of the invention 1:The first sieve methods of 1 chloroazotic acid Water bath-ICP-MS determine the correction of Guizhou Province's red soil lead content
The specific embodiment and application example of the factor.
Embodiment 1：
1st, embodiment
(1) for examination soil
" the whole nation in Inst. of Soils and Fertilizers, Guizhou Academy of Agricultural Sciences's sample library is taken from for trying pedotheque《Agricultural product are produced
Ground heavy metal pollution of soil preventing and treating》GeneraI investigation " project pedotheque.Pedotheque quantity is 80, and soil types is red soil, soil
Earth granularity was 100 mesh sieve fine earths.
(2) main agents and instrument
1. main agents：Nitric acid (Merck KGaA is analyzed pure)；Hydrochloric acid (traditional Chinese medicines, top pure grade)；Perchloric acid (try, excellent by Kingsoftization
Level is pure)；Fluohydric acid. (Shanghai Shen is won, top pure grade)；Deionized water；ICP-MS standard reserving solutions (GSB 04-1767-2004, it is polynary
Plain standard solution, 100 μ g/mL, national non-ferrous metal and electronic material Institute of Analysis)；Rhodium (Rh) standard liquid (GSB 04-
1746-2004,1000 μ g/mL, national non-ferrous metal and electronic material Institute of Analysis)；Lead (Cr) standard liquid (GSB 04-
1723-2004 (a), 1000 μ g/mL, national non-ferrous metal and electronic material Institute of Analysis)；Diammonium phosphate (Tianjin section
Close Europe, top pure grade).
2. key instrument：8 hole electric-heated thermostatic water baths (Tianjin Stettlen)；Icp mses (ICP-
MS) (the silent winged generation that of match, Icap Q)；Hard glass color comparison tube (50mL, day glass)；A ten thousandth electronic balance (prunus mume (sieb.) sieb.et zucc. Teller support profit
It is many, AL240)；Electric hot plate (LabTech)；Flame atomic absorption spectrophotometer (Varian, AA240FS).
(3) detecting instrument condition
1. Instrument working parameter
ICP-MS detection patterns are KED；The detection target isotope of lead is Cr (52)；RF power is 1500W；Nebulizer stream
Amount, secondary air amount, cooling gas flow are respectively 0.9630,0.8000,14.000L/min；CCT throughputs are 5.1250L/
min。
Flame Atomic Absorption Spectrometry instrument condition：Wavelength 357.9nm is determined, passband width 0.7nm, flame properties are reproducibility,
Burner height 8mm.
2. interference and the correction of matrix effect
1:When the first sieve methods of 1 chloroazotic acid Water bath-ICP-MS determine the content of lead in Guizhou Province's red soil, due to having used king
Water, therefore mainly disturbed by multi-atomic ion 35Cl+16O+1H.To remove this interference, detection pattern selects KED (kinetic energy discriminations
Depending on pattern), meanwhile, in this mode, instrument parameter meets 59Co≤8000,59Co/35Cl16O≤18.It is molten to reduce sample
The matrix effect of liquid, correction is compensated from rhenium (Re) as internal standard substance.
(4) sample pre-treatments
Immersion method：0.1000g (being accurate to 0.0002g) Guizhou Province red soil sample is weighed respectively in 50mL color comparison tubes, plus
Enter 1:1 chloroazotic acid 3mL, vibration；2h, midway shake 1~2 time are heated in boiling water bath；Cooling is taken out, deionized water is settled to
50mL；Stand, upper machine testing.
Standard technique：0.2g (being accurate to 0.0002g) samples are accurately weighed in 50ml politef crucibles, water-wet is used
10ml hydrochloric acid is added afterwards, and low-temperature heat on the electric hot plate in fume hood makes sample preliminary exposition, to be evaporated when about 3ml is remained,
Remove slightly cold, be subsequently adding 5ml nitric acid, 5ml Fluohydric acid .s, 3ml perchloric acid, add a cover middle temperature heating 1h or so on electric hot plate,
Then uncap, electric plate temperature is controlled at 150 DEG C, continue plus evanescence of heat silicon, in order to reach good winged silicon effect, answer Jing often to shake
Crucible.When being heated to emitting dense perchloric acid white cigarette, add a cover, decompose black organic carbon compound.Treat that the black on sidewall of crucible has
After machine thing disappears, uncap, it is in sticky shape to drive white cigarette and steam to content.Depending on clearing up situation, 3ml nitric acid, 3ml hydrogen can be again added
Fluoric acid, 1ml perchloric acid, repeat above digestion process.Remove crucible slightly cold, add 3ml hydrochloric acid solutions, warm dissolving solubility is residual
Slag, full dose is transferred in 50ml volumetric flasks, adds 5ml ammonium dibasic phosphate aqueous solutions, and graticule is settled to water after cooling, is shaken up,
Examination with computer.
(5) result and analysis
With 1:Just sieve method determines Guizhou Province's red soil lead content to 1 chloroazotic acid Water bath-ICP-MS and the result of correction factor is shown in
Table 1.
Table 11:Just sieve method determines Guizhou Province's red soil lead content and correction factor to 1 chloroazotic acid Water bath-ICP-MS
By the testing result of two kinds of pre-treating methods, standard technique result is the pedotheque with the ratio of immersion method result
Correction coefficient, the meansigma methodss of all pedotheque correction coefficients are 1:Just sieve method determines expensive to 1 chloroazotic acid Water bath-ICP-MS
The correction factor of state province red soil lead content, is 1.24.
With immersion method result as the longitudinal axis, standard technique result is transverse axis, draws two kinds of pre-treating method dependency diagrams (figure
1)。
The dependency of two kinds of pre-treating methods is 0.9707, and dependency is good.Prove that the correction factor that the method draws is accurate
It is really reliable.
2nd, application example as shown in table 1, adopts 1:Just sieve method measures Guizhou Province's red soil sample to 1 chloroazotic acid Water bath-ICP-MS
The immersion method content of product lead, is multiplied by correction factor 1.24, obtains immersion method correction result.Compared with the true value that standard technique is measured
Compared with all result relative erroies are in the range of 50%.Therefore, the correction factor coordinates 1:At the beginning of 1 chloroazotic acid Water bath-ICP-MS
Sieve method is used, and has very big using value in the census operations of Guizhou Province's red soil lead element.
The above, is only presently preferred embodiments of the present invention, non-to make any pro forma restriction to the present invention, although
The present invention is disclosed above with preferred embodiment, but not to limit the present invention, any those skilled in the art,
In the range of technical solution of the present invention, when making a little change using the method and technology contents of the disclosure above or repair
The Equivalent embodiments for equivalent variations are adornd, as long as being an off the content of technical solution of the present invention, according to the technical spirit according to invention
Any simple modification, equivalent variations and the modification made to above example, still falls within the range of technical solution of the present invention.
Claims (3)
1. a kind of method of measure Guizhou Province red soil lead content, it is characterised in that：Guizhou Province's red soil pedotheque is chosen, each soil
Earth sample makees parallel pair of sample；Atomic absorption spectrophotometry and 1 is used respectively:The first sieve methods pair of 1 chloroazotic acid Water bath-ICP-MS
Lead content in pedotheque is detected；With the measured value of atomic absorption spectrophotometry as the pedotheque lead content
True value, with 1:The measured value of the first sieve methods of 1 chloroazotic acid Water bath-ICP-MS is the non-correction value of the pedotheque lead content；Will
The ratio of the true value of the pedotheque lead and non-correction value is used as a correction coefficient；The meansigma methodss of the correction coefficient of all samples
As 1:The first sieve methods of 1 chloroazotic acid Water bath-ICP-MS determine the correction factor of Guizhou Province's red soil lead content；It is logical with the correction factor
Cross 1:Lead content in the first sieve method quick detection Guizhou Province red soil soil of 1 chloroazotic acid Water bath-ICP-MS.
2. a kind of correction factor of measure Guizhou Province's red soil lead content that method according to claim 1 is obtained, it is characterised in that：Should
Correction factor is used for 1:Lead content in the first sieve method quick detection Guizhou Province red soil soil of 1 chloroazotic acid Water bath-ICP-MS, the correction
The factor refers to the measured value and 1 of the atomic absorption spectrophotometry of all pedotheque lead element contents:1 chloroazotic acid water-bath disappears
The meansigma methodss of the ratio of the measured value of the first sieve methods of solution-ICP-MS.
3. the correction factor of measure Guizhou Province red soil lead content according to claim 2, it is characterised in that：The correction factor
For 1.24.
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Application publication date: 20170517 |