CN101271072A - Method for measuring kalium in soil by tetraphenylboron sodium nephelometery and its screening agent - Google Patents
Method for measuring kalium in soil by tetraphenylboron sodium nephelometery and its screening agent Download PDFInfo
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Abstract
The invention discloses a method for measuring potassium by the sodium tetraphenylborate turbidimetry and a masking agent which is used by the method. The masking agent is a water solution containing 0.01 to 0.04mol/l of Cu<2+>, 0.04 to 0.10mol/l of tartaric acid and 5 to 10mol/l of H<+>; the method for measuring the potassium by the sodium tetraphenylborate turbidimetry is that: the masking agent is used for masking ammonium ion and other interfering ions in liquid under test, basic EDTA disodium salt solution is further added to carry out the auxiliary masking, basic sodium tetraphenylborate water solution is finally added, and the turbidity measurement is immediately carried out after shaking the reaction solution well. The measurement method has the advantages of simple operation, rapid and accurate measurement and low cost; the linear range thereof meets the requirements of the rapid measurement, which is suitable for the application of grass roots and agriculture popularization departments; and the masking agent used does extremely small harm to the human body and the environment.
Description
Technical field
The present invention relates to the assay field, be specifically related to the method for potassium in a kind of tetraphenylboron sodium turbidimetry for Determination soil and the environment-friendly type screening agent of low toxicity thereof.
Background technology
The trophic level of soil potassium depends primarily on the content of soil available potassium, the content of available potassium is the efficiency index that evaluation soil potassium level and pre-measuring plants are executed nak response in the soil, in time measure the soil quick-acting potassium content, understanding its variation tendency, is very necessary to instructing rationally using of potash fertilizer.
At present, the available potassium method for measuring mainly contains gravimetric method, volumetric method, colourimetry, turbidimetry, flare photometer, atomic absorption method, electrode method and plasma emission spectroscopy method (ICP-AES) in the soil.NH wherein
4OAc lixiviate-flame photometry is the most commonly used, but the instrument of its used flame photometer, atomic absorption and so on costs an arm and a leg, and is not only not portable, and its working service is loaded down with trivial details, competency profiling to operating personnel is higher, thus its be difficult in the township, at village level soil detects the unit popularization and application; And the operation of gravimetric method, volumetric method is too complicated, and the error effect factor is too many; Potassium electrode complex manufacturing technology that the electrode method is used and life-span are short, are difficult in the short time apply.Basic unit to the requirement of the assay method of soil potassium be: testing equipment is simple, test operation is easy, quick, and turbidimetry, colourimetry can satisfy the requirement of this respect.Colourimetry mainly refers to crown ether DPDB-18-C-6 and Bromothymol blue ion pair extraction luminosity colourimetry, because complicated extraction step is arranged in this method, thereby few the application; Turbidimetry mainly contains tetraphenylboron sodium method and nitrous acid cobalt nanofarad, because natrium cobaltinitrosum reagent has severe toxicity and costs an arm and a leg, thereby nitrous acid cobalt nanofarad is also seldom used, the tetraphenylboron sodium turbidimetry is a method the most commonly used for many years, and this method operation is easier, has certain simplicity and reliability, meet the requirement that speed is surveyed, use comparatively extensive, but in the tetraphenylboron sodium method is surveyed potassium, the NH in the sample
4 +Also generate white precipitate { K with the tetraphenylboron sodium reaction
++ Na (B (C
6H
5) X)=K (B (C
6H
5)
4The Na of) ↓+
+, thereby the mensuration of interference potassium.Traditional tetraphenylboron sodium method is united with formaldehyde-EDTA and is sheltered NH
4 +With other metallic ion [4NH
4 ++ 6HCHO=(CH
2)
6N
4+ 6H
2O+4H
+], its masking effect still can (reach 100mg/kg), but the problem that can not be ignored below also existing: 1. used formaldehyde is poisonous and volatile, the formaldehyde that evaporates is a kind of colourless harmful gas that the obvious irritation smell is arranged, long-term contact may cause nasal cavity, oral cavity, throat, skin and alimentary tract cancer, contaminated environment not only, and the harm lab assistant is healthy; 2. formaldehyde is difficult for long-term storage, forms polymkeric substance easily and loses efficacy; 3. waste liquid is difficult to handle.
Based on this, seek a kind of screening agent of environment-friendly type, can effectively shelter NH4+, can avoid environmental pollution and the able-bodied adverse consequences of harm lab assistant to become the task of top priority again.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of easy and simple to handle, measure quick and precisely, tetraphenylboron sodium turbidimetry that cost is low surveys the method for potassium, and a kind of environment-friendly type screening agent that human body is not had harm is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of tetraphenylboron sodium turbidimetry is surveyed the screening agent of potassium, and it is to contain 0.01～0.04mol/L Cu
2+, 0.04～0.10mol/L tartrate, [H
+The aqueous solution of]=5～10mol/L.
The compound method of above-mentioned screening agent is as follows:
Take by weighing CuSO
45H
2O 2.5～10.0g or CuCl
22H
2O 1.7～6.8g, tartrate 6.0～15.0g are dissolved in 100～800mL water, add the concentrated sulphuric acid (H
2SO
418.6mol/L) 135.9～271.7mL or concentrated hydrochloric acid (mass percent concentration is 38%) 407.7～815.1mL, be cooled to room temperature after, be diluted to 1000mL, shake up.
The preferable range of agents useful for same: CuSO
45H
2O 4.0～7.5g, tartrate 9.0～13.5g, the concentrated sulphuric acid 163.0～217.4mL.
Agents useful for same is preferably: CuSO
45H
2O 5.0g, tartrate 12.0g, concentrated sulphuric acid 200.0mL.
A kind of tetraphenylboron sodium turbidimetry is surveyed the method for potassium, may further comprise the steps:
(1) reagent preparation
1. screening agent takes by weighing CuSO
45H
2O 2.5～10.0g or CuCl
22H
2O 1.7～6.8g, tartrate 6.0～15.0g are dissolved in 100～800mL water, add the concentrated sulphuric acid 135.9～271.7mL or concentrated hydrochloric acid 407.7～815.1mL, be cooled to room temperature after, be diluted to 1000mL, shake up;
2. help and cover agent and take by weighing EDTA disodium salt 60.0～80.0g, NaOH 100～150g is dissolved in 100～800mL water, is diluted with water to 1000mL after the cooling, mixing;
3. turbidity agent weighing sodium hydroxide 5.0～10.0g is dissolved in 50～90mL water, is settled to 100mL after the cooling, and is standby; Other takes by weighing tetraphenylboron sodium 55.0～70.0g, is dissolved in 500～900mL water, is diluted to 1000mL with water, and adds the above-mentioned sodium hydroxide solution of 0.3～0.7mL, shakes up, and is filtered to the solution clarification;
4. standard solution is got at least a water-soluble in potassium dihydrogen phosphate, potassium nitrate, glazier's salt, the potassium chloride, is mixed with known K
2The aqueous solution of O concentration is diluted to 100 times with soil extractant solution with it again;
(2) draw equal volume V respectively than turbid survey liquid preparation
0Digestion agent solution, standard solution, soil lixiviate filtrate (being soil liquid to be measured) in different reaction vessels, add available potassium screening agent V respectively
1, add available potassium after shaking up again respectively and help and cover agent V
2, add at last and quicken to imitate potassium turbidity agent V respectively
3, carry out turbidimetric assay, wherein volume ratio V after shaking up immediately
0: V
1=13～30: 1, V
0: V
2=4～8: 1, V
0: V
3=8～14: 1; Can come to determine V as required
0Size, for example when colorimetric estimation, use the 10mm cuvette, consider the needs of saving reagent cost, get V
0=2mL promptly can satisfy the mensuration needs; Also can increase V
0, unnecessary reagent rinse cuvette is then arranged, can further improve measuring accuracy like this.
(3) turbidimetric assay is adjusted light path wavelength to the 500～700nm of photometer or photolometer, with digestion agent solution is blank reference, absorbance at absorbance measuring shelves difference bioassay standard liquid and liquid to be measured, or the measurement of concetration shelves with titer transfer with reference to dense (the mg/kg) * liquid of scale value R[R=titer sample than], then liquid to be measured is inserted in the light path, read or calculate quick-acting potassium content in the testing sample.
Above-mentioned soil extractant can be to contain 0.40～0.50mol/LNaHCO
3, 0.020～0.030mol/LNa
2CO
3, 0.30～0.40mol/L Na
2SO
4, the pH value is 8.4～8.6 aqueous solution; Described soil filtrate is meant above-mentioned aqueous solution with liquid: the mass ratio of soil=5～25: 1 joins in the soil to be measured, and under 20～30 ℃ temperature conditions, vibration or stirring and leaching 4～20 minutes are filtered back gained solution.
Above-mentioned soil extractant can also be conventional digestion agent, promptly contains 1molL
-1NH
4The aqueous solution of OAc; Described soil filtrate is meant above-mentioned aqueous solution with liquid: 10: 1 mass ratio of soil joins in the soil to be measured, under 20～30 ℃ temperature conditions, with 150～180 rev/mins frequency lixiviate 30 minutes, filters back gained solution at vibrating machine.
Above agents useful for same is except that indicating the person to be analyzed pure or top grade is pure, and water is for meeting three grades of water quality standards that " assay laboratory's water specification and test method " (GB6682-92) stipulate, down together.
The present invention has actively useful effect:
1. the Cu in good this screening agent of environment-protecting asepsis and masking performance
2+, under alkali condition, make the ammonium root in the solution change ammonium molecule (NH into
4 ++ OH-=NH
3.H
2O), then with solution in copper ion complexing [Cu
2++ 4NH
3=Cu (NH
3)
4 2+], generate the stabilized copper ammonium complex ion, thereby eliminate NH
4 +To the interference of potassium measurement result, experimental result shows, this screening agent can effectively shelter with potassium ion with isoconcentration NH
4 +, and do not influence the linearity of this reaction system; Avoid using the chemical reagent of grievous injury human body, effectively reduced environmental pollution.
2. all ingredients that is made into, the shelf-life long (all more than half a year, and the reagent shelf-life of conventional method preparation is short, is with using with joining mostly), be easy to realize the finished product supply of all ingredients, effectively improve testing efficiency, reduce testing cost.
3. the range of linearity satisfies fast measuring and requires to make solvent preparation variable concentrations K with soil extractant
2O solution is measured different K by method of the present invention
2O concentration solution absorbency, the result shows K in the solution
2O concentration is best in 2.0～20 μ g/mL scope internal linear, regression equation y=0.0186x+0.0242, R
2=0.9904, lowest detection is limited to 0.45 μ g/mL, sees Table 1, and linearity curve is seen Fig. 1.
4. method of testing favorable reproducibility, error is little of determining the Repeatability and Reproducibility of the inventive method measurement result, entrust 4 independently laboratory [Gansu Province's agricultural product quality and safety supervision inspection centers, fertilizer quality supervision and inspection center of the Ministry of Agriculture (Zhengzhou), fertilizer quality supervision and inspection center of the Ministry of Agriculture (Shenyang), Hunan Province farmingization inspection center of Academy of Agricultural Sciences, down together], with associating lixiviate rapid method, choose the control experiment that national standard soil and representational pedotheque have carried out available potassium, twice replication made to each sample in each laboratory, all does parallel at every turn.The result shows: the inventive method measurement result has good Repeatability and Reproducibility, and its parallel error satisfies the desired error level of conventional method of analysis, sees Table 2.
5. the method for testing among the present invention is simple to operate, test speed is fast, is suitable for the application of basic unit and agricultural extension department.
Description of drawings
Fig. 1 surveys the linearity curve of potassium for the tetraphenylboron sodium turbidimetry.
Embodiment
1 one kinds of tetraphenylboron sodium turbidimetrys of embodiment are surveyed the screening agent of potassium, contain 0.02mol/L Cu
2+, 0.08mol/L tartrate, [H
+The aqueous solution of]=7.36mol/L.
Survey the method for potassium with the tetraphenylboron sodium turbidimetry of above-mentioned screening agent, may further comprise the steps:
(1) reagent preparation
1. screening agent takes by weighing copper sulphate (CuSO
45H
2O) 5.0g, tartrate (C
4H
6O
6) 12.0g, be dissolved in about 500mL water, add concentrated sulphuric acid 200.0mL, be cooled to room temperature after, be settled to 1000mL with distilled water, be sub-packed in the small droplet bottles standby after shaking up;
2. help and cover agent and take by weighing EDTA disodium salt 75.0g, NaOH 130.0g is dissolved in the suitable quantity of water, after the cooling, is settled to 1000mL with distilled water, and mixing is sub-packed in the small droplet bottles standby;
3. turbidity agent weighing sodium hydroxide 8.0g is dissolved in about 80mL water, is settled to 100mL after the cooling, and is standby; Other takes by weighing tetraphenylboron sodium [NaB (C
6H
5)
4] 62.5g, be dissolved in about 900mL water, be settled to 1000mL with distilled water, and add the sodium hydroxide solution of the 2N that the 0.5mL front is made into, shake up, be filtered to the solution clarification, the filtrate of clarification is sub-packed in the small droplet bottles standby;
4. standard solution takes by weighing potassium dihydrogen phosphate 0.4602g, ammonium sulfate 1.1319g, potassium nitrate 1.7323g, glazier's salt 0.0611g is dissolved in about 800mL water, adds concentrated sulphuric acid 10.0mL, fully after the dissolving, be settled to 1000mL with distilled water, shake up, be and contain 240 μ g/mL NH
4 +-N, 240 μ g/mL P
2O
5, 1000 μ g/mLK
2The hybrid standard stock solution of O (simultaneously double as is surveyed the standard reserving solution of nitrogen, phosphorus) is got this solution 1.0mL, and is standby after accurately being diluted to 100 times with soil extractant solution.
(2) drawing soil extractant solution 2.0mL than turbid liquid preparation does blank in a little reaction bulb, draw soil mixed standard solution 2.0mL in another little reaction bulb, draw soil lixiviate filtrate 2.0mL in the 3rd little reaction bulb, add screening agent 2 (calibrated dropper or drop bottles respectively successively, every 0.051 ± 0.003mL, down with), help and cover 6 of agent, 4 of turbidity agent, all shake up after whenever adding a kind of reagent, carry out turbidimetric assay immediately.
Above-mentioned soil extractant is for containing 0.45mol/L NaHCO
3, 0.0255mol/L Na
2CO
3, 0.37mol/LNa
2SO
4, the pH value is 8.5 combined digestion agent aqueous solution; Described soil filtrate is meant above-mentioned aqueous solution with liquid: the mass ratio of soil=20: 1 joins in the soil to be measured, and under 25 ℃ temperature conditions, vibration lixiviate 10 minutes is filtered back gained solution, referring to Chinese patent application 200810049443.4.
(3) turbidimetric assay is adjusted the light path wavelength of photometer or photolometer to 685nm, with soil extractant solution serves as blank with reference to after the zeroing, at the measurement of concetration shelves titer tone pitch is made as 200.0, then liquid to be measured is inserted in the light path, show that numerical value is quick-acting potassium content in the testing sample (mg/kg).When measuring a plurality of sample simultaneously (soil lixiviate filtrate has a plurality of), the liquid to be measured that only needs to prepare is put into light path successively, and reading gets final product.
2 one kinds of tetraphenylboron sodium turbidimetrys of embodiment are surveyed the screening agent of potassium, contain 0.01mol/L Cu
2+, 0.067mol/L tartrate, [H
+The aqueous solution of]=6.62mol/L.Survey the method for potassium with the tetraphenylboron sodium turbidimetry of this screening agent, may further comprise the steps:
(1) reagent preparation
1. screening agent takes by weighing copper sulphate (CuSO
45H
2O) 4.0g, tartrate (C
4H
6O
6) 10.0g, be dissolved in the 700mL water, add concentrated sulphuric acid 180.0mL, be cooled to room temperature after, be settled to 1000mL with distilled water, shake up;
2. help and cover agent and take by weighing EDTA disodium salt 65.0g, NaOH 140.0g is dissolved in the suitable quantity of water, after the cooling, is settled to 1000mL with distilled water, mixing;
3. turbidity agent weighing sodium hydroxide 7.0g is dissolved in the 70mL water, is diluted to 100mL after the cooling, and is standby; Other takes by weighing tetraphenylboron sodium 65.0g, is dissolved in the 900mL water, is settled to 1000mL with distilled water, and adds the sodium hydroxide solution that the 0.4mL front is made into, and is filtered to the solution clarification after shaking up;
4. the standard solution potassium chloride is dissolved in the 600mL water in right amount, adds concentrated sulphuric acid 8.0mL, be settled to 1000mL with water after, shake up, be mixed with and contain 1000 μ g/mL K
2The standard inventory solution of O is got this solution, with soil extractant solution it is diluted to 100 times and gets final product.
(2) drawing soil extractant solution 10.0mL than turbid liquid preparation does blank in a reaction bulb, draw standard solution 10.0mL in another reaction bulb, draw soil lixiviate filtrate 10.0mL in the 3rd reaction bulb, add screening agent 0.75mL respectively successively, help and cover agent 1.8mL, turbidity agent 1.3mL, whenever all to shake up after adding a kind of reagent, and measure immediately.
Above-mentioned soil extractant is conventional digestion agent, promptly contains 1molL
-1NH
4The aqueous solution of OAc; Soil filtrate is meant above-mentioned aqueous solution with liquid: 10: 1 mass ratio of soil joins in the soil to be measured, under 25 ℃ temperature conditions, with 170 rev/mins frequency lixiviate 30 minutes, filters back gained solution at vibrating machine.
(3) turbidimetric assay is adjusted the light path wavelength of photometer or photolometer to 680nm, with the soil extractant is blank with reference to after the zeroing, absorbance at absorbance measuring shelves difference bioassay standard liquid and liquid to be measured, the content of available potassium is represented with mark X in the sample, calculate by following formula, be accurate to behind the radix point one.
In the formula: X---quick-acting potassium content in the sample, unit are every kilogram (mg/kg) of milligram; A
1---the absorbance of titer; A
2---the absorbance of liquid to be measured.
3 one kinds of tetraphenylboron sodium turbidimetrys of embodiment are surveyed the screening agent of potassium, contain 0.032mol/L Cu
2+, 0.087mol/L tartrate, [H
+The aqueous solution of]=9.2mol/L.Survey the method for potassium with the tetraphenylboron sodium turbidimetry of this screening agent, may further comprise the steps:
(1) reagent preparation
1. screening agent takes by weighing CuSO
45H
2O 8.0g, tartrate (C
4H
6O
6) 13.0g, be dissolved in the 250mL water, add concentrated sulphuric acid 250.0mL, be cooled to room temperature after, water is settled to 1000mL, shakes up.
2. help and cover agent and take by weighing EDTA disodium salt 70.0g, NaOH 120.0g is dissolved in the suitable quantity of water, after the cooling, is settled to 1000mL with distilled water, mixing;
3. turbidity agent weighing sodium hydroxide 6.0g is dissolved in the 70mL water, is settled to 100mL after the cooling, and is standby; Other takes by weighing tetraphenylboron sodium 60.0g, is dissolved in the 800mL water, is settled to 1000mL with distilled water, and adds the sodium hydroxide solution that the 0.6mL front is made into, and shakes up, and is filtered to the solution clarification;
4. standard solution is got glazier's salt and is dissolved in right amount in the 700mL water, adds concentrated sulphuric acid 9.0mL, be settled to 1000mL with distilled water after, shake up, be mixed with and contain 1000 μ g/mL K
2The standard inventory solution of O is got this solution, with soil extractant solution it is diluted to 100 times and gets final product.
(2) draw equal volume V respectively than turbid liquid preparation
0The soil extractant solution of=5.0mL, standard solution, soil lixiviate filtrate add available potassium screening agent V respectively in different reaction vessels
1, add available potassium after shaking up again respectively and help and cover agent V
2, add at last and quicken to imitate potassium turbidity agent V respectively
3, carry out turbidimetric assay, wherein volume ratio V after shaking up immediately
0: V
1=20: 1, V
0: V
2=6: 1, V
0: V
3=10: 1.
Above-mentioned soil extractant is for containing 0.40mol/L NaHCO
3, 0.026mol/L Na
2CO
3, 0.35mol/LNa
2SO
4The combined digestion agent aqueous solution; The described soil filtrate of used soil lixiviate filtrate is meant above-mentioned aqueous solution with liquid: the mass ratio of soil=20: 1 joins in the soil to be measured, under 25 ℃ temperature conditions, back gained solution is filtered in vibration lixiviate 15 minutes, sees Chinese patent application 200810049443.4 for details.
(3) turbidimetric assay is adjusted the light path wavelength of photometer or photolometer to 690nm, after the blank solution zeroing, at the measurement of concetration shelves titer tone pitch is made as 200.0, then liquid to be measured is inserted in the light path, show that numerical value is quick-acting potassium content in the testing sample (mg/kg).When measuring a plurality of sample simultaneously (soil lixiviate filtrate has a plurality of), only the soil for preparing liquid to be measured need be put into light path successively, reading gets final product.
Embodiment 4 soil available potassium assay methods are substantially the same manner as Example 1: difference is: 1. use CuSO in the screening agent preparation
45H
2O 3.0g, tartrate (C
4H
6O
6) 6.5g; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 65.0g, NaOH 110.0g; 3. weighing sodium hydroxide 5.5g, tetraphenylboron sodium 65.0g during the turbidity agent is prepared; 4. water-soluble with glazier's salt, potassium chloride in standard solution preparation, be mixed with and contain 1000 μ g/mLK
2The standard inventory solution of O; 5. in than turbid liquid preparation process screening agent, help the addition of covering agent, turbidity agent to be respectively 3,8,5.
Embodiment 6 soil available potassium assay methods are substantially the same manner as Example 3: difference is: 1. use CuSO in the screening agent preparation
45H
2O 7.0g, tartrate (C
4H
6O
6) 9.0g; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 78.0g, NaOH 145.0g; 3. weighing sodium hydroxide 8.0g, tetraphenylboron sodium 60.0g during the turbidity agent is prepared; 4. the liquor capacity V that gets in than turbid liquid preparation process
0With add screening agent, help the volume ratio of covering agent, turbidity agent to be respectively V
0: V
1=15: 1, V
0: V
2=5: 1, V
0: V
3=9: 1.
Embodiment 7 soil available potassium assay methods are substantially the same manner as Example 1: difference is: 1. use CuSO in the screening agent preparation
45H
2O 4.5g, tartrate (C
4H
6O
6) 13.5g; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 61.5g, NaOH 125.0g; 3. weighing sodium hydroxide 6.5g, tetraphenylboron sodium 51.5g during the turbidity agent is prepared; 4. in than turbid liquid preparation process screening agent, help the addition of covering agent, turbidity agent to be respectively 2,7,5.
Embodiment 8 soil available potassium assay methods are substantially the same manner as Example 2: difference is: 1. use CuSO in the screening agent preparation
45H
2O 5.8g, tartrate (C
4H
6O
6) 11.5g; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 69.0g, NaOH 135.0g; 3. weighing sodium hydroxide 9.5g, tetraphenylboron sodium 58.5g during the turbidity agent is prepared; 4. in than turbid liquid preparation process screening agent, help the addition of covering agent, turbidity agent to be respectively 0.25mL, 1.78mL, 1.27mL.
Embodiment 9 soil available potassium assay methods are substantially the same manner as Example 3: difference is: 1. use CuCl in the screening agent preparation
22H
2O 2.0g, tartrate (C
4H
6O
6) 13.5g; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 65.5g, NaOH 125.0g; 3. weighing sodium hydroxide 7.8g, tetraphenylboron sodium 63.5g during the turbidity agent is prepared; 4. the liquor capacity V that gets in than turbid liquid preparation process
0With add screening agent, help the volume ratio of covering agent, turbidity agent to be respectively V
0: V
1=18: 1, V
0: V
2=7: 1, V
0: V
3=12: 1.
Embodiment 11 soil available potassium assay methods are substantially the same manner as Example 2: difference is: 1. use CuCl in the screening agent preparation
22H
2O 6.5g, tartrate (C
4H
6O
6) 10.5g, concentrated hydrochloric acid 810.0mL; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 62.0g, NaOH 145.0g; 3. weighing sodium hydroxide 7.5g, tetraphenylboron sodium 56.5g during the turbidity agent is prepared.
Embodiment 12 soil available potassium assay methods are substantially the same manner as Example 3: difference is: 1. use CuCl in the screening agent preparation
22H
2O 5.0g, tartrate (C
4H
6O
6) 10.5g, concentrated hydrochloric acid 610.0mL; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 72.0g, NaOH 125.0g; 3. weighing sodium hydroxide 7.0g, tetraphenylboron sodium 66.5g during the turbidity agent is prepared.
Embodiment 13 soil available potassium assay methods are substantially the same manner as Example 2: difference is: 1. use CuCl in the screening agent preparation
22H
2O 3.8g, tartrate (C
4H
6O
6) 13.5g, concentrated sulphuric acid 271.0mL; 2. help to cover in the agent preparation and take by weighing EDTA disodium salt 62.0g, NaOH 145.0g; 3. weighing sodium hydroxide 9.8g, tetraphenylboron sodium 59.5g during the turbidity agent is prepared.
The masking performance test of embodiment 14 screening agents
For the check screening agent is done following test to the screening ability of ammonium nitrogen in the solution: make solvent with soil extractant and prepare 14.0mgkg respectively
-1K
2O, 14.0mgkg
-1K
2O+12mgkg
-1NH
4 +-N solution adds all ingredients with the method among the embodiment 1, measures its absorbance, and the result shows imitates the potassium screening agent to containing in the liquid to be measured≤12mgkg
-1NH
4 +-N can shelter fully, sees Table 3.
Press system-working specification of being formulated, entrust 4 independently laboratories respectively, with this method and conventional method (1molL
-1NH
4OAc lixiviate--flame photometry), to local 30 representative pedotheques, carries out available potassium mensuration, and analyzed the correlativity that has compared two kinds of detection methods, the results are shown in Table 4.
Table 1 is surveyed the available potassium test of linearity
Table 2 different experiments chamber soil available potassium error at measurment comparison unit: (%)
Ammonium nitrogen interference test in table 3 potassium solution
The correlation test of table 4 quick tests for soils and conventional method
Claims (7)
1. a tetraphenylboron sodium turbidimetry is surveyed the screening agent of potassium, and it is to contain 0.01～0.04mol/L Cu
2+, 0.04～0.10mol/L tartrate, [H
+The aqueous solution of]=5～10mol/L.
2. tetraphenylboron sodium turbidimetry according to claim 1 is surveyed the screening agent of potassium, it is characterized in that its compound method is as follows:
Take by weighing CuSO
45H
2O 2.5～10.0g or CuCl
22H
2O 1.7～6.8g, tartrate 6.0～15.0g are dissolved in 100～800mL water, add the concentrated sulphuric acid 135.9～271.7mL or concentrated hydrochloric acid 407.7～815.1mL, be cooled to room temperature after, be diluted to 1000mL, shake up and get final product.
3. tetraphenylboron sodium turbidimetry according to claim 2 is surveyed the screening agent of potassium, it is characterized in that used CuSO
45H
2O 4.0～7.5g, tartrate 9.0～13.5g, the concentrated sulphuric acid 163.0～217.4mL.
4. tetraphenylboron sodium turbidimetry according to claim 3 is surveyed the screening agent of potassium, it is characterized in that used CuSO
45H
2O is that 5.0g, tartrate are that 12.0g, the concentrated sulphuric acid are 200.0mL.
5. the method for potassium in the tetraphenylboron sodium turbidimetry for Determination soil may further comprise the steps:
(1) reagent preparation
1. screening agent takes by weighing CuSO
45H
2O 2.5～10.0g or CuCl
22H
2O 1.7～6.8g, tartrate 6.0～15.0g are dissolved in 100～800mL water, add the concentrated sulphuric acid 135.9～271.7mL or concentrated hydrochloric acid 407.7～815.1mL, be cooled to room temperature after, be diluted to 1000mL, shake up;
2. help and cover agent and take by weighing EDTA disodium salt 60.0～80.0g, NaOH 100～150g is dissolved in 100～800mL water, is diluted with water to 1000mL after the cooling, mixing;
3. turbidity agent weighing sodium hydroxide 5.0～10.0g is dissolved in 50～90mL water, is settled to 100mL after the cooling, and is standby; Other takes by weighing tetraphenylboron sodium 55.0～70.0g, is dissolved in 500～900mL water, is diluted to 1000mL with water, and adds the above-mentioned sodium hydroxide solution of 0.3～0.7mL, shakes up, and is filtered to the solution clarification;
4. standard solution is got at least a water-soluble in potassium dihydrogen phosphate, potassium nitrate, glazier's salt, the potassium chloride, is mixed with known K
2The aqueous solution of O concentration is diluted to 100 times with soil extractant solution with it again;
(2) draw equal volume V respectively than turbid liquid preparation
0Soil extractant solution, standard solution, soil lixiviate filtrate in different reaction vessels, add available potassium screening agent V respectively
1, add available potassium after shaking up again respectively and help and cover agent V
2, add available potassium turbidity agent V after shaking up again respectively
3, carry out turbidimetric assay, wherein volume ratio V after shaking up immediately
0: V
1=13～30: 1, V
0: V
2=4～8: 1, V
0: V
3=8～14: 1;
(3) turbidimetric assay is adjusted light path wavelength to the 500～700nm of photometer or photolometer, with soil extractant solution is blank reference, absorbance at absorbance measuring shelves difference bioassay standard liquid and liquid to be measured, or transfer with reference to the scale value with titer at the measurement of concetration shelves, then liquid to be measured is placed light path, read or calculate the content of available potassium in the pedotheque to be measured.
6. the method for potassium is characterized in that described soil extractant is for containing NaHCO in the tetraphenylboron sodium turbidimetry for Determination soil according to claim 5
30.40～0.50mol/L, Na
2CO
30.020～0.030mol/L, Na
2SO
40.30～0.40mol/L, pH value are 8.4～8.6 aqueous solution; Described soil filtrate is meant above-mentioned aqueous solution with liquid: the mass ratio of soil=5～25: 1 joins in the pedotheque to be measured, and under 20～30 ℃ temperature conditions, vibration or stirring and leaching 4～20 minutes are filtered back gained solution.
7. the method for potassium is characterized in that in the tetraphenylboron sodium turbidimetry for Determination soil according to claim 5, and described soil extractant is conventional digestion agent, promptly contains 1molL
-1NH
4The aqueous solution of OAc; Described soil filtrate is meant above-mentioned aqueous solution with liquid: the mass ratio of soil=10: 1 joins in the pedotheque to be measured, under 20～30 ℃ temperature conditions, with 150～180 rev/mins frequency lixiviate 30 minutes, filters back gained solution with vibrating machine.
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| CN102937587A (en) * | 2012-11-08 | 2013-02-20 | 成武县农业局 | Method for rapidly measuring rapidly available potassium content in compound fertilizer through flame photometry |
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