CN110068648A - Utilize the method for full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content - Google Patents
Utilize the method for full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content Download PDFInfo
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- CN110068648A CN110068648A CN201910356255.4A CN201910356255A CN110068648A CN 110068648 A CN110068648 A CN 110068648A CN 201910356255 A CN201910356255 A CN 201910356255A CN 110068648 A CN110068648 A CN 110068648A
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- G01N31/002—Determining nitrogen by transformation into ammonia, e.g. KJELDAHL method
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- G—PHYSICS
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- 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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Abstract
The invention discloses a kind of methods using full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content, it is desirable that full-automatic Kjeldahl determination device need to have delay function, have distillation cascade shield sensor, and distillation end point has volume and terminates two kinds of time selections；Ammonia nitrogen or ammonium nitrogen content in water sample or soil sample are first surveyed, recycling slops that Devardasalloy is added and sufficiently reacts reducing nitrate radical is ammonium ion, surveys pin state nitrogen content.It portion water sample or soil sample can be used to measure ammonia nitrogen or ammonium nitrogen content and nitrate nitrogen content simultaneously, and can not interfered by factors such as metal ion, organic matter, water body color, water body muddinesses in water body, pretreatment can be saved, the quick measurement of suitable batch samples；Soil sample measurement does not need to extract yet, and can directly measure.
Description
Technical field
The present invention relates to nitrogen content detection fields, and in particular to a kind of to use a sample using full-automatic Kjeldahl determination device
The method that product quickly measure water body or soil ammonia (ammonium) nitrogen and nitrate nitrogen content simultaneously.
Technical background
Water eutrophication is a kind of excessive caused water pollution phenomenon of the plant nutrient substances contents such as nitrogen, phosphorus.It is rich
Algae undue growth breeding, meeting under certain meteorological condition in the sunny range in water body surface layer in nutritive water
Break out cyanobacterial bloom.The dissolved oxygen content of breakout of cyanobacteria blooms Shi Shuizhong is extremely low, causes a large amount of aquatiles dead, dead is aquatic
Biogenic deposit is decomposed by the microorganisms to lakebed, this process consumes a large amount of dissolved oxygen, make water body dissolved oxygen content further sharply under
Drop causes water quality deterioration, smelly.The Eutrophication Status of the current water body in China is very severe, and the eutrophic extent of lake and reservoir is high,
Cyanobacterial bloom, which is frequently broken out, to be had become the norm, and region ecology safety and drinking water safety are severely impacted.2009 China Nian Shi 66% with
On lake and reservoir be in eutrophication (horse high honour etc., 2009), all lakes of the middle and lower reach of Yangtze River are at present
Eutrophic state, therefore the eutrophication monitoring of water body and improvement are particularly important.
Nitrogen is an important indicator of eutrophication water monitoring.Nitrogen in water body is mainly inorganic nitrogen and organic nitrogen.
Inorganic nitrogen includes ammonia nitrogen and nitrate nitrogen, wherein ammonia nitrogen include free ammoniacal nitrogen () and ammonium salt state nitrogen (), nitre state
Nitrogen include nitrate nitrogen () and nitrite nitrogen ().Organic nitrogen mainly has urea, amino acid, protein, core
The itrogenous organic substances such as acid, uric acid, fatty amine.Soluble organic nitrogen mainly exists with urea and protein form, can pass through ammonia
The effects of change, is converted to ammonia nitrogen.
Ammonia nitrogen detects common Na's colorimetry, phenol-hypochlorite colorimetric method etc., colorimetric method high sensitivity, but water body
In metal ion, organic matter, water body color, water body muddiness etc. can interference measurement；Nitrate often uses Pbenoldisulfonic Acid spectrophotometric
The measurement of the methods of method, ultraviolet spectrophotometry, but chloride, organic matter, carbonate and water body color and water body in water body
Muddiness etc. can generate interference to measurement.In order to eliminate interference when above-mentioned measurement, water sample need to do different pretreatments, but pre-process
The complexity of measurement process is increased, such as plus suitable zinc sulfate is in water sample, and adding sodium hydroxide makes to generate hydrogen-oxygen in alkalinity
Change zinc precipitating, using filtering off except color and muddiness etc., metal ion need to be added suitable screening agent and be eliminated.
Nitrogen is a great number of elements necessary to plant growth, the influence of spatial distribution crop of nitrogen content and nitrogen in soil
Yield and agricultural product quality.Nitrogen in soil measures in soil mainly with the presence of ammonium nitrogen, nitrate nitrogen and organic
Nitrogen content can study influence of the different agronomic measures to nitrogen utilization efficiency, to targetedly improve farming operations.Have
Machine state nitrogen can be converted into ammonium nitrogen or nitrate nitrogen is measured again, after the ammonium nitrogen in soil, nitrate nitrogen are often extracted with KCl at present
Again using the methods of distillation titration, colorimetric measurement, but sample needs to pre-process, and extraction time is long, is unfavorable for the fast of batch samples
Speed measurement.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of utilization to solve the above problems entirely certainly
The method of dynamic kjeldahl apparatus rapid survey water body or Soil Nitrogen Content measures ammonia (ammonium) nitrogen and nitre using a sample simultaneously
State nitrogen, and can not interfered by the factors such as metal ion, organic matter, water body color, water body muddiness in water body example, save pre- place
Reason；Soil sample does not need to extract, and can directly measure, and is suitble to the quick measurement of batch samples.
To achieve the above object, the present invention provides the following technical scheme that
Using the method for full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content, full-automatic Kjeldahl determination device needs to have
There is delay function, there is distillation cascade shield sensor, distillation end point has volume and terminates two kinds of time selections；
(1) blank value is measured
A. take not nitrogenous pure water 30-100ml that distillation cascade, distillation cascade capacity >=750ml is added, distillation cascade capacity is the bigger the better, can
It avoids being added after Devardasalloy because reacting acutely, liquid overflows into machine pipeline from distillation cascade when distillation, by full-automatic kelvin
The blank value of azotometer is set as 0, analyzes parameterDosage is set as 0ml,Dosage should be between 20-50ml, containing titration
The boric acid dosage of indicator is 30ml, and automatic Titration in distillation process, distillation termination condition is that volume terminates, slops not oneself
Dynamic to empty for measuring nitrate nitrogen content, when the dosage of Titrable acid is ammonia nitrogen or the measurement of ammonium nitrogen at the end of distillation blank value,
It is expressed as；
Blank when b. being measured immediately using Devardasalloy using the waste liquid measurement nitrate nitrogen in distillation cascade after a step
It is worth, the liquid at the end of a step in distillation cascade just restores nitrate nitrogen for Devardasalloy and provides alkaline environment in alkalinity, and
Fluid temperature in distillation cascade is very high, and especially up to 100 DEG C at the end of distillation just, the change of nitrate nitrogen is restored for starting Devardasalloy
It learns reaction and provides temperature condition, the blank value of full-automatic Kjeldahl determination device is set as 0, if analysis parameterFor 0ml,For 0ml, the boric acid containing titrate indicator is 30ml, and automatic Titration in distillation process, be delayed waiting time >=300S, delay
It waits the time for being to provide for abundance to react Devardasalloy sufficiently reducing nitrate radical ammonium ion, distills termination condition
For time termination, the time is located between 300S-450S, after the completion of parameter setting, is opened the shield on the outside of machine distillation cascade, is pressed
Machine starts the key of measurement, but because shield is opened, and machine can be prompted to close shield and is waited at this time, with
The nozzle plug of distillation cascade and machine is separated into a small distance in 30S afterwards, the Devardasalloy of 1.5-4.0g is poured into distillation
Bottom of the tube, and rapidly reinstall distillation cascade, nozzle closes shield by plug seal, and machine automatically begins to measure, distillation titration
At the end of Titrable acid dosage be nitrate nitrogen measurement when blank value, be expressed as；
(2) measurement of sample nitrogen content
C. need water sampling or soil sample that distillation cascade, distillation cascade capacity >=750ml is added by research, distillation cascade capacity is the bigger the better,
It can avoid being added after Devardasalloy because reacting acutely, liquid overflows into machine pipeline from distillation cascade when distillation；
The measurement of ammonia nitrogen or ammonium nitrogen content: blank value is inputted in instrument, water sample analysis parameterDosage is set as 0ml,
Soil sample analyzes parameterDosage is set as 20ml,Dosage should be between 20-50ml, and the boric acid containing titrate indicator is used
Amount is 30ml, and automatic Titration in distillation process distills termination condition for volume termination, and automatic-discharging is not used to measure slops
Nitrate nitrogen content needs to set the unit of machine output result, the ammonia nitrogen (ammonium of sample is obtained at the end of distillation titration according to research
Nitrogen) content；
D. the measurement of nitrate nitrogen content: after c the end of the step, nitrate nitrogen content is surveyed using the waste liquid in distillation cascade immediately: defeated in instrument
Enter blank valueIf the analysis measurement parameter of machine,For 0ml,For 0ml, the boric acid containing titrate indicator is
30ml, automatic Titration, be delayed waiting time >=300S, and delay waits the time for being to provide for abundance to keep Devardasalloy sufficiently anti-
It should be ammonium ion by reducing nitrate radical, distillation termination condition is to terminate the time, and the time is located between 300S-450S, according to grinding
Study carefully and need to set the unit that machine exports result, after the completion of parameter setting, the shield on the outside of machine distillation cascade is opened, by machine
Start the key of measurement, but because shield is opened, machine can be prompted to close shield and is waited at this time, then be existed
The nozzle plug of distillation cascade and machine is separated into a small distance in 30S, the Devardasalloy of 1.5-4.0g is poured into distillation cascade bottom
Portion, and rapidly reinstall distillation cascade, nozzle closes shield by plug seal, and machine automatically begins to measure, and distillation titration terminates
When obtain the nitrate nitrogen content of sample.
Further, distillation cascade domestic demand adds 1.0-5.0g KCl when c pacing amount soil sample.Rapidly by ammonium ion in soil
It cements out, prevents still having ammonium ion in soil at the end of measuring, influence the accuracy of detection data.
Further, b is walked, slops does not empty in d step.Because of the residue after thering is Devardasalloy to react in liquid, such as
Then residue may be stuck at the valve of machine pipeline fruit automatic-discharging.
Further, b is walked, be delayed waiting time preferred 390-450S in d step.Give appropriate reaction period.
Still further, in a step, c stepThe preferred 30ml of dosage.C step water sample preferentially takes 10-100ml that distillation cascade is added；
Or distillation cascade is added in the preferential 5-25g of soil sample.It is suitableIt is added in sample, builds suitable alkaline environment, additional amount is few, no
Ammonia element can be made to distill out completely, additional amount forms unnecessary waste too much.
The superiority of this method
This method is suitable for the measurement of heavy polluted water nitrogen, can use a water sample while measuring ammonia-nitrogen content and nitrate nitrogen
Content, and can not interfered by factors such as metal ion, organic matter, water body color, water body muddinesses in water body, pre- place can be saved
Reason is suitble to the quick measurement of batch samples；After organic nitrogen in water sample is changed into nitrate nitrogen or ammonium nitrogen, this method is also
It can measure the organic nitrogen content in water sample；This method is also suitable for the measurement of nitrogen content in soil, can use a soil sample
Ammonium nitrogen content and nitrate nitrogen content are measured simultaneously, soil sample does not need to extract, and can directly measure, and is suitble to the fast of batch samples
Speed measurement；After organic nitrogen resolution in soil sample is changed into ammonium nitrogen, this method also can measure the organic nitrogen content in soil sample.
Specific embodiment
The measurement of nitrogen content in one water sample of experimental example:
The complete dynamic kjeldahl apparatus used is OPSIS KD-310, and the capacity of distillation cascade is 750ml.
(1) blank value is measured
A. it takes not nitrogenous pure water 30-100ml that distillation cascade is added, the blank value of full-automatic Kjeldahl determination device is set as 0, if analysis ginseng
NumberFor 0ml,For 30ml, the boric acid containing titrate indicator is 30ml, and automatic Titration, distillation termination condition is that volume is whole
Only, slops does not empty, and the dosage of Titrable acid is 0.0256ml at the end of distillation, then blank value when ammonia nitrogen measures；
B. after a the end of the step, blank value when nitrate nitrogen measures is surveyed using the waste liquid in distillation cascade immediately: full-automatic kelvin is determined
The blank value of nitrogen instrument is set as 0, if analysis parameterFor 0ml,For 0ml, the boric acid containing titrate indicator is 30ml, automatically
Titration, delay waiting time are 400S, distill termination condition for time termination, the time is set as 450S, and slops does not empty, ginseng
After number is provided with, opens the shield on the outside of machine distillation cascade and be in an open state by start button in machine prompts shield
Afterwards, the nozzle plug of distillation cascade and machine is separated into a small distance in 10S, the Devardasalloy of 2.0g is poured into distillation cascade bottom
Portion, and rapidly reinstall distillation cascade, nozzle closes shield by plug seal, and machine automatically begins to measure, and distillation titration terminates
When Titrable acid dosage be 0.0424ml, then nitrate nitrogen measure when blank value；
(2) measurement of heavily contaminated water sample nitrogen content
C. heavily contaminated water sample 50ml is taken, distillation cascade is added, distillation cascade capacity is 750ml,
The measurement of ammonia-nitrogen content: inputting blank value 0.0256 in instrument, the analysis parameter of instrument is setFor 0ml,For
30ml, the boric acid 30ml containing titrate indicator, automatic Titration distill termination condition for volume termination, and slops does not empty, if
The unit for determining machine output result is mgN, and the ammonia-nitrogen content that sample is obtained at the end of distillation is 0.790mgN；
D. after c the end of the step, nitrate nitrogen content, instrument input the measurement of nitrate nitrogen content: are surveyed using the waste liquid in distillation cascade immediately
Blank value 0.0424, if the analysis measurement parameter of machine,For 0ml,For 0ml, the boric acid containing indicator is 30ml,
Automatic Titration, be delayed waiting time 400S, distills termination condition for time termination, and the time is set as 450S, and slops does not empty,
The unit of machine output result is set as mgN.After the completion of parameter setting, the shield on the outside of machine distillation cascade is opened, by beginning
The nozzle plug of distillation cascade and machine is separated a small distance, by 2.0g after machine prompts shield is in an open state by key
Devardasalloy pour into distillation bottom of the tube, and distillation cascade is reinstalled rapidly, nozzle closes shield by plug seal.Distillation drop
The nitrate nitrogen content that sample is obtained at the end of fixed is 1.106mgN.
The measurement of nitrogen content in two soil sample of experimental example
The complete dynamic kjeldahl apparatus used is OPSIS KD-310, and the capacity of distillation cascade is 750ml；
(1) blank value is measured.Using one numerical value of experimental example,,；
(2) measurement of soil sample nitrogen content
C. distillation cascade is added in soil sampling 10g, adds 2.0gKCl, and distillation cascade capacity is 750ml,
The measurement of ammonium nitrogen content: inputting blank value 0.0256 in instrument, the analysis parameter of instrument is setFor 20ml,For
30ml, the boric acid 30ml containing titrate indicator, automatic Titration distill termination condition for volume termination, and slops does not empty, if
The unit for determining machine output result is mgN, and the ammonium nitrogen content that sample is obtained at the end of distillation is 0.650mgN；
D. after c the end of the step, nitrate nitrogen content, instrument input the measurement of nitrate nitrogen content: are surveyed using the waste liquid in distillation cascade immediately
Blank value 0.0424, if the analysis measurement parameter of machine,For 0ml,For 0ml, the boric acid containing indicator is 30ml,
Automatic Titration, be delayed waiting time 450S, distills termination condition for time termination, and the time is set as 450S, and slops does not empty,
The unit of machine output result is set as mgN, after the completion of parameter setting, the shield on the outside of machine distillation cascade is opened, by beginning
The nozzle plug of distillation cascade and machine is separated a small distance, by 3.0g after machine prompts shield is in an open state by key
Devardasalloy pour into distillation bottom of the tube, and distillation cascade is reinstalled rapidly, nozzle closes shield by plug seal.Distillation drop
The nitrate nitrogen content that sample is obtained at the end of fixed is 1.002mgN.
Claims (6)
1. utilizing the method for full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content, it is characterised in that:
Full-automatic Kjeldahl determination device need to have delay function, have distillation cascade shield sensor, and distillation end point has volume and end
Only two kinds of time selections；
(1) blank value is measured
A. take not nitrogenous pure water 30-100ml that distillation cascade, distillation cascade capacity >=750ml, by full-automatic Kjeldahl determination device is added
Blank value is set as 0, analyzes parameterDosage is set as 0ml,Dosage should be between 20-50ml, containing titrate indicator
Boric acid dosage is 30ml, and automatic Titration in distillation process, distillation termination condition is that volume terminates, slops not automatic-discharging,
The blank value when dosage of Titrable acid is ammonia nitrogen or the measurement of ammonium nitrogen at the end of distillation, is expressed as；
B. the blank value of full-automatic Kjeldahl determination device is set as 0 immediately after a the end of the step, if analysis parameterFor 0ml,
For 0ml, the boric acid containing titrate indicator is 30ml, and automatic Titration in distillation process, be delayed waiting time >=300S, and distillation terminates
Condition is time termination, and the time is located between 300S-450S, after the completion of parameter setting, opens the protection on the outside of machine distillation cascade
Cover is started the key of measurement by machine, but because shield is opened, and machine can prompt to close shield and in waiting shape at this time
The nozzle plug of distillation cascade and machine is then separated a small distance in 30S, the Devardasalloy of 1.5-4.0g is poured by state
Bottom of the tube is distilled, and rapidly reinstalls distillation cascade, nozzle closes shield by plug seal, and machine automatically begins to measure,
The blank value when dosage of Titrable acid is nitrate nitrogen measurement at the end of distillation titration, is expressed as；
(2) measurement of sample nitrogen content
C. water sampling or soil sample is needed to be added distillation cascade by research, distillation cascade capacity >=750ml,
The measurement of ammonia nitrogen or ammonium nitrogen content: blank value is inputted in instrument, water sample analysis parameterDosage is set as 0ml,
Soil sample analyzes parameterDosage is set as 20ml,Dosage should be between 20-50ml, and the boric acid containing titrate indicator is used
Amount is 30ml, and automatic Titration in distillation process, distillation termination condition is that volume terminates, slops not automatic-discharging, according to grinding
Study carefully the unit for needing to set machine output result, the ammonia nitrogen or ammonium nitrogen content of sample are obtained at the end of distillation titration；
D. after c the end of the step, blank value the measurement of nitrate nitrogen content: is inputted in instrumentIf the analysis measurement parameter of machine,For 0ml,For 0ml, the boric acid containing titrate indicator is 30ml, and automatic Titration, be delayed waiting time >=300S, is steamed
Termination condition is evaporated for time termination, and the time is located between 300S-450S, needs to set the list of machine output result according to research
, after the completion of parameter setting, the shield on the outside of machine distillation cascade is opened, starts the key of measurement by machine, but because of shield
It is opened, machine can be prompted to close shield and is waited at this time, then by the nozzle of distillation cascade and machine in 30S
Plug separates a small distance, the Devardasalloy of 1.5-4.0g is poured into distillation bottom of the tube, and rapidly reinstall distillation cascade, nozzle
By plug seal, shield is closed, machine automatically begins to measure, and the nitrate nitrogen content of sample is obtained at the end of distillation titration.
2. the side according to claim 1 using full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content
Method, it is characterised in that: distillation cascade domestic demand adds 1.0-5.0gKCl when c pacing amount soil sample.
3. the side according to claim 1 using full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content
Method, it is characterised in that: slops does not empty in b step, d step.
4. the side according to claim 1 using full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content
Method, it is characterised in that: be delayed waiting time preferred 390-450S in b step, d step.
5. the side according to claim 1 using full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content
Method, it is characterised in that: in a step, c stepThe preferred 30ml of dosage.
6. the side according to claim 1 using full-automatic Kjeldahl determination device rapid survey water body or Soil Nitrogen Content
Method, it is characterised in that: c step water sample preferentially takes 10-100ml that distillation cascade is added；Or distillation cascade is added in the preferential 5-25g of soil sample.
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Application publication date: 20190730 |