CN111141859A - Analysis system and method for nitrogen element in fertilizer - Google Patents

Analysis system and method for nitrogen element in fertilizer Download PDF

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Publication number
CN111141859A
CN111141859A CN202010102043.6A CN202010102043A CN111141859A CN 111141859 A CN111141859 A CN 111141859A CN 202010102043 A CN202010102043 A CN 202010102043A CN 111141859 A CN111141859 A CN 111141859A
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China
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fertilizer
unit
intermediate product
acid
nitrogen
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CN202010102043.6A
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徐开群
曹学军
袁康
刘洪伟
罗建文
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Changsha Kaiyuan Instruments Co Ltd
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Changsha Kaiyuan Instruments Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/64Electrical detectors
    • G01N30/66Thermal conductivity detectors

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a method for analyzing nitrogen elements in a fertilizer, which comprises the following steps: adding a catalyst to a fertilizer sample; combusting the fertilizer sample; sequentially carrying out deacidification treatment and dewatering treatment on the intermediate product generated by the fertilizer sample; reducing the intermediate product and detecting the content of nitrogen element. Also discloses an analysis system of nitrogen element in fertilizer and an analysis method applying the nitrogen element in fertilizer. Compared with a Dumas combustion method adopted in the prior art, the method for analyzing the nitrogen element in the fertilizer adds two steps of adding the catalyst and performing deacidification and dewatering treatment, the adding of the catalyst is favorable for improving the decomposition speed and the decomposition degree of nitrate nitrogen, and the deacidification and dewatering treatment of the intermediate product formed after the fertilizer sample is combusted is favorable for prolonging the service life of relevant instruments corresponding to other operations after the combustion operation.

Description

Analysis system and method for nitrogen element in fertilizer
Technical Field
The invention relates to the field of element analysis and detection, in particular to an analysis method of nitrogen elements in a fertilizer. The invention also relates to an analysis system of the nitrogen element in the fertilizer and an analysis method applying the nitrogen element in the fertilizer.
Background
Current methods of determining nitrogen content in fertilizers include: firstly, a titration method after distillation or a back titration method; second, Dumas combustion method. The post-distillation titration method or the back titration method has long test time and large human error. The method for measuring the nitrogen content by adopting the direct sample introduction and decomposition of the Domas combustion method has the advantages that the nitrogen in the fertilizer sample exists in various forms such as ammonium nitrogen, nitrate nitrogen, amide nitrogen and the like, the nitrate nitrogen is difficult to decompose thoroughly in the combustion process of the sample, the nitrogen measurement result of the nitrate nitrogen is low, and the nitrogen element analysis result of the sample is lower than the actual level; in addition, the moisture content in the fertilizer sample is high, and the moisture content is easy to remain in pipelines to influence the reduction of nitrogen oxides, and influence the maintenance period of instruments and the use of subsequent instruments.
Disclosure of Invention
The invention aims to provide an analysis method of nitrogen in a fertilizer, which can improve the analysis and measurement precision of the nitrogen and prolong the service life of an instrument. The invention also aims to provide an analysis system for the nitrogen element in the fertilizer, and an analysis method for the nitrogen element in the fertilizer is applied.
In order to achieve the above object, the present invention provides a method for analyzing nitrogen in a fertilizer, comprising:
s1: adding a catalyst to a fertilizer sample;
s2: combusting the fertilizer sample;
s3: sequentially carrying out deacidification treatment and dewatering treatment on the intermediate product generated by the fertilizer sample;
s4: reducing the intermediate product and detecting the content of nitrogen element.
Preferably, the step of adding the catalyst into the fertilizer sample specifically comprises:
sucrose was added to the fertilizer samples.
Preferably, the step of performing acid removal treatment on the intermediate product generated by the fertilizer sample specifically comprises:
introducing an intermediate product generated by the fertilizer sample into an acid removal pipe added with halide;
the step of performing water removal treatment on the intermediate product generated by the fertilizer sample specifically comprises the following steps:
and introducing the intermediate product flowing out of the acid removal pipe into a water removal pipe.
Preferably, between the step S3 and the step S4, further comprising:
s30: storing all intermediate products;
the step of reducing the intermediate product comprises:
reducing the intermediate product quantitatively.
Preferably, the step of reducing the quantitative intermediate product specifically comprises:
and introducing the intermediate product into a quantitative valve, and pushing the quantitative intermediate product to flow into a reduction furnace from the quantitative valve by using carrier gas.
Preferably, the step of combusting the fertilizer sample further comprises:
monitoring the combustion state of the fertilizer sample;
the step of storing all intermediate products further comprises:
and monitoring whether all the intermediate products are stored in the gas storage tank, and if so, entering the step S4.
Preferably, the step of detecting the content of nitrogen element specifically comprises:
and introducing the reduced intermediate product into a thermal conductivity cell detector and collecting an electric signal of the thermal conductivity cell detector.
The invention also provides an analysis system of the nitrogen element in the fertilizer, and an analysis method of the nitrogen element in the fertilizer is applied, and the analysis method comprises the following steps:
a combustion unit; the combustion unit is used for combusting a fertilizer sample doped with a catalyst;
an acid and water removal unit; the acid and water removing unit is connected in series with the outlet end of the combustion unit and is used for sequentially removing acid substances and water in an intermediate product formed after the fertilizer sample is combusted;
a reduction unit; the reduction unit is connected in series with the outlet end of the acid and water removal unit and is used for reducing the intermediate product discharged by the acid and water removal unit;
a nitrogen element detection unit; the nitrogen element detection unit is connected in series with the outlet end of the reduction unit and is used for detecting the intermediate product discharged by the reduction unit and outputting a detection result.
Preferably, the acid and water removing unit comprises an acid removing pipe and a water removing pipe which are sequentially connected in series with the combustion unit.
Preferably, the device also comprises a quantitative supply unit and a carrier gas pushing unit; the acid and water removing unit and the carrier gas pushing unit are connected in parallel to the inlet end of the quantitative supply unit, and the outlet end of the quantitative supply unit is connected to the inlet end of the reduction unit.
Compared with the background art, the method for analyzing the nitrogen element in the fertilizer provided by the invention comprises the steps of adding a catalyst into a fertilizer sample; combusting the fertilizer sample; sequentially carrying out deacidification treatment and dewatering treatment on the intermediate product generated by the fertilizer sample; the four steps of reducing the intermediate product and detecting the content of nitrogen elements are basically the same as the operation of the prior art, and the steps of adding the catalyst in the first step and removing acid and water in the third step are the improvement points of the invention compared with the prior art.
The method for analyzing the nitrogen element in the fertilizer improves the decomposition speed and the decomposition degree of nitrate nitrogen by adding a catalyst such as sucrose into a fertilizer sample, and ensures that all nitrogen elements in the fertilizer sample are contained in an intermediate product obtained by combustion; through the acid removal treatment and the water removal treatment of the intermediate product formed after the fertilizer sample is combusted, the intermediate product is kept in a dry state before reduction and detection, acid components are reduced, and the phenomenon that water is reserved in related instruments corresponding to other operations after the combustion operation or the acid components damage the instruments is avoided.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a system for analyzing nitrogen in a fertilizer according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method for analyzing nitrogen in a first fertilizer according to an embodiment of the present invention;
fig. 3 is a schematic flow chart of a method for analyzing nitrogen in a second fertilizer according to an embodiment of the present invention.
The device comprises a gas storage tank 1, a quantitative supply device 2, a quantitative valve 21, a reduction furnace 3, a second purification pipe 4, a thermal conductivity cell detection device 5, a flow valve 611, a flow meter 612, a combustion part 62, a filter 63, a carrier gas input port 71, a first purification pipe 72, a pressure control valve 73, a flow stabilizing device 8, a combustion monitoring part 9, a pressure sensor 10, an acid removal pipe 11 and a water removal pipe 12.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order that those skilled in the art will better understand the disclosure, the invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Referring to fig. 1 to 3, fig. 1 is a schematic structural diagram of a system for analyzing nitrogen in a fertilizer according to an embodiment of the present invention; FIG. 2 is a schematic flow chart of a method for analyzing nitrogen in a first fertilizer according to an embodiment of the present invention; fig. 3 is a schematic flow chart of a method for analyzing nitrogen in a second fertilizer according to an embodiment of the present invention.
The invention provides a method for analyzing nitrogen elements in a fertilizer, which comprises the following steps:
s1: adding a catalyst to a fertilizer sample;
s2: combusting the fertilizer sample;
s3: sequentially carrying out deacidification treatment and dewatering treatment on the intermediate product generated by the fertilizer sample;
s4: reducing the intermediate product and detecting the content of nitrogen element.
The quality of the catalyst depends on the type of the catalyst and the quality of the fertilizer sample, and the fertilizer sample added with a proper amount of the catalyst can be placed in a combustion device such as a U-shaped combustion tube or a high-temperature combustion furnace for combustion, so that the fertilizer sample is decomposed at high temperature to obtain an intermediate material containing the analyzed gas.
The analysis method of the nitrogen element in the fertilizer provided by the invention aims at analyzing and measuring the nitrogen element in the fertilizer, so that the catalyst such as sucrose and the like only containing the hydrocarbon element can be selected as the type of the catalyst, and the interference of other elements on the measurement result of the nitrogen element is avoided.
When the fertilizer samples are combusted, all the fertilizer samples added into the combustion device are ensured to be fully and completely combusted, and then all the analysis gas obtained by combusting all the fertilizer samples enters the subsequent steps.
In the step of removing acid and water from the intermediate product containing the analyzed gas, the intermediate product may be introduced into a pipeline containing halide during acid removal, and the intermediate product subjected to acid removal may be cooled or introduced into a pipeline containing a drying agent during water removal.
As for the means for reducing the intermediate product and detecting nitrogen, reference is made to the related art apparatus and the operation thereof.
In summary, compared with the dumas combustion method adopted in the prior art, the method for analyzing the nitrogen element in the fertilizer adds two steps of adding the catalyst and performing the acid and water removal treatment, the adding of the catalyst is beneficial to improving the decomposition speed and the decomposition degree of nitrate nitrogen, and the acid and water removal treatment of the intermediate product formed after the fertilizer sample is combusted is beneficial to prolonging the service life of relevant instruments corresponding to other operations after the combustion operation.
The method for analyzing nitrogen element in fertilizer provided by the invention is further explained with reference to the attached drawings and the embodiment.
In a specific embodiment provided by the invention, the catalytic effect and the raw material cost of the catalyst are comprehensively considered, and if the catalyst adopts sucrose, the step one is specifically to add the sucrose into the fertilizer sample.
On the basis of the above embodiment, the present invention adopts the acid-removing pipe 11 and the water-removing pipe 12 connected in series and in communication to realize the acid-removing and acid-removing operation, the inlet end of the acid-removing pipe 11 is connected in series and in communication with the outlet end of the combustion device for performing the combustion operation, and the outlet end of the water-removing pipe 12 is connected in series and in communication with the inlet end of the reduction device for performing the reduction operation.
The acid-removing pipe 11 is embodied as a pipe containing halide, so the above-mentioned operation of removing acid and water is equivalent to first introducing the intermediate product generated by the fertilizer sample into the acid-removing pipe 11 added with halide, and then introducing the intermediate product flowing out from the acid-removing pipe 11 into the water-removing pipe 12.
Further, between the step S3 and the step S4, the method further includes:
s30: storing all intermediate products;
the step of reducing the intermediate product related to the invention is as follows:
reducing the intermediate product quantitatively.
In order to facilitate the analysis and measurement and improve the accuracy of the measurement result, the method provided by the invention carries out quantitative and fractional measurement on all intermediate products obtained after the fertilizer sample is combusted, therefore, after the acid and water removal treatment, all intermediate products generated in the stage of starting to combust and finishing to combust are gradually stored, and then quantitative intermediate products are taken out from the stored intermediate products in a fractional manner and are introduced into a reduction device for realizing reduction.
Since the intermediate product after the acid and water removal treatment is an analysis gas containing gaseous nitrogen elements, the analysis gas can be stored by using the gas storage tank 1.
As for the specific step of reducing a fixed amount of the intermediate product, the intermediate product may be introduced into the metering valve 21 and the fixed amount of the intermediate product may be pushed by the carrier gas to flow from the metering valve 21 into a reduction apparatus having a reduction function, such as the reduction furnace 3.
It should be noted that the carrier gas may be supplied by a carrier gas device.
In order to more accurately analyze and measure the content of the nitrogen element, the step of burning the fertilizer sample further comprises:
monitoring the combustion state of the fertilizer sample;
and the step of storing all intermediate products further comprises:
whether all the intermediate products are stored in the gas tank 1 is monitored, and if yes, the process proceeds to step S4.
The step of monitoring the combustion state of the fertilizer sample can be realized by adopting the principle and the device of infrared detection. In addition, when the combustion device is specifically set as a combustion furnace, the pressure of the intermediate material collected at the bottom end of the hearth can be detected.
In any of the above embodiments, the thermal conductivity cell detection device 5 may be used to detect the content of the nitrogen element, that is, the steps of detecting the content of the nitrogen element specifically include: and introducing the reduced intermediate product into the thermal conductivity cell detection device 5 and collecting the electric signal of the thermal conductivity cell detection device 5.
Of course, the intermediate product after reduction can also be introduced into other nitrogen element detection devices.
The invention also provides an analysis system of the nitrogen element in the fertilizer, and an analysis method of the nitrogen element in the fertilizer is applied, and the analysis method comprises the following steps:
a combustion unit; the combustion unit is used for combusting a fertilizer sample doped with a catalyst;
an acid and water removal unit; the acid and water removing unit is connected in series with the outlet end of the combustion unit and is used for sequentially removing acid substances and water in an intermediate product formed after the fertilizer sample is combusted;
a reduction unit; the reduction unit is connected in series with the outlet end of the acid and water removal unit and is used for reducing the intermediate product discharged by the acid and water removal unit;
a nitrogen element detection unit; the nitrogen element detection unit is connected in series with the outlet end of the reduction unit and is used for detecting the intermediate product discharged by the reduction unit and outputting a detection result.
The combustion unit may be provided as a U-shaped combustion tube as shown in fig. 1 or a high temperature combustion furnace; the acid and water removing unit can be arranged in series with the acid removing pipe 11 and the water removing pipe 12 of the combustion unit in sequence; the reduction unit can be arranged as a reduction furnace 3 which is connected in series with the outlet end of the acid and water removing unit; the nitrogen element detection unit may be provided as a thermal conductivity cell detection device 5 connected in series to the outlet end of the reduction unit.
The reduction furnace 3 and the thermal conductivity cell detection device 5 can also be connected in series and communicated with a second purification pipe 4 and a flow stabilizer 8, so that the analyzed gas entering the thermal conductivity cell detection device 5 is purified and the flow stability of the analyzed gas is improved; a filter 63 and a gas storage tank 1 can be connected between the water removing pipe 12 and the reducing furnace 3.
In order to facilitate detection and monitoring of the combustion state of the fertilizer sample and the collection state of the analyzed gas in the U-shaped combustion tube or the high-temperature combustion furnace, a combustion monitoring part 9 for monitoring the combustion state of the fertilizer sample in the U-shaped combustion tube or the high-temperature combustion furnace and a pressure detection part for detecting the pressure of the analyzed gas collected at the bottom of the U-shaped combustion tube or the high-temperature combustion furnace are connected between the U-shaped combustion tube or the high-temperature combustion furnace serving as the combustion device and the gas storage tank 1. The pressure detecting part may include a pressure sensor 10, and the pressure sensor 10 may be connected to an outlet of the gas storage tank 1 to close the outlet of the gas storage tank 1 when the analyzed gas is not completely collected at the bottom end of the furnace. This process can be accomplished using a solenoid valve.
The inlet end of the U-shaped combustion pipe or the high-temperature combustion furnace is used for feeding a fertilizer sample to be detected and also used for introducing combustion-supporting gas required by combustion of the fertilizer sample, therefore, the inlet end of the U-shaped combustion pipe or the high-temperature combustion furnace is connected in series and communicated with a combustion-supporting gas supply device, a flow valve 611 and a flow meter 612, and a proper amount of sufficient combustion-supporting gas is introduced into the combustion part 62 according to the reading of the flow meter 612 and the opening of a combustion state regulating valve of the material to be detected in the combustion part 62, wherein the combustion-supporting gas mostly adopts oxygen.
On the basis of the embodiment, the system for analyzing the nitrogen element in the fertilizer further comprises a quantitative supply unit and a carrier gas pushing unit; the acid and water removing unit and the carrier gas pushing unit of the system are connected in parallel with the inlet end of the quantitative supply unit, and the outlet end of the quantitative supply unit is connected with the inlet end of the reduction unit.
The carrier gas pushing unit may include a carrier gas input port 71 and a first purge pipe 72 and a pressure control valve 73 connected in series between the carrier gas input port 71 and the dosing unit in this order. The carrier gas may be oxygen. The first purge tube 72 is used to remove impurities such as moisture from the carrier gas, ensuring that the carrier gas entering the dosing unit does not interfere with the composition of the analyte gas. The pressure control valve 73 is used for the pressure of the carrier gas when it enters the dosing unit.
The dosing unit is provided as dosing means 2 comprising a dosing valve 21. The pressure control valve 73 of the carrier gas pushing unit and the gas storage tank 1 for storing the analysis gas formed by the combustion of the material to be measured are both communicated with the proportional valve 21, and the carrier gas pushes the quantitative intermediate product to be transported to the thermal conductivity cell measuring device 5.
The system and the method for analyzing the nitrogen element in the fertilizer provided by the invention are described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (10)

1. A method for analyzing nitrogen elements in a fertilizer is characterized by comprising the following steps:
s1: adding a catalyst to a fertilizer sample;
s2: combusting the fertilizer sample;
s3: sequentially carrying out deacidification treatment and dewatering treatment on the intermediate product generated by the fertilizer sample;
s4: reducing the intermediate product and detecting the content of nitrogen element.
2. The method for analyzing nitrogen elements in fertilizer according to claim 1, wherein the step of adding catalyst to the fertilizer sample comprises:
sucrose was added to the fertilizer samples.
3. The method for analyzing nitrogen elements in fertilizer according to claim 2, wherein the step of performing acid removal treatment on the intermediate product generated by the fertilizer sample comprises the following steps:
introducing an intermediate product generated by the fertilizer sample into an acid removal pipe (11) added with halide;
the step of performing water removal treatment on the intermediate product generated by the fertilizer sample specifically comprises the following steps:
the intermediate product flowing out of the acid removal pipe is led into a water removal pipe (12).
4. The method for analyzing nitrogen elements in fertilizer according to any one of claims 1 to 3, wherein between the step S3 and the step S4, further comprising:
s30: storing all intermediate products;
the step of reducing the intermediate product comprises:
reducing the intermediate product quantitatively.
5. The method for analyzing nitrogen element in fertilizer according to claim 4, wherein the step of reducing the quantitative intermediate product comprises the following steps:
and introducing the intermediate product into a quantitative valve (21) and pushing the quantitative intermediate product to flow into the reduction furnace (3) from the quantitative valve (21) by using carrier gas.
6. The method of analyzing elemental nitrogen in a fertilizer of claim 4, wherein said step of combusting said fertilizer sample further comprises:
monitoring the combustion state of the fertilizer sample;
the step of storing all intermediate products further comprises:
whether all the intermediate products are stored in the gas storage tank (1) is monitored, and if yes, the process goes to step S4.
7. The method for analyzing nitrogen in fertilizer according to any one of claims 1 to 3, wherein the step of detecting the content of nitrogen specifically comprises:
and introducing the reduced intermediate product into a thermal conductivity cell detector (5) and collecting an electric signal of the thermal conductivity cell detector (5).
8. An analysis system for nitrogen element in fertilizer, characterized in that, the analysis method for nitrogen element in fertilizer according to any one of claims 1 to 7 is applied, comprising:
a combustion unit; the combustion unit is used for combusting a fertilizer sample doped with a catalyst;
an acid and water removal unit; the acid and water removing unit is connected in series with the outlet end of the combustion unit and is used for sequentially removing acid substances and water in an intermediate product formed after the fertilizer sample is combusted;
a reduction unit; the reduction unit is connected in series with the outlet end of the acid and water removal unit and is used for reducing the intermediate product discharged by the acid and water removal unit;
a nitrogen element detection unit; the nitrogen element detection unit is connected in series with the outlet end of the reduction unit and is used for detecting the intermediate product discharged by the reduction unit and outputting a detection result.
9. The system for analyzing nitrogen elements in fertilizer according to claim 8, wherein the acid and water removing unit comprises an acid removing pipe (11) and a water removing pipe (12) which are sequentially connected in series with the combustion unit.
10. The system for analyzing nitrogen elements in a fertilizer according to claim 8, further comprising a dosing unit and a carrier gas pushing unit; the acid and water removing unit and the carrier gas pushing unit are connected in parallel to the inlet end of the quantitative supply unit, and the outlet end of the quantitative supply unit is connected to the inlet end of the reduction unit.
CN202010102043.6A 2020-02-19 2020-02-19 Analysis system and method for nitrogen element in fertilizer Pending CN111141859A (en)

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Citations (5)

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Publication number Priority date Publication date Assignee Title
US5612225A (en) * 1992-08-31 1997-03-18 Fisons Instruments S.P.A. Process and apparatus for determining total nitrogen content by elemental analysis
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CN211627474U (en) * 2020-02-19 2020-10-02 长沙开元仪器有限公司 Analysis system for nitrogen element in fertilizer

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Publication number Priority date Publication date Assignee Title
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CN103512858A (en) * 2013-09-13 2014-01-15 广东电网公司电力科学研究院 Measuring method of carbon, hydrogen and nitrogen contents in biomass fuel
JP2015210111A (en) * 2014-04-24 2015-11-24 株式会社三菱化学アナリテック Nitrogen analysis method
CN106092946A (en) * 2016-05-27 2016-11-09 鼎泰(湖北)生化科技设备制造有限公司 A kind of for determining nitrogen analysis and there is series connection except the system of water purification unit
CN211627474U (en) * 2020-02-19 2020-10-02 长沙开元仪器有限公司 Analysis system for nitrogen element in fertilizer

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