CN107957478A - A kind of device and method of total soil nitrogen measure - Google Patents
A kind of device and method of total soil nitrogen measure Download PDFInfo
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- CN107957478A CN107957478A CN201810003981.3A CN201810003981A CN107957478A CN 107957478 A CN107957478 A CN 107957478A CN 201810003981 A CN201810003981 A CN 201810003981A CN 107957478 A CN107957478 A CN 107957478A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
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Abstract
The invention discloses a kind of device and method of total soil nitrogen measure, described device mainly includes steam unit, disappears and boil device, gas-liquid separation device, condensing unit and titration bottle；Steam unit boils device and is connected with disappearing, and disappears and boils device connection and be connected with gas-liquid separation device, gas-liquid separation device is connected and is connected with condensing unit, and condensing unit is connected and is connected with titration bottle；The described method includes：The inspection and cleaning of device；Soil sample, which disappears, boils；The distillation of ammonia in the boil liquid that disappears；Standard solution is titrated；The configuration of the present invention is simple, and cost of the present invention is cheap, is adapted to large-scale popularization.
Description
Technical field
The present invention relates to Soil K+adsorption technical field, and in particular to a kind of device and method of total soil nitrogen measure.
Background technology
Soil refers to one layer of loose material of earth surface, by various particulate minerals, organic substance, moisture, sky
Gas, microorganism etc. form, can growing plant.Mineral matter that soil is formed by rock weathering, animals and plants, the production of microorganism residuum decomposition
Raw organic matter, geobiont (solid matter) and moisture (liquid phase substance), air (gaseous substance), the humus of oxidation etc.
Composition.Solid matter includes soil mineral, organic matter and microorganism and passes through nutriment for being obtained after the antibacterial sterilizing of illumination etc..Liquid
Material refers mainly to soil moisture.Gas is the air being present in soil aperture.This three classes material constitutes a lance in soil
The entity of shield.They are interknited, and are conditioned each other, living condition necessary to be provided for crop, are the material bases of soil fertility
Plinth.
Soil plough horizon is for the soil of farming, is without this for the soil still in natural form
Concept.The structure under natural conditions of soil has been upset in the agricultural planting activity for being formed as the mankind of soil plough horizon, is
Upper soll layer about 0-20cm.Level below soil plough horizon is known as ploughing bottom.Have how more thickness are on earth for soil plough horizon
Division, Xibei Univ. of Agricultural ＆ Forest Science ＆ Technology agrology expert professor Wang Yiquan thinks that distinguishing soil plough horizon mainly has two to set out
Point：First, the fertility of soil, that is, the concentrated layer of the main nutrient organic matter of soil；Second, the extent of the root system of soil, is ploughed
Make layer naturally will with root system of plant corresponding to.It is inconsistent according to this 2 points each local topsoils, but for the side of research
Just we are in general using the topsoil thickness from native this vertical thickness of surface 0-20cm as soil.Soil plough horizon is on the one hand rich
The main fertility of soil is collected, has on the other hand been also the main concentrated part of soil root.Can be according to reality during specific research
Situation determines the topsoil thickness of soil.Because some plants are shallower as the root system of cucumber and strawberry ratio, the root system of broad-leaved arbor
Than shallower, and the root system of Cereal is with regard to deep.The experiment of soil planing surface shows place of origin Yang Ling in China's agricultural, less than eight meters
Still the root system of visible wheat.
Total nitrogen content in China's soil plough horizon is probably changed 0.05%~0.25%.The black earth of wherein the Northeast is
China's soil is averaged the highest soil of nitrogen content, and generally 0.15%~0.35%.And northwest loess plateau and the North China Plain
Soil nitrogenous amount is relatively low, and generally 0.05%~0.1%.Central China South China, total nitrogen content of soil have larger luffing, generally
For 0.04%~0.18%.In the case of condition is substantially similar, the nitrogen content in paddy field is often higher than dryland soil.China is big absolutely
Part soil application nitrogenous fertilizer has certain effect of increasing production.
The height of total nitrogen content in soil, the potential fertility for reflecting soil are horizontal.Therefore, the full nitrogen in soil analysis point
Analysis is one of important indicator；Protein is nitrogenous organic compound.Protein and sulfuric acid and catalyst together hot digestion, make
Breaks down proteins, the ammonia of decomposition are combined generation ammonium sulfate with sulfuric acid.Then alkalization distillation ammonia is dissociated, after being absorbed with boric acid again with
Sulfuric acid or hydrochloric acid standard solution titration, are multiplied by conversion coefficient, and be converted into protein content according to the consumption of acid.
Soda acid bucket no pressure often occurs using nitrogen auto analyzer distillation soil digested solusion, azotometer in the prior art, acid
Alkali pipeline or air pump gas leakage, damage.During instrument long-time service, there is incrustation scale on heater, the cleaning of distiller, when titration can not
Acid ＆ alkali liquid etc. frequent produced problem is added dropwise.
The content of the invention
For above-mentioned problem, first technical problem that the present invention solves there is provided it is a kind of it is easy to operate, can
Dismounting, the device of easy cleaned total soil nitrogen measure, another technical problem that the present invention solves there is provided a kind of soil
The method of full nitrogen determination.
To solve above-mentioned first technical problem, the technical scheme is that：A kind of device of total soil nitrogen measure, it is main
To include steam unit, disappear and boil device, gas-liquid separation device, condensing unit and titration bottle；The steam unit is boiled with described disappear
Device connect, disappear boil device connection be connected with the gas-liquid separation device, gas-liquid separation device connection and the condensing unit company
Connect, condensing unit connection is connected with the titration bottle；
The steam unit includes steam chest, case lid, heating unit and strainer, be provided with the steam chest water inlet,
Discharge outlet and limit fastener, the row's of being provided with steam unit on the case lid；The side box wall that the water inlet is arranged on steam chest leans on
Upper position, the discharge outlet are arranged on steam chest side box wall lower end and put, and the limiting card is buckled with two, is separately positioned on steam chest
On left and right tank wall；The case lid is flexibly connected with steam chest, and the heating unit is arranged in steam chest, heating unit with it is outer
Portion's power supply connection, the strainer is opening up cylindrical shape or cuboid, and strainer is arranged in steam chest, is enclosed in heating
The periphery of device, the convex shoulder activity on strainer top are placed on limit fastener, and the convex shoulder on strainer top is less than water inlet；
Described disappear boils device and includes disappearing and boiling Bottle and bottle cap, exhaust apparatus, charging hopper is provided with the bottle cap and into steaming
Steam pipe；Described disappear boils Bottle and bottle cap flexible connection, and through bottle cap upper end is arranged on, the charging hopper runs through the exhaust apparatus
Be arranged on bottle cap, and the lower port of charging hopper boils a bottle inner upper end position positioned at disappearing, the steam lead by hose with
Row's steam unit connection, steam lead, which runs through, to be arranged on bottle cap, and steam lead lower port boils subordinate in bottle positioned at disappearing
End position；
The gas-liquid separation device includes collector and separator, and the separator is arranged on inside collector, the receipts
Collection port and exhaust outlet are provided with storage, the separator includes separating plate and separation convex mouth, is provided with the separating plate
Liquid-leaking nozzle；The collection port is arranged on collector lower surface center, and collection port is connected by hose with exhaust apparatus；It is described
Exhaust outlet has multiple, is uniformly arranged on the outer side position in collector upper surface；The separating plate is arranged on collector bosom
Section, the separation convex mouth are arranged on separating plate upper surface center, and the liquid-leaking nozzle has multiple, is evenly distributed on separating plate
On, positioned at the surrounding of separation convex mouth；
The condensing unit includes condensed water container and crosses tracheae, and the tracheae of crossing is through being arranged on the interior of condensed water container
Portion；Condensation water inlet and condensation-water drain are provided with the condensed water container；The condensation water inlet is arranged on the condensation water capacity
The lower end of device, the condensation-water drain are arranged on the upper end of condensed water container；The tracheae upper port excessively passes through soft with exhaust outlet
Pipe connects, and crosses tracheae lower port and is connected by pipeline pipe with the titration bottle.
Further, aperture of filter screen 0.5mm-2mm；Effectively the incrustation scale produced on heating unit can be intercepted and filtered
Online side, periodically can clean strainer, scale removal, avoid incrustation scale and block outlet pipe, and influence heating unit can not
Effectively heated, influence the duration of experiment.
Further, arranging steam unit includes gas collection flaring one, connecting tube one and connection pipe port one, the gas collection flaring
One has two, and two gas collection flarings one are arranged on case lid, positioned at the inner upper end of steam chest, leads between two gas collection flarings one
The connecting tube one is crossed to connect, the connection pipe port one is arranged in connecting tube one, and connect pipe port one be used for into steaming
Steam pipe connects；Exhaust apparatus includes gas collection flaring two, connecting tube two and connection pipe port two, and the gas collection flaring two has two,
Two gas collection flarings two are arranged on bottle cap upper end, are connected between two gas collection flarings two by the connecting tube two, the connection
Pipe port two is arranged in connecting tube two, and is connected pipe port two and be used to be connected with collection port；It can effectively be collected, make
More high efficiency must be tested.
Further, port is both provided with bayonet with hose junction；The company between hose and device port can be reinforced
Connect, effectively avoid the failure of an experiment caused by the coming off of hose in experimentation again.
Further, filler cap is movably set with charging hopper；After being fed, filler cap is covered tightly, is made
It must disappear to boil and sealing state is presented in device so that experimental result is more rigorous.
Further, tracheae caliber excessively is thicker than hose caliber, and it is spiral to be arranged on the tracheae of crossing inside condensed water container
Shape, can more effectively carry out condensation process.
To solve above-mentioned second technical problem, the technical scheme is that：A kind of total soil nitrogen method for measuring, bag
Include following steps：
Step 1：The inspection and cleaning of device
After device is connected, from water inlet plus water, open heating unit, first check device whether gas leakage, and pass through water
Distillate pipeline and device are cleaned；After inspection, heating unit is closed, is discharged from discharge outlet by superfluous water, place 1h,
It is stand-by after device naturally dry；
Step 2：Soil sample, which disappears, boils
Opening, which disappears, boils the bottle cap of device, and soil sample is sent into disappear and is boiled in bottle, after adding 0.5-1ml deionized waters moistening soil sample, adds
Enter 2g accelerators and 5ml sulfuric acid, shake up；It will disappear and boil bottle 21 and be placed on 300W alternating temperature electric furnaces, and heat 10-15min with small fire, treat
When reaction relaxes in bottle, strengthen the firepower native liquid boiled that makes to disappear and keep slightly boiling, the part of heating is no more than the liquid level in bottle, to prevent bottle
Wall temperature is excessive and is thermally decomposed ammonium salt, causes nitrogen loss；The temperature boiled of disappearing with sulfuric acid vapor at the pre- top 1/3 of bottle it is cold
Solidifying reflux is advisable；After boil liquid is disappeared and grogs is all changed into greyish white slightly band green, it is further continued for disappearing and boils 1h；Disappear to boil and finish, cool down, treat
Distillation；Disappear boil soil sample while, do two parts of blank determinations, in addition to soil sample is not added with, other operation all with measure soil sample it is identical；
Step 3：The distillation of ammonia in the boil liquid that disappears
After the boil liquid cooling that disappears, it will disappear and boil bottle and bottle cap and be connected in device；Added into titration bottle 5ml 2% boric acid-
Indicator mixed liquor, is placed on condensing unit lower end so that the lower end mouth of pipe for the pipeline pipe being connected with crossing tracheae lower end is placed in boric acid
At liquid level above 3-4cm；Filler cap is opened, 20ml10mol/L sodium hydroxide solutions is slowly added to by crossing charging hopper, opens
Heating unit, is passed through steam distillation, when liquid product to be distillated is about 50ml, i.e. distillation finishes；With being adjusted to pH4.5's on a small quantity
The end for the pipeline pipe that water washing condensing unit is connected with buret；
Step 4：Standard solution is titrated
Aubergine is changed into from blue-green with 0.005mol/L sulfuric acid standard solution titration distillate；
Step 5：Interpretation of result
According to the soil sample weight weighed and detect that the concentration of digestion solution calculates the content of full nitrogen in sample：
Total soil nitrogen (%)=(V-V0) * 0.014*CH*100/m
V------ titrates the volume of sour standard solution used during test solution, ml；
V0------ titrates the volume of sour standard solution used during blank, ml；
CHThe concentration of --- --- sour standard solution, mol/L；
The quality of soil sample, g after m------- drying.
Compared with prior art, beneficial effects of the present invention：Steam unit of the present invention is set using flexible connection
Case lid is put, periodically effectively the incrustation scale inside steam unit can be cleared up, and sets strainer to clear up incrustation scale
Work become succinct, only need to be by strainer periodic cleaning；Meanwhile disappear used by our invention boil device using bottle, lid separation,
It can effectively be boiled using disappearing after bottle disappear and boil, combine, examined that will disappear to boil bottle and be attached with other devices of the invention
Survey step, can flexibly, be efficiently completed test experience；In addition, the gas-liquid separation device of the present invention can be effectively to gas-liquid
Separated, enable to experiment accurately to complete；The configuration of the present invention is simple, can reduce user when being operated
Error, and cost of the present invention is cheap, is adapted to large-scale popularization.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention；
Fig. 2 is the structure diagram of row's steam unit of the present invention；
Fig. 3 is the top view of the bottle cap of the present invention；
Fig. 4 is the structure diagram of the gas-liquid separation device of the present invention；
Fig. 5 is the structure diagram of the separator of the present invention；
Wherein, 1- steam units, 11- steam chests, 111- water inlets, 112- discharge outlet, 113- limit fasteners, 12- case lids,
13- heating units, 14- strainers, 15- rows steam unit, 151- gas collections flaring one, 152- connecting tubes one, 153- connection pipe ports
First, 2- disappear boil device, 21- disappear boil bottle, 22- bottle caps, 221- exhaust apparatus, 222- charging hoppers, 2220- filler caps, 223- into
Steam pipe, 3- gas-liquid separation devices, 31- collectors, 311- collection ports, 312- exhaust outlets, 32- separators, 321- separating plates,
3210- liquid-leaking nozzles, 322- separation convex mouth, 4- condensing units, 41- condensed water containers, 411- condensations water inlet, 412- condensed waters go out
Mouth, 42- cross tracheae, 5- titration bottles.
Embodiment
Embodiment：A kind of device of total soil nitrogen measure as shown in Figs. 1-5, mainly includes steam unit 1, disappears and boil device
2nd, gas-liquid separation device 3, condensing unit 4 and titration bottle 5；
Steam unit 1 includes steam chest 11, case lid 12, heating unit 13 and strainer 14, is provided with steam chest 11 into water
Mouthfuls 111, discharge outlet 112 and limit fastener 113, the row's of being provided with steam unit 15 on case lid 12；Water inlet 111 is arranged on steam chest
11 side box wall upper position, discharge outlet 112 are arranged on 11 side box wall lower end of steam chest and put, and limit fastener 113 has two, respectively
It is arranged on 11 left and right tank wall of steam chest；Case lid 12 is flexibly connected with steam chest 11, and heating unit 13 is arranged on steam chest 11
Interior, heating unit 13 is connected with external power supply, and strainer 14 is opening up cylindrical shape or cuboid, and strainer 14 is arranged on steaming
In vapour case 11, the periphery of heating unit 13 is enclosed in, the convex shoulder activity on 14 top of strainer is placed on limit fastener 113, and is filtered
The convex shoulder on 14 top of net is less than water inlet 111, and 14 aperture of strainer is 1mm；Arranging steam unit 15 includes gas collection flaring 1, connects
Adapter 1 and connection pipe port 1, gas collection flaring 1 have two, and two gas collection flarings 1 are arranged on case lid 12
On, positioned at the inner upper end of steam chest 11, connected between two gas collection flarings 1 by connecting tube 1, connect pipe port
One 153 are arranged in connecting tube 1；
Disappear and boil device 2 and include disappearing and boiling bottle 21 and bottle cap 22, exhaust apparatus 221,222 and of charging hopper are provided with bottle cap 22
Steam lead 223；Disappear and boil bottle 21 and bottle cap 22 is flexibly connected, exhaust apparatus 221 is through being arranged on 22 upper end of bottle cap, exhaust apparatus
221 include gas collection flaring two, connecting tube two and connection pipe port two, and gas collection flaring two has two, and two gas collection flarings two are set
Connected between 22 upper end of bottle cap, two gas collection flarings two by connecting tube two, connection pipe port two is arranged in connecting tube two；
Charging hopper 222, which runs through, to be arranged on bottle cap 22, and the lower port of charging hopper 222 boils 21 inner upper end position of bottle positioned at disappearing,
Filler cap 2220 is movably set with charging hopper 222, steam lead 223 is connected by hose with row's steam unit 15, into steaming
223 upper port of steam pipe is connected with being connected pipe port 1, and steam lead 223, which runs through, to be arranged on bottle cap 22, and steam lead
223 lower ports boil 21 interior lower end position of bottle positioned at disappearing；
Gas-liquid separation device 3 includes collector 31 and separator 32, and separator 32 is arranged on inside collector 31, collector
Collection port 311 and exhaust outlet 312 are provided with 31, separator 32 includes separating plate 321 and separates convex mouth 322, on separating plate 321
It is provided with liquid-leaking nozzle 3210；Collection port 311 is arranged on 31 lower surface center of collector, and collection port 311 passes through hose and row
Device of air 221 connects, and collection port 311 is connected with being connected pipe port two；Exhaust outlet 312 has four, is uniformly arranged on collector 31
The outer side position in upper surface；Separating plate 321 is arranged on 31 bosom section of collector, and separation convex mouth 322 is arranged on separating plate 321
Upper surface center, liquid-leaking nozzle 3210 have four, are evenly distributed on separating plate 321, positioned at the surrounding of separation convex mouth 322；
Condensing unit 4 includes condensed water container 41 and crosses tracheae 42, crosses tracheae 42 through being arranged on condensed water container 41
It is internal；Condensation water inlet 411 and condensation-water drain 412 are provided with condensed water container 41；Condensation water inlet 411 is arranged on condensation
The lower end of water container 41, condensation-water drain 412 are arranged on the upper end of condensed water container 41；42 caliber of tracheae is crossed than hose caliber
Slightly, and be arranged on inside condensed water container 41 cross tracheae 42 be helical form, mistake 42 upper port of tracheae with exhaust outlet 312 by soft
Pipe connects, and crosses 42 lower port of tracheae and is connected by pipeline pipe with titration bottle 5.
Wherein, port is both provided with bayonet with hose junction.
Using the present apparatus to total soil nitrogen method for measuring, comprise the following steps：
Step 1：The inspection and cleaning of device
After device is connected, from water inlet 111 plus water, open heating unit 13, first check device whether gas leakage, and lead to
The distillate for crossing water cleans pipeline and device；After inspection, heating unit 13 is closed, arranges superfluous water from discharge outlet 112
Go out, place 1h, it is stand-by after device naturally dry；
Step 2：Soil sample, which disappears, boils
Opening, which disappears, boils the bottle cap 22 of device 2, and soil sample is sent into disappear and is boiled in bottle 21, after adding 1ml deionized waters moistening soil sample, adds
Enter 2g accelerators and 5ml sulfuric acid, shake up；It will disappear and boil bottle 21 and be placed on 300W alternating temperature electric furnaces, and heat 15min with small fire, treat bottle
When interior reaction relaxes, strengthen the firepower native liquid boiled that makes to disappear and keep slightly boiling, the part of heating is no more than the liquid level in bottle, to prevent bottle wall
Temperature is excessive and is thermally decomposed ammonium salt, causes nitrogen loss；The temperature boiled that disappears is condensed with sulfuric acid vapor at the pre- top 1/3 of bottle
Reflux is advisable；After boil liquid is disappeared and grogs is all changed into greyish white slightly band green, it is further continued for disappearing and boils 1h；Disappear to boil and finish, cool down, wait to steam
Evaporate；Disappear boil soil sample while, do two parts of blank determinations, in addition to soil sample is not added with, other operation all with measure soil sample it is identical；
Step 3：The distillation of ammonia in the boil liquid that disappears
After the boil liquid cooling that disappears, it will disappear and boil bottle 21 and bottle cap 22 and be connected in device；5ml 2% is added into titration bottle 5
Boric acid-indicator mixed liquor, is placed on 4 lower end of condensing unit so that the lower end mouth of pipe for the pipeline pipe being connected with crossing 42 lower end of tracheae
It is placed at boric acid liquid level above 3-4cm；Filler cap 2220 is opened, 20ml10mol/L hydrogen is slowly added to by crossing charging hopper 222
Sodium hydroxide solution, opens heating unit 13, is passed through steam distillation, when liquid product to be distillated is about 50ml, i.e. distillation finishes；With less
Amount is adjusted to the end for the pipeline pipe that the water washing condensing unit 4 of pH4.5 and buret 5 connect；
Step 4：Standard solution is titrated
Aubergine is changed into from blue-green with 0.005mol/L sulfuric acid standard solution titration distillate；
Step 5：Interpretation of result
According to the soil sample weight weighed and detect that the concentration of digestion solution calculates the content of full nitrogen in sample：
Total soil nitrogen %=(V-V0) * 0.014*CH*100/m
V------ titrates the volume of sour standard solution used during test solution, ml；
V0------ titrates the volume of sour standard solution used during blank, ml；
CHThe concentration of --- --- sour standard solution, mol/L；
The quality of soil sample, g after m------- drying.
With the present invention to Purple Soils In Sichuan Province (ASA-3a), Hubei rice soil (ASA-4a), Heilungkiang black earth (ASA-7), peace
Four kinds of soil of emblem moisture soil (ASA-10) four regions carry out ten groups of test experience respectively；Table 1 is to soil using the present invention
The testing result of standard items；Table 2 is the metallic element actual content of the pedotheque；
Table 1：Testing result using the method for the present invention to Soil standard product
Table 2：The metallic element actual content of the pedotheque
By the Comparative result of above Tables 1 and 2 as it can be seen that between data and actual value that the method for the present invention detects
Deviation is especially small, within standard value deviation range.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
To modify to the technical solution described in previous embodiment, or equivalent substitution is carried out to which part technical characteristic；And
These modifications are replaced, and the essence of appropriate technical solution is departed from the spirit and model of technical solution of the embodiment of the present invention
Enclose.
Claims (7)
- A kind of 1. device of total soil nitrogen measure, it is characterised in that mainly including steam unit (1), disappear and boil device (2), gas-liquid Separator (3), condensing unit (4) and titration bottle (5)；The steam unit (1) includes steam chest (11), case lid (12), heating unit (13) and strainer (14), the steam chest (11) water inlet (111), discharge outlet (112) and limit fastener (113) are provided with, the row's of being provided with steam on the case lid (12) Device (15)；The water inlet (111) is arranged on the side box wall upper position of steam chest (11), and the discharge outlet (112) is set Put in steam chest (11) side box wall lower end, the limit fastener (113) there are two, is separately positioned on steam chest (11) left and right box On wall；The case lid (12) is flexibly connected with steam chest (11), and the heating unit (13) is arranged in steam chest (11), heating Device (13) is connected with external power supply, and the strainer (14) is opening up cylindrical shape or cuboid, and strainer (14) is set In steam chest (11), the periphery of heating unit (13) is enclosed in, the convex shoulder activity on strainer (14) top is placed on limit fastener (113) on, and the convex shoulder on strainer (14) top is less than water inlet (111)；Described disappear boils device (2) and includes disappearing and boiling bottle (21) and bottle cap (22), and exhaust apparatus is provided with the bottle cap (22) (221), charging hopper (222) and steam lead (223)；Described disappear boils bottle (21) and bottle cap (22) flexible connection, the exhaust Through bottle cap (22) upper end is arranged on, the charging hopper (222) is run through to be arranged on bottle cap (22) device (221), and is fed The lower port of funnel (222) boils bottle (21) inner upper end position positioned at disappearing, and the steam lead (223) passes through hose and the row Steam unit (15) connects, and steam lead (223), which runs through, to be arranged on bottle cap (22), and steam lead (223) lower port is located at Disappear and boil bottle (21) interior lower end position；The gas-liquid separation device (3) includes collector (31) and separator (32), and the separator (32) is arranged on collector (31) it is internal, collection port (311) and exhaust outlet (312) are provided with the collector (31), the separator (32) includes dividing From plate (321) and separation convex mouth (322), liquid-leaking nozzle (3210) is provided with the separating plate (321)；The collection port (311) Collector (31) lower surface center is arranged on, collection port (311) is connected by hose with exhaust apparatus (221)；The row Gas port (312) has multiple, is uniformly arranged on the outer side position in collector (31) upper surface；The separating plate (321) is arranged on receipts Storage (31) bosom section, the separation convex mouth (322) are arranged on separating plate (321) upper surface center, the leakage Hole (3210) has multiple, is evenly distributed on separating plate (321), positioned at the surrounding of separation convex mouth (322)；The condensing unit (4) includes condensed water container (41) and excessively tracheae (42), and the tracheae (42) excessively is cold through being arranged on The inside of condensate container (41)；Condensation water inlet (411) and condensation-water drain are provided with the condensed water container (41) (412)；The condensation water inlet (411) is arranged on the lower end of condensed water container (41), and the condensation-water drain (412) is arranged on The upper end of condensed water container (41)；Tracheae (42) upper port of crossing is connected with exhaust outlet (312) by hose, crosses tracheae (42) Lower port is connected by pipeline pipe with the titration bottle (5).
- 2. the device of a kind of total soil nitrogen measure according to claim 1, it is characterised in that strainer (14) aperture is 0.5mm-2mm。
- 3. the device of a kind of total soil nitrogen measure according to claim 2, it is characterised in that the net (14), which is enclosed in, to be added The surrounding of thermal (13).
- 4. the device of a kind of total soil nitrogen measure according to claim 1, it is characterised in that the port is connected with hose Place is both provided with bayonet.
- A kind of 5. device of total soil nitrogen measure according to claim 1, it is characterised in that the charging hopper (222) On be movably set with filler cap (2220).
- 6. the device of a kind of total soil nitrogen measure according to claim 1, it is characterised in that described to cross tracheae (42) caliber It is thicker than hose caliber, and it is helical form to be arranged on the internal tracheae (42) of crossing of condensed water container (41).
- 7. a kind of total soil nitrogen method for measuring, it is characterised in that comprise the following steps：Step 1：The inspection and cleaning of deviceAfter device is connected, from water inlet (111) plus water, open heating unit (13), first check device whether gas leakage, and lead to The distillate for crossing water cleans pipeline and device；After inspection, heating unit (13) is closed, will be unnecessary from discharge outlet (112) Water is discharged, and places 1h, stand-by after device naturally dry；Step 2：Soil sample, which disappears, boilsOpening, which disappears, boils the bottle cap (22) of device (2), and soil sample is sent into disappear and is boiled in bottle (21), adds 0.5-1ml deionized water humid soils After sample, 2g accelerators and 5ml sulfuric acid are added, is shaken up；It will disappear and boil bottle (21) and be placed on 300W alternating temperature electric furnaces, be heated with small fire 10-15min, when reaction relaxes in the bottle, strengthens the firepower native liquid boiled that makes to disappear and keeps slightly boiling, the part of heating is no more than in bottle Liquid level, it is excessive and thermally decomposed ammonium salt to prevent bottle wall temperature, cause nitrogen loss；The temperature boiled that disappears is pre- in bottle with sulfuric acid vapor Condensing reflux is advisable at top 1/3；After boil liquid is disappeared and grogs is all changed into greyish white slightly band green, it is further continued for disappearing and boils 1h；Disappear and boil Finish, cool down, it is to be distilled；Disappear boil soil sample while, do two parts of blank determinations, in addition to soil sample is not added with, other operation all with survey It is identical to determine soil sample；Step 3：The distillation of ammonia in the boil liquid that disappearsAfter the boil liquid cooling that disappears, it will disappear and boil bottle (21) and bottle cap (22) and be connected in device；5ml is added into titration bottle (5) 2% boric acid-indicator mixed liquor, is placed on condensing unit (4) lower end so that under the pipeline pipe being connected with crossing tracheae (42) lower end End pipe mouth is placed at boric acid liquid level above 3-4cm；Filler cap (2220) is opened, is slowly added to by crossing charging hopper (222) 20ml10mol/L sodium hydroxide solutions, open heating unit (13), are passed through steam distillation, when liquid product to be distillated is about 50ml, I.e. distillation finishes；The end of the pipeline pipe connected with the water washing condensing unit (4) and buret (5) for being adjusted to pH4.5 on a small quantity End；Step 4：Standard solution is titratedAubergine is changed into from blue-green with 0.005mol/L sulfuric acid standard solution titration distillate；Step 5：Interpretation of resultAccording to the soil sample weight weighed and detect that the concentration of digestion solution calculates the content of full nitrogen in sample：Total soil nitrogen (%)=(V-V0) * 0.014*CH*100/mV------ titrates the volume of sour standard solution used during test solution, ml；V0------ titrates the volume of sour standard solution used during blank, ml；CHThe concentration of --- --- sour standard solution, mol/L；The quality of soil sample, g after m------- drying.
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|---|---|---|---|---|
| CN108732169A (en) * | 2018-06-02 | 2018-11-02 | 彭春剑 | A kind of soil fertility detection method |
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