CN2733355Y - Device for determining ammonium state nitrogen and nitrate nitrogen in soil - Google Patents
Device for determining ammonium state nitrogen and nitrate nitrogen in soil Download PDFInfo
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- CN2733355Y CN2733355Y CN 200420069946 CN200420069946U CN2733355Y CN 2733355 Y CN2733355 Y CN 2733355Y CN 200420069946 CN200420069946 CN 200420069946 CN 200420069946 U CN200420069946 U CN 200420069946U CN 2733355 Y CN2733355 Y CN 2733355Y
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Abstract
The utility model relates to a device for determining ammonium state nitrogen and nitrate nitrogen in soil, specifically relating to a device for determining ammonium state nitrogen and nitrate nitrogen in soil, comprising a steam generator, a still, a condensing tube, a heater and a liquid recovery container. A gas outlet, a gas inlet and a feeding opening are arranged on the still, the steam outlet of the steam generator is connected with the gas inlet of the still via a catheter, and the gas outlet of the still is connected with the inlet of the inner pipeline of the condensing tube via the catheter. The outlet of the inner pipeline of the condensing tube extends in the liquid recovery container, and a cooling water inlet and a cooling water outlet are arranged on the outer pipeline of the condensing tube, respectively is connected with the pipeline of cooling water. The utility model has the advantages of simple technics, convenient operation, good repeatability and stability, accurate determining result, durable apparatus, simple maintenance and reasonable design of structure and scheme.
Description
Technical field
The utility model relates to the mensuration of soil ammonium-state and nitrate nitrogen, a kind of specifically device of measuring soil ammonium and nitrate nitrogen.
Background technology
Nitrogen is one of necessary macronutrient of crop growth in Agro-ecological System.Now having verified nitrogen is the important composition composition of phytoprotein, nucleic acid, nucleoprotein, chlorophyll, many enzymes, vitamin substances, alkaloid and plant hormone etc., in making object, have many-sided trophism, agricultural production is had very important influence.But a large amount of using of chemical nitrogen fertilizer have been aggravated the great and thorny environmental problem that these mankind of nitrate pollution face in agricultural production.Since 1970's, the problem of environmental pollution of nitrogen has caused widely in the world to be paid close attention to.(document 1: Zhu Zhaoliang, Wen Qixiao, Chinese soil nitrogen, Jiangsu: Jiangsu science tech publishing house, 1992:267～288) (its chemical general formula is NO to the gaseous oxidation thing of the nitrate nitrogen, ammonium nitrogen and the nitrogen that produce by biological chemistry action in farmland ecosystem of chemical nitrogen fertilizer
x) to wait be exactly one of major reason that causes groundwater contamination, closure or semiclosed property water environment eutrophication, pollution ecological effect.Simultaneously, the excessive of chemical nitrogen fertilizer applies, and also can influence the quality of agricultural product, increased the cancered danger of eater, is detrimental to health.Therefore, for preventing that excessive nitrogenous fertilizer from applying farmland ecosystem, avoid it to the pollution of environment and unnecessary waste, the soil testing and fertilizer recommendation system has just been carried out in succession as far back as 60～seventies of last century by some agriculture developed countries, according to the reasonable applied nitrogen of Soil Nitrogen Supplying.In recent years, China has also carried out a large amount of correlative study work.Why soil testing and fertilizer recommendation has remarkable economical and environmental benefit is because it can overcome China's existing shortcoming in the fertilizing method in the past, promote balance fertilizing, balancedly supply with the required Different Nutrition of crops, when bringing into play the fertilizer production-increasing function fully, limited the abuse of nitrogenous fertilizer, reduced the pollution of nitrogen to environment, improve the biological quality of agricultural product, reduced because the excessive increase of using the production cost that is brought of chemical fertilizer further promotes the economic benefit of agricultural production.
In the modern soil scientific research, to the evaluation of Soil Nitrogen Supplying except that the total soil nitrogen content's index, also to see the easiest by ammonium nitrogen that crop absorbed and nitrate nitrogen content what in the soil, this is a key of estimating Soil Nitrogen Supplying, also two important indicators of required mensuration in the soil testing and fertilizer recommendation system often.
(MgO-Devarda) way of distillations that adopt in the method for the ammonium nitrogen of inorganic states and nitrate nitrogen can be measured the NH in the leaching liquor more in the present stage domestic mensuration soil
4 +, NO
3 -And NO
2 -, measure ammonium nitrogen with the MgO way of distillation, measure NH with the MgO and the Devarda alloy way of distillation again
4 +, NO
3 -And NO
2 -Total amount, this is just recording on the ammonium nitrogen basis, obtains the content (document 2: Lu Rukun, soil agrochemistry analytical approach, Beijing: Chinese agriculture science and technology publishing house, 2000:156～159) of nitrate nitrogen in the soil by both differences.But what the distillation equipment that uses was more now is that homemade semi-automatic semimicro Kelvin is decided the nitrogen distiller, the existing shortcoming of this distillation equipment is: 1. the sample distillery is after adding the sample leaching liquor, be in a kind of closed state, the interpolation of MgO and Devarda alloy after being unfavorable for; 2. because this instrument distillery structural limitations, after finishing last sample, be difficult to the residue of the residual sample in the distillery and MgO and Devarda alloy suspension is cleaned up, its residual effect will cause totally unfavorable influence the mensuration of sample thereafter; 3. the substep that is not easy to MgO and Devarda alloy adds, so each sample will be measured ammonium nitrogen and nitrate nitrogen must carry out twice mensuration, but the measurement result of nitrate nitrogen is influenced by remaining ammonium nitrogen still easily; 4. if it will be cleaned up, distillery in the instrument partly must be pulled down, because front and back and below all be connected with emulsion tube, and instrument temperature is higher in the sample determination process, and like this operation is difficult to carry out; 5. most links of instrument are glass and emulsion tube, if any misoperation or long-time use the damage that all easily causes parts and aging.
The utility model content
The purpose of this utility model provides a kind of easy to use, the mensuration soil ammonium that is easy to safeguard and the device of nitrate nitrogen.
For achieving the above object, the technical solution adopted in the utility model is as follows: adopt the MgO and the Devarda alloy way of distillation, sample leaching liquor 20ml is placed distillery (being formed by the transformation of Kelvin bottle) bottom, add the appropriate MgO suspension from the distillery lateral opening, feed steam distillation, the BAS that is added with indicator with the triangular flask splendid attire in the condenser pipe lower end absorbs the ammonium nitrogen distill out, when liquid to be recycled reaches 30～40ml, add the Devarda alloy from distillery side mouth, the triangular flask that reclaims liquid is contained in the condenser pipe lower end to be replaced with the new triangular flask that BAS is housed, continue distillation, by the time reclaim and stop distillation when liquid reaches 30～40ml, take off to be equipped with and reclaim the triangular flask that liquid is used, two triangular flasks in front and back are used the standard acid titration respectively, can draw the ammonium nitrogen in the sample and the content of nitrate nitrogen.
Detailed process is as follows:
1) in distillery, adds testing sample leaching liquor and MgO, realize heating by importing steam to the distillery bottom, steam imports to liquid level and all can up and down, the purpose of heating is for promoting leaching liquor and the MgO generation ammonia that reacts, ammonia is condensed after deriving by conduit with steam again, reclaim condensed fluid with concentration known HCl titration, to determine ammonium nitrogen content;
2) add the Devarda alloy in distillery, continue to be blown into steam to the distillery bottom, nitrate nitrogen is reduced to ammonium nitrogen, and then generation ammonia, it is condensed mix the rear tube derivation with vapours after, reclaims condensed fluid with concentration known HCl titration, can obtain nitrate nitrogen content in the sample.
In testing sample leaching liquor 10-20ml, MgO (suspension of powder or respective amount all can) consumption is 0.2 gram or surpasses 0.2 gram; Devarda alloy (powder) consumption 0.2 restrains or surpasses 0.2 and restrains; Usually contain the boric acid aqueous solution 5ml that concentration is 20g/L in the container of recovery condensed fluid, wherein contain micro-indicator (1-2 drips and gets final product); Described indicator can be methyl red-bromcresol green indicator, and it is that 0.1 gram methyl red and 0.5 gram bromcresol green are added in the 100ml ethanol, grinds dissolving and obtain in agate mortar.When the condensed fluid that reclaims is 25-35ml, can carry out titration;
The isolated plant of described assay method comprises steam raising plant, distillery, condenser pipe, well heater and liquids recovery container; Distillery is provided with gas inlet and outlet and charge door, the steam (vapor) outlet of steam raising plant links to each other with the gas feed of distillery by conduit, the gas vent of distillery links to each other with the interior pipeline inlet of condenser pipe by conduit, and the interior pipeline outlet of condenser pipe extend in the liquids recovery container; The outer pipeline of condenser pipe is provided with cooling water inlet and outlet, and they link to each other with the pipeline of chilled water respectively.
Steam raising plant is made up of distilling flask and well heater, and the liquids recovery container is a triangular flask; Well heater can be external heater (as: Electric stove, spirit lamp), or the electric furnace heating wire of inner heating; Between distillery and distilling flask the catherer connection tube road be provided with the stainless steel connector; When described steam raising plant and well heater were one, these three devices of distillery, condenser pipe and liquids recovery container can be respectively 1 group, 2 groups, 3 groups or 4 groups.
Principle of the present utility model is: adopt MgO and Devarda alloy way of distillation principle, as distillery, make the interpolation of some reagent in the mensuration process more convenient in the Kelvin bottle of improved.Add the MgO suspension at the sample determination initial stage, ammonium nitrogen in the sample is taken away by steam and do not influenced the existence of nitrate nitrogen in the sample, this has also removed the ammonium nitrogen under the original state in the leaching liquor, eliminates it measures (is that ammonium nitrogen is measured it again with the nitrate-nitrogen reduction in the sample by adding the Devarda alloy) to nitrate nitrogen in the sample influence.
The utlity model has following advantage:
1. technology is simple, is convenient to operation.This method and instrument are improved old-fashioned Kelvin bottle, directly use it as distillery, and production technology and uncomplicated, and through this improvement is greatly simplified the step of adding MgO and Devarda alloy in the mensuration process of whole sample.Because distillery is convenient to change, therefore, finish after the batch sample if standby distillery is arranged, promptly replaceable distillery, this makes under the situation that does not stop whole mensuration process, and the replacing of finishing sample and distillery becomes possibility.The equipment of changing can clean at once, with standby.
2. repeated, good stability, measurement result is accurate.Because the utility model can add MgO and Devarda alloy by substep in the sample leaching liquor, therefore ammonium nitrogen in the sample leaching liquor and nitrate nitrogen separated measuring can have been removed the influence that ammonium nitrogen is measured nitrate nitrogen, make measurement result more accurate.
3. durable in use, safeguard simple.The link of key and rapid wear all adopts stainless steel to make in the utility model, and the long duct that steam is fed the distillery bottom also adopts stainless steel, and this design can not cause when changing distillery, and long service life takes place the phenomenon of damaging conduit.That distillery cleans is very convenient, has overcome the not shortcoming that easily sample determination thereafter impacted of easy cleaning, residual effect of existing equipment.Therefore operation and maintenance of the present utility model is very simple and direct, convenient.
4. structure and conceptual design are reasonable.Because the utility model can allow to add MgO earlier among the mensuration process, the ammonium nitrogen that exists in the working sample then adds the Devarda alloy, is ammonium nitrogen with the nitrate-nitrogen reduction that remains in the sample, measures again.Therefore each sample can obtain required two results (ammonium nitrogen, nitrate nitrogen) through once measuring, and can use manpower and material resources sparingly like this, reduces the error that causes owing to the experiment pre-treatment.
Description of drawings
Fig. 1 is the utility model method equipment therefor (soil ammonium and nitrate nitrogen determinator) structural representation;
Fig. 2 is the side view of stainless steel connector in used soil ammonium of the utility model method and the nitrate nitrogen determinator;
Fig. 3 connects the upward view in street corner for stainless steel in used soil ammonium of the utility model method and the nitrate nitrogen determinator;
1 is electric power connection line among the figure, and 2 is electric furnace heating wire, and 3 is conduit, 4 is the distilling flask plug, and 5 is distilling flask, and 6 is support, 7 is stainless joint, and 8 are fixing stainless joint clip, and 9 is that skin one encloses plug, 10 are long stainless steel pipe, and 11 is the outlet of second condenser pipe, and 12 is condenser, 13 is the charge door bottle stopper, and 14 is the distillery charge door, and 15 is distillery, 16 is second condenser pipe inlet, and 17 is support spring, and 18 is spring suppport, 19 communicate for the stainless steel steam pipeline, 20 is triangular flask, and 21 is the gas vent conduit of distillery, and 22 is the outlet of first condenser pipe, 23 is coolant guide pipe, 24 is first condenser pipe inlet, and 25 is carriage, and 26 is base.
Embodiment
The utility model assay method equipment therefor: as shown in Figure 1, mainly comprise the conduit between stainless steel connector, condenser pipe, the each several part between distilling flask, distillery, distillery and distilling flask, support, support is with spring and base and be used for the compositions such as triangular flask that splendid attire plays the BAS of absorption.Wherein, distilling flask 5 places on the carriage 25, and be connected in distillery 15 by conduit 3, stainless joint 7, acting as of long stainless steel pipe 10 imports the distillery bottom with steam, simultaneously, stainless joint 7 communicates with stainless steel steam pipeline 19 again, and steam is condensed after by condenser 12, is recovered in the triangular flask 20; Each device all is placed on the support, after steam steams from distilling flask, enters distillery by conduit and stainless steel connector, and the ammonia that the reaction in the distillery generates promptly with steam process condenser pipe, is collected in the triangular flask that fills BAS at last.
Operation steps is as follows:
1) add distilled water in distilling flask 5, the water yield is about 3/4 of a distilling flask.Enter the mouth from first condenser pipe and 24 constantly to inject cold water, it will fill with two condenser pipes with cold water by first condenser pipe outlet, 22, second condenser pipe inlet 16 and coolant guide pipe 23, from the second condenser pipe exit cold water is derived, cold water promptly is recycled and adds in the condenser pipe like this, to playing condensation through the steam of stainless steel steam lead 19 by wherein.Adding the concentration that has 2 indicator (0.1 gram methyl red and 0.5 gram bromcresol green are added in the 100ml ethanol, grind dissolving and obtain in agate mortar) in triangular flask 20 is the boric acid aqueous solution 5ml of 20g/L; BAS is used to absorb the ammonium nitrogen that distills out;
2) sample thief leaching liquor 20ml injects distillery 15 bottoms, and distillery is connected in plug 9 places, uses fixedly distillery of lower support spring simultaneously;
3) add MgO powder or suspension from distillery charge door 14, connect the electric power connection line 1 in distilling flask 5 exits, electric furnace heating wire 2 begins the water in the bottle is heated in the distilling flask, steam is promptly by conduit 3 and stainless steel connector 7, import distillery 15 bottoms by long stainless steel pipe 10, sample reacts herein, and the ammonia of generation, is recovered in the triangular flask 20 after conduit 21,19 is condensed with steam.When liquid to be recycled reaches 30～40ml, behind a small amount of distilled water cleaning pipe 19 exits, change the triangular flask that is added with BAS.The triangular flask of changing is with known standard concentration HCl (concentration of hydrochloric acid is near 0.01mol/L) titration, to determine ammonium nitrogen content;
4) in distillery, add the Devarda alloy from distillery charge door 14, it can be an ammonium nitrogen with nitrate-nitrogen reduction in the sample leaching liquor, finally generates ammonia, and it also will be recovered in the triangular flask 20 at last with steam, when recovery liquid reaches 30～40ml, change triangular flask.With concentration known HCl titration, can obtain nitrate nitrogen content in the sample;
5) stop distillation, depress support spring 17, take off distillery 15, clean, with standby, change the standby distillery that has added sample, energized continues distillation, measures;
Because two cover distillery and relevant devices (Fig. 1) are housed on this covering device, therefore can measure two samples respectively at every turn, if any special requirement, also the number of distillery can be expanded to 4.
This critical component of distillery that the utility model adds distillery charge door 14 makes in the test process substep add medicine becomes possibility, and experimental implementation is easier, and is more prone to hold on the time that adds reagent.The ammonium nitrogen in this substep adding medicine working sample and the method for nitrate nitrogen cooperate this instrument, have simplified experimental procedure, have improved work efficiency, have strengthened the feasibility of this method.Many places rapid wear, easy parts aging, corrosion all use stainless steel to make in the utility model, make this instrument more durable, and are not fragile.
Be check this method and the repeatability of instrument and the accuracy of mensuration, special compound concentration is ammonium nitrogen and the nitrate nitrogen standard solution of 50ppm, reclaims determination experiment, and experimental result sees Table 1, table 2.By measurement result as can be seen, result of experiment repeatability is very good several times, and the coefficient of variation is very little, and ammonium nitrogen and nitrate nitrogen all can accurately be measured in the interpret sample.
Table 1 ammonium nitrogen recovery measuring result
| Repeat number | Consume HCl amount (ml) | Ammonium nitrogen concentration (ppm) | The recovery (%) |
| 1 | 11.37 | 49.74 | 99.5 |
| 2 | 11.35 | 49.66 | 99.3 |
| 3 | 11.45 | 50.09 | 100.2 |
| 4 | 11.32 | 49.53 | 99.1 |
| 5 | 11.31 | 49.48 | 99.0 |
| Mean value | 11.36 | 49.70 | 99.4 |
| Standard deviation | 0.056 | 0.241 | 0.476 |
| The coefficient of variation (%) | 0.49 | 0.49 | 0.48 |
Annotate: HCl concentration is 0.00625mol/L
Table 2 nitrate nitrogen recovery measuring result
| Repeat number | Consume HCl amount (ml) | Nitrate nitrogen concentration (ppm) | The recovery (%) |
| 1 | 7.93 | 50.35 | 100.7 |
| 2 | 7.95 | 50.47 | 100.9 |
| 3 | 7.81 | 49.59 | 99.2 |
| 4 | 7.86 | 49.90 | 99.8 |
| 5 | 7.82 | 49.65 | 99.3 |
| Mean value | 7.87 | 49.99 | 99.98 |
| Standard deviation | 0.063 | 0.403 | 0.008 |
| The coefficient of variation (%) | 0.806 | 0.806 | 0.806 |
Annotate: HCl concentration is 0.00907mol/L
Claims (5)
1. a device of measuring soil ammonium and nitrate nitrogen is characterized in that: comprise steam raising plant, distillery, condenser pipe, well heater and liquids recovery container; Distillery is provided with gas inlet and outlet and charge door, the steam (vapor) outlet of steam raising plant links to each other with the gas feed of distillery by conduit, the gas vent of distillery links to each other with the interior pipeline inlet of condenser pipe by conduit, and the interior pipeline outlet of condenser pipe extend in the liquids recovery container; The outer pipeline of condenser pipe is provided with cooling water inlet and outlet, and they link to each other with the pipeline of chilled water respectively.
2. according to the device of described mensuration soil ammonium of claim 1 and nitrate nitrogen, it is characterized in that: described steam raising plant is made up of distilling flask and well heater, and the liquids recovery container is a triangular flask.
3. according to the device of described mensuration soil ammonium of claim 2 and nitrate nitrogen, it is characterized in that: described well heater can be external heater, or the electric furnace heating wire of inner heating.
4. according to the device of described mensuration soil ammonium of claim 2 and nitrate nitrogen, it is characterized in that: the catherer connection tube road between described distillery and distilling flask is provided with the stainless steel connector.
5. according to the device of described mensuration soil ammonium of claim 1 and nitrate nitrogen, it is characterized in that: when described steam raising plant and well heater were one, these three devices of distillery, condenser pipe and liquids recovery container can be respectively 1 group, 2 groups, 3 groups or 4 groups.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200420069946 CN2733355Y (en) | 2004-07-23 | 2004-07-23 | Device for determining ammonium state nitrogen and nitrate nitrogen in soil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200420069946 CN2733355Y (en) | 2004-07-23 | 2004-07-23 | Device for determining ammonium state nitrogen and nitrate nitrogen in soil |
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| CN2733355Y true CN2733355Y (en) | 2005-10-12 |
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| CN 200420069946 Expired - Fee Related CN2733355Y (en) | 2004-07-23 | 2004-07-23 | Device for determining ammonium state nitrogen and nitrate nitrogen in soil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106872385A (en) * | 2016-12-31 | 2017-06-20 | 新昌县迪斯曼科技有限公司 | A kind of chemical fertilizer it is water-soluble go out nitrogen nutrient on-line measuring device |
-
2004
- 2004-07-23 CN CN 200420069946 patent/CN2733355Y/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106872385A (en) * | 2016-12-31 | 2017-06-20 | 新昌县迪斯曼科技有限公司 | A kind of chemical fertilizer it is water-soluble go out nitrogen nutrient on-line measuring device |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20051012 |