CN111122287A - Method for rapidly determining total phosphorus content in organic fertilizer for tobacco - Google Patents
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Abstract
The invention discloses a method for rapidly determining the total phosphorus content in an organic fertilizer for cigarettes. The method comprises the steps of detecting the total phosphorus content in the organic fertilizer for the tobacco by using a continuous flow analyzer for the first time, digesting the phosphorus in the organic fertilizer for the tobacco by using sulfuric acid-hydrogen peroxide, converting the phosphorus into phosphate ions, and reacting the phosphate ions in a sample solution with metavanadate and molybdic acid under a certain acidity condition to form yellow ternary heteropoly acid. Measuring the response value of the sample solution at 420nm with a continuous flow analyzer, and determining the response value according to the response value and P in the sample solution2O5The total phosphorus content in the organic fertilizer sample for tobacco can be calculated by the quantitative relation between the concentrations. The method is simple and convenient to operate, rapid, high in accuracy, good in precision and good in stability, has the same detection result with a standard method, and provides a new choice for related detection of tobacco organic fertilizer componentsAnd (6) selecting.
Description
Technical Field
The invention belongs to the technical field of organic fertilizer component detection, and particularly relates to a method for rapidly and accurately detecting the total phosphorus content in a tobacco organic fertilizer by using a continuous flow method.
Background
The organic fertilizer for the tobacco is a fertilizer formed by decomposing or fermenting natural organic matters through microorganisms, and researches show that the organic fertilizer can coordinate the nutrition of tobacco plants, improve the utilization rate of the fertilizer, balance nutrients, improve soil, reduce production cost and be beneficial to the growth and development of the tobacco plants and the improvement of the qualities of the tobacco leaves, such as luster, elasticity, oil content, aroma and the like. However, the quality of the organic fertilizer for tobacco in the market is not uniform, so that the popularization effect of the organic fertilizer for tobacco is influenced to a certain extent, and the quality of the organic fertilizer for tobacco is imperatively monitored. Phosphorus is taken as one of important nutrient elements forming the organic fertilizer and is always considered, the currently widely used method for determining the total phosphorus content in the organic fertilizer is a spectrophotometric method in NY/T298-1995 organic fertilizer total phosphorus determination and NY/T525-2012 organic fertilizer 5.4, and the detection efficiency is low due to the defects that the number of manual operation steps is large in the detection process, data needs post-processing and the like. The continuous flow method has the advantages of online color development, online mixing and dilution, continuous sample introduction, immediate data processing and the like, can realize continuous detection of samples, and greatly improves the detection working efficiency. However, no report for measuring the total phosphorus content in the organic fertilizer for cigarettes by using a continuous flow method is found at present.
Disclosure of Invention
The invention aims to provide a method for rapidly, simply, quantitatively and accurately measuring the total phosphorus content in an organic fertilizer for cigarettes aiming at the defects of the prior art.
The purpose of the invention is realized by the following technical scheme.
All percentages used in the present invention are mass percentages unless otherwise indicated.
A method for rapidly determining the total phosphorus content in an organic fertilizer for tobacco comprises the following steps:
(1) preparation of standard working solution: mixing KH with water2PO4Drying at 105 deg.C for 2 hr, accurately weighing 4.79g (to 0.0001g), placing in 50mL beaker, adding water for dissolving, transferring into 500mL volumetric flask, adding water to constant volume to scale, and mixing to obtain P2O5Reserving the stock solution for later use; respectively removing 1, 2, 4, 8, 16 and 20mLP2O5Placing the stock solution into a 100mL volumetric flask, diluting with a sample injector cleaning solution to a constant volume to obtain P2O5The concentration is 50, 100, 200, 400, 800, 1000mg/L series of standard working solutions respectively;
(2) drawing a standard working curve: the response value of a series of standard working solutions is measured at 420nm by a continuous flow analyzer as the P of the solution2O5The concentration is abscissa, the response value is ordinate, a standard working curve is drawn, the linear equation is that Y is 0.0002X +0.0004, and the correlation coefficient R21 is ═ 1; and (3) arranging pipelines of the continuous flow analyzer: using a yellow/white pump tube for the sample solution, wherein the flow rate is 0.23 mL/min; h2SO4The solution is pumped by a yellow/yellow pump tube at the flow rate of 1.20 mL/min; FFD6 solution was pumped through a yellow/blue pump tube at a flow rate of 1.40 mL/min; the color developing agent is an orange/orange pump tube, and the flow rate is 0.42 mL/min; highest P for linear correspondence2O5The content is 1000 mg/L;
(3) measurement of sample moisture: drying and crushing the organic fertilizer for the tobacco to be detected, sieving the organic fertilizer with a sieve with the aperture of 1mm to be used as a sample, and then determining the moisture content of the sample according to the specification of NY/T3021995 organic fertilizer moisture determination;
(4) sample treatment: weighing 0.5-1.0 g (accurate to 0.0001g) of a sample, placing the sample at the bottom of a 100mL digestion tube, washing the sample adhered to the tube wall with 3mL water, then slowly adding 5mL sulfuric acid, slowly and dropwise adding 1.5mL hydrogen peroxide, carefully shaking up, inserting a pear-shaped glass funnel into the tube opening, and standing overnight; heating the digester to 100 ℃ for 20min, taking out the digester, and slowly adding 0.5mL of hydrogen peroxide along the wall of the digester for three times until the solution is colorless or light yellow clear liquid; then placing the digestion tube in a digester which is preheated to 370 ℃ in advance, and digesting for 1 h; cooling for 10min after digestion, adding 10mL of water, cooling to room temperature, fixing the volume to the scale with the water, and shaking up to obtain a sample solution;
(5) analysis of the sample solution: measuring the response value of the sample solution at 420nm by using a continuous flow analyzer, and calculating the total phosphorus concentration in the sample solution through a standard working curve; and (3) arranging pipelines of the continuous flow analyzer: using a yellow/white pump tube for the sample solution, wherein the flow rate is 0.23 mL/min; h2SO4For solutionsA yellow/yellow pump pipe with the flow rate of 1.20 mL/min; FFD6 solution was pumped through a yellow/blue pump tube at a flow rate of 1.40 mL/min; the color developing agent is an orange/orange pump tube, and the flow rate is 0.42 mL/min; highest P for linear correspondence2O5The content is 1000 mg/L;
(6) and (4) calculating a result:
in the formula:
P2O5(%) -total phosphorus content in organic fertilizer for tobacco, unit is percentage (%);
c-total phosphorus concentration in milligrams per liter (mg/L) in the sample solution;
v-total volume of sample solution in milliliters (mL);
m-mass of the sample in grams (g);
w-moisture content of the sample in percent (%);
the calculation result is accurate to two decimal places, and the arithmetic mean value of 2 parallel measurements is taken as the measurement result.
In the step (5), if the total phosphorus concentration in the sample solution is beyond the range of the standard working solution, the sample mass should be reduced, and the sample solution is prepared again according to the step (4).
Compared with the prior art, the invention has the following advantages: the invention firstly uses a continuous flow analyzer to detect the total phosphorus content in the organic fertilizer for tobacco. Phosphorus in the organic fertilizer for the tobacco is digested by sulfuric acid-hydrogen peroxide and converted into phosphate ions. Under a certain acidity condition, phosphate ions in the sample solution react with metavanadate and molybdic acid to form yellow ternary heteropoly acid. Measuring the response value of the sample solution at 420nm by using a continuous flow analyzer, and determining the response value according to the response value and the P in the sample solution2O5The total phosphorus content in the organic fertilizer sample for tobacco can be calculated by the quantitative relation between the concentrations. Plotting the maximum P2O5Standard working curve with standard solution concentration of 1000mg/L and linear correlation coefficient R21 is ═ 1; standard deviation of blank solution according to 10 repeated measurementsRespectively calculating the detection limit and the quantification limit of the method to be 1.372mg/L and 4.574mg/L by 3 times and 10 times; within the precision range of result expression required by the method, the variation coefficients in and among batches of 3 samples with different total phosphorus contents are all 0.00 percent after repeated measurement for 3 times; the recovery rate range of 3 adding levels of 3 samples is 99.99-100.01%, and the variation coefficient range of the secondary parallel measurement for calculating each recovery rate is 0.00-0.01%; compared with the method of 'NY 525-2012 organic fertilizer' 5.4, the absolute value difference of the measured value is mostly less than 0.01%. The method is simple and convenient to operate, rapid, high in accuracy, good in precision and good in stability, and the detection result of the method is consistent with that of a standard method, so that a new choice is provided for related detection of tobacco organic fertilizer components.
Drawings
FIG. 1 is a standard operating curve;
FIG. 2 is a schematic diagram of a pipeline arrangement of a continuous flow analyzer for measuring the total phosphorus content of the organic fertilizer for tobacco.
Detailed Description
The present invention is further described in detail with reference to the drawings and examples, which are not intended to limit the technical scope of the present invention, and all changes and equivalents which come within the spirit of the teachings of the present invention shall fall within the scope of the present invention.
Examples
1 materials and methods
1.1 principle of the method
Phosphorus in the organic fertilizer for the tobacco is digested by sulfuric acid-hydrogen peroxide and converted into phosphate ions. Under a certain acidity condition, phosphate ions in the sample solution react with metavanadate and molybdic acid to form yellow ternary heteropoly acid. Measuring the response value of the sample solution at 420nm by using a continuous flow analyzer, and determining the response value according to the response value and the P in the sample solution2O5The content of the total phosphorus in the organic fertilizer sample for the cigarettes can be calculated by the quantitative relation among the concentrations.
1.2 materials, reagents and instruments
Samples 1-11# are commercial organic fertilizers for tobacco.
Concentrated sulfuric acid (H)2SO4) (Tianjin Fuchen chemical reagent factory); ammonium metavanadate (NH)4VO3) (chemical agents of the national drug group Co., Ltd.); ammonium molybdate ((NH)4)6Mo7O24.4H2O) (national drug group chemical agents limited); hydrogen peroxide (Tianjin Fuchen chemical reagent factory); potassium dihydrogen phosphate (KH)2PO4) (ii) a Sodium dodecylsulfate diphenoxy salt (FFD6, Skalar).
Sulfuric acid solution: slowly add 40mL of H to 800mL of water2SO4Stirring while adding, transferring into a 1000mL volumetric flask, and fixing the volume to the scale.
FFD6 solution: 2mL of FFD6 was added to 1000mL of water and mixed well.
Sample injector cleaning solution: remove 50mL H2SO4Slowly adding water into a 1000mL volumetric flask, and fixing the volume to the scale.
Color developing agent: weighing NH4VO31.0g was dissolved in 200mL of hot water and cooled. Weighing (NH)4)6Mo7O24.4H2O20 g was dissolved in 200mL of hot water and cooled. Reacting NH4VO3The solution was added to 400mL of distilled water, and 60mL of H was slowly added2SO4Stirring and mixing the mixture evenly while adding the (NH) solution, cooling the mixture, and slowly adding the (NH) solution while stirring4)6Mo7O24.4H2And cooling the O solution, and then fixing the volume to 2L.
Continuous flow analyzers (SKALAR, netherlands); an electric heating air blast drying oven (DHG-9240, Shanghai-Heng scientific instruments Co., Ltd.); electronic balance (AR2140, Onhaus (OHAUS) Corp., accuracy 0.0001 g).
1.3 methods
1.3.1 preparation of Standard working solutions
Phosphorus pentoxide (P)2O5) Stock solution (5 g/L): accurately weighing 4.79g (accurate to 0.0001g) of potassium dihydrogen phosphate (KH) dried at 105 deg.C for 2 hr2PO4) Dissolving in 50mL beaker with water, transferring into 500mL volumetric flask, adding water to constant volume to scale, and mixing.
1, 2, 4, 8, 16 and 20mL of P were removed2O5The stock solution is put into a 100mL volumetric flask and diluted to a constant volume by a sample injector cleaning solution to obtain P2O5The concentration is 50, 100, 200, 400, 800, 1000mg/L series of standard working solutions respectively.
The response of the series of standard working solutions was measured at 420nm with a continuous flow analyzer as the P of the solution2O5The concentration is abscissa, the response value is ordinate, a standard working curve is drawn, the linear equation is that Y is 0.0002X +0.0004, and the correlation coefficient R21. FIG. 1 is a typical standard operating curve. And (3) arranging pipelines of the continuous flow analyzer: using a yellow/white pump tube for the sample solution, wherein the flow rate is 0.23 mL/min; h2SO4The solution is pumped by a yellow/yellow pump tube at the flow rate of 1.20 mL/min; FFD6 solution was pumped through a yellow/blue pump tube at a flow rate of 1.40 mL/min; the color developing agent is an orange/orange pump tube, and the flow rate is 0.42 mL/min; highest P for linear correspondence2O5The content is 1000 mg/L; as shown in particular in fig. 2.
1.3.2 sample moisture determination
The moisture content of the sample was measured with reference to "determination of moisture of organic fertilizer NY/T3021995".
1.3.2.1 sample drying
And (3) treating an air-dried sample: after the organic fertilizer for the tobacco to be detected is taken and dried, the organic fertilizer is reduced to 100g by a quartering method, the organic fertilizer is crushed and completely passes through a sieve with the aperture of 1mm, and the crushed organic fertilizer is filled into a sample bottle for later use, namely a sample.
Treatment of fresh laboratory samples: weighing fresh laboratory samples as soon as possible, putting the samples into an electric heating blast constant-temperature drying oven at 80-90 ℃ for drying for 15-30min, then cooling to 65 ℃, keeping for 12-24h, then processing according to air-dried samples to prepare samples, and bottling for later use.
1.3.2.2 treatment of aluminum boxes: placing the aluminum box obliquely into a box cover, placing the box cover into an electric heating blowing constant-temperature drying box with the temperature of 100-105 ℃, drying for 30min, taking out the box cover, moving the box cover into a dryer, balancing for 20min, taking out and weighing. And baking for 30min, weighing under the same conditions until the mass difference between the two times is not more than 1mg, thus obtaining the constant weight.
1.3.2.3 weigh about 5g of sample, accurately to 0.001g, flatly spread on an aluminum box with known constant weight, covered, moved to an electrothermal blowing constant temperature drying oven preheated to 105 ℃, opened and put the box cover obliquely, closed, dried at 105 ℃ for 8h at 2 ℃, taken out after covered, moved to a dryer for balancing for 30min, taken out and weighed.
1.3.2.4 the moisture content is expressed in mass percent (%) and is calculated as follows:
in the formula: w (%) -sample moisture content in percent (%);
m1-sample and aluminum box mass in grams (g);
m2the mass of the dried sample and the aluminum box is gram (g);
m0-aluminum box mass in grams (g).
The results should be expressed as one decimal place. The arithmetic mean of the results of the replicates was taken as the measurement result. The absolute difference of the parallels is not more than 0.2%.
1.3.3 sample treatment
Weighing 0.5-1.0 g (accurate to 0.0001g) of the sample, placing the sample at the bottom of a 100mL digestion tube, washing the sample adhered to the tube wall with 3mL water, slowly adding 5mL sulfuric acid, slowly and carefully adding 1.5mL hydrogen peroxide dropwise, carefully shaking up, inserting a pear-shaped glass funnel at the tube opening, and standing overnight. Heating the digester to 100 ℃ for 20min, taking out the digester, and slowly adding 0.5mL of hydrogen peroxide along the wall of the digester three times until the solution is colorless or light yellow clear liquid. The digestion tube was placed in a digester pre-warmed to 370 ℃ for 1 h. Cooling for 10min after digestion, adding 10mL of water, cooling to room temperature, fixing the volume to the scale with the water, and shaking up to obtain a sample solution.
1.3.4 sample analysis
Measuring the response value of the sample solution at 420nm by using a continuous flow analyzer, and calculating the total phosphorus concentration in the sample solution by using a standard working curve; and (3) arranging pipelines of the continuous flow analyzer: using a yellow/white pump tube for the sample solution, wherein the flow rate is 0.23 mL/min; h2SO4The solution is pumped by a yellow/yellow pump tube at the flow rate of 1.20 mL/min; FFD6 solution forA yellow/blue pump tube with the flow rate of 1.40 mL/min; the color developing agent is an orange/orange pump tube, and the flow rate is 0.42 mL/min; highest P for linear correspondence2O5The content is 1000 mg/L;
if the total phosphorus concentration in the sample solution is out of the range of the standard working solution, the sample mass should be reduced and the sample solution is again prepared according to step (1.3.3).
1.3.5 results calculation
In the formula:
P2O5(%) -total phosphorus content in organic fertilizer for tobacco, unit is percentage (%);
c-total phosphorus concentration in milligrams per liter (mg/L) in the sample solution;
v-total volume of sample solution in milliliters (mL);
m-mass of the sample in grams (g);
w-moisture content of the sample in percent (%);
the calculation results are shown to two decimal places, and the arithmetic mean of 2 replicates is taken as the measurement result.
2 results and discussion
2.1 Instrument Condition optimization
Under a certain acidity condition, phosphate ions in the sample solution react with metavanadate and molybdic acid to form yellow ternary heteropoly acid, and 420nm is the maximum absorption wavelength of the colored solution, so 420nm is selected as the detection wavelength.
Respectively transferring 1, 2, 4, 8, 16, 20mL of 5g/L P2O5The stock solution is put into a 100mL volumetric flask and diluted to a constant volume by a sample injector cleaning solution to obtain P2O5The concentration is 50, 100, 200, 400, 800, 1000mg/L series of standard working solutions respectively. Three main agents were examined in combination: h2SO4Under the condition that the solution, the FFD6 solution and the color developing agent are arranged in different pipelines, the peak shape, the separation degree, the gain and the color developing agent of the series of standard working solutions,And selecting and determining a proper flow path for measuring the total phosphorus content in the organic fertilizer for the cigarettes under the influence of linear correlation coefficients and the like. The piping configuration shown in fig. 2 is finally determined: sample solution was pumped through a yellow/white pump tube (flow rate 0.23mL/min), H2SO4The solution was pumped through a yellow/yellow pump tube (flow rate 1.20mL/min), the FFD6 solution was pumped through a yellow/blue pump tube (flow rate 1.40mL/min), and the developer was pumped through an orange/orange pump tube (flow rate 0.42 mL/min). In the case of this pipe configuration, the highest P corresponds to the linearity2O5The content is 1000 mg/L.
2.2 methodological investigation
2.2.1 Standard Curve, detection Limit, quantification Limit of method
Standard working solution was prepared as 1.3.1, as P of solution2O5The concentration is abscissa, the response value is ordinate, a standard working curve is drawn, the linear equation is that Y is 0.0002X +0.0004, and the correlation coefficient R21. See fig. 1.
By not adding P2O5The Standard Deviation (SD) of 10 parallel measurements of the blank solution was calculated using the stock solution as a sample cleaning solution, and the detection limit and the quantification limit were calculated as 1.372mg/L and 4.574mg/L for 3-fold SD and 10-fold SD, respectively, and the detection data are shown in Table 1.
Table 1 blank solution 10 replicates
2.2.2 precision and stability of the method
Taking 1#, 3#, 10# samples to test 3 batches at different time respectively, testing each batch for 3 times in parallel, and investigating precision and stability of the method, as shown in table 2, within the precision range of result expression required by the method, the variation coefficient between batches is 0.00%, and the precision and stability of the method are both good.
TABLE 2 precision and stability of the method
2.2.3 recovery rate by adding standard
Adding a certain amount of P into a sample with a known content2O5And comparing the measured addition amount with the theoretical addition amount to obtain the recovery rate. The recovery rate range of 3 addition levels of 3 samples is 99.99-100.01%, and the variation coefficient range of secondary parallel measurement for each recovery rate is 0.00-0.01% (see table 3), which indicates that the detection method has accurate and reliable results.
TABLE 3 recovery with addition of standard
2.2.4 sample detection and method comparison
The method is used for detecting 11 commercially available organic fertilizers for cigarettes, and the 1#, 3#, and 10# are parallelly measured for 3 times, and the rest samples are parallelly measured for 2 times. And meanwhile, detecting according to a method of 'NY 525-2012 organic fertilizer' 5.4, and comparing the difference between the two. As can be seen from Table 4, the coefficient of variation of the test results of 11 samples in the method of the invention is less than 0.02%; the absolute difference in the measured values is also mostly less than 0.01% compared with the standard method. The precision of the method is high, and the result is consistent with that of the standard method.
TABLE 4 sample detection and method comparison
The average value of 2 parallel measurements, the measurement precision meets the requirement of NY525-2012 method
3. Conclusion
The method disclosed by the invention is simple and convenient to operate, rapid, high in accuracy, good in precision and good in stability, has the same detection result with a standard method, and can completely meet the requirement of detecting the total phosphorus content of the organic fertilizer for the cigarettes.
Claims (2)
1. A method for rapidly determining the total phosphorus content in an organic fertilizer for tobacco comprises the following steps:
(1) preparation of standard working solution: mixing KH with water2PO4Drying at 105 ℃ for 2h, accurately weighing 4.79g, placing in a 50mL beaker, adding water for dissolution, transferring into a 500mL volumetric flask, adding water to a constant volume to a scale, and mixing uniformly to obtain P2O5Reserving the stock solution for later use; 1, 2, 4, 8, 16 and 20mL of P were removed2O5Placing the stock solution into a 100mL volumetric flask, diluting with a sample injector cleaning solution to a constant volume to obtain P2O5The concentration is 50, 100, 200, 400, 800, 1000mg/L series of standard working solutions respectively;
(2) drawing a standard working curve: the response value of a series of standard working solutions is measured at 420nm by a continuous flow analyzer as the P of the solution2O5The concentration is abscissa, the response value is ordinate, a standard working curve is drawn, the linear equation is that Y is 0.0002X +0.0004, and the correlation coefficient R21 is ═ 1; and (3) arranging pipelines of the continuous flow analyzer: using a yellow/white pump tube for the sample solution, wherein the flow rate is 0.23 mL/min; h2SO4The solution is pumped by a yellow/yellow pump tube at the flow rate of 1.20 mL/min; FFD6 solution was pumped through a yellow/blue pump tube at a flow rate of 1.40 mL/min; the color developing agent is an orange/orange pump tube, and the flow rate is 0.42 mL/min; highest P for linear correspondence2O5The content is 1000 mg/L;
(3) measurement of sample moisture: drying and crushing the organic fertilizer for the tobacco to be detected, sieving the organic fertilizer with a sieve with the aperture of 1mm to be used as a sample, and then determining the moisture content of the sample according to the specification of NY/T3021995 organic fertilizer moisture determination;
(4) sample treatment: weighing 0.5-1.0 g of sample, placing the sample at the bottom of a 100mL digestion tube, washing the sample adhered to the tube wall with 3mL of water, slowly adding 5mL of sulfuric acid, slowly and dropwise adding 1.5mL of hydrogen peroxide, carefully shaking up, inserting a pear-shaped glass funnel into the tube opening, and placing the tube opening overnight; heating the digester to 100 ℃ for 20min, taking out the digester, and slowly adding 0.5mL of hydrogen peroxide along the wall of the digester for three times until the solution is colorless or light yellow clear liquid; then placing the digestion tube in a digester which is preheated to 370 ℃ in advance, and digesting for 1 h; cooling for 10min after digestion, adding 10mL of water, cooling to room temperature, fixing the volume to the scale with the water, and shaking up to obtain a sample solution;
(5) analysis of the sample solution: determination at 420nm with continuous flow AnalyzerCalculating the total phosphorus concentration of the sample solution through a standard working curve according to the response value of the sample solution; and (3) arranging pipelines of the continuous flow analyzer: using a yellow/white pump tube for the sample solution, wherein the flow rate is 0.23 mL/min; h2SO4The solution is pumped by a yellow/yellow pump tube at the flow rate of 1.20 mL/min; FFD6 solution was pumped through a yellow/blue pump tube at a flow rate of 1.40 mL/min; the color developing agent is an orange/orange pump tube, and the flow rate is 0.42 mL/min; highest P for linear correspondence2O5The content is 1000 mg/L;
(6) and (4) calculating a result:
in the formula:
P2O5(%) -total phosphorus content in organic fertilizer for tobacco, unit is percentage (%);
c-total phosphorus concentration in milligrams per liter (mg/L) in the sample solution;
v-total volume of sample solution in milliliters (mL);
m-mass of the sample in grams (g);
w-moisture content of the sample in percent (%);
the calculation result is accurate to two decimal places, and the arithmetic mean value of 2 parallel measurements is taken as the measurement result.
2. The method of claim 1, wherein: in the step (5), if the total phosphorus concentration in the sample solution is beyond the range of the standard working solution, the sample mass should be reduced, and the sample solution is prepared again according to the step (4).
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