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    • 专利摘要:
    A method and system for preparing a slurry sample for online detection of one or more nutrients, in particular the content of ammonium N, total nitrogen (N), total phosphorus (P) and/or potassium (K) in a slurry contained in a tank (1) of a slurry tanker or tank trailer. The sampling and nutrient detection system comprises a slurry sample preparation and detection loop comprising a first sample preparation loop (2) with one or more pumps (3) for pumping slurry through the sample preparation loop (2) and a macerator (3) arranged in the sample preparation loop, e.g. integrated into the pump (3) for cutting or grinding particulates contained in the slurry. One or more means (4, 11) for diverting a sub flow of the macerated sample flow from the sample loop preparation (2) to the sensor loop (6). The sensor loop (6) comprises an inline nuclear magnetic resonance (NMR) sensor (7) for detecting the content of ammonium–nitrogen (N), total (Nitrogen) N, total phosphorous (P) and/or potassium (K) in slurry present in a slurry tanker or a truck tanker.
    公开号:DK201970684A1
    申请号:DKP201970684
    申请日:2019-11-07
    公开日:2021-05-21
    发明作者:Nørlund Thomsen Carsten；Mejlstrup Jensen Søren
    申请人:Samson Agro As；
    IPC主号:
    专利说明:

    DK 2019 70684 A1 1 [Method for preparing a slurry sample for online detection of one or more nutri- ents and a slurry tanker or tank trailer with a slurry sampling and online nutri- ent detection system] Field of the Invention The present invention relates to a slurry tanker or truck tank trailer comprising a slurry sampling and online nutrient detection system mounted on the mobile slurry tanker or the tank trailer unit.
    The present invention also relates to a method for preparing a slurry sample for online detection of one or more nutrients.
    Background of the Invention Crops need nutrients to be able to grow properly. Especially, compounds such as ni- trogen, phosphor and potassium are important to promote an efficient yield. To pro- vide the crops with sufficient amounts of nutrients, nutrients are added separately to the crops by fertilization and/or by applying manure or slurry to the crops, for exam- ple by distributing slurry in the field.
    It should be emphasised that throughout the application the term “slurry” is to be in- terpreted as any kind of liquid manure, organic fertilizer, sludge or similar liquids or semi-liquids in the form of a watery mixture of primarily insoluble matter. In particu- lar, the term “slurry” refers to dung, urine and/or mixtures thereof.
    Typically, slurry originates from animal husbandry and is collected in stables as a waste fraction. The dung and/or urine from the animals is typically mixed with bed- ding e.g. straw, wood chips or other particulates in the waste fractions leaving the sta- bles.
    The slurry could also come from a biogas plant as a waste product after the biogas production is done.
    DK 2019 70684 A1 2 The slurry is usually stored in large stationary slurry storage tanks at the farm until it is time to apply the slurry in the fields/application site for fertilization purposes. Then a slurry tanker is filled with slurry pumped from the stationary slurry storage tank and into the tank on the slurry tanker. The slurry tanker then transports the slurry to the application site/the field and starts applying the slurry with distribution means ar- ranged on the slurry tanker. If the field is far from the farm’s stationary slurry storage, the slurry storage is often transported from the slurry storage to the application site by trucks with tank trailers.
    Furthermore, it should be emphasised that throughout the application the term “appli- cation site” is to be interpreted as any kind of field, ground or the like, wherein the fertilizing and/or nutritive qualities of the slurry is utilized, in particular for fertilizing crops growing on the particular field.
    Nutrients/fertilizers such as nitrogen, phosphor and potassium are present in high amounts in the slurry. Nitrogen is present as inorganic N, in particular ammonium—N (NH4+ -N) and/or nitrate- N (NO3' -N) as well as N bound to/in organic molecules. The sum of inorganic and organic N is normally called Total -N. Roughly speaking, ammonium- N is representing all dissolved N and typically amounts to 40-70 % (by weight) of the total-N (the rest of the total- N is roughly considered to be organic N. Phosphor is likewise present as inorganic phosphor and organic bound P. Inorganic P is usually calculated as phosphate -P (PO, -P). Phosphate —P is present in dissolved form as well as solid forms. The sum of inorganic P and organic P is the total- P con- tent. Potassium is mostly present in inorganic and dissolved form in manure or slurry fractions. The specific amounts of nutrients present in the slurry depend on which an- imal the slurry originates from. Additionally, the content of each of the nutrients may vary significantly depending on the season as well as the storage conditions and/or storage time of the slurry as well as sedimentation in the storage tanks. The latter im- ply highly inhomogeneous distribution of the nutrients even within the same slurry storage tank.
    Chemical characterization using standard laboratory methods at best only provides averaged information masking intrinsic big variations, and they are time consuming and costly. Further, off-line laboratory tests determining contents of N, P and K nutri-
    DK 2019 70684 A1 3 ents are impractical for Total N and total P. The sampling and the treatment of the samples during transport to the laboratory is demanding due to essential pre- degradation of the solid fractions. Furthermore, it is difficult to take representative samples from large slurry storage tanks, e.g. tanks of 5000m” or more, and make sure that these samples are representative for the whole storage tank. Therefore, the amount of NPK nutrients delivered to the fields through spreading of animal slurry is today mainly determined on the basis of standard values based on general information on animal and housing type, without accurate knowledge of the potential fertilizer value or environmental impact.
    The need for the individual nutrients in a specific field varies depending on the type of crop present on the field along with the specific type of soil present in the field. Hence, the amount of slurry to be distributed depends not only on from where and when the slurry is derived but also on the crops onto which it is to be distributed along with the soil type and/or quality in a specific field.
    Undertreating of a specific field with one or more nutrients, will likely result in insuf- ficient growth of the crops. In order to counteract insufficient growth, additional ferti- lizer may have to be added to the field. Overdosing one or more nutrients will result in eutrophication caused by surplus nutrients leaching from the soil into lakes or rivers. It may also cause over-growth of the crops which often results in the crop tipping over and ending up lying on the ground. This will make it difficult to harvest the crop and the yield quality will also be affected.
    The eutrophication by nutrients being emitted to the environment are caused by ferti- lizing fields, e.g. by slurry/manure when and/or after the slurry is applied in the field for fertilizing purposes.
    Slurry is typically applied to the fields by tractors towing a slurry tanker comprising a container/tank to hold slurry as well as slurry distributing means for allowing the slur- ry to be placed on the application site. The tractor with the slurry tanker transports the slurry from the slurry storage at the farm to the field and then applies the slurry to the field. It typically takes a few minutes to fill the slurry tanker’s primary tank with slur-
    DK 2019 70684 A1 4 ry and up to e.g. five minutes for the slurry tanker to drive to the field. Alternatively, a truck with a tank trailer transports the slurry from the slurry storage to the field where the slurry is transferred to the slurry tanker for application to the application site. Trucks are mostly used where the application site is remote from the slurry storage facility. Typically, there is at least a 5 kilometres drive between the slurry storage fa- cility and the application site. This dedicates the use of the slurry tanker to distributing the slurry in the field, while transport of the slurry is done by fast driving trucks. Recently, there have been several attempts to reduce the emission of such fertilizers by controlling the amount of fertilizers in the slurry being applied to a certain field in order to reduce or eliminate overdosing with one or more nutrients, such as N, P and/or K.
    Such systems include a control system that controls the amount of slurry being applied to a certain field. The control system is typically mounted in the tractor and controls a slurry pump, which delivers slurry from the tank to the distributing means. The con- troller receives data from a database in which each field of farm land is identified, and a calculated amount of slurry (in m3 per hectares) is stored for each field. The control system then controls the amount of slurry applied to the field based on the tractor’s position, e.g. by means of GPS signals.
    This method is based on using an average content of the nutrients in slurry (see also further above) and is therefore inaccurate and may still lead to overdosing or under- dosing of one or more nutrients in a certain field.
    Recently attempts have been made to overcome this problem by applying online measurement of one or more nutrients, e.g. installed at the slurry tanker/trailer that transports the slurry from the slurry storage at the farm to the application site.
    One example is a sensor system based on the Near Infra-Red (NIR) technology. It is a problem for this technology to be approved by authorities. The problem is providing sufficiently reliable measurement as NIR based detection of nutrients N, P, K show problems with accuracy relative to standardized laboratory measurements.
    DK 2019 70684 A1 Another solution is proposed in the article: NPK NMR Sensor: "Online Monitoring of Nitrogen, Phosphorus, and Potassium in Animal Slurry”, Morten K. Sørensen et al ; Analytical Chemistry, 2015, 87 (13), 6446-6450 (DOL
    10.1021/acs.analchem.5b01924). This article proposes using a low field NMR (nucle- 5 ar magnetic field) sensor for detecting Ammonium —N, total- N, total P, and K in ani- mal slurry in an online monitoring application. The article describes the principle of detection of the nutrients by measuring certain isotopes of N, O, P and K. This NMR sensor is now marketed under the tradename “Tveskaeg” by Nano Nord A/S in Den- mark. At present the NMR sensor is only available in bench top versions with or with- out an integrated sample pump and in limited online uses in other fields (online meas- urements in water or (fuel) oil applications. This type of NMR sensor shows reliable results when detecting ammonium —N, total- N, total P, and K and when compared to standardized laboratory tests and is therefore applicable as a combined NPK (nitrogen, phosphorous, potassium) sensor. Aimed at direct detection of dissolved N (mainly ammonium N), total P, and K, the sensor has been modified to multinuclear operation tuned for "N, *'P, and ”K detection. ”'O detection is applied for determination of the organic N (and dry matter) fraction. The NMR sensor is based on the use of a cylin- drical Halbach magnet with a static magnetic field, e.g. of 1.5 T, a digital field- programmable gate array (FPGA) console, a 400 W power amplifier and a shielded probe with an elongate radio frequency (rf) coil. The sensor hardware may be installed in a temperature controlled cabinet to avoid or minimize drift. The sample flow is provided in a hose or pipe directly in the probe bore inside the coil. This sensor has however not yet been applicable for online applications in detection of Ammonium —N, total N, total P, and K in slurry present in a slurry tanker or a truck tanker. This is due to the fact that the sensor requires a narrow sample tube diameter of as little as 8-12 mm within the magnetic field. This is a challenge since animal slur- ry is highly inhomogeneous and easily clogs such a narrow tube. Further, the size dis- tribution of the particles and solid matter is much too large to allow use on an unfil- tered fraction of the slurry. Filtering the slurry will however not provide correct results as the filtered off solids also contain nutrients, in particular organic N and organic P. Filtering of the slurry before detection of nutrients in the NMR online sensor will not provide reliable results at least in relation to total N and total P. Therefore, the NMR nutrient sensor technology as described in the above mentioned article has in practice
    DK 2019 70684 A1 6 never been applied in an online monitoring solution on slurry tankers as it has been a challenge to provide a slurry sample flow which is suitable for being subjected to reli- able online NMR sensor detection of the nutrients as described in the article men- tioned above.
    Thus, there is still a need for providing systems and methods for online monitoring of ammonium —N, total N, total P, and K in slurry being pumped into the slurry tanker or tank trailer or in a tanker or truck tank trailer. There is also a need to provide a system that provides sampling and preparing of a slurry sample flow in order to allow reliable detection of the content of nutrients in the slurry tanker or truck tank trailer. Object of the Invention Thus, it is an object of the present invention to provide a system and a method for pre- paring a sample of slurry for online monitoring of ammonium —N, total N, total P, and K in slurry being pumped into the slurry tanker or tank trailer or in a slurry tanker or truck tank trailer. Further, it is an object of the present invention to provide a system and a method for providing a slurry sample flow and preparing a slurry sample flow in order to allow reliable detection of the content of nutrients in the slurry inside the slurry tanker or truck tank trailer. Further, it is an object of the present invention to provide a system and a method for providing a slurry sample flow and to prepare a slurry sample flow in order to allow reliable detection of the content of nutrients in the slurry inside the slurry tanker or truck tank trailer by a nuclear magnetic resonance (NMR) sensor installed on the slur- ry tanker or on the tank trailer for online monitoring of nutrients Description of the Invention These objects are met by a slurry tanker comprising a slurry sampling and online nu- trient detection system mounted on the mobile slurry tanker or the tank trailer unit. The sampling and nutrient detection system is special in that it comprises a slurry sample loop comprising a first slurry sample preparation loop with one or more pumps for pumping slurry through the sample preparation loop, and/or a sensor loop, a mac- erator arranged in the sample preparation loop for cutting or grinding particulates con-
    DK 2019 70684 A1 7 tained in the slurry to a particle size of less than the inner diameter of the sensor loop tube, such as to a particle size of below 8-10 mm, - one or more means for diverting a sub flow of the macerated sample flow from the sample loop to the sensor loop, wherein the sensor loop comprises an inline nuclear magnetic resonance (NMR) sensor for detecting the content of ammonium —Nitrogen (N), total (Nitrogen) N, total phosphorous (P), and/or potassium (K) in slurry present in a slurry tanker or a truck tanker in the sample flow in the sensor loop. Hereby is obtained a uniform and reliable preparation of the sample flow to the NMR sensor. The NMR sensor is provided with a sample flow tube of a very narrow diame- ter, typically of an inner diameter of 9 to 12mm. By means of the sample and online detection system according to the present invention it is possible to provide a sample flow that reduces or eliminates blockages in the sample flow to or through the NMR sensor.
    This sample preparation and nutrient detection system on the slurry tanker or tank trailer provides stable readouts from the NMR sensor that determines the actual con- tent of nutrients present in the slurry contained in the tank on the slurry tanker or the tank trailer.
    If untreated slurry is transferred to the sample flow to the NMR sensor, it would result in immediate blockage of this sample flow tube by large particulates contained in the slurry. This would render the NMR sensor useless. It is possible to provide a filtered sample flow to the NMR sensor, but this is also highly unwanted. This is because fil- tering out particulates will affect the content of nutrients present in the filtered sample and affect the detected amounts of total P and total N. The particulates present in the slurry contains nutrients bound in particulate form, in particular organic —N as well as organic —P and precipitated inorganic phosphorous containing salts. Removing the particulate matter in the slurry by filtration will therefore remove nutrients and result in the NMR sensor detecting too low amounts of especially total —-N and total P. The slurry sampling and online nutrient detection system ensures that particulates are ground to a well-defined particle size of no more than 8-10 mm whereby a homoge- nous sample is transferred to the sensor loop. This eliminates blockages in the sensor
    DK 2019 70684 A1 8 loop as the particle size is reduced to below the inner diameter of the sample tube in the sensor loop. This further ensures stable, reliable and reproducible measurements of the above-mentioned nutrients in the slurry by the NMR sensor.
    The stable readouts from the NMR sensor can be transferred to the control system of a tractor towing the slurry tanker while distributing the slurry in the fields. The tractor’s control system can then be allowed to control the amount (e.g. per hectare) of slurry distributed to the field according to the composition of nutrients in the slurry in the particular load of slurry present in the tank of the slurry tanker. The system is further equally applicable on a slurry tanker as on a tank trailer that transports slurry to the application site for subsequent distribution by a slurry tanker. The measurement data on nutrient content data in the slurry provided by the NMR sensor can be transferred to the control system in the tractor towing the slurry by conventional connection means, e.g. a wired connection or a wireless connection, e.g. Bluetooth, or via the internet, e.g. in a cloud based configuration. If the sample preparation and nutrient detection system is mounted on a truck’s tank trailer, the data from the sensor will typically be transferred to the tractor’s control system via a wireless connection.
    This further allows for optimizing the fertilising effect for the crops which are grow- ing or are to grow in that specific field where the tank load of slurry in the slurry tank- er is distributed. By optimizing the amount of nutrients it is also possible to optimize plant growth in the field by avoiding undertreatment with nutrients while also avoid- ing overtreatment and the resulting eutrophication (see background section).
    These objects of the present invention and the effects discussed above are therefore also met by a method for preparing a slurry sample for online detection of one or more nutrients, in particular the content of ammonium N, total Nitrogen (N), total Phospho- rus (P) and/or Potassium (K) in a slurry contained in a tank of a slurry tanker or tank trailer or a slurry flow entering into the tank of a mobile slurry tanker or a tank trailer unit. The method comprises -extracting a sample flow from the tank or the flow of slurry being pumped into the tank, -directing the sample flow to a sample preparation loop comprising at least one pump- ing means for circulating the slurry flow and macerating particulates in the slurry
    DK 2019 70684 A1 9 sample flow to a particle size of less than the inner diameter of the sensor loop tube, such as to a particle size of below 8-10 mm, in a macerator arranged in the sample preparation loop - extracting a sample sub flow of the macerated slurry, - directing the macerated sample sub flow to a sensor loop, wherein the sensor loop comprises an inline NMR sensor for detection of the content of ammonium —N, total N, total P, and/or K in slurry present in a slurry tanker or a truck tanker in the sample flow in the sensor loop.
    A flow of slurry is directed to the sample preparation loop from the slurry tank (also called the primary tank) on the slurry tanker. This can be done from a filled tank or alternatively during filling of the primary tank. It is preferred to extract the sample flow to the sample preparation loop from the primary tank, because the slurry content in this tank is thoroughly mixed inside the primary tank. This ensures that the concen- tration of nutrients is more uniform in the entire volume of slurry in the primary tank. Therefore, the NMR sensor in the sensor loop will provide more reliable and repro- ducible results on the detection and concentration of each of the above-mentioned nutrients.
    The sample preparation loop preferably comprises a pipe loop with an inlet end and an outlet end connected to the primary tank on the slurry tanker or tank trailer. Slurry is extracted from the slurry tanker by a first pump installed in the sample preparation loop. This pump directs the slurry sample flow through the sample preparation loop and back to the primary tank.
    The sample preparation loop comprises a macerator. The macerator is preferably built into the pump or a separate macerator is arranged downstream to the pump. The mac- erator grinds particulates in the slurry to a particle size of less than the inner diameter of the sensor loop tube. The sensor loop tube has an inner diameter of 9-12 mm. Thus, the macerator grinds the particulate matter to a maximum particle size of less than 10mm, preferably less than 8 mm.
    The slurry may also be extracted from the primary tank by a slurry sampling automat. The samples extracted by the slurry sampling automat are then directed to the slurry
    DK 2019 70684 A1 10 sample preparation loop. The slurry sampling automat is e.g. installed in a circulation pipe that circulates slurry, e.g. for stirring or mixing the slurry in the primary tank. Alternatively, the slurry sampling automat may be arranged at the inlet pipe used for filling slurry into the primary tank. Suitable slurry sampling automats are available on the market. For example, the Dutch companies D-Tec and Eijkelkamp market suitable slurry sampling automats for mounting on slurry tankers or tank trailers. A sample flow is withdrawn from the sample preparation loop to the sensor loop. This can be done simply by providing pipe branch to divert a prepared sample flow to the sensor loop, by arranging at least one valve to control the flow in the sensor loop and/or by a second pump arranged in the sensor loop. The at least one valve is prefer- ably arranged upstream to the NMR sensor. Alternatively, a valve may instead or ad- ditionally be arranged downstream to the NMR sensor. A second pump may be ar- ranged upstream to the NMR sensor, such as between the accumulation tank (see fur- ther below) and the NMR sensor to control the sample flow through the NMR sensor and thereby through the sensor loop. It is also possible to provide a sample automat see above) in the sample preparation loop for directing a sample flow to the sensor loop.
    It is possible to transfer a sample flow to the sample loop and thus also to the sensor loop during filling of the slurry tanker. When repeating detection of especially total — N and/or total —P such repeated measurements may show variations in the content of these nutrients in the slurry. These variations may e.g. relate to the composition of dry matter or suspended solids in the slurry. For example, slurry pumped from the top of a slurry storage facility contains relatively low amounts of suspended solids and thus a lower total —P and lower organic —N. Thus, continued monitoring of these nutrients in the composition of the slurry by repeating measurements of the slurry during filling of the slurry tanker will show such variations.
    Each sample is transferred to the sensor and held in the NMR sensor for a period of time depending on the time necessary for detecting each nutrient. The NMR sensor is at present able to provide reliable results on each nutrient with a sample holding time as mentioned in table 1. Further optimisation of the necessary holding time is expected
    DK 2019 70684 A1 11 within the near future. It is expected that the NMR sensor will be able to provide at least Ammonium-N, Total- N and total- P within a holding time of 5 minutes. Nutrient Sample holding time in NMR sensor em Table 1: NMR sensor time necessary to detect nutrients.
    Therefore, a sequence of such continued online detection of each of the nutrients Ammonium —N, total -N (represented by ”O measurements) and/or total -P meas- urements may be time consuming and it may be difficult to do during the time it takes to fill the primary tank on the slurry tanker.
    Preferably, the sensor loop further comprises an accumulation tank upstream to the NMR sensor for pooling the sub flow of the macerated sample flow. Hereby it be- comes possible to accumulate the sample flow in the sensor loop in the accumulation tank, in particular upstream to the NMR sensor. The content of each of the nutrients in the sample accumulation tank is then the same in all samples transferred to the sensor. This evens out variations in the nutrient content throughout the sample volume present in the sample accumulation tank. This corresponds to calculating an average concen- tration of nutrients in the slurry pumped into the primary tank. Thereby it is possible to reduce the number of measurements necessary for reliably measuring the content of each of the nutrients (ammonium- N, total —N, total- P, K), which reduces the overall time necessary for detecting the nutrient content in the slurry in the NMR sensor. Therefore, the method also comprises the step of collecting a sample flow in a sample accumulation tank upstream to the NMR sensor for pooling the sub flow of the macer- ated sample flow in the sample accumulation tank. The accumulation tank preferably may further comprise a vent valve. This vent valve allows for emptying the accumulation tank, when a measurement cycle is finished.
    DK 2019 70684 A1 12 This may e.g. occur in advance of each time the slurry tanker is re-filled with a new portion of slurry.
    The accumulation tank is emptied by opening the vent valve and e.g. activating a pump (see further below) arranged in the sensor loop, such as arranged between the accumulation tank and the NMR sensor.
    Alternatively, the vent valve is opened and a valve is opened, which is arranged between the accumulation tank and point where the sensor flow re-enters the sample preparation loop.
    Thereby the con- tent of the accumulation tank is sucked into the sample preparation loop.
    Optionally, an agitator is installed in the accumulation tank.
    The agitator ensures uni- form distribution of any solid matter and ensures uniform samples being transferred from the accumulation tank to the NMR sensor.
    Preferably, the sensor loop comprises a second pump for pumping the sample sub flow to the NMR sensor.
    The second pump is preferably arranged between the accu- mulation tank and the NMR sensor unit.
    Downstream to the sensor, the sensor loop flow is directed back into the sample prep- aration loop.
    The sample flow preparation loop preferably comprises an ejector, an injector, a nozzle or a mixing valve for mixing the exit flow from the NMR sensor into the sample loop.
    Alternatively, the sensor flow may be added to the sample prepa- ration loop downstream to the ejector or the nozzle.
    This provides a simple and relia- ble way of disposing of the outlet flow from the NMR sensor unit.
    When using an ejector this further creates a vacuum in the outlet line from the from the NMR sensor, which creates a suction effect in the sensor loop, which eliminates the need for provid- ing a pump in the sensor sub flow loop.
    A nozzle arranged downstream to the pump provides a counter pressure to the pump.
    This forces a sub flow of the sample prepara- tion loop into the sensor loop.
    The ejector also provides a tearing effect on the particulate matter present in the slurry passing through the ejector.
    This provides a more homogenous slurry fraction exiting from the ejector.
    This can be utilized for sample preparation in the sample preparation loop.
    Thus, in a variant of the sample preparation system, the sub flow to the sensor loop is withdrawn from the sample preparation loop downstream to the ejector.
    The outflow from the NMR sensor in the sensor loop is then preferably transferred to the
    DK 2019 70684 A1 13 sample preparation loop upstream to the ejector, where it is mixed into the sample flow from the macerator or macerating pump. Likewise, the method preferably comprises directing the sample sub flow or the pooled sample sub flow to the to the NMR sensor by means of a sample flow pump arranged upstream or downstream to the NMR sensor or by sucking the sample flow through the NMR sensor by connecting a sample outlet of the NMR sensor to an ejec- tor arranged in the sample flow loop. The sample preparation loop is then directed into the slurry tank on the slurry tanker or tank trailer. The content of dissolved nutrients, i.e. ammonium-N and/or Potassium (K) is substan- tially the same throughout a volume of slurry present in a slurry storage facility. The content of organic —N and/or organic —P varies because particulate matter tends to settle to the bottom in a slurry storage facility throughout the storage period. Thus, when pumping slurry from a slurry storage, the nutrient content of dissolved nutrients, i.e. Ammonium-N and/or Potassium (K) is substantially the same in the entire volume of slurry.
    Thus, the method preferably further comprises the steps of initially detecting the con- tent of potassium (K) and/or ammonium-N in a slurry extracted from a single station- ary slurry storage tank once by i) providing a first portion of the sample flow to the NMR sensor, i1) detecting the content of Potassium (K) and/or Ammonium-N in this first sample portion, and -optionally repeating steps i-ii one or more times, such as up to five times. This minimizes the overall time needed for determining the nutrient content of the nutrients, i.e. ammonium-N and/or potassium (K), which is substantially the same throughout a volume of slurry present in a slurry storage facility. In addition, the over- all detection time for nutrient content of ammonium-N and/or potassium (K), as well as for total-N and/or total-P is optimized to allow the sensor to complete detection of the nutrients in the slurry sample before spreading it at the application site. This fur-
    DK 2019 70684 A1 14 ther allows that the control unit that controls slurry application can use the NMR sen- sor’s signals relating to the content of one or more of these nutrients to control the amount of slurry applied to the application site. This further reduces risks for over- fertilising or under-fertilising the crops that are growing or planned to grow on the particular application site/field. As mentioned above, the content of organic —N and/or organic —P varies present in each body of slurry contained in the primary tank on the slurry tanker depending on whether it was pumped from the top of the slurry storage facility or the bottom there- of. Thus, the method preferably further comprises detecting the content of phosphorous as total P and/or the total Nitrogen content for every filling of the primary tank on the slurry tanker or tank trailer by ii1) providing a second portion of the sample flow to the NMR sensor, iv) detecting at least the content of phosphorous as total P and/or total Nitrogen in the second sample portion, -optionally repeating steps iii-iv one or more times, such as up to five times for each filled tank of the slurry tanker or tank trailer.
    This allows detection of variations of the total nitrogen content and/or total — P con- tent in each load of slurry. Thus, when transferring sensor data on the content thereof to the tractor’s control unit, it is possible to adjust the distribution of the slurry to the application site and to vary the amount of slurry added (ton or m” per hectare) while taking into account the variations in the content of these nutrients from load to load of slurry distributed to the application site. This reduces the risk of overdosing or under- dosing of one or more nutrients in a certain field even further. Preferably, the sequence of sampling and detection of nutrients is carried out while filling slurry into the primary tank and/or while driving the filled slurry tanker or tank trailer truck to the application site. For example, ammonium —N and/or Total -N is detected during filling of the slurry tanker or tank trailer. After completing filling of the tanker or after finishing measurement of the content of anmonium-N and/or total- N in the first sample, a new sample is transferred from the accumulation tank and into
    DK 2019 70684 A1 15 the NMR sensor for detection of total-P and/or K content in the slurry.
    The detection of total-P and/or K can then continue while the filled slurry tanker or tank trailer truck drives to the application site.
    This utilises the time where the slurry tanker drives to the application site for detecting the nutrients that have a longer detection time in the NMR sensor.
    This further reduces idle time for the slurry tanker and/or reduces or eliminates waiting time (while waiting for results from the NMR sensor) for the slurry tanker, which further optimizes the utilisation of the slurry tanker for spreading slurry to the application site.
    The sequence of sampling and detection of nutrients therefore preferably comprises 1) providing a first sample flow to the NMR sensor one or more times and detecting ammonium-N and/or total —N, i1) transferring a sample flow to the second sample accumulation tank while detecting ammonium-N and/or total —N, 111) transferring a second sample one or more times to the NMR sensor and detecting total- P and/or K.
    This sequence optimizes the sequence and allows for the longer holding times neces- sary for detection of total- P and/or K.
    Description of the Drawing The present invention will now be described in details with reference to the drawings in which Figs. la-lg shows different diagrams with layouts of the sample preparation loop and the sensor preparation loop with an NMR sensor unit in the sensor loop Figs. 2a-2e shows different diagrams with layouts of the sample preparation loop and the sensor preparation loop in diagram form in which an accumulation tank is arranged in the sensor sub loop upstream to the NMR sensor, and Figs. 3a-3b show graphics of the results of tests of the correlation of the content of nutrient data ( total N, total P) in two different types of slurry and
    DK 2019 70684 A1 16 at different positions of the sample loop, the sensor loop and the primary tank. Detailed Description of the Invention The different layouts shown in figs la-1g and 2a-2e are discussed briefly in the fol- lowing. In the following we have described the sample preparation and nutrient detec- tion system as mounted on a slurry tanker. As indicated above, the sample preparation and nutrient detection system is equally applicable on a tank trailer that transports slurry from a slurry storage facility to the application field.
    The same reference signs are used for the same features in all figures. Fig. 1a shows in diagram form a first variant of the sample preparation and nutrient detection system.
    A slurry tanker having a primary tank 1 comprises a slurry sample loop 2 and a sensor loop 6. The slurry sample preparation loop 2 is connected to either the primary tank 1 or a slurry inlet pipe (not shown) e.g. by a slurry sampling automat (not shown). The slurry preparation loop’s 2 outlet end is connected to the primary tank 1 for circulating the slurry sample flow back into the primary tank 1. The sample preparation loop 2 comprises a pump 3 for pumping slurry through the sample preparation loop 2. In all figures, the macerator is integrated into the pump 3. It is noted that the macerator may be provided as a separate unit in the sample preparation loop 2. The macerator inte- grated in the pump 3 is for cutting or grinding particulates contained in the slurry to a particle size of less than the inner diameter of the sensor loop tube 6. This means that the slurry particulates are cut/grinded to a particle size of below 8mm or 10 mm in the macerator. A pipe branch diverts/extracts a sub flow of the macerated sample flow from the sam- ple preparation loop 2 to the sensor loop 6. The sensor loop comprises an inline nucle- ar magnetic resonance (NMR) sensor 7 for detecting the content of ammonium — Nitrogen (N), total (Nitrogen) N, total phosphorous (P) and/or potassium (K) in slurry present in a slurry tanker or a truck tanker in the sample flow in the sensor loop. The
    DK 2019 70684 A1 17 functioning of this NMR sensor is described further in the background section. The NMR sensor detects the content of nutrients in the slurry sample flow in the sensor loop 6 as mentioned above and provides control signals which can be used by the trac- tor (not shown) towing the slurry tanker when applying slurry to the application site.
    A valve 12 mounted downstream to the NMR sensor 7 controls the sample flow through the sensor loop 6. The sample preparation loop comprises an ejector 5 (or a nozzle, a mixing valve or an injector, in the following just mentioned as ejector 5). The sensor loop’s 6 downstream end is connected to the ejector 5 and expels the sen- sor loop flow into the ejector 5 for mixing with the circulating sample preparation flow 2 before being reintroduced into the primary tank 1 of the slurry tanker.
    Fig. 1b shows in diagram form a second variant of the sample preparation and nutrient detection system. Fig. 1b has all features of fig. la. In fig 1b, a further valve 11 is pro- vided to control the sample flow from the sample preparation loop 2 and into the sen- sor loop 6.
    Fig. 1c shows in diagram form a third variant of the sample preparation and nutrient detection system. Fig. lc has all features of fig. la. In fig. 1c the sensor loop’s 6 downstream end/outflow is connected downstream to a nozzle 5 and expels the sensor loop flow 6 into the sample preparation loop 2 downstream to the nozzle 5 for mixing with the circulating sample preparation flow 2 before being reintroduced into the pri- mary tank 1 of the slurry tanker. The nozzle 5 provides a counter pressure to the pump 3, which forces a sub flow of the sample preparation loop 2 into the sensor loop 6.
    Fig. 1d shows in diagram form a fourth variant of the sample preparation and nutrient detection system. Fig. 1d has all features of fig. la. In fig 1d a second sensor loop pump 8 is further provided to control the sample flow through the sensor loop 6.
    Fig. le shows in diagram form a fifth variant of the sample preparation and nutrient detection system. Fig. le has all features of fig. 1c. In fig. le a further valve 11 is fur- ther provided to control the sample flow from the sample preparation loop 2 and into the sensor loop 6.
    DK 2019 70684 A1 18 Fig. 1f shows in diagram form a sixth variant of the sample preparation and nutrient detection system. Fig. 1f has all features of fig. lc. In fig. 1f a second sensor loop pump 8 is further provided to control the sample flow through the sensor loop 6.
    Fig 1g shows in diagram form a seventh variant of the sample preparation and nutrient detection system. In fig. 1g the ejector 5 also provides a tearing effect on the particu- late matter present in the slurry passing through the ejector 5 resulting in a more ho- mogenous slurry fraction exiting from the ejector 5. Thus, in the sample preparation system, the sub flow 4 to the sensor loop 6 is withdrawn from the sample preparation loop 2 downstream to the ejector. The outflow from the NMR sensor 7 in the sensor loop is then preferably transferred to the sample preparation loop 2 upstream to the ejector 5, where it is mixed into the sample flow 2 from the macerator or macerating pump 3.
    Fig. 2a shows in diagram form an eighth variant of the sample preparation and nutri- ent detection system. Fig. 2a has all features of fig. 1b. In fig. 2a the sensor loop fur- ther comprises an accumulation tank 9 upstream to the NMR sensor 7 for pooling the sub flow of the macerated sample flow in the accumulation tank 9. Hereby it becomes possible to accumulate the sample flow in the sensor loop 6 in the accumulation tank 9, in particular upstream to the NMR sensor 7. This evens out variations in the nutri- ent content throughout the sample volume present in the sample accumulation tank 9. Thereby it is possible to reduce the number of measurements necessary for reliably measuring the content of each of the nutrients (ammonium- N, total —N, total- P, K), which reduces the overall time necessary for detecting the nutrient content in the slur- ry in the NMR sensor 7.
    The accumulation tank 9 preferably may further comprise a vent valve 10. This vent valve 10 allows for emptying the accumulation tank 9 in advance of each time the primary tank 1 is re-filled with a new portion of slurry. Further, the vent valve allows for transferring part of the accumulated sample in the accumulation tank 9 to the NMR sensor by opening the vent valve 10 during transfer of the sample. When emptying the accumulation tank 9, the vent valve 10 is opened and the valve 12 is opened, which is arranged between the NMR sensor 7 and the point where the sensor loop 6 re-enters
    DK 2019 70684 A1 19 the sample preparation loop 2. Thereby the content of the accumulation tank 9 is sucked into the sample preparation loop 2. Optionally, an agitator (not shown) is installed in the accumulation tank 9. The agita- tor ensures uniform distribution of any solid matter and ensures uniform samples be- ing transferred from the accumulation tank to the NMR sensor 7. Fig. 2b shows in diagram form a ninth variant of the sample preparation and nutrient detection system. Fig. 2b has all features of fig. 2a. The pooled sample is transferred from the accumulation tank 9 to the NMR sensor 7 by activating the second pump 8 (see further below) arranged in the sensor loop 6 between the accumulation tank 9 and the NMR sensor 7. Fig. 2c shows in diagram form a tenth variant of the sample preparation and nutrient detection system. Fig. 2c has all features of fig. 2a. In fig. 2c the sensor loop’s 6 downstream end/outflow is connected downstream to the nozzle 5 and expels the sen- sor loop flow 6 into the sample preparation loop 2 downstream to the ejector/nozzle 5 for mixing with the circulating sample preparation flow 2 before being reintroduced into the primary tank 1 of the slurry tanker.
    Fig. 2d shows in diagram form an eleventh variant of the sample preparation and nu- trient detection system. Fig. 2d has all features of fig. 2c. In fig. 2d the pooled sample is further transferred from the accumulation tank 9 to the NMR sensor by activating the second pump 8 (see further below) arranged in the sensor loop 6 between the ac- cumulation tank 9 and the NMR sensor 7. Fig. 2e shows in diagram form a twelfth variant of the sample preparation and nutrient detection system. In fig. 2e the ejector 5 also provides a tearing effect on the particu- late matter present in the slurry passing through the ejector 5 resulting in a more ho- mogenous slurry fraction exiting from the ejector 5. Thus, in the sample preparation system, the sub flow 4 to the sensor loop 6 is withdrawn from the sample preparation loop 2 downstream to the ejector 5 and is transferred to the sample accumulation tank
    9. The outflow from the NMR sensor 7 in the sensor loop is then preferably trans- ferred to the sample preparation loop 2 upstream to the ejector 5, where it is mixed
    DK 2019 70684 A1 20 into the sample flow 2 from the macerator or macerating pump 3. Otherwise, the twelfth variant functions as outlined for the variant shown in fig. 2a. Reference numbers:
    1. Slurry tanker’s tank (primary tank)
    2. Sample preparation loop
    3. Pump and/or macerator
    4. Sample extraction
    5. Ejector, nozzle, injector or mixing valve
    6. Sensor loop
    7. NMR sensor
    8. Second pump
    9. Accumulation tank
    10. Vent valve
    11. Valve
    12. valve Examples A sample preparation and nutrient detection system as shown in fig. 1b was installed on a slurry tanker and tested for reliability of the sample preparation used for prepar- ing the sample flow for detection of the content of nutrients as mentioned further above. The example focusses on comparing of the content of dry matter, total N and total P in the sensor loop relative to the slurry present in the primary tank 1. This is because these values are sensitive to changes in the content of particulates present in the slurry. The test aims at verifying if the sample preparation used herein results in a sample flow to the NMR sensor, which is comparable to the slurry contained in the primary tank. Cattle slurry was filled into the primary tank 1 on the slurry tanker.
    Five samples of the slurry were taken from the primary tank (represented as A in fig 3), five samples of the slurry were taken in the sample preparation loop downstream to the macerator pump 3 (represented as B in fig 3) and five samples were taken from the sensor loop downstream to the NMR sensor 7 (represented as C in fig 3).
    DK 2019 70684 A1 21 The samples from A-C were all tested for total-N and total —P in a laboratory. The samples from A-C were filled in 500-1000 mL containers for external laboratory analysis. All samples were kept cold (2—5 °C), and the sample containers for the la- boratories were sent with cooling items in insulated boxes. Laboratory results were obtained for dry matter, total N, total P. The cattle slurry contained 8.5 % by weight dry matter (in average over the 5 samples taken at A-B, C) at all positions A-C.
    The results of laboratory tests are shown in fig. 3a. Relative standard deviation bars (RSD) are shown in fig. 3a. The RSD deviations relate to “normal” deviations that are connected with taking samples of animal slurry which is highly inhomogeneous.
    The test was repeated with biogas slurry (as outlined above).
    The biogas slurry contained 6-7 % by weight dry matter (in average over the 5 sam- ples taken at A-B, C) at all positions A-C.
    The results of laboratory tests are shown in fig. 3b. Relative standard deviation bars (RSD) are also shown in fig. 3b.
    The RSD deviation in cattle slurry between A and C is 4.7 % for total -P and 0.9 % for total —N respectively.
    The RSD deviation in degassed slurry between A and C is 8.2 % for total —P and 0.1 % for total —N respectively. RSD deviations between measurements internally in each group A-C was 7-30 %. Thus, it can be concluded that the sample present at C, i.e. in the sensor loop is representative for the slurry contained in the primary tank 1, and that the sample preparation made in the sample preparation loop does not change the content of nutrients in slurry flow in the sensor loop 6 relative to the slurry present in the primary tank 1.
    权利要求:
    Claims (11)
    [1] 1. Slurry tanker or truck tank trailer comprising a slurry sampling and online nutrient detection system mounted on the mobile slurry tanker or the tank trailer unit, wherein the sampling and nutrient detection system comprises a slurry sample loop comprising a first loop with one or more pumps for pumping slurry through the sample prepara- tion loop, and/or a sensor loop, a macerator arranged in the sample preparation loop for cutting or grinding particulates contained in the slurry to a particle size of less than the inner diameter of the sensor loop tube, such as to a particle size of below 8-10 mm, - one or more means for diverting a sub flow of the macerated sample flow from the sample loop to the sensor loop, wherein the sensor loop comprises an inline nuclear magnetic resonance (NMR) sensor for detecting the content of ammonium —Nitrogen (N), total (Nitrogen) N, total phosphorous (P), and/or potassium (K) in slurry present in a slurry tanker or a truck tanker in the sample flow in the sensor loop.
    [2] 2. Slurry tanker or truck tank trailer according to claim 1, characterized in that the sensor loop further comprises an accumulation tank upstream to the NMR sensor for pooling the sub flow of the macerated sample flow.
    [3] 3. Slurry tanker or truck tank trailer according to claim 1 or 2, characterized in that the accumulation tank comprises a vent valve and optionally an agitator.
    [4] 4. Slurry tanker or truck tank trailer according to any of claims 1 to 3, characterized in that the sensor loop comprises a pump for pumping the sample sub flow to the NMR sensor.
    [5] 5. Slurry tanker or truck tank trailer according to any of claims 1 to 4, characterized in that the sample flow loop comprises an ejector, an injector, a nozzle or a mixing valve for mixing the exit flow from the NMR sensor into the sample loop.
    [6] 6. A method for preparing a slurry sample for online detection of one or more nutri- ents, in particular the content of ammonium N, total Nitrogen (N), total Phosphorus (P) and/or Potassium (K) in a slurry contained in a tank of a slurry tanker or tank trail-
    DK 2019 70684 A1 23 er or a slurry flow entering into the tank of a mobile slurry tanker or a tank trailer unit, wherein the method comprises -extracting a sample flow from the tank or the flow of slurry being pumped into the tank, -directing the sample flow to a sample preparation loop comprising at least one pump- ing means for circulating the slurry flow -macerating particulates in the slurry sample flow to a particle size of less than the inner diameter of the sensor loop tube, such as to a particle size of below 8-10 mm, in a macerator arranged in the sample preparation loop, - extracting a sample sub flow of the macerated slurry, - directing the macerated sample sub flow to a sensor loop, wherein the sensor loop comprises an inline NMR sensor for detection of the content of ammonium —N, total N, total P and/or K in slurry present in a slurry tanker or a truck tanker in the sample flow in the sensor loop.
    [7] 7. A method for preparing a slurry sample according to claim 6, characterized in fur- ther comprising the step of collecting a sample flow in a sample accumulation tank upstream to the NMR sensor for pooling the sub flow of the macerated sample flow in the sample accumulation tank.
    [8] 8. A method for preparing a slurry sample according to claim 6-7, characterized in further comprising the steps of initially detecting the content of potassium (K) and/or ammonium-N in a slurry extracted from a single stationary slurry storage tank once by i) providing a first portion of the sample flow to the NMR sensor, 11) detecting the content of potassium (K) and/or ammonium-N in this first sample portion, and -optionally repeating steps 1-11 one or more times, such as up to five times,
    [9] 9. A method for preparing a slurry sample according to any of the claims 6-8, charac- terized in detecting the content of phosphorous as total P and/or total Nitrogen for every filling of the mobile tank on the slurry tanker or tank trailer by 111) providing a second portion of the sample flow to the NMR sensor, iv) detecting at least the content of phosphorous as total P and/or total Nitrogen in the second sample portion,
    DK 2019 70684 A1 24 -optionally repeating steps iii-iv one or more times, such as up to five times for each filled tank of the slurry tanker or tank trailer.
    [10] 10. A method for preparing a slurry sample according to any of the claims 6-9, char- acterized in directing a the sample sub flow or the pooled sample sub flow to the NMR sensor by means of a sample flow pump arranged upstream or downstream to the NMR sensor or by sucking the sample flow through the NMR sensor by connect- ing a sample outlet of the NMR sensor to an ejector or pump arranged in the sample flow loop.
    [11] 11. A method for preparing a slurry sample according to any of the claims 6-10, char- acterized in that sequence of sampling and detection of nutrients comprises i) providing a first sample flow to the NMR sensor one or more times and detecting ammonium-N and/or total —N, i1) transferring a sample flow to the second sample accumulation tank while detecting ammonium-N and/or total —N, 111) transferring a second sample one or more times to the NMR sensor and detecting total- P and/or K.
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    同族专利:
    公开号 | 公开日
    WO2021089096A1|2021-05-14|
    DK180483B1|2021-05-27|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE102004010217A1|2004-02-27|2005-09-15|Carl Zeiss Jena Gmbh|Arrangement and method for the spectroscopic determination of the constituents and concentrations of pumpable organic compounds|
    DK177351B1|2011-12-12|2013-02-11|Nanonord As|A method of determining catalytic fines in an oil|
    WO2015070872A1|2013-11-13|2015-05-21|Nanonord A/S|A method for quantitative determination of nitrogen in an aqueous fluid|
    法律状态:
    2021-05-21| PAT| Application published|Effective date: 20210508 |
    2021-05-27| PME| Patent granted|Effective date: 20210527 |
    优先权:
    申请号 | 申请日 | 专利标题
    DKPA201970684A|DK180483B1|2019-11-07|2019-11-07|Method for preparing a slurry sample for online detection of one or more nutrients and a slurry tanker or tank trailer with a slurry sampling and online nutrient detection system|DKPA201970684A| DK180483B1|2019-11-07|2019-11-07|Method for preparing a slurry sample for online detection of one or more nutrients and a slurry tanker or tank trailer with a slurry sampling and online nutrient detection system|
    PCT/DK2020/050300| WO2021089096A1|2019-11-07|2020-11-05|Method for preparing a slurry sample for online detection of one or more nutrients and a slurry tanker or tank trailer with a slurry sampling and online nutrient detection system|
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