CN110412018A - The detection method of P elements in a kind of plant - Google Patents
The detection method of P elements in a kind of plant Download PDFInfo
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- CN110412018A CN110412018A CN201910847336.4A CN201910847336A CN110412018A CN 110412018 A CN110412018 A CN 110412018A CN 201910847336 A CN201910847336 A CN 201910847336A CN 110412018 A CN110412018 A CN 110412018A
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Abstract
The present invention provides a kind of detection methods of P elements in plant, belong to detection of content of element technical field.The present invention is cleared up and is cleared up in advance to plant sample using hydrogen peroxide and concentrated nitric acid, highly shortened the plant sample resolving time, and resolution is more complete, and reagent dosage is few, has lower cross contamination and volatilization loss；It is tested in conjunction with ICP-OES, so that the detection method has high sensitivity, precision good, wide dynamic range, opposite interference are small, analyze fireballing feature, can largely improve test quality and test speed.Embodiment statistics indicate that: the phosphorous recovery of detection method provided by the invention be 91~103%, detection be limited to 8.2 μ g/g.
Description
Technical field
The present invention relates to detection of content of element technical field more particularly to a kind of detection methods of plant species P elements.
Background technique
Phosphorus is the essential nonmetalloid of plant normal growth, belongs to the nonmetalloid that fusing point is low, volatile, because
This reasonably pre-processes plant, and to microelement phosphorus carry out accurate quantitative analysis be one merit attention the problem of.At present
Dry method digestion and wet digesting pretreatment sample are mostly used, colorimetric method for determining is reused.Such methods are complicated for operation, time-consuming long,
Poor sensitivity, Volatile Elements loss is larger, and pollution is not easy to control.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of detection methods of P elements in plant.Detection of the invention
Method highly shortened the plant sample resolving time, and resolution is more complete, and reagent dosage is few, has lower cross contamination and waves
Hair loss；Have the characteristics that analysis speed is fast, measurement quality is high.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of detection methods of P elements in plant, comprising the following steps:
Establish phosphorus standard solution mass concentration-absorbance value standard curve；
Plant sample, concentrated nitric acid and hydrogen peroxide are mixed, is successively cleared up and is cleared up in advance, obtain digestion solution；
ICP-OES test is carried out to the digestion solution, the absorbance value of the digestion solution is obtained, according to the phosphorus mark
Quasi- concentration of polymer solution-absorbance value standard curve, obtains the content of phosphorus in the plant sample；
The amount ratio of the plant sample, concentrated nitric acid and hydrogen peroxide is 0.1g:6~7mL:0.2~2mL；The hydrogen peroxide
Mass concentration be 30%.
Preferably, the mixed time is 15min.
Preferably, the temperature of the pre- resolution is 80~90 DEG C, and the time is 10~20min.
Preferably, the temperature of the resolution is 170~190 DEG C, and the time is 50~60min.
Preferably, rate >=5 DEG C/min of the temperature of the resolution is warming up to by the temperature for clearing up temperature in advance.
Preferably, after the resolution, including by gained digestion solution catch up with acid to 0.5mL, be then with mass concentration
0.5% nitric acid is settled to 10mL.
Preferably, when establishing phosphorus standard solution mass concentration-absorbance value standard curve, comprising the following steps:
Compound concentration is respectively the phosphorus standard solution of 0,1,2,5,10,20,50ppm, is carried out to the phosphorus standard solution
ICP-OES test, obtains the absorbance value of the phosphorus standard solution, obtains phosphorus standard solution mass concentration-absorbance value standard
Curve.
Preferably, the compound concentration is respectively the detailed process packet of the phosphorus standard solution of 0,1,2,5,10,20,50ppm
Include following steps:
The phosphorus standard solution is using the national standard sample phosphorus single element standard solution that concentration is 1000 μ g/mL as phosphorus standard
Stoste is prepared to obtain；The preparation method of the phosphorus standard solution the following steps are included:
Drawing 5,2.5mL concentration respectively is the phosphorus standard stock solution of 1000 μ g/ml into volumetric flask, dilute with 0.5% nitric acid
It releases to 50mL, prepares and obtain the phosphorus standard solution that concentration is 100ppm and 50ppm；Draw the phosphorus that 5,2.5mL concentration is 100ppm
Standard solution is diluted to 25mL into volumetric flask, with 0.5% nitric acid, and it is that 20, the phosphorus standard of 10ppm is molten that preparation, which obtains concentration,
Liquid；Drawing 1mL concentration is the phosphorus standard solution of 50ppm into volumetric flask, is diluted to 10mL with 0.5% nitric acid, preparation obtains
Concentration is the phosphorus standard solution of 5ppm；Drawing 5,2.5mL concentration is the phosphorus standard solution of 10ppm into volumetric flask, with 0.5%
Nitric acid is diluted to 25mL, prepares and obtains the phosphorus standard solution that concentration is 2,1ppm.
Preferably, the parameter of the ICP-OES test includes:
RF power is 1150W；Pump speed is 60r/min；Secondary air amount is 0.5L/min；Atomization gas flow is 0.7L/
min；Observed direction is vertical, observed altitude 12mm；Wavelength is 177.495nm or 178.284nm.
The present invention provides a kind of detection methods of P elements in plant, comprising the following steps: establishes phosphorus standard solution matter
Measure concentration-absorbance value standard curve；Plant sample, concentrated nitric acid and hydrogen peroxide are mixed, is successively cleared up and is cleared up in advance, obtained
To digestion solution；ICP-OES test is carried out to the digestion solution, the absorbance value of the digestion solution is obtained, according to described
Phosphorus standard solution mass concentration-absorbance value standard curve, obtains the content of phosphorus in the plant sample；The plant sample,
The amount ratio of concentrated nitric acid and hydrogen peroxide is 0.1g:6~7mL:0.2~2mL；The mass concentration of the hydrogen peroxide is 30%.
The present invention is cleared up and is cleared up in advance to plant sample using hydrogen peroxide and concentrated nitric acid, highly shortened plant sample
The product resolving time, resolution is more complete, and reagent dosage is few, has lower cross contamination and volatilization loss；It is surveyed in conjunction with ICP-OES
Examination, so that the detection method has high sensitivity, precision good, wide dynamic range, opposite interference are small, analyze fireballing spy
Point can largely improve test quality and test speed.Embodiment statistics indicate that: the phosphorus of detection method provided by the invention
The rate of recovery is 91~103%, and detection is limited to 8.2 μ g/g.
Specific embodiment
The present invention provides a kind of detection methods of P elements in plant, comprising the following steps:
Establish phosphorus standard solution mass concentration-absorbance value standard curve；
Plant sample, concentrated nitric acid and hydrogen peroxide are mixed, is successively cleared up and is cleared up in advance, obtain digestion solution；
ICP-OES test is carried out to the digestion solution, the absorbance value of the digestion solution is obtained, according to the phosphorus mark
Quasi- concentration of polymer solution-absorbance value standard curve, obtains the content of phosphorus in the plant sample；The plant sample, dense nitre
The amount ratio of acid and hydrogen peroxide is 0.1g:6~7mL:0.2~2mL；The mass concentration of the hydrogen peroxide is 30%.
The present invention establishes phosphorus standard solution mass concentration-absorbance value standard curve.
In the present invention, when establishing phosphorus standard solution mass concentration-absorbance value standard curve, following step is preferably included
It is rapid:
Compound concentration is respectively the phosphorus standard solution of 0,1,2,5,10,20,50ppm, is carried out to the phosphorus standard solution
ICP-OES test obtains the absorbance value of the phosphorus standard solution, and establishes and obtain phosphorus standard solution mass concentration-absorbance
It is worth standard curve.
In the present invention, the compound concentration is respectively the specific mistake of the phosphorus standard solution of 0,1,2,5,10,20,50ppm
Journey preferably includes following steps:
The phosphorus standard solution is preferably using the national standard sample phosphorus single element standard solution that concentration is 1000 μ g/mL as phosphorus
Standard stock solution is prepared to obtain；The national standard sample phosphorus single element standard solution is preferably GSB 04-1741-2004 (a).
In the present invention, the preparation method of the phosphorus standard solution preferably includes following steps:
Drawing 5,2.5mL concentration respectively is the phosphorus standard stock solution of 1000 μ g/mL into volumetric flask, dilute with 0.5% nitric acid
It releases to 50mL, prepares and obtain the phosphorus standard solution that concentration is 100ppm and 50ppm；Draw the phosphorus that 5,2.5mL concentration is 100ppm
Standard solution is diluted to 25mL into volumetric flask, with 0.5% nitric acid, and it is that 20, the phosphorus standard of 10ppm is molten that preparation, which obtains concentration,
Liquid；Drawing 1mL concentration is the phosphorus standard solution of 50ppm into volumetric flask, is diluted to 10mL with 0.5% nitric acid, preparation obtains
Concentration is the phosphorus standard solution of 5ppm；Drawing 5,2.5mL concentration is the phosphorus standard solution of 10ppm into volumetric flask, with 0.5%
Nitric acid is diluted to 25mL, prepares and obtains the phosphorus standard solution that concentration is 2,1ppm.
In the present invention, the parameter of the ICP-OES test preferably includes:
RF power is preferably 1150W；Pump speed is preferably 60r/min；Secondary air amount is preferably 0.5L/min；Atomization air flow
Amount is preferably 0.7L/min；Observed direction is preferably vertical, and observed altitude is preferably 12mm；Wavelength be preferably 177.495nm,
178.284nm。
The present invention mixes plant sample, concentrated nitric acid and hydrogen peroxide, is successively cleared up and is cleared up in advance, obtains clearing up molten
Liquid.
In the present invention, the plant sample is preferably pre-processed before mixing with concentrated nitric acid and hydrogen peroxide；It is described
Pretreatment includes, and by plant in 105 DEG C of drying 2h, crushes and sieves with 100 mesh sieve after then drying to constant weight in 60 DEG C, extracting screen underflow storage
It deposits, obtains plant crushed material；Before being cleared up, get damp in order to prevent, by the plant crushed material in 105 ± 5 DEG C of drying 2h,
It is balanced in drying basin later for 24 hours, obtain plant sample.
In the present invention, the mass concentration of the hydrogen peroxide is preferably 30%；The plant sample, concentrated nitric acid and hydrogen peroxide
Amount ratio be 0.1g:6~7mL:0.2~2mL, further preferably 0.1g:6~7mL:0.5~1.5mL, more preferably
0.1g:6~7mL:1.0mL.
In the present invention, after the plant sample, concentrated nitric acid and hydrogen peroxide mixing, preferably standing 15min.In the present invention
In, the mixing carries out preferably in counteracting tank.
In the present invention, the temperature of the pre- resolution is preferably 80~90 DEG C, and further preferably 85 DEG C；The pre- resolution
Time be preferably 10~20min, further preferably 15min.In the present invention, the pre- resolution is preferably catching up with sour plate enterprising
Row, it may be assumed that be placed in catch up with by the counteracting tank equipped with plant sample, concentrated nitric acid and hydrogen peroxide and be cleared up in advance on sour plate.
In the present invention, the temperature of the resolution is preferably 170~190 DEG C, and further preferably 180 DEG C；The resolution
Time be preferably 50~60min, further preferably 55min.In the present invention, resolution is warming up to by the temperature cleared up in advance
The heating rate of temperature is preferably >=5 DEG C/min, further preferably 5~10 DEG C/min；That is, by the temperature by clearing up in advance
The time for spending the temperature for being warming up to resolution is preferably controlled to be no more than 30min.In the present invention, the resolution preferably disappears in microwave
It is carried out on Xie Yi, it may be assumed that by counteracting tank after catching up with and being taken off on sour plate, counteracting tank is put into microwave dissolver and is cleared up.
In the present invention, it after resolution, preferably includes to catch up with gained digestion solution acid to 0.5mL, then uses mass concentration
It is settled to 10mL for 0.5% nitric acid, obtains digestion solution.In the present invention, described that acid is caught up with preferably to carry out on catching up with sour plate.
After obtaining digestion solution, the present invention carries out ICP-OES test to the digestion solution, obtains the digestion solution
Absorbance value obtains containing for phosphorus in the plant sample according to the phosphorus standard solution mass concentration-absorbance value standard curve
Amount.
In the present invention, the parameter of ICP-OES test is carried out to the digestion solution and to establish phosphorus standard solution quality dense
Degree-absorbance value standard curve parameter is consistent, and details are not described herein.
It is described in detail below with reference to detection method of the embodiment to P elements in plant provided by the invention, still
They cannot be interpreted as limiting the scope of the present invention.
The running parameter of progress ICP-OES test includes: in embodiment
RF power is 1150W；Pump speed is 60r/min；Secondary air amount is 0.5L/min；Atomization gas flow is 0.7L/
min；Observed direction is vertical, observed altitude 12mm；Wavelength is 177.495nm or 178.284nm.
Embodiment 1
Compound concentration is respectively the phosphorus standard solution of 0,1,2,5,10,20,50ppm, is carried out to series of phosphorus standards solution
ICP-OES tests and establishes standard curve, obtains phosphorus standard solution mass concentration-absorbance value standard curve, is y=
174.738*x+0.323。
It selects GSB-11 citrus leaf, GSB-3 corn, GSB-4 soya bean as plant sample to be measured, weighs the plant of 0.1g respectively
Object sample is separately added into concentrated nitric acid 6mL and hydrogen peroxide (quality 30%) 0.5mL in micro-wave diminishing pot, stands 15min, is put into
It catches up in sour plate, in 85 DEG C of pre- resolution 15min.Corresponding temperature program, 180 DEG C of guarantors are arranged to micro-wave diminishing pot according to sample size
Hold 50min；After resolution, micro-wave diminishing pot is taken out, catches up with acid to 0.5mL on catching up with sour plate, is settled to using 0.5% nitric acid
10mL obtains GSB-11 citrus leaf digestion solution, GSB-3 corn digestion solution and GSB-4 soya bean digestion solution；To gained GSB-
11 citrus leaf digestion solutions, GSB-3 corn digestion solution and GSB-4 soya bean digestion solution digestion solution carry out ICP-OES test；
Each plant sample to be measured implements 8 Duplicate Samples, averaged, as a result such as table 1.
P elements measurement result in table 1, detection method plant sample to be measured
Blank solution (the preparation method of blank solution are as follows: the hydrogen peroxide for being 30% by concentrated nitric acid 6mL and mass concentration
0.5mL mixing, stands 15min, is put into and catches up in sour plate, after 85 DEG C of pre- resolution 15min, then in 180 DEG C of holding 50min；Disappear
After solution, micro-wave diminishing pot is taken out, catches up with acid to 0.5mL, is settled to 10mL using 0.5% nitric acid, obtains blank sample) measurement
After 11 times, 3 times of instrument detection limits for being determined as P elements by blank solution measurement concentration standard deviation are that content is
0.082mg/L, according to sample sample weighting amount (0.1000g) and final constant volume (10mL), the detection limit of detection method
Are as follows: 0.082mg/L × 10mL/0.1000g=8.2 μ g/g.
Embodiment 2
Agricultural industry criteria method standard curve is established: using the anti-absorption photometry of molybdenum antimony, drawing phosphorus standard respectively makes
With liquid (10mg/L) 0.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL in 50mL volumetric flask, blank solution is added, it is dilute with water
It releases to about 30mL, 1~2 drop dinitrophenol dinitrophenolate indicator (2g/L) is added, 240g/L sodium hydroxide solution is added dropwise and is neutralized to just in Huang
Color adds 1 drop 2mol/L sulfuric acid solution, takes off solution yellow, and the anti-color developing agent 5.0mL of molybdenum antimony is added, shakes up, fixed with water
Hold to get 0.0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L phosphorus standard serial solution, room temperature condition
Lower placement 30min measures its absorbance, using phosphorus mass concentration as abscissa, absorbance with spectrophotometer at wavelength 700nm
Value is ordinate, and calculating standard curve is y=0.5066x-0.0046.
According to phosphorus yield method in plant in " People's Republic of China's agricultural industry criteria " NY/T2017-2011, point
It also known as takes 0.1g (citrus leaf, corn, soya bean standard sample) in digest tube, 1mL water infiltration is added, 5mL sulfuric acid is added, shakes
It is even, it is added in two portions hydrogen peroxide, each 2mL after vigorous reaction, is placed in heating on digestion furnace and disappears and boil, make solid matter
Disappearing becomes solution, whitens cigarette to sulfuric acid, and solution is brown, stops heating, and few drops of hydrogen peroxide are added after slightly cold, continue to heat
Disappear and boil about 5min, it is cooling, add few drops of hydrogen peroxide, repeatedly to solution in colourless or limpid, continue heating remove it is more
Remaining hydrogen peroxide, the process duration are about 8~12h；After cooling, digestive juice is fully transferred to 100mL capacity with water
In bottle, constant volume obtains series of samples solution, for measuring phosphorus content；Reagent blank test is done simultaneously.
Accurate 1~10mL (V1) series of samples solution of drawing is in 50mL (V2) volumetric flask, according to " agricultural industry criteria side
Method standard curve establish part ' be diluted with water to about 30mL ' " rise and operate according to methods, while blank test is done, with blank tune
Zero.Phosphorus content in the prepare liquid looked into the absorbance value measured by standard curve, if absorbance value is more than the extinction of 1.0mg/L
When spending, then redeterminated after diluting prepare liquid.
Phosphorus content is below standard recommendation value, the rate of recovery 84 in final testing result display citrus leaf, corn and soya bean
~91%, and blank pollution is more serious.
The above method and (0.1g is diluted to 100mL) after sample size unification in the present invention are compared, as a result such as table 2
It is shown.
Table 2, detection method of the invention are compared with agricultural industry criteria method
Embodiment 3
Concentrated nitric acid+the hydrogen peroxide (mass concentration 30%) for having selected different volumes to match respectively, concentrated nitric acid+hydrofluoric acid (matter
40%) measuring concentration is that nitric acid+hydrochloric acid (mass concentration 36%) is to citrus leaf standard sample, Standard for Maize sample and soya bean mark
Quasi- sample is tested (digestion time is 60min at this time) respectively, after reagent conditions optimize well, when to different resolutions
Between be also optimized.The results are shown in Table 3.
The rate of recovery (%) of P elements in the lower three kinds of standard samples of 3 different condition of table
As can be seen from Table 3: in the case where different acid solution different amounts proportions, citrus leaf standard sample, Standard for Maize
Sample is different with the rate of recovery of soya bean standard sample, not exclusively within an acceptable range, only in concentrated nitric acid+hydrogen peroxide (quality
Concentration is dosage 30%) when being 6~7mL+0.2~2mL, and the rate of recovery of three kinds of standard samples is in 90~110% models simultaneously
In enclosing, belong to the preferable result of effect.When digestion time is 30~40min, the rate of recovery is unsatisfactory, 50min or more the rate of recovery
Reach acceptable level, therefore, digestion time can be set to 50min.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. the detection method of P elements in a kind of plant, which comprises the following steps:
Establish phosphorus standard solution mass concentration-absorbance value standard curve；
Plant sample, concentrated nitric acid and hydrogen peroxide are mixed, is successively cleared up and is cleared up in advance, obtain digestion solution；
ICP-OES test is carried out to the digestion solution, obtains the absorbance value of the digestion solution, it is molten according to the phosphorus standard
Liquid mass concentration-absorbance value standard curve, obtains the content of phosphorus in the plant sample；
The amount ratio of the plant sample, concentrated nitric acid and hydrogen peroxide is 0.1g:6~7mL:0.2~2mL；The matter of the hydrogen peroxide
Measuring concentration is 30%.
2. detection method according to claim 1, which is characterized in that the mixed time is 15min.
3. detection method according to claim 1, which is characterized in that the temperature of the pre- resolution is 80~90 DEG C, the time
For 10~20min.
4. detection method according to claim 1, which is characterized in that the temperature of the resolution is 170~190 DEG C, the time
For 50~60min.
5. detection method described according to claim 1 or 3 or 4, which is characterized in that be warming up to described disappear by the temperature cleared up in advance
Rate >=5 DEG C of the temperature of solution/min.
6. detection method according to claim 1, which is characterized in that after the resolution, including by gained digestion solution
It catches up with acid to 0.5mL, is then settled to 10mL with the nitric acid that mass concentration is 0.5%.
7. detection method according to claim 1, which is characterized in that establish phosphorus standard solution mass concentration-absorbance value
When standard curve, comprising the following steps:
Compound concentration is respectively the phosphorus standard solution of 0,1,2,5,10,20,50ppm, carries out ICP-OES to the phosphorus standard solution
Test, obtains the absorbance value of the phosphorus standard solution, and it is bent to obtain the phosphorus standard solution mass concentration-absorbance value standard
Line.
8. detection method according to claim 7, which is characterized in that the compound concentration is respectively 0,1,2,5,10,20,
The detailed process of the phosphorus standard solution of 50ppm the following steps are included:
The phosphorus standard solution is using the national standard sample phosphorus single element standard solution that concentration is 1000 μ g/mL as phosphorus standard stock solution
Preparation obtains；The preparation method of the phosphorus standard solution the following steps are included:
Drawing 5,2.5mL concentration respectively is the phosphorus standard stock solution of 1000 μ g/ml into volumetric flask, is diluted to 0.5% nitric acid
50mL is prepared and is obtained the phosphorus standard solution that concentration is 100ppm and 50ppm；Draw the phosphorus standard that 5,2.5mL concentration is 100ppm
Solution is diluted to 25mL into volumetric flask, with 0.5% nitric acid, prepares and obtains the phosphorus standard solution that concentration is 20,10ppm；It inhales
It takes the phosphorus standard solution that 1mL concentration is 50ppm into volumetric flask, is diluted to 10mL with 0.5% nitric acid, preparation obtains concentration and is
The phosphorus standard solution of 5ppm；Drawing 5,2.5mL concentration is the phosphorus standard solution of 10ppm into volumetric flask, dilute with 0.5% nitric acid
It releases to 25mL, prepares and obtain the phosphorus standard solution that concentration is 2,1ppm.
9. detection method according to claim 1 or claim 7, which is characterized in that the parameter of ICP-OES test includes:
RF power is 1150W；Pump speed is 60r/min；Secondary air amount is 0.5L/min；Atomization gas flow is 0.7L/min；It sees
Surveying direction is vertical, observed altitude 12mm；Wavelength is 177.495nm or 178.284nm.
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| CN113720828A (en) * | 2021-09-27 | 2021-11-30 | 江苏省地质工程勘察院 | Method for determining phosphorus and sulfur in fresh plant sample by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method |
| CN117990772A (en) * | 2024-04-07 | 2024-05-07 | 中国科学院生态环境研究中心 | Method for determining phosphorus element in plant by utilizing ICP-MS |
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