CA1121916A - Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizers - Google Patents
Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizersInfo
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- CA1121916A CA1121916A CA000325290A CA325290A CA1121916A CA 1121916 A CA1121916 A CA 1121916A CA 000325290 A CA000325290 A CA 000325290A CA 325290 A CA325290 A CA 325290A CA 1121916 A CA1121916 A CA 1121916A
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Abstract
RADIOACTIVATION METHOD FOR SIMULTANEOUS DETERMINATION
OF NITROGEN, PHOSPHORUS AND POTASSIUM CONTENT IN PLANTS
AND FERTILIZERS
Abstract of the Disclosure According to the invention, the radioactivation method for simultaneous determination of the nitrogen, phosphorus and potassium content in plants and fertilizers consists in exposing samples to be analyzed and standard samples to neutron irradiation and recording the spectra of the gamma radiation induced in said samples, whereupon the samples are laid aside for a period of time determined by the half-life of the interfering isotope. This is followed by again recor-ding the spectra of the samples being analyzed and of the standard samples and superposing the first and second spectra of the samples being analyzed and of the standard samples.
These spectra are then shifted relative to each other along the energy axis, and the contents of the elements being ana-lyzed are determined by thus comparing the spectra of the samples being analyzed and of the standard samples.
OF NITROGEN, PHOSPHORUS AND POTASSIUM CONTENT IN PLANTS
AND FERTILIZERS
Abstract of the Disclosure According to the invention, the radioactivation method for simultaneous determination of the nitrogen, phosphorus and potassium content in plants and fertilizers consists in exposing samples to be analyzed and standard samples to neutron irradiation and recording the spectra of the gamma radiation induced in said samples, whereupon the samples are laid aside for a period of time determined by the half-life of the interfering isotope. This is followed by again recor-ding the spectra of the samples being analyzed and of the standard samples and superposing the first and second spectra of the samples being analyzed and of the standard samples.
These spectra are then shifted relative to each other along the energy axis, and the contents of the elements being ana-lyzed are determined by thus comparing the spectra of the samples being analyzed and of the standard samples.
Description
~ 9 ~6 Titl~ o~ the Invention RADIOACTIVATION i~T~OD FOR SIMULTANEOUS DET~RMrl~ATIO~
OF Nii~ROGEN, PHOSPHORUS AND PCrASSIUM CON~NT IN PLANTS
AND VEGE~ABLES
Field of the Invention The present invention relates to tbe determination of tbe content o~ chemical elements in plants and fertiliæers and, mDre particularly,.to radioactivation methods for simul-taneous determi~ation o~ the nitrogen, potassium a~d ph~spho-ru~ content in plants and fertili2ers. Tbe inventiDn can be used in agriculture a~d forestr~
Background of the Invantion There is knDwn a method for simultaneous determination of the co~tent o~ several c~emical elements, such a~ nitro-g2n, phosphorus and potassium, in plant samples. AccDrdi~g to this methDd, samples to be analyzed a~d sta~dard samples are exposed to a fast neutron flux. A~ter a certain periDd of time, the spectrum o~ the gamma radiatio~ induced in tbe samples is recorded and analyzed with reference to the spectra o~ tbe standard samples b~ using the least squares method (cf. R.A. Srapen~a~ts, J.L. ~ovtoun, E. Vernin~ G. Aude, C. AxelrDd, "~éthode et installa~iDn de dosage automatique par acti~ation neutronique de N, P, E, Ca dans les végétau~", Proceadings of the Symposium on Nuclear Activation Techniques in ths Life Sciences~ April 10-14, 1972, Bled, Jugoslavia, I~ter~ational Atomic Energy Agency, Vie~na, 1972).
1 12 1 ~ 1 6 The method under revi~w is disadvantageous because o~
its low accurac~9 especially when analyzing plant samples with a silicon content of mDre than 0005 per cent by wei~ht.
This is due to tha fact that the pbDsphorus content is deter-mined from the radioactive isotope Al28 whicb is also produ-cad from silicon as a result o~ a competitive nuclsar reac-tiDn. In the case o~ phospborus deter~ination, t~e time bet~een the end of irradiation and tke moment the spectrum is ta~en is suc~ that the contributions of phosphorus and silicon to the spectrum of tbe irradiated plant sample practi-cally cannot be differentiat~d.
Summary of tbe Invention It 7 5 an objec~ o~ the present invention tD prDvide a method for simultane3us determination Df the ~itrogen, phos-ph~rus and potassium cDntent in plants and fertilizers, wbicb would ensure a higher accuracy of the analysis by resorting tD repeated recording of the spectra Df samples being analyzed and sta~dard samples~
~ he foregDing ob~ect is attained b~ providing a radio-activation method for simultaneous determinatiDn of the nitrogen, phosphorus and pDtaSSiUm content in plants and fer-tilizers~ wbereby samples to be analyzed and standard samples are exposed to neutrDn irradiation, the spactra of ga~ma radiation induced in said 9amples are recorded, and the nitrogan, phosphorus and potassium content is determined from said spactra, wAic~ method is characterized, according ~ ", . ~
~lZ1916 to the invention9 in that after recording tbe spectra, the samples being analyzed and standard ~amples are laid aside for a period of time determi~ d by the half-life of the in-terfering isotDpe, whersupon tbe spectra of the samples being analyzed and of the standard samples ara recorded again, the ~irst and ~econd spectra of the samples being analyzed and of the standard samples are superposed and shifted relative to each other along the e~ergy axis, and the content of the elements being analyzed is determined by comparing the spectra of the samples being analyzed and of the standard samples.
Detailed Description of t~e Invention The radioactivation method acco~ding to the invention is carriea out as follows.
~ tandard samples of nitrogen, phosphorus, potassium and silicDn and samples t~ be analyzed are exposed to a neutron flux emitted by a neutron gene~ator. After a periDd o~ time of 1 to 5 minutes, i.e. after a period o~ time sufficiently long for the decay to take place, the gamma radiation spectrum of the irradiated sample~ is rec~rded ~ith the use of spectromatric aquipment.
The standard samples and those being analyzed are then laid aside fDr a second period of timo of 5 tD 25 minutes, whereafter their spectra are recorded again. T~e first and second spectra are superposed; the discontinuities of the ~ 6 first spectra a~e filled ~ith por~ions of th~ secDnd spectra of tha respectivo samples, and the first and second spectra are shiftad relative to each other along the energy axis.
~he infor~ation thus receiwed is illustrated by the attached plots ~qhers i is the channel numb~r proportional to the energy of gamma radiationt and S is the number of pulses re-corded in a given cbannel.
The nitrogen, phosphDrus and potassium c~ntent is deter-mined by comparing the sp~ctra Df the standard samples with tbose o~ the samples being analyzed, which is done by using the conventional mathematical methods, such as the least sauares method~
The method according to the invention is fundamentally different from c~nventional methods serving the same purpose in tha~ instead of measuring the actual gamma radiation spectrum, the object of measuraments is a composite spectrum produced by superposing t~v~ spectra take~ after different periods of timeO Apart from the information on the gamma ra-diation energy distribution, the spectra thus suparposed also carry informatiQn on the change of this distribution with time, ~qhich accDunts for a higher accuracg o~ the analysis.
The fQllowing table CDmpareS the rasults of analyzing plant samples with the use of the conventional method and the one according to the in~ention. The analysis covered 4 types of control plant samples, ~amely, oat, barley, maize and grass mixture. Tùe c~nten~ of N? P and K in the sampl~s was det~rmin~d b~ ch~mical anal~sis.
Table _ _ .
q~ype Che Result Average Variation Ab~lute of mical C~emi- Value, wt.,o C~ffici~t ~f Difference Sample El~ cal M~t~Dd Prior Single from ment A~laly_ Accor- Ar~ Measurement, Results ~f sis, ding to ~,q~thOd 5~o Relat. Ch~mical wt.% Inven~ Anal~sis tion %
Method Pri~r ~ethod P~iDr Accor- Ar~ Accor- Art ding MethDd ding Met~od t~ to Inven- Inven-ti~n = ~ . .. .
OF Nii~ROGEN, PHOSPHORUS AND PCrASSIUM CON~NT IN PLANTS
AND VEGE~ABLES
Field of the Invention The present invention relates to tbe determination of tbe content o~ chemical elements in plants and fertiliæers and, mDre particularly,.to radioactivation methods for simul-taneous determi~ation o~ the nitrogen, potassium a~d ph~spho-ru~ content in plants and fertili2ers. Tbe inventiDn can be used in agriculture a~d forestr~
Background of the Invantion There is knDwn a method for simultaneous determination of the co~tent o~ several c~emical elements, such a~ nitro-g2n, phosphorus and potassium, in plant samples. AccDrdi~g to this methDd, samples to be analyzed a~d sta~dard samples are exposed to a fast neutron flux. A~ter a certain periDd of time, the spectrum o~ the gamma radiatio~ induced in tbe samples is recorded and analyzed with reference to the spectra o~ tbe standard samples b~ using the least squares method (cf. R.A. Srapen~a~ts, J.L. ~ovtoun, E. Vernin~ G. Aude, C. AxelrDd, "~éthode et installa~iDn de dosage automatique par acti~ation neutronique de N, P, E, Ca dans les végétau~", Proceadings of the Symposium on Nuclear Activation Techniques in ths Life Sciences~ April 10-14, 1972, Bled, Jugoslavia, I~ter~ational Atomic Energy Agency, Vie~na, 1972).
1 12 1 ~ 1 6 The method under revi~w is disadvantageous because o~
its low accurac~9 especially when analyzing plant samples with a silicon content of mDre than 0005 per cent by wei~ht.
This is due to tha fact that the pbDsphorus content is deter-mined from the radioactive isotope Al28 whicb is also produ-cad from silicon as a result o~ a competitive nuclsar reac-tiDn. In the case o~ phospborus deter~ination, t~e time bet~een the end of irradiation and tke moment the spectrum is ta~en is suc~ that the contributions of phosphorus and silicon to the spectrum of tbe irradiated plant sample practi-cally cannot be differentiat~d.
Summary of tbe Invention It 7 5 an objec~ o~ the present invention tD prDvide a method for simultane3us determination Df the ~itrogen, phos-ph~rus and potassium cDntent in plants and fertilizers, wbicb would ensure a higher accuracy of the analysis by resorting tD repeated recording of the spectra Df samples being analyzed and sta~dard samples~
~ he foregDing ob~ect is attained b~ providing a radio-activation method for simultaneous determinatiDn of the nitrogen, phosphorus and pDtaSSiUm content in plants and fer-tilizers~ wbereby samples to be analyzed and standard samples are exposed to neutrDn irradiation, the spactra of ga~ma radiation induced in said 9amples are recorded, and the nitrogan, phosphorus and potassium content is determined from said spactra, wAic~ method is characterized, according ~ ", . ~
~lZ1916 to the invention9 in that after recording tbe spectra, the samples being analyzed and standard ~amples are laid aside for a period of time determi~ d by the half-life of the in-terfering isotDpe, whersupon tbe spectra of the samples being analyzed and of the standard samples ara recorded again, the ~irst and ~econd spectra of the samples being analyzed and of the standard samples are superposed and shifted relative to each other along the e~ergy axis, and the content of the elements being analyzed is determined by comparing the spectra of the samples being analyzed and of the standard samples.
Detailed Description of t~e Invention The radioactivation method acco~ding to the invention is carriea out as follows.
~ tandard samples of nitrogen, phosphorus, potassium and silicDn and samples t~ be analyzed are exposed to a neutron flux emitted by a neutron gene~ator. After a periDd o~ time of 1 to 5 minutes, i.e. after a period o~ time sufficiently long for the decay to take place, the gamma radiation spectrum of the irradiated sample~ is rec~rded ~ith the use of spectromatric aquipment.
The standard samples and those being analyzed are then laid aside fDr a second period of timo of 5 tD 25 minutes, whereafter their spectra are recorded again. T~e first and second spectra are superposed; the discontinuities of the ~ 6 first spectra a~e filled ~ith por~ions of th~ secDnd spectra of tha respectivo samples, and the first and second spectra are shiftad relative to each other along the energy axis.
~he infor~ation thus receiwed is illustrated by the attached plots ~qhers i is the channel numb~r proportional to the energy of gamma radiationt and S is the number of pulses re-corded in a given cbannel.
The nitrogen, phosphDrus and potassium c~ntent is deter-mined by comparing the sp~ctra Df the standard samples with tbose o~ the samples being analyzed, which is done by using the conventional mathematical methods, such as the least sauares method~
The method according to the invention is fundamentally different from c~nventional methods serving the same purpose in tha~ instead of measuring the actual gamma radiation spectrum, the object of measuraments is a composite spectrum produced by superposing t~v~ spectra take~ after different periods of timeO Apart from the information on the gamma ra-diation energy distribution, the spectra thus suparposed also carry informatiQn on the change of this distribution with time, ~qhich accDunts for a higher accuracg o~ the analysis.
The fQllowing table CDmpareS the rasults of analyzing plant samples with the use of the conventional method and the one according to the in~ention. The analysis covered 4 types of control plant samples, ~amely, oat, barley, maize and grass mixture. Tùe c~nten~ of N? P and K in the sampl~s was det~rmin~d b~ ch~mical anal~sis.
Table _ _ .
q~ype Che Result Average Variation Ab~lute of mical C~emi- Value, wt.,o C~ffici~t ~f Difference Sample El~ cal M~t~Dd Prior Single from ment A~laly_ Accor- Ar~ Measurement, Results ~f sis, ding to ~,q~thOd 5~o Relat. Ch~mical wt.% Inven~ Anal~sis tion %
Method Pri~r ~ethod P~iDr Accor- Ar~ Accor- Art ding MethDd ding Met~od t~ to Inven- Inven-ti~n = ~ . .. .
2 3 4 5 6 7 8 9 0 at N 2.02 2.02 2.18 1.5 3.0 0.0 +8.0 P 0.43 0.46 0.30 8.1 13.0 +7.0 -3.02 0.51 0.56 0.57 8.8 15.1 +9.8 Gras9 N3 .35-3 .41 3 5 3-39 -9 2.8 +2,6 0.0 ~ixture p0.30~0.34 0;35 0.38 6.5 9.6 +2.9 ~11.8 E 2.10-2.30 2.26 2.60 4.3 6.9 0.0 ~13.0 Barle~ ~1. 94 1. 95 1. 94 3.0 2.7 l0.5 0.0 P0.39 0.40 0.41 7.216.6 +2.5 +5.1 K0.43 0-45 0.48 6.012.6 ~4.6 +11.6 Maize N1,62 1t64 1,64 3.22.7 +1.2 ~1.2 P0,37 0,38 ~39 7,810.7 ~2.7 +5.4 K0.38 0.35 0.24 ~.911.3 -10.2 -36.8 ~0 _ ~Zl!316 T~e forego~ng table ~akes it clear t~at the discrepancy between tha results of the chemical analysis and those ob--tained ~vith the use of the method according tD the invention are not greater than 10 per cent; t~e av~rage discrepancy is
3 per cent for N and 5 to 7 per cent fDr P and K. The con-vergence of tho rasults is also satisfactory, being 3 per cent for ~ and 6 to 9 per cent for P and E. On the contrary, the prior art method shows strong deviations in determining P and ~, which in a number of cases are as hig~ as 11 to 30 per cent; the variation cosfficients ars often as high as 10 to 15 per cent, vlhich is unacceptable.
A better understanding of the present i~vention ~i~ll be had from a co~sideratiDn of t~e following examples illustra-ting preferred embodiments t~ereofO
EXample 1 Standard samples of nitrogen, phosphorus, silicon and potassium and samples of oat are put intD polyethyle~e cap-sules Df a constant volums, egposed to a neutron flux of 14.5 Mev and put asids for a period of time of 1 to 2 minutas for tha decay to ta~s place~ A gamma radiation spectrum is taken wit~ the aid of a scintillatiDn detector and a multi-channel pulse-hsight analyzer; the spectrum is take~ in 100 channels of the analyzsr. The standard samples and thoss being analyzed are thsn laid aside for a second period of time of 16 minutes, whereupDn they are transferred to a se-cond detector~
~21916 ~ scintil1atio~ gamma radiati3n spectrum is again taken in 100 channels of the analyzer and added to the first spectra of the respecti~e standard samplas and samples being anal~zed as channel~ 101 throu~h 200.
P1DtS 1 through 15 repxesent the informa~io~ thus ob-tained.
~ IG. 1, where i is the cha~nel number proportiDnal to the Oamma radiation energy and S i9 t~e number of pulses re-c~rded in the channel, shows the spectrum of a standard sample of nitrogen, recorded 2 minutes a~ter the end of tbe irradiation~
FIG. 2 is plotted in t~e same coordinates as FIG~ 1 and ~ho~s tpe spectrum of the standard sa~ple o~ nitrogen, recar-ded 16 minutes after the end of the irradiatiDn.
FIG. 3 is plDtted in tha samq coordinates as ~IG. 1 and shDws a composite spectrum of the standard sample o~ nitrogen, produced b~ adding the first and second spectra tDgether FIGS 4 through 15 are plotted i~ t~e same cDordinates as FIG. 1 and show first and second sp ctra, as well as com-posite spectra of phosphorus9 silicon and potassium, and t~ose o~ the sar~ple bein~ analyzed, obtained as the spectra o~ FI~S 1, 2 and 3~
I~ order to find the concentrations o~ nitrogen, phos-phorus and potassium, the least squares method is used to divide t~e composite spectrum of the samp~e subjected to ~1219~6 anal~sis into those of the standard samples.
The period of time between the end of irradiation and the moment the first spcctrum i9 taken is 2 minutes. This period is sufficiently long for short-lived isotopes to decay (this applied, for example, to N16 whereof T1/2 =
=7.4 sec); yet tbis period is short enough fDr the activity o~ Al2~ produced from phosphorus and silicon to bs maintained at a reasDnabl~ ~igh level (~1/2 of Al 8 is 2.3 min). The second period of time during which thc sampl~s are put aside is 1~ minutes and is selected with due regard for t~e decay of the activity of A128.
20 weighed portions o~ oat wers used in the determina-tion of the nitrogen, phosphorus and potassium contant; The percentage by weig~t concentratiDns of these elemeats were as follows: N, 2.02; P~ 0.46; ~, 0.56.
Exa~ple 2 T~e analysis is carried out as in Exa~ple 1, but this time the ob~ect of the analysis is grass mixture.
The percentage b~ weight concentration~ of the ~hree elements are as follows: N~ 3.50; P~ 0~35; K, 2.26.
E~ample 3 The analysis is carried out as in ~xample 1, but the object of the a~alysis is barle~.
The parcentage by weight concentrations of the three elements are as follows: N, 1.95; P, 0.40; E, 00~5.
_g_ ~2~916 EXample 4 The analysis is carried ~ut as in EXample 1, but th9 object of the analysis is maize.
The percentage by weight concantrations Df the three elements are as follows: N, 1.64; P, 0~38; ~, 0 35.
A better understanding of the present i~vention ~i~ll be had from a co~sideratiDn of t~e following examples illustra-ting preferred embodiments t~ereofO
EXample 1 Standard samples of nitrogen, phosphorus, silicon and potassium and samples of oat are put intD polyethyle~e cap-sules Df a constant volums, egposed to a neutron flux of 14.5 Mev and put asids for a period of time of 1 to 2 minutas for tha decay to ta~s place~ A gamma radiation spectrum is taken wit~ the aid of a scintillatiDn detector and a multi-channel pulse-hsight analyzer; the spectrum is take~ in 100 channels of the analyzsr. The standard samples and thoss being analyzed are thsn laid aside for a second period of time of 16 minutes, whereupDn they are transferred to a se-cond detector~
~21916 ~ scintil1atio~ gamma radiati3n spectrum is again taken in 100 channels of the analyzer and added to the first spectra of the respecti~e standard samplas and samples being anal~zed as channel~ 101 throu~h 200.
P1DtS 1 through 15 repxesent the informa~io~ thus ob-tained.
~ IG. 1, where i is the cha~nel number proportiDnal to the Oamma radiation energy and S i9 t~e number of pulses re-c~rded in the channel, shows the spectrum of a standard sample of nitrogen, recorded 2 minutes a~ter the end of tbe irradiation~
FIG. 2 is plotted in t~e same coordinates as FIG~ 1 and ~ho~s tpe spectrum of the standard sa~ple o~ nitrogen, recar-ded 16 minutes after the end of the irradiatiDn.
FIG. 3 is plDtted in tha samq coordinates as ~IG. 1 and shDws a composite spectrum of the standard sample o~ nitrogen, produced b~ adding the first and second spectra tDgether FIGS 4 through 15 are plotted i~ t~e same cDordinates as FIG. 1 and show first and second sp ctra, as well as com-posite spectra of phosphorus9 silicon and potassium, and t~ose o~ the sar~ple bein~ analyzed, obtained as the spectra o~ FI~S 1, 2 and 3~
I~ order to find the concentrations o~ nitrogen, phos-phorus and potassium, the least squares method is used to divide t~e composite spectrum of the samp~e subjected to ~1219~6 anal~sis into those of the standard samples.
The period of time between the end of irradiation and the moment the first spcctrum i9 taken is 2 minutes. This period is sufficiently long for short-lived isotopes to decay (this applied, for example, to N16 whereof T1/2 =
=7.4 sec); yet tbis period is short enough fDr the activity o~ Al2~ produced from phosphorus and silicon to bs maintained at a reasDnabl~ ~igh level (~1/2 of Al 8 is 2.3 min). The second period of time during which thc sampl~s are put aside is 1~ minutes and is selected with due regard for t~e decay of the activity of A128.
20 weighed portions o~ oat wers used in the determina-tion of the nitrogen, phosphorus and potassium contant; The percentage by weig~t concentratiDns of these elemeats were as follows: N, 2.02; P~ 0.46; ~, 0.56.
Exa~ple 2 T~e analysis is carried out as in Exa~ple 1, but this time the ob~ect of the analysis is grass mixture.
The percentage b~ weight concentration~ of the ~hree elements are as follows: N~ 3.50; P~ 0~35; K, 2.26.
E~ample 3 The analysis is carried out as in ~xample 1, but the object of the a~alysis is barle~.
The parcentage by weight concentrations of the three elements are as follows: N, 1.95; P, 0.40; E, 00~5.
_g_ ~2~916 EXample 4 The analysis is carried ~ut as in EXample 1, but th9 object of the analysis is maize.
The percentage by weight concantrations Df the three elements are as follows: N, 1.64; P, 0~38; ~, 0 35.
Claims
1. A radioactivation method for simultaneous deter-mination of the nitrogen, phosphorus and potassium content in plants and fertilizers, whereby samples to be analyzed and standard samples are exposed to neutron irradiation, the spectra of gamma radiation induced in said samples are re-corded, and said samples are laid aside for a period of time determined by the half-life of the interfering isotope, whereupon the spectra of the samples being analyzed and those of the standard samples are recorded again, the first and second spectra of the samples being analyzed and standard samples are superposed and shifted relative to each other along the energy axis, and the content of the elements being analyzed is determined by comparing the spectra of the samples being analyzed and of the standard samples.
Priority Applications (1)
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CA000325290A CA1121916A (en) | 1979-04-06 | 1979-04-06 | Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizers |
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CA000325290A CA1121916A (en) | 1979-04-06 | 1979-04-06 | Radioactivation method for simultaneous determination of nitrogen, phosphorus and potassium content in plants and fertilizers |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110749612A (en) * | 2019-11-27 | 2020-02-04 | 湖北富邦科技股份有限公司 | Novel method for measuring potassium content in fertilizer |
CN110749613A (en) * | 2019-11-27 | 2020-02-04 | 湖北富邦科技股份有限公司 | Method for on-line analysis of phosphate ore |
-
1979
- 1979-04-06 CA CA000325290A patent/CA1121916A/en not_active Expired
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110749612A (en) * | 2019-11-27 | 2020-02-04 | 湖北富邦科技股份有限公司 | Novel method for measuring potassium content in fertilizer |
CN110749613A (en) * | 2019-11-27 | 2020-02-04 | 湖北富邦科技股份有限公司 | Method for on-line analysis of phosphate ore |
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