CN108645882A - X-ray fluorescence method measures the scaling method of sulfur content in sulfur-coated urea - Google Patents
X-ray fluorescence method measures the scaling method of sulfur content in sulfur-coated urea Download PDFInfo
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Abstract
The present invention relates to the scaling methods that x-ray fluorescence method measures sulfur content in sulfur-coated urea, prepare calibration object：It weighs the higher sulphur of purity respectively to mix in proportion with urea, control sulfur content is 0%~60wt%, then utilizes the above-mentioned calibration substance of excitation of X-rays, and standard curve is established with element sulphur response signal and sulfur content；Measure sulfur content：According to calibration substance preparation method, sample to be tested is handled, then carries out quantitative analysis using X-ray fluorescence spectra, the sulfur content in sample to be tested is obtained by standard curve.Compared with prior art, the present invention has many advantages, such as easy to operate, quick, safe.
Description
Technical field
The present invention relates to a kind of scaling methods, and measuring sulphur in sulfur-coated urea more particularly, to a kind of x-ray fluorescence method contains
The scaling method of amount.
Background technology
China is large agricultural country, and agricultural is the basis of national economy, and chemical fertilizer occupies in China's grain-production and its
Consequence is maximum goods and materials investment in peasant's productive investment, accounts for about the 50% of its whole productive expenditure.According to system
Meter, the total output of China's chemical fertilizer account for a quarter in the world, and total amount of application of chemical fertilizer accounts for the one third in the world.In China, change
Fertilizer is about 46.3% to the contribution rate that grain increases.With the growth of population, in order to meet people's goods and materials needs, grain production is improved
Amount, increasing the input of fertilizer can not avoid.But mass data shows that the utilization rate of fertilizer in China is still universal relatively low, and also
Largely use caused problem of environmental pollution, such as body eutrophication, Total Nitrogen effusion special to atmosphere with fertilizer
It is the influence etc. of ozone layer.In addition, the problems such as also often resulting in the ordinary people trust whether healthy and safe to agricultural product.Now such as
What combines fertilizer and food security, environmental protection, how to keep agricultural high-efficiency continuous sound development at
The problem of being had received special attention in being studied for fertilizer.
Countries in the world are susceptible to loss and pollute environment all low for general chemistry utilization rate of fertilizer during use
The problems such as, it is numerous and confused to develop nutrient controlled release fertilizer, it is desirable that the release rule of fertilizer nutrient matches with the Nutrient Absorption of crop,
Not only it can realize that single fertilization saving of labor was efficient, but also utilization rate of fertilizer can be increased substantially.In order to improve the utilization rate of chemical fertilizer, from 20
Beginning of the century people just propose the imagination of slow release chemical fertilizer, and release and release control fertilizer is the advanced form of slow release fertilizer.Compared with conventional fertilizers,
The appearance of release and release control fertilizer has very big advantage, can not only improve utilization rate of fertilizer, reduces fertilizer amount, and it is rich to reduce water body
Nutrient laden, or even to a certain extent, release and release control fertilizer is not only a kind of agricultural material product, even more a kind of environmental product, because forming
For a research hotspot of current fertilizer circle and forward position.Release and release control fertilizer can significantly improve the utilization rate of fertilizer, reduce nutrient
Volatilization and elution loss, mitigate fertilising to the pollution of environment, the growth and development state that improves crop, the yield for improving crop and
Product quality.Since the coated fertilizer used in release and release control fertilizer is very expensive, cause the price of release and release control fertilizer generally excessively high, this is system
The major obstacle that about this concentrated fertilizer is widely applied.Use sulphur as main packet for this purpose, many experts and scholar explore
Membrane material and be manufactured that sulfur coated slow release fertilizer.
Sulfur-coated urea is to be developed for the first time by U.S. Tennessee Valley Authority country chemical fertilizer center for 1961, and in 1967
A kind of coated slow-release nitrogenous fertilizer of year formal commodity production.It is made by wrapping up sulphur and sealant outside urea, one
As nitrogenous 30%~40%, sulfur-bearing 10%~30%.And the characteristic of sulphur and sealant, packaging method, quantity will determine this
The release characteristics of product slow-release nitrogen.Sulphur coating use can effectively reduce fertilizer harm high in salt, reduce nutrient loss,
Sulphur nutrition is provided, adjusts nutrients release pattern, reaches the Fertilizer application rate that improves, reduces Effects of Fertilization Frequency, saves labour, to environment
Purpose that is friendly, improving plant economic quality and economic flow rate.Therefore the content high degree influence slow-release fertilizer of element sulphur is
Fertilizer release efficiency.
However mainly have for the assay method of sulfur content at present：(1) calcium, magnesium, sulphur contain in 19203 complex fertilizers of GB/T
The measurement of amount；(2) in AOAC in fertilizer " gravimetry of sulphur "；(3) three kinds of methods of GB 29401-2012 sulfur-coated ureas.
The assay method of sulphur in used measurement sulfur-coated urea is to be surveyed according to " GB29401-2012 sulfur-coated ureas " method
It is fixed, using the dissolution characteristics of sulphur, the acetone dissolution hydrotrope and the molten object of acetone for using water and sulphur to be saturated respectively, then it is molten with carbon disulfide
Go out whole sulphur, the content of sulphur is calculated by Subtraction method.But this assay method is complicated for operation, time-consuming and laborious and high temperature item
Existing security risk under part, and also have certain pollution to environment.
Therefore, there is an urgent need to study a kind of new method easy to operate, quick, safe to replace existing experimental method, with
Meet the needs of sulphur coated slow release fertilizer process quality control and the inspection of field of circulation fertilizer quality.
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of easy to operate, fast
Speed, safe x-ray fluorescence method measure the scaling method of sulfur content in sulfur-coated urea.
The purpose of the present invention can be achieved through the following technical solutions：
X-ray fluorescence method measures the scaling method of sulfur content in sulfur-coated urea, using following steps：
(1) calibration object is prepared：The higher sulphur of purity is weighed respectively to mix in proportion with urea, controls sulfur content model
It encloses and is built with sulfur content with element sulphur response signal then using the above-mentioned calibration substance of excitation of X-rays for 0%~60wt%
Day-mark directrix curve；
(2) sulfur content is measured：According to calibration substance preparation method, sample to be tested is handled, then utilizes X-ray glimmering
Light spectrum carries out quantitative analysis, and the sulfur content in sample to be tested is obtained by standard curve.
Sulphur is placed in urea and sample to be tested in sample cell component, which is followed successively by from bottom to top：Spiral shell
The wealthy mouth plastic bottle of spiral cover, polyethylene film, plastics inner supporting circle and screw top closure.Its plastics inner supporting circle can put down polyethylene film
Whole is fixed at the wealthy mouth plastic bottle inner ring position of bottleneck of screw lid, and when being detected, Xray fluorescence spectrometer can pass through should
Smooth polyethylene film window carries out element sulphur measurement.
Urea in step (1) is the urea of non-sulphur coating.
The sulphur weighed and urea are placed in agate mortar in step (1) and ground in fine-powdered, then by the mixing of milled
Object is placed in the wealthy mouth plastic bottle of screw lid, covers upper polyethylene film in bottleneck, plastics inner supporting circle is used in combination to put down polyethylene film
Site preparation is fixed at position of bottleneck, is inverted, and is shaken the wealthy mouth plastic bottle of screw lid and is uniformly distributed on polyethylene film to mixture,
Bottle cap finally is screwed under inversion state, is saved backup.
Step (1) weighs sulphur and urea is accurate to 0.0001g.
Sample to be tested in step (2) is placed in the wealthy mouth plastic bottle of screw lid, is covered upper polyethylene film in bottleneck, is used in combination
Polyethylene film is entirely fixed at position of bottleneck by plastics inner supporting circle, is inverted, and shakes the wealthy mouth plastic bottle of screw lid to mixing
Object is uniformly distributed on polyethylene film, is finally screwed on bottle cap under inversion state, is saved backup.
The Xray fluorescence spectrometer is commercial instruments, carries out element sulphur measurement through polyethylene film window, is carrying out
When detection, test window as shown in Fig. 2, bottleneck downward, sample is uniformly distributed in by the fixed smooth poly- second of plastics inner supporting circle
Alkene film surface, Xray fluorescence spectrometer can pass through the smooth polyethylene film window and carry out element sulphur measurement.
Compared with prior art, the present invention has the following advantages：
It has the following advantages：
1, the scaling method calibration substance that the present invention uses can be prepared once, long-term preservation, Reusability；
2, the scaling method that the present invention uses avoids laboratory without using having cytotoxic carbon disulfide reagent
The security risk that operating personnel accidentally inhale, eat by mistake；
3, the scaling method that the present invention uses, can quick determination sample without carrying out the pre-treatment such as digesting to chemical fertilizer sample
In specific components；
4, the scaling method that the present invention uses can be used commercially available commodity-type portable X-Ray Fluorescence spectrometer and is coated to sulphur
Sulfur content is measured in urea, and it is accurate to examine, simple and fast；
If 5, the scaling method that the present invention uses does not have test site equipped with portable X-Ray Fluorescence spectrometer
It is required that can be not only used for experimental determination, it is also suitable for the measurement of the online quality control and field place of factory.
6, the scaling method that the present invention uses reduces the dosage of chemical reagent, meets the requirement of Green Chemistry, reduces
Pollution to environment；
7, it is even need to only to crush sample mill for the scaling method that uses of the present invention, reduce laboratory operating procedures, reduce
Human error.
Description of the drawings
Fig. 1 is the decomposition texture schematic diagram of sample cell component；
Fig. 2 is structural schematic diagram when sample cell component uses；
Fig. 3 is 2 prepared canonical plotting of embodiment.
In figure, 1- screw top closures, 2- plastics inner supporting circle, 3- polyethylene films, the wealthy mouth plastic bottle of 4- screw lids, 5-X rays
Fluorescence Spectrometer test window, 6- demarcate object.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment
X-ray fluorescence method measures the scaling method of sulfur content in sulfur-coated urea, using following steps：
(1) calibration object is prepared：The higher sulphur of purity is weighed respectively mixed in proportion with urea (non-sulphur coating) be accurate to
0.0001g, for control sulfur content in the range of 0-60wt%, it is 0%, 5%, 10% that the present embodiment prepares content respectively,
15%, 25%, the sulphur weighed and urea are placed in agate mortar and grind in fine-powdered by 30% calibration object, then by milled
Mixture be placed in sample cell, the sample cell of use is as shown in Figs. 1-2, including screw top closure 1, plastics inner supporting circle 2, polyethylene
The wealthy mouth plastic bottle of film 3, screw lid 4.Plastics inner supporting circle 2 is hollow cylindrical device, and 2 diameter of plastics inner supporting circle is slightly less than described
Wealthy 4 bottleneck diameter of mouth plastic bottle of screw lid, plastics inner supporting circle 2 can be embedded at wealthy 4 position of bottleneck of mouth plastic bottle of screw lid,
And it can be fixed on polyethylene film 3 is smooth at wealthy 4 position of bottleneck of mouth plastic bottle of screw lid and do not move
It is dynamic.Plastics inner supporting circle 2 is placed in inside the wealthy mouth plastic bottle of screw lid 4, the top of the wealthy mouth plastic bottle of 1 lower end of screw top closure and screw lid 4
End is connected, and screw top closure 1 can be with the wealthy mouth plastic bottle of seal spiral cover 4.Calibration object 6 is uniform to be scattered in the polyethylene
At film 3, and realize that the fluorescence data of calibration object 6 acquires through Xray fluorescence spectrometer test window 5.
(2) sulfur content is measured：According to calibration substance preparation method, sample to be tested is handled, sample to be tested is placed in spiral shell
In the wealthy mouth plastic bottle of spiral cover, upper polyethylene film is covered in bottleneck, plastics inner supporting circle is used in combination entirely to fix polyethylene film
It at position of bottleneck, is inverted, shakes the wealthy mouth plastic bottle of screw lid and be uniformly distributed on polyethylene film to mixture, finally falling
It sets and screws on bottle cap under state, save backup, then carry out quantitative analysis using X-ray fluorescence spectra, obtained by standard curve
Sulfur content in sample to be tested.
Embodiment 2
Accurately weigh respectively 0.5000g sulphur (analysis pure, similarly hereinafter) and 9.5000g urea (analyze pure, similarly hereinafter),
1.0000g sulphur and 9.0000g urea, 1.5000g sulphur and 8.5000g urea, 2.0000g sulphur and 8.0000g urea,
2.5000g sulphur and 7.5000g urea, 3.0000g sulphur and 7.0000g urea, are respectively placed in agate by said mixture and grind
It is carefully milled to fine-powdered in alms bowl, then the mixture of milled is placed in the wealthy mouth plastic bottle of screw lid, upper poly- second is covered in bottleneck
Alkene film is used in combination plastics inner supporting circle to be entirely fixed on polyethylene film at position of bottleneck, is inverted.Then it is wealthy to shake screw lid
Mouth plastic bottle is uniformly distributed to mixture on polyethylene film, finally screws on bottle cap under inversion state.Above-mentioned calibration is used mixed
It is respectively 0%, 5%, 10%, 15%, 25%, 30% to close sulfur content in object.With the production of match Mo Feishier companies of the U.S.
The Xray fluorescence spectrometer of model ARL QUANTX measures above-mentioned calibration mixture, measured above-mentioned calibration mixing
The intensity value of object be respectively 141.34cps/mA, 4631.96cps/mA, 8183.08cps/mA, 11452.98cps/mA,
17982.09cps/mA, 21920.34cps/mA establish standard curve, standard by element sulphur response signal and sulfur content
Curvilinear equation is that (y is element sulphur response intensity value to y=704.89x+732.68, and x is sulfur content, coefficient R2=
0.9976), standard curve is as shown in Figure 3.Then sample to be tested is accurately weighed --- sulfur-coated urea sample is demarcated according to preparing
The same mode of object prepares sample to be tested, i.e., is placed on sulfur-coated urea sample to be carefully milled to fine-powdered in agate mortar,
The mixture of milled is placed in the wealthy mouth plastic bottle of screw lid again, upper polyethylene film is covered in bottleneck, plastics inner supporting circle is used in combination
Polyethylene film is entirely fixed at position of bottleneck, is inverted.Then the wealthy mouth plastic bottle of screw lid is shaken to mixture poly-
It is uniformly distributed on vinyl film, finally screws on bottle cap under inversion state.It is equally measured, is led to Xray fluorescence spectrometer
It is 11.1% to cross the sulfur content that standard curve returns to obtain sample to be tested sulfur-coated urea.
Embodiment 3
Accurately weigh respectively 0.5000g sulphur (analysis pure, similarly hereinafter) and 9.5000g urea (analyze pure, similarly hereinafter),
1.0000g sulphur and 9.0000g urea, 1.5000g sulphur and 8.5000g urea, 2.0000g sulphur and 8.0000g urea,
2.5000g sulphur and 7.5000g urea, 3.0000g sulphur and 7.0000g urea, are respectively placed in agate by said mixture and grind
It is carefully milled to fine-powdered in alms bowl, then the mixture of milled is placed in the wealthy mouth plastic bottle of screw lid, upper poly- second is covered in bottleneck
Alkene film is used in combination plastics inner supporting circle to be entirely fixed on polyethylene film at position of bottleneck, is inverted.Then it is wealthy to shake screw lid
Mouth plastic bottle is uniformly distributed to mixture on polyethylene film, finally screws on bottle cap under inversion state.Above-mentioned calibration is used mixed
It is respectively 0%, 5%, 10%, 15%, 25%, 30% to close sulfur content in object.With the production of match Mo Feishier companies of the U.S.
The Xray fluorescence spectrometer of model ARL QUANTX measures above-mentioned calibration mixture, measured above-mentioned calibration mixing
The intensity value of object be respectively 141.34cps/mA, 4631.96cps/mA, 8183.08cps/mA, 11452.98cps/mA,
17982.09cps/mA, 21920.34cps/mA establish standard curve, standard by element sulphur response signal and sulfur content
Curvilinear equation is that (y is element sulphur response intensity value to y=704.89x+732.68, and x is sulfur content, coefficient R2=
0.9976).Then sample to be tested is accurately weighed --- sulphur is coated complex fertilizer sample 1.5000g, and according to preparing, calibration object is same
Mode prepare sample to be tested, i.e., by sulphur coating complex fertilizer sample be placed on carefully being milled to fine-powdered in agate mortar, then
The mixture of milled is placed in the wealthy mouth plastic bottle of screw lid, upper polyethylene film is covered in bottleneck, is used in combination plastics inner supporting circle will
Polyethylene film is entirely fixed at position of bottleneck, is inverted.Then the wealthy mouth plastic bottle of screw lid is shaken to mixture in poly- second
It is uniformly distributed on alkene film, finally screws on bottle cap under inversion state.It is equally measured, is passed through with Xray fluorescence spectrometer
Standard curve returns to obtain the sulfur content of sample to be tested sulphur coating complex fertilizer to be 15.2%.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (7)
1.X ray fluorescences measure the scaling method of sulfur content in sulfur-coated urea, which is characterized in that this method uses following step
Suddenly：
(1) calibration object is prepared：It weighs the higher sulphur of purity respectively to mix in proportion with urea, control sulfur content is ranging from
Then 0%~60wt% utilizes the above-mentioned calibration substance of excitation of X-rays, established and marked with element sulphur response signal and sulfur content
Directrix curve；
(2) sulfur content is measured：According to calibration substance preparation method, sample to be tested is handled, then utilizes x-ray fluorescence light
Spectrum carries out quantitative analysis, and the sulfur content in sample to be tested is obtained by standard curve.
2. x-ray fluorescence method according to claim 1 measures the scaling method of sulfur content in sulfur-coated urea, feature exists
In the urea in step (1) is the urea of non-sulphur coating.
3. x-ray fluorescence method according to claim 1 measures the scaling method of sulfur content in sulfur-coated urea, feature exists
In the sulphur weighed and urea are placed in agate mortar in step (1) and ground in fine-powdered, then the mixture of milled is placed in
In the wealthy mouth plastic bottle of screw lid, upper polyethylene film is covered in bottleneck, plastics inner supporting circle be used in combination that polyethylene film is entirely solid
It at position of bottleneck, is inverted, shakes the wealthy mouth plastic bottle of screw lid and be uniformly distributed on polyethylene film to mixture, finally existed
Bottle cap is screwed under inversion state, is saved backup.
4. x-ray fluorescence method according to claim 1 measures the scaling method of sulfur content in sulfur-coated urea, feature exists
In step (1) weighs sulphur and urea is accurate to 0.0001g.
5. x-ray fluorescence method according to claim 1 measures the scaling method of sulfur content in sulfur-coated urea, feature exists
In the sample to be tested in step (2) is placed in the wealthy mouth plastic bottle of screw lid, covers upper polyethylene film in bottleneck, plastics are used in combination
Polyethylene film is entirely fixed at position of bottleneck by inner supporting circle, is inverted, and is shaken the wealthy mouth plastic bottle of screw lid to mixture and is existed
It is uniformly distributed on polyethylene film, finally screws on bottle cap under inversion state, save backup.
6. the x-ray fluorescence method according to claim 3 or 5 measures the scaling method of sulfur content in sulfur-coated urea, special
Sign is, element sulphur measurement is carried out through polyethylene film window using Xray fluorescence spectrometer.
7. x-ray fluorescence method according to claim 6 measures the scaling method of sulfur content in sulfur-coated urea, feature exists
In the Xray fluorescence spectrometer is commercial instruments.
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Application publication date: 20181012 |