CN105116021A - Device and method for rapidly detecting nutrient releasing rate of controlled-release fertilizer based on electric conductivity method - Google Patents
Device and method for rapidly detecting nutrient releasing rate of controlled-release fertilizer based on electric conductivity method Download PDFInfo
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- CN105116021A CN105116021A CN201510567563.3A CN201510567563A CN105116021A CN 105116021 A CN105116021 A CN 105116021A CN 201510567563 A CN201510567563 A CN 201510567563A CN 105116021 A CN105116021 A CN 105116021A
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Abstract
The invention belongs to the technical field of a test for detecting the nutrient releasing rate of a controlled-release fertilizer, relates to a device and method for rapidly detecting the nutrient releasing rate of the controlled-release fertilizer based on an electric conductivity method, and particularly relates to a device and method for rapidly detecting the still water dissolution rate and the accumulation releasing rate of the controlled-release fertilizer based on the electric conductivity method. The device comprises a bracket, a water feeding device, a glass container, a digital display electric conductivity instrument, an electronic stirrer, a PCL control system for controlling detection steps and the like. With the adoption of the special device, an uneven concentration distribution phenomenon caused by external temperature fluctuation and long-time standing of a solution to be detected is avoided; and the detected electric conductivity value of a nutrient solution is relatively reliable and accurate, and meanwhile, the operation time is greatly shortened.
Description
Technical field
The invention belongs to the technical field detecting the test of release and release control fertilizer nutrient release rate, relate to a kind of device and method detecting release and release control fertilizer nutrient release rate based on electrical conductivity method fast, particularly relate to a kind of device and method based on electrical conductivity method Fast Measurement release and release control fertilizer hydrostatic dissolution rate and preparation.
Background technology
The slow/controlled release performance of coated fertilizer evaluates one of its quality and important indicator of effectively using, and at present, the method evaluating the slow/controlled release performance of coated fertilizer mainly contains hydrostatic leaching and soil leaching etc.Be compared to soil leaching, hydrostatic leaching due to have easy and simple to handle, fast and the advantage such as result is reproducible, extensively adopted by domestic and international Ge great slowly/controlled releasing fertilizer manufacturing enterprise and scientific research institutions.
Also the Nutrient Release of hydrostatic Determination by Stripping coated fertilizer is adopted in slow release fertilizer national standard (GB/T-23348-2009), for the nutrient solution in hydrostatic leaching, usual employing chemical method directly measures nutrient content, such as nitrogen auto analyzer measures nutrients of nitrogen content, adopt molybdenum antimony anti-turbidimetry for Determination nutrient phosphorus content, flame photometry or tetraphenylboron sodium turbidimetry for Determination nutrient potassium content etc.But, due in chemical method directly mensuration process, complex operation step, consuming time longer, the corresponding increase of the error that manual operation brings.
At present, have certain associating for the conductivity of Different Nutrients solution or index of refraction with the concentration of solution itself, HG/T4216-2011 has worked out experimental implementation and the data processing method of detailed quick detection slowly/controlled releasing fertilizer hydrostatic dissolution rate.The mensuration conductivity of nutrient solution or the change of index of refraction is utilized to carry out its concentration change of accurate characterization, not only need careful experimental implementation and rational data processing method, and for the characteristic of slowly/controlled releasing fertilizer nutrient solution, specific Special experimental apparatus should be designed assisted.Only in this way, the slow/controlled release behavior that coated fertilizer shows in hydrostatic immersion test just can better be described.
Summary of the invention
For the characteristic of slowly/controlled releasing fertilizer nutrient solution, the invention provides a kind of based on electrical conductivity method can fast, the device of Accurate Determining release and release control fertilizer nutrient release rate and method of operating, have detect rapidly, advantage that error is little.
For achieving the above object, the present invention takes following technical scheme:
A kind of device detecting release and release control fertilizer nutrient release rate based on electrical conductivity method fast, it is characterized in that: comprise support, water feed apparatus, glass container, digital display conductivity meter, electronic stirrer, outlet is provided with bottom described glass container, this exit lower end is rising pipe, this rising pipe is provided with out water solenoid valve, the described water solenoid valve that goes out is controlled by PLC, and this glass container is fixed on the first dividing plate of support; The stirring end of described electronic stirrer is placed in glass container inside, and the other end of this electronic stirrer is fixed on the push rod of support, and described electronic stirrer is controlled by PLC; The expansion link that described digital display conductivity meter is fixed on support is placed in the top of glass container, the conductivity test probe side of this digital display conductivity meter is provided with cleaning water pipe, this digital display conductivity meter is controlled by electric device, and described electric device is controlled by PLC; Described water feed apparatus is used for supplying water to glass container and cleaning water pipe.
As preferably, described glass container indicates scale, is pyramidal structure bottom glass container, is easier to liquid and changes.
The top of described glass container is provided with foldable cover, on the cover board offers inlet opening, electronic stirrer hole and bag with fertilizer fixed orifice.
Another object of the present invention is to, a kind of method detecting release and release control fertilizer nutrient release rate based on electrical conductivity method is fast provided, comprises the steps:
(1) mensuration of fertilizer standard solution to be measured and the drafting of typical curve: according to method described in HG/T4216-2011, fertilizer to be measured is carried out to the configuration of standard solution, standard solution to be measured is transferred in the glass container of said apparatus, by PLC control desk, open electronic stirrer and foundation liquid fluctuating situation, regulate and fix stir speed (S.S.), then folding cover plate is covered, and device entirety is placed in constant temperature oven, temperature constant is 25 DEG C and places after half an hour, by PLC control desk, mobile conductivity test probe, carry out conductivity test, digital display conductivity meter records the conductivity values of now solution automatically, after being completed, open out water solenoid valve and water feed apparatus successively, glass container is cleaned, conductivity test probe is cleaned simultaneously, aforesaid operations can be repeated after cleaning, obtain the conductivity values under fertilizer different solutions concentration to be measured successively, print conductivity data and obtain equation of linear regression: Y=KX+C
Y: fertilizer simulation nutrient release rate to be measured, %;
X: the conductivity values of fertilizer standard solution to be measured, μ scm
-1;
K, C are coefficient;
(2) lixiviate of fertilizer control release nutrient to be measured and mensuration:
Method according to HG/T4216-2011, in constant temperature oven, adopt said apparatus to carry out hydrostatic stripping experiment to fertilizer to be measured, load weighted fertilizer is placed in bag with fertilizer, and hang in glass container, first close water delivering orifice and go out water solenoid valve, water feed apparatus is adopted to fill pure water by glass container, then electronic stirrer is opened, regulate and fixed rotating speed, start timing and set inlet/outlet and conductance measurement program, 1, 3, 5, 7, 10, 13, 16, 19, 22, 25, 35, 42, 49, 56, 63, 70, 77, 84, 91, 98d time point carries out electric conductivity automatic test, each measurement terminates, conductivity test probe shifts out solution to be measured, and automatically perform cleaning conductivity test probe program, use in order to next time, then water solenoid valve and water feed apparatus is opened out successively, change pure water leaching liquor, the automatic record of conductivity data, finally obtain the solution conductivity rate score under the different soak time of fertilizer to be measured.
The conductivity values obtained is brought successively into the standard solution equation of linear regression of step (1), obtain the release rate of surveyed solution, then be converted into fertilizer to be measured accumulation nutrient release rate under such condition, finally obtain the accumulation nutrients release rate curve under 25 DEG C of different soak time points, and carry out S type curvilinear regression analysis, obtain regression equation, Regression Equations is: Y=A2+ (A1-A2)/(1+ (X/X0)
p),
Y: fertilizer simulation nutrient release rate to be measured, %;
X: the conductivity values of fertilizer standard solution to be measured, μ scm
-1;
X0: midrange; A1, A2: initial value and stop value; P: formula index.
Method of the present invention takes hydrostatic cultivation, and sampling mode is with reference to HG/T4216-2011.
For test condition, conductance measurement is all carried out in constant temperature oven, at temperature remains on 25 ± 2 DEG C.
Method of the present invention is applicable to the detection of release and release control fertilizer, but does not comprise control release urea.
Beneficial effect of the present invention is:
1. adopt the higher hydrostatic cultivation of current scholar's degree of recognition to detect release and release control fertilizer, sample soaks and carries out with test simultaneously, and the replacing of leachate adopts PLC to control, the automatic record of conductivity data.
2. adopt and measure the concentration change that Crystal by Solution Conductivity Measurement characterizes solution, have simple, convenient, the advantages such as analysis time is short.
3. digital display conductivity meter is placed in the electric device controlled by PLC, and electric device shift position is accurate, avoids the experimental error that people brings for multi-pass operations; Conductivity meter is furnished with temperature indicator simultaneously, can the temperature variation of control measurement liquid at any time, conductivity meter range used is 0.055 μ S/cm ~ 199.9mS/cm, arranges 5 range abilities, measuring accuracy: conductivity: ± 0.5%FS.
4. the introducing of electronic stirrer, avoids solution to be measured causes CONCENTRATION DISTRIBUTION inequality phenomenon because of static for a long time, and electronic stirrer adopts powered battery mode, and structure is detachable, and it is controlled that rotating speed is adjustable.
5. the glass cylinder placing testing liquid indicates scale mark, and folder cover with holes is arranged at top, avoids external impurities and pollutes testing liquid.
6. EC-device structure of the present invention is simple, and except PCL controls dress, all the other devices all can be positioned in constant temperature oven, avoids ambient temperature and to fluctuate the measuring error brought.
A kind of based on electrical conductivity method test nutrient release rate special purpose device and method, equipment therefor is simple to operate, easy-to-use flexibly, and test process adopts PLC to control, and robotization is higher, and data reappearance is good.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
1-electronic stirrer, 2-cover plate, 3-bag with fertilizer, 4-glass container, 5-goes out water solenoid valve, and 7-cleans water pipe, 8-conductivity test probe, 9-support, 10-first dividing plate, 11-push rod, 12-expansion link, 13-inlet opening, 14-electronic stirrer hole, 15-bag with fertilizer fixed orifice, 16-digital display conductivity meter, 17-water feed apparatus.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment
Device entirety need be positioned in constant temperature oven (25 DEG C) when carrying out conductance measurement.
Carry out validation test to the release and release control fertilizer of a series of known fertilizer releasing period, sample is respectively the resin coated controlled release fertilizer (16-16-16) that fertilizer releasing period is 60,90 days, and numbering is respectively P1, P2.Known release and release control fertilizer fertilizer releasing period adopts chemical direct method to carry out (GB/T-23348-2009) measured.
The concrete assay method of preparation and release period is soaked for P1 interpret sample hydrostatic in special purpose device of the present invention.
(1) mensuration of standard solution and the drafting of typical curve.According to method described in HG/T4216-2011, P1 is carried out to the configuration of standard solution.Standard solution to be measured is transferred in device of the present invention, by PCL control desk, open electronic stirrer and according to liquid fluctuating situation, regulate and fix stir speed (S.S.), then covering folding lid, and device entirety is placed in constant temperature oven, temperature constant is 25 DEG C and places after half an hour, by PCL operation bench, and mobile conductivity probe, carry out conductivity test, instrument records the conductivity values of now solution automatically.After being completed, opening out water solenoid valve 5 and water feed apparatus successively, glass container is cleaned.Can aforesaid operations be repeated after cleaning, obtain the conductivity values under P1 different solutions concentration successively.Print conductivity data and obtain equation of linear regression.
table 1coated fertilizer P1 standard solution conductivity/(mscm
-1, under 25 DEG C of conditions)
Linear regression analysis is carried out to the standard solution of P1 sample, obtains the conductivity of standard solution and the equation of linear regression of simulation nutrient release rate, as follows.Linear correlation property coefficient r
2=0.99613.
Y
1=0.36573X
1+8.68964
Y
1: P1 simulates nutrient release rate, %;
X
1: the conductivity values of P1 standard solution, μ scm
-1.
Testing sample is replaced by P2, according to method described in HG/T4216-2011, P2 is carried out to the configuration of standard solution.And according to the method described above, in conductance measurement special purpose device of the present invention, carry out the conductance measurement of P2 standard solution.Print conductivity data and obtain equation of linear regression.
table 2coated fertilizer P2 standard solution conductivity/(mscm
-1, under 25 DEG C of conditions)
Linear regression analysis is carried out to the standard solution of P2 sample, obtains the conductivity of standard solution and the equation of linear regression of simulation nutrient release rate, as follows.Linear correlation property coefficient r
2=0.99982.
Y
2=0.34736X
2+8.7906；
Y
2: P2 simulates accumulation nutrient release rate, %;
X
2: the conductivity values of P2 standard solution, μ scm
-1;
The lixiviate of (2) 25 DEG C of controlled release nutrients and mensuration.
Method according to HG/T4216-2011, in constant temperature oven, (25 DEG C) adopt conductance measurement special purpose device of the present invention to carry out hydrostatic stripping experiment to P1, load weighted P1 is placed in Nylon Bag, and hangs in container.First open water intaking valve, close outlet valve, fill leaching liquor (pure water), then open electronics stirring apparatus, regulate and fixed rotating speed.Start timing and also set inlet/outlet and conductance measurement program, 1,3,5,7,10,13,16,19,22,25,35,42,49,56,63,70,77,84,91,98d ... equi-time point carries out electric conductivity automatic test.Each measurement terminates, and conductivity probe shifts out solution to be measured, and automatically performs cleaning electrode program, uses in order to next time, then opens outlet valve and water intaking valve successively, changes pure water leaching liquor.The automatic record of conductivity data, finally obtains the solution conductivity rate score under the different soak time of P1.
The conductivity values obtained is brought successively into the standard solution regression equation of P1, obtain the release rate of surveyed solution, be then converted into P1 accumulation nutrient release rate under such condition.Finally obtain the accumulation nutrients release rate curve under 25 DEG C of different soak time points, and carry out S type curvilinear regression analysis, obtain regression equation.So far, the hydrostatic of P1 under 25 DEG C of conditions soaks and conductance measurement data processing completes.
table 3release and release control fertilizer P1 electrical conductivity method measures release rate (25 DEG C)
Carry out curve fitting sample time to accumulation nutrient release rate in P1 the data obtained and test, the equation of matching S type curve (Logistic) is:
Y
1: P1 accumulation nutrient release rate, %;
X
1: P1 conductivity of the present invention tests sample time, d;
(3) P1 is replaced with P2, repeat above operation, based on conductance measurement special purpose device of the present invention, obtain the accumulation nutrient release rate of P2 under 25 DEG C of hydrostatic soaking conditionses and fertilizer releasing period.
table 4release and release control fertilizer P2 electrical conductivity method measures release rate (25 DEG C)
Continued 4
Carry out curve fitting sample time to accumulation nutrient release rate in P2 the data obtained and test, the equation of matching S type curve (Logistic) is:
Y
2: P2 accumulation nutrient release rate, %;
X
2: P2 conductivity of the present invention tests sample time, d;
From test data, 60 days and 90 days are respectively for the release and release control fertilizer P1 of known release period and P2(release period), under 25 DEG C of conditions, adopt conductance measurement special purpose device of the present invention, the release period recording P1 is 53 days (during preparation >80%), the fertilizer releasing period of P2 is 88 days (during accumulation nutrient release rate >80%), both release period relative errors about 10%.
From above data, conductivity test method of the present invention and special purpose device completely can as the effective means detecting release and release control fertilizer fertilizer releasing period.
Claims (8)
1. one kind is detected the device of release and release control fertilizer nutrient release rate fast based on electrical conductivity method, it is characterized in that: comprise support, water feed apparatus, glass container, digital display conductivity meter, electronic stirrer, outlet is provided with bottom described glass container, this exit lower end is rising pipe, this rising pipe is provided with out water solenoid valve, the described water solenoid valve that goes out is controlled by PLC, and this glass container is fixed on the first dividing plate of support; The stirring end of described electronic stirrer is placed in glass container inside, and the other end of this electronic stirrer is fixed on the push rod of support, and described electronic stirrer is controlled by PLC; The expansion link that described digital display conductivity meter is fixed on support is placed in the top of glass container, the conductivity test probe side of this digital display conductivity meter is provided with cleaning water pipe, this digital display conductivity meter is controlled by electric device, and described electric device is controlled by PLC; Described water feed apparatus is used for supplying water to glass container and cleaning water pipe.
2. a kind of device detecting release and release control fertilizer nutrient release rate based on electrical conductivity method fast according to claims 1, it is characterized in that, described glass container indicates scale.
3. a kind of device detecting release and release control fertilizer nutrient release rate based on electrical conductivity method fast according to claims 1, is characterized in that, is pyramidal structure bottom described glass container.
4. a kind of device detecting release and release control fertilizer nutrient release rate based on electrical conductivity method fast according to claims 1, it is characterized in that, the top of described glass container is provided with foldable cover, on the cover board offers inlet opening, electronic stirrer hole and bag with fertilizer fixed orifice.
5. detect a method for release and release control fertilizer nutrient release rate based on electrical conductivity method fast, comprise the steps:
(1) mensuration of fertilizer standard solution to be measured and the drafting of typical curve: according to method described in HG/T4216-2011, fertilizer to be measured is carried out to the configuration of standard solution, standard solution to be measured is transferred in the glass container of said apparatus, by PLC control desk, open electronic stirrer and foundation liquid fluctuating situation, regulate and fix stir speed (S.S.), then folding cover plate is covered, and device entirety is placed in constant temperature oven, temperature constant is 25 DEG C and places after half an hour, by PLC control desk, mobile conductivity test probe, carry out conductivity test, digital display conductivity meter records the conductivity values of now solution automatically, after being completed, open out water solenoid valve and water feed apparatus successively, glass container is cleaned, conductivity test probe is cleaned simultaneously, aforesaid operations can be repeated after cleaning, obtain the conductivity values under fertilizer different solutions concentration to be measured successively, print conductivity data and obtain equation of linear regression: Y=KX+C
Y: fertilizer simulation nutrient release rate to be measured, %;
X: the conductivity values of fertilizer standard solution to be measured, μ scm
-1;
K, C are coefficient;
(2) lixiviate of fertilizer control release nutrient to be measured and mensuration:
Method according to HG/T4216-2011, in constant temperature oven, adopt said apparatus to carry out hydrostatic stripping experiment to fertilizer to be measured, load weighted fertilizer is placed in bag with fertilizer, and hang in glass container, first close water delivering orifice and go out water solenoid valve, water feed apparatus is adopted to fill pure water by glass container, then electronic stirrer is opened, regulate and fixed rotating speed, start timing and set inlet/outlet and conductance measurement program, 1, 3, 5, 7, 10, 13, 16, 19, 22, 25, 35, 42, 49, 56, 63, 70, 77, 84, 91, 98d time point carries out electric conductivity automatic test, each measurement terminates, conductivity test probe shifts out solution to be measured, and automatically perform cleaning conductivity test probe program, use in order to next time, then water solenoid valve and water feed apparatus is opened out successively, change pure water leaching liquor, the automatic record of conductivity data, finally obtain the solution conductivity rate score under the different soak time of fertilizer to be measured,
The conductivity values obtained is brought successively into the standard solution equation of linear regression of step (1), obtain the release rate of surveyed solution, then be converted into fertilizer to be measured accumulation nutrient release rate under such condition, finally obtain the accumulation nutrients release rate curve under 25 DEG C of different soak time points, and carry out S type curve (Logistic equation) regretional analysis, obtain regression equation, Regression Equations is: Y=A2+ (A1-A2)/(1+ (X/X0)
p),
Y: fertilizer simulation nutrient release rate to be measured, %;
X: the conductivity values of fertilizer standard solution to be measured, μ scm
-1;
X0: midrange; A1, A2: initial value and stop value; P: formula index.
6. detect the method for release and release control fertilizer nutrient release rate according to claim 5 based on electrical conductivity method fast, it is characterized in that, take hydrostatic cultivation, sampling mode is with reference to HG/T4216-2011.
7. detect the method for release and release control fertilizer nutrient release rate according to claim 5 based on electrical conductivity method fast, it is characterized in that, conductance measurement is all carried out in constant temperature oven, at temperature remains on 25 ± 2 DEG C.
8. detect the method for release and release control fertilizer nutrient release rate according to claim 5 based on electrical conductivity method fast, it is characterized in that, this method is applicable to the detection of release and release control fertilizer, but does not comprise control release urea.
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Cited By (5)
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| CN107505359A (en) * | 2017-08-31 | 2017-12-22 | 沃博特生态农业科技有限公司 | Fertilizer slow release nutrient detection means and detecting system |
| CN108088874A (en) * | 2017-12-12 | 2018-05-29 | 西南石油大学 | A kind of leaching method of black shale soluble salt |
| CN111189888A (en) * | 2020-01-14 | 2020-05-22 | 中国科学院合肥物质科学研究院 | Water fertilizer nitrogen phosphorus potassium element concentration analysis method based on two-stage water fertilizer dilution treatment system |
| CN112462010A (en) * | 2020-12-23 | 2021-03-09 | 广东海洋大学 | Inspection processing technology for production of special controlled release fertilizer for pineapples |
| CN117871823A (en) * | 2024-01-12 | 2024-04-12 | 北京中化联合认证有限公司 | Green intelligent design evaluation authentication method and system for fertilizer product |
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| CN112462010A (en) * | 2020-12-23 | 2021-03-09 | 广东海洋大学 | Inspection processing technology for production of special controlled release fertilizer for pineapples |
| CN117871823A (en) * | 2024-01-12 | 2024-04-12 | 北京中化联合认证有限公司 | Green intelligent design evaluation authentication method and system for fertilizer product |
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Application publication date: 20151202 |
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