CN113933451A - Method for inspecting active humic acid organic fertilizer product - Google Patents
Method for inspecting active humic acid organic fertilizer product Download PDFInfo
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- CN113933451A CN113933451A CN202010623773.0A CN202010623773A CN113933451A CN 113933451 A CN113933451 A CN 113933451A CN 202010623773 A CN202010623773 A CN 202010623773A CN 113933451 A CN113933451 A CN 113933451A
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- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000004021 humic acid Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000003895 organic fertilizer Substances 0.000 title claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 71
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 69
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000005303 weighing Methods 0.000 claims abstract description 45
- 238000005406 washing Methods 0.000 claims abstract description 41
- 238000001816 cooling Methods 0.000 claims abstract description 30
- 238000004458 analytical method Methods 0.000 claims abstract description 23
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 239000005416 organic matter Substances 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 103
- 239000000523 sample Substances 0.000 claims description 67
- 239000012086 standard solution Substances 0.000 claims description 48
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 30
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 29
- 239000011790 ferrous sulphate Substances 0.000 claims description 27
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 27
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 239000000047 product Substances 0.000 claims description 23
- 239000002244 precipitate Substances 0.000 claims description 18
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 15
- 238000007865 diluting Methods 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 239000012085 test solution Substances 0.000 claims description 9
- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 claims description 9
- 239000011449 brick Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004380 ashing Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000012496 blank sample Substances 0.000 claims description 3
- 150000001721 carbon Chemical group 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000012937 correction Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 230000020477 pH reduction Effects 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000004448 titration Methods 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- 238000012372 quality testing Methods 0.000 abstract description 2
- 239000003337 fertilizer Substances 0.000 description 7
- 230000002195 synergetic effect Effects 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000004151 quinonyl group Chemical group 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- -1 humic acid compound Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003415 peat Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for inspecting active humic acid organic fertilizer products, which comprises the following steps: firstly, measuring the organic matter content: step 1: weighing 0.2-0.5 g of an analysis sample passing through a sieve with the diameter of 0.5mm, placing the analysis sample in a 500mL triangular flask, accurately adding 50mL of 0.8mol/L potassium dichromate solution, adding 50mL of concentrated sulfuric acid, adding a small funnel with a bent neck, placing the funnel in boiling water, and keeping the funnel for 30min after the water is boiled; step 2: removing the small funnel from the boiling water, cooling to room temperature, washing the small funnel with water, and collecting the washing liquid in a triangular flask. By sequentially measuring and analyzing the organic matter content, the activated brown black humic acid content and the active humic acid content, the method has clear operation steps, is simple and convenient to operate, can quickly test the active humic acid organic fertilizer product, has high test accuracy, can meet the operation requirements of most enterprises and quality testing units, and is convenient to popularize and use.
Description
Technical Field
The invention relates to the technical field related to organic fertilizer detection, in particular to a method for detecting an active humic acid organic fertilizer product.
Background
Humic acid is animal and plant residues, mainly plant residues, and is a heterogeneous aliphatic aromatic amorphous organic polymer mixture rich in various active functional groups such as carboxyl, phenolic hydroxyl, quinonyl, carbonyl, methoxyl and the like through microbial decomposition and synthesis and a series of geophysical and chemical interaction processes. Humic acid is mainly activated, extracted and separated from weathered coal, lignite and peat, and can also be converted from clean biomass resources through humification by a special microorganism fermentation means; the basic structure of the macromolecule of humic acid is aromatic ring and alicyclic ring, the functional groups of carboxyl, hydroxyl, carbonyl, quinonyl, methoxyl, etc. are connected on the ring, the humic acid is a mixture of aromatic amorphous high molecular compounds rich in oxygen-containing functional groups of carboxyl, phenolic hydroxyl, methoxyl, etc., the synergistic effect of the humic acid on fertilizer is very obvious, and the humic acid is widely used as a synergist of the fertilizer. The humic acid compound fertilizer has huge capacity, the main part of the humic acid synergistic fertilizer is activated humic acid, and the activated humic acid is usually used for representing the activation degree of the humic acid in the fertilizer.
In order to control the product quality of the humic acid organic fertilizer and promote the healthy development of the humic acid synergistic fertilizer, the active humic acid organic fertilizer in the product needs to be detected; however, no scientific and accurate determination method exists at present, so that finding a method for accurately, quickly and efficiently determining the product quality of the humic acid organic fertilizer has an important influence on the product quality of humic acid.
Disclosure of Invention
The invention aims to provide a method for inspecting active humic acid organic fertilizer products, which aims to solve the problems that the quality of the humic acid organic fertilizer products is controlled, the healthy development of humic acid synergistic fertilizer is promoted, and the active humic acid organic fertilizer in the products needs to be inspected; however, there is no scientific and accurate measurement method.
In order to achieve the purpose, the invention provides the following technical scheme: the method for inspecting the active humic acid organic fertilizer product comprises the following steps:
firstly, measuring the organic matter content:
step 1: weighing 0.2-0.5 g of an analysis sample passing through a sieve with the diameter of 0.5mm, placing the analysis sample in a 500mL triangular flask, accurately adding 50mL of 0.8mol/L potassium dichromate solution, adding 50mL of concentrated sulfuric acid, adding a small funnel with a bent neck, placing the funnel in boiling water, and keeping the funnel for 30min after the water is boiled;
step 2: taking out the small funnel with bent neck from boiling water, cooling to room temperature, washing the small funnel with water, and collecting the washing liquid in a triangular flask;
and step 3: taking down the triangular flask, transferring reactants into a 250mL volumetric flask without damage, cooling to room temperature, fixing the volume, sucking 50mL of solution into the 250mL triangular flask, adding water to about 100mL, adding 2-3 drops of an o-phenanthroline indicator, titrating the solution with 0.2mol/L ferrous sulfate standard solution to be near the end point, changing the solution from green to dark green, and then dropwise adding the ferrous sulfate standard solution until brick red is generated;
and 4, step 4: simultaneously weighing 0.2g of silicon dioxide instead of a sample, and carrying out a blank test by using the same reagent according to the same analysis steps of the steps 1 to 3;
and 5: the dry-basis organic matter content omega in the sample is expressed by mass fraction and calculated according to the formula:
secondly, measuring the content of activated brown black humic acid:
step 1: weighing 1.0g to 3.0g of a sample (accurate to 0.0002g, weighing 3.0g to 1.0g according to the sample weighing of 1 percent to 3 percent of the content of activated humic acid) from the sample into a 250mL conical flask, adding 100mL of citric acid-sodium citrate extraction solution, shaking to wet the sample, placing the sample into a boiling water bath through a small funnel at the opening of the conical flask, heating and extracting for 60min, wherein the amplitude is 20r/min to 30r/min, and uniformly extracting the sample;
step 2: taking out the conical flask, cooling to room temperature, transferring all the extract and residues into a 200mL volumetric flask, diluting to a scale with water, and shaking up to obtain solution A; dry-filtering with medium-speed qualitative filter paper, discarding the initial solution of about 5mL, and filtering to obtain filtrate of 150-180 mL to obtain solution B, and performing blank test;
and step 3: accurately sucking 100mL of the B solution by using a 50mL pipette, slowly adding a sulfuric acid solution into a centrifuge cup to adjust the pH value of the solution to 2.00, centrifuging the suspension at 3000r/min for 30min, decanting the supernatant, collecting, washing the centrifugation residue for 3 times by using a sulfuric acid washing solution, wherein the dosage of the supernatant and the washing solution is 20mL each time, and combining the supernatant and the washing solution to obtain a C solution;
and 4, step 4: dissolving the precipitate in the centrifuge cup with 50mL of sodium hydroxide solution, transferring the precipitate to a 200mL volumetric flask, washing the centrifuge cup with 20mL of water each time, repeating the washing for 3-4 times, transferring the washing liquid into the volumetric flask, and fixing the volume to obtain solution D;
10. and 5: accurately sucking 10mL of D liquid into a 250mL conical flask, accurately adding 5mL of 0.4mol/L potassium dichromate solution and 15mL of sulfuric acid by using a pipette, placing the solution in a boiling water bath, oxidizing for 30min, and carrying out amplitude of 20r/min-30r/min, then taking down the solution, cooling to room temperature, diluting to about 100mL by using water, adding 3-inch phenanthroline indicator after cooling, and titrating to brick red by using a ferrous ammonium sulfate standard solution; simultaneously, measuring a blank value according to the steps;
step 6: the content of active brown black humic acid BHAad is calculated according to the formula, wherein the numerical value is expressed by percent:
thirdly, active humic acid determination:
step 1: weighing 0.3g-0.5g of an analysis sample in a 250mL conical flask, adding 100mL of water, shaking to wet the sample, placing the sample in a water bath at 100 +/-1 ℃ in a small funnel at the opening of the conical flask, heating and extracting for 1h, and shaking once every 20min to uniformly extract the sample; simultaneously, performing a blank experiment;
step 2: taking out the conical flask, cooling to room temperature, transferring the extract to a 200mL volumetric flask, washing with water to constant volume, and shaking up; filtering with slow-speed fixed filter paper, discarding the initial 10mL of filtrate, accurately transferring 100mL of filtrate into a 250mL beaker, placing the beaker on an electromagnetic stirrer, regulating the pH to 1 with 2mol/L hydrochloric acid solution under stirring, stabilizing for 5min, placing the solution into a centrifuge cup, centrifuging for 30min at 3000r/min, transferring the centrifuged clear solution onto the filter paper which is dried at 105-110 ℃ in advance and has constant weight and slow fixed amount, adding 50mL of 2mol/L hydrochloric acid solution into the centrifuged residue, stirring uniformly, centrifuging for 30min at 3000r/min, transferring the acid-washed clear solution onto the filter paper, repeating acid washing for three times, transferring the residue onto the filter paper, and washing with acid until the color is formed;
and step 3: transferring the precipitate and filter paper into a weighing bottle, drying in a drying oven at 105-110 ℃ for 2h, taking a certain amount of sample, putting the sample into a dryer, cooling to room temperature, and weighing; performing checking drying until the difference value of two continuous times is not more than 0.001g, calculating the mass, and weighing the mass of the blank sample;
and 4, step 4: transferring the dried precipitate with constant weight and filter paper into a constant-weight and weighed net bottom ceramic crucible, placing the crucible into a muffle furnace, leaving a gap of 15-20 mm on a furnace door, slowly ashing the dried precipitate and the filter paper from room temperature to 250-300 ℃, closing the furnace door after ashing, burning for 1h at 815 +10 ℃, taking the crucible out of the muffle furnace, cooling the crucible in the air for 5min, placing the crucible into a drier, cooling to room temperature (about 20min), weighing, performing inspection burning until the difference value of two continuous times is not more than 0.001g, and calculating the quality of the burned residues of humic acid and the weight of blank burned residues;
and 5: the content omega of the dry-based active humic acid in the sample is expressed by mass fraction and calculated according to a formula:
preferably, in step 1 of measuring the organic content, the potassium dichromate solution is prepared as follows: weighing 39.2g of potassium dichromate, dissolving with a small amount of water, transferring into a 1L volumetric flask, diluting to a scale, and shaking up.
Preferably, in step 3 of measuring the organic content, the ferrous sulfate standard solution is prepared as follows: weighing 55.6g of ferrous sulfate heptahydrate, dissolving in 900mL of water, adding 20mL of sulfuric acid for dissolving, diluting to a constant volume of 1L, and shaking up for later use; the preparation method of the o-phenanthroline indicator is as follows: weighing 0.695g of ferrous sulfate and 1.485g of o-phenanthroline, dissolving in 100mL of water, and shaking uniformly.
Preferably, in the step 5 of measuring the organic matter content, omega is the dry-basis organic matter content; c is the molar concentration of the ferrous sulfate standard solution, and the unit is mol/L; v. of0When the test is a blank test, the volume of the ferrous sulfate standard solution is consumed, and the unit is mL; v is the volume of the ferrous sulfate standard solution consumed in the sample determination, and the unit is mL; 0.003 is the molar mass of a quarter of a carbon atom in g/mmol; 1.724 is a coefficient converted from organic carbon to organic matter; m is the mass of the air-dried sample, and the unit is g; mad is the moisture of the analysis sample; d is the volume multiple of the volume to be measured/volume to be measured, 250/50; and taking the arithmetic mean of the parallel analysis results as a determination result, and keeping four significant digits of the analysis results.
Preferably, in the step 1 of measuring the content of the activated brown black humic acid, the citric acid-sodium citrate extract is prepared by mixing 70mL of citric acid solution and 930mL of sodium citrate solution and shaking up, wherein the concentration of the citric acid-sodium citrate extract is 0.1mol/L, and the pH value is 6-7.
Preferably, in step 3 of measuring the content of activated brown black humic acid, the preparation method of the sulfuric acid solution is as follows: diluting 28ml of 98% sulfuric acid with water, metering to 1000ml volumetric flask, and shaking up; the sulfuric acid washing liquor is prepared by mixing and shaking up sulfuric acid solution and water according to the volume ratio of 1: 9.
Preferably, in the step 5 of measuring the content of the activated brown black humic acid, the sulfuric acid is concentrated sulfuric acid with the concentration of 98%; the preparation method of the potassium dichromate solution comprises the following steps: weighing 20g of potassium dichromate, dissolving in a proper amount of water, fixing the volume to a volumetric flask of 1000ml, and shaking up; the standard solution of ferrous ammonium sulfate is prepared by the following steps: weighing 40g of ferrous ammonium sulfate, dissolving the ferrous ammonium sulfate in water, adding 20mL of sulfuric acid with the concentration of 98%, metering the volume to a 1000mL brown volumetric flask, and shaking up.
Preferably, in step 6 of the determination of the content of activated humic acid brown black, v0The volume of the blank consumed ammonium ferrous sulfate standard solution is titrated, and the unit is mL; v. of1The volume of the standard solution of ferrous ammonium sulfate consumed by the titration test solution is a numerical value, and the unit is milliliter (mL); c is an accurate value of the concentration of the ammonium ferrous sulfate standard solution, and the unit is mol/L; r is the carbon content of humic acid, and the value is 0.58; m is the numerical value of the mass of the sample, and the unit is g; a is the numerical value of the total volume of the extract after constant volume, the unit is mL, and a is 200 in the method; d is the numerical value of the total volume of the acid precipitate after alkali dissolution and volume fixing, the unit is mL, and d is 200 in the method; b is the numerical value of the volume of the test solution taken in the acidification, the unit is mL, and b is 100 in the method; e is the volume value of the test solution taken in the oxidation measurement, the unit is mL, and e is 10 in the method; 0.003 is a number corresponding to a mass of carbon in g for 1.00mL of a 1.000mol/L solution of ferrous ammonium sulfate C (Fe2 +); 1.05 is an oxidation correction factor.
Preferably, in step 2 of active humic acid determination, the hydrochloric acid solution is prepared as follows: 166mL of concentrated hydrochloric acid was accurately transferred and slowly placed in a 1L beaker into which 600mL of distilled water had been added, stirred uniformly, cooled, and transferred to a 1000mL volumetric flask.
Preferably, in step 5 of active humic acid determination, in the formula, ω is dry-based active humic acidAcid content, m is sample mass, and unit is g; m is1The unit is the dry mass of humic acid, and is g; m is2The dry mass of blank filter paper is gram; m is3The unit is g of the quality of residue burned by humic acid; m is4The mass of the residue after blank filter paper firing is given in gram; d is the volume multiple of the volume to be measured/volume to be measured, 200/100; madTo analyze the moisture content of a sample; and during calculation, the arithmetic mean value of the parallel measurement results is taken as the measurement result, and the result is reserved to one digit behind the decimal point.
The invention provides a method for inspecting an active humic acid organic fertilizer product, which has the following beneficial effects:
according to the invention, through sequentially measuring and analyzing the organic matter content, the activated brown black humic acid content and the active humic acid content, the operation steps are clear, the operation is simple and convenient, the active humic acid organic fertilizer product can be quickly tested, the testing accuracy is high, the operation requirements of most enterprises and quality testing units can be met, the measuring error can be better controlled, and the popularization and the use are convenient.
Detailed Description
Example (b):
the method for inspecting the active humic acid organic fertilizer product comprises the following steps:
the method comprises the following steps:
firstly, measuring the organic matter content:
step 1: weighing 0.2-0.5 g of an analysis sample passing through a sieve with the diameter of 0.5mm, placing the analysis sample in a 500mL triangular flask, accurately adding 50mL of 0.8mol/L potassium dichromate solution, adding 50mL of concentrated sulfuric acid, adding a small funnel with a bent neck, placing the funnel in boiling water, and keeping the funnel for 30min after the water is boiled; wherein, the potassium dichromate solution is prepared as follows: weighing 39.2g of potassium dichromate, dissolving with a small amount of water, transferring into a 1L volumetric flask, diluting to scale, and shaking up
Step 2: taking out the small funnel with bent neck from boiling water, cooling to room temperature, washing the small funnel with water, and collecting the washing liquid in a triangular flask;
and step 3: taking off the triangular flask, transferring the reactant into a 250mL volumetric flask without damage, and cooling to room temperatureDiluting to a constant volume, sucking 50mL of solution into a 250mL triangular flask, adding about 100mL of water, adding 2-3 drops of an o-phenanthroline indicator, titrating with 0.2mol/L of a ferrous sulfate standard solution to a near-end point, changing the solution from green to dark green, and then dropwise adding the ferrous sulfate standard solution until brick red is generated; wherein the preparation method of the o-phenanthroline indicator is as follows: weighing 0.695g of ferrous sulfate and 1.485g of o-phenanthroline, dissolving in 100mL of water, and shaking uniformly; the ferrous sulfate standard solution was prepared as follows: weighing 55.6g of ferrous sulfate heptahydrate, dissolving in 900mL of water, adding 20mL of sulfuric acid for dissolving, diluting to a constant volume of 1L, and shaking up for later use; the accurate concentration of the ferrous sulfate standard solution is calibrated by 0.1mol/L potassium dichromate standard solution in the following way: absorbing 20mL of potassium dichromate standard solution, adding into a 150mL triangular flask, adding 3-5 mL of sulfuric acid and 2-3 drops of an admenation indicator, and titrating with ferrous sulfate standard solution; calculating the accurate concentration C according to the consumption of the ferrous sulfate standard solution drop at regular time by the following formula2:In the formula: c1The concentration of the standard solution of potassium dichromate is shown in mol/L; c2The concentration of the ferrous sulfate standard solution is shown in mol/L; v1In order to absorb the volume of the potassium dichromate standard solution, the unit is mL; v2 isThe volume of the ferrous sulfate standard solution is consumed in milliliter mL when the solution is dripped;
and 4, step 4: simultaneously weighing 0.2g of silicon dioxide instead of a sample, and carrying out a blank test by using the same reagent according to the same analysis steps of the steps 1 to 3;
and 5: the dry-basis organic matter content omega in the sample is expressed by mass fraction and calculated according to the formula:in the formula, omega is the content of dry organic matters; c is the molar concentration of the ferrous sulfate standard solution, and the unit is mol/L; v. of0When the test is a blank test, the volume of the ferrous sulfate standard solution is consumed, and the unit is mL; v is the body consuming the ferrous sulfate standard solution when the sample is measuredProduct, in mL; 0.003 is the molar mass of a quarter of a carbon atom in g/mmol; 1.724 is a coefficient converted from organic carbon to organic matter; m is the mass of the air-dried sample, and the unit is g; mad is the moisture of the analysis sample; d is the volume multiple of the volume to be measured/volume to be measured, 250/50; taking the arithmetic mean value of the parallel analysis results as a determination result, and keeping four significant digits in the analysis results;
secondly, measuring the content of activated brown black humic acid:
step 1: weighing 1.0g to 3.0g of a sample (accurate to 0.0002g, weighing 3.0g to 1.0g according to the sample weighing of 1 percent to 3 percent of the content of activated humic acid) from the sample into a 250mL conical flask, adding 100mL of citric acid-sodium citrate extraction solution, shaking to wet the sample, placing the sample into a boiling water bath through a small funnel at the opening of the conical flask, heating and extracting for 60min, wherein the amplitude is 20r/min to 30r/min, and uniformly extracting the sample; the citric acid-sodium citrate extraction liquid is prepared by mixing 70mL of citric acid solution and 930mL of sodium citrate solution and shaking up, the concentration of the citric acid-sodium citrate extraction liquid is 0.1mol/L, and the pH value is 6-7;
step 2: taking out the conical flask, cooling to room temperature, transferring all the extract and residues into a 200mL volumetric flask, diluting to a scale with water, and shaking up to obtain solution A; dry-filtering with medium-speed qualitative filter paper, discarding the initial solution of about 5mL, and filtering to obtain filtrate of 150-180 mL to obtain solution B, and performing blank test;
and step 3: accurately sucking 100mL of the B solution by using a 50mL pipette, slowly adding a sulfuric acid solution into a centrifuge cup to adjust the pH value of the solution to 2.00, centrifuging the suspension at 3000r/min for 30min, decanting the supernatant, collecting, washing the centrifugation residue for 3 times by using a sulfuric acid washing solution, wherein the dosage of the supernatant and the washing solution is 20mL each time, and combining the supernatant and the washing solution to obtain a C solution; the preparation method of the sulfuric acid solution comprises the following steps: diluting 28ml of 98% sulfuric acid with water, metering to 1000ml volumetric flask, and shaking up; the sulfuric acid washing liquor is prepared by mixing and shaking up a sulfuric acid solution and water according to the volume ratio of 1: 9;
and 4, step 4: dissolving the precipitate in the centrifuge cup with 50mL of sodium hydroxide solution, transferring the precipitate to a 200mL volumetric flask, washing the centrifuge cup with 20mL of water each time, repeating the washing for 3-4 times, transferring the washing liquid into the volumetric flask, and fixing the volume to obtain solution D;
and 5: accurately sucking 10mL of D liquid into a 250mL conical flask, accurately adding 5mL of 0.4mol/L potassium dichromate solution and 15mL of sulfuric acid by using a pipette, placing the solution in a boiling water bath, oxidizing for 30min, and carrying out amplitude of 20r/min-30r/min, then taking down the solution, cooling to room temperature, diluting to about 100mL by using water, adding 3-inch phenanthroline indicator after cooling, and titrating to brick red by using a ferrous ammonium sulfate standard solution; simultaneously, measuring a blank value according to the steps; wherein, the sulfuric acid adopts concentrated sulfuric acid with the concentration of 98 percent; the preparation method of the potassium dichromate solution comprises the following steps: weighing 20g of potassium dichromate, dissolving in a proper amount of water, fixing the volume to a volumetric flask of 1000ml, and shaking up; the standard solution of ferrous ammonium sulfate is prepared by the following steps: weighing 40g of ferrous ammonium sulfate, dissolving the ferrous ammonium sulfate in water, adding 20mL of sulfuric acid with the concentration of 98%, metering the volume to a 1000mL brown volumetric flask, and shaking up; before the ammonium ferrous sulfate standard solution is used, a 0.1mol/L potassium dichromate solution is used for calibration according to the following method: accurately sucking 25ml of potassium dichromate standard solution, putting the solution into a 250ml conical flask, then adding 70ml to 80ml of distilled water and 10ml of 98% sulfuric acid, cooling, adding 3 drops of phenanthroline indicator, and titrating the solution by using ammonium ferrous sulfate standard solution until the solution is changed from orange to brick red; the preparation method of the phenanthroline indicator comprises the following steps: weighing 1.5g of phenanthroline, 1g of ammonium ferrous sulfate or 0.7g of ferrous sulfate, dissolving in 100ml of water, and uniformly mixing; the concentration of the ammonium ferrous sulfate standard solution is C, the unit is moL/L, and the calculation formula is as follows:wherein v is the numerical value of the volume of the ammonium ferrous sulfate standard solution for titrating 25ml of potassium dichromate standard solution, and the unit is ml;
step 6: the content of active brown black humic acid BHAad is calculated according to the formula, wherein the numerical value is expressed by percent:v0the volume of the blank consumed ammonium ferrous sulfate standard solution is titrated, and the unit is mL; v. of1The volume value of the standard solution of ferrous ammonium sulfate consumed by the titration test solution,the unit is mL; c is an accurate value of the concentration of the ammonium ferrous sulfate standard solution, and the unit is mol/L; r is the carbon content of humic acid, and the value is 0.58; m is the numerical value of the mass of the sample, and the unit is g; a is the numerical value of the total volume of the extract after constant volume, the unit is mL, and a is 200 in the method; d is the numerical value of the total volume of the acid precipitate after alkali dissolution and volume fixing, the unit is mL, and d is 200 in the method; b is the numerical value of the volume of the test solution taken in the acidification, the unit is mL, and b is 100 in the method; e is the volume value of the test solution taken in the oxidation measurement, the unit is mL, and e is 10 in the method; 0.003 is a number corresponding to a mass of carbon in g for 1.00mL of a 1.000mol/L solution of ferrous ammonium sulfate C (Fe2 +); 1.05 is the oxidation correction factor;
thirdly, active humic acid determination:
step 1: weighing 0.3g-0.5g of an analysis sample in a 250mL conical flask, adding 100mL of water, shaking to wet the sample, placing the sample in a water bath at 100 +/-1 ℃ in a small funnel at the opening of the conical flask, heating and extracting for 1h, and shaking once every 20min to uniformly extract the sample; simultaneously, performing a blank experiment;
step 2: taking out the conical flask, cooling to room temperature, transferring the extract to a 200mL volumetric flask, washing with water to constant volume, and shaking up; filtering with slow-speed fixed filter paper, discarding the initial 10mL of filtrate, accurately transferring 100mL of filtrate into a 250mL beaker, placing the beaker on an electromagnetic stirrer, regulating the pH to 1 with 2mol/L hydrochloric acid solution under stirring, stabilizing for 5min, placing the solution into a centrifuge cup, centrifuging for 30min at 3000r/min, transferring the centrifuged clear solution onto the filter paper which is dried at 105-110 ℃ in advance and has constant weight and slow fixed amount, adding 50mL of 2mol/L hydrochloric acid solution into the centrifuged residue, stirring uniformly, centrifuging for 30min at 3000r/min, transferring the acid-washed clear solution onto the filter paper, repeating acid washing for three times, transferring the residue onto the filter paper, and washing with acid until the color is formed; the preparation method of the hydrochloric acid solution comprises the following steps: accurately transferring 166mL of concentrated hydrochloric acid into a 1L beaker into which 600mL of distilled water is added, uniformly stirring, cooling, and transferring the concentrated hydrochloric acid into a 1000mL volumetric flask;
and step 3: transferring the precipitate and filter paper into a weighing bottle, drying in a drying oven at 105-110 ℃ for 2h, taking a certain amount of sample, putting the sample into a dryer, cooling to room temperature, and weighing; performing checking drying until the difference value of two continuous times is not more than 0.001g, calculating the mass, and weighing the mass of the blank sample;
and 4, step 4: transferring the dried precipitate with constant weight and filter paper into a constant-weight and weighed net bottom ceramic crucible, placing the crucible into a muffle furnace, leaving a gap of 15-20 mm on a furnace door, slowly ashing the dried precipitate and the filter paper from room temperature to 250-300 ℃, closing the furnace door after ashing, burning for 1h at 815 +10 ℃, taking the crucible out of the muffle furnace, cooling the crucible in the air for 5min, placing the crucible into a drier, cooling to room temperature (about 20min), weighing, performing inspection burning until the difference value of two continuous times is not more than 0.001g, and calculating the quality of the burned residues of humic acid and the weight of blank burned residues;
and 5: the content omega of the dry-based active humic acid in the sample is expressed by mass fraction and calculated according to a formula:in the formula, omega is the content of dry-base active humic acid, m is the mass of a sample, and the unit is g; m is1The unit is the dry mass of humic acid, and is g; m is2The dry mass of blank filter paper is gram; m is3The unit is g of the quality of residue burned by humic acid; m is4The mass of the residue after blank filter paper firing is given in gram; d is the volume multiple of the volume to be measured/volume to be measured, 200/100; madTo analyze the moisture content of a sample; and during calculation, the arithmetic mean value of the parallel measurement results is taken as the measurement result, and the result is reserved to one digit behind the decimal point.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The method for inspecting the active humic acid organic fertilizer product is characterized by comprising the following steps:
firstly, measuring the content of organic matters;
step 1: weighing 0.2-0.5 g of an analysis sample passing through a sieve with the diameter of 0.5mm, placing the analysis sample in a 500mL triangular flask, accurately adding 50mL of 0.8mol/L potassium dichromate solution, adding 50mL of concentrated sulfuric acid, adding a small funnel with a bent neck, placing the funnel in boiling water, and keeping the funnel for 30min after the water is boiled;
step 2: taking out the small funnel with bent neck from boiling water, cooling to room temperature, washing the small funnel with water, and collecting the washing liquid in a triangular flask;
and step 3: taking down the triangular flask, transferring reactants into a 250mL volumetric flask without damage, cooling to room temperature, fixing the volume, sucking 50mL of solution into the 250mL triangular flask, adding water to about 100mL, adding 2-3 drops of an o-phenanthroline indicator, titrating the solution with 0.2mol/L ferrous sulfate standard solution to be near the end point, changing the solution from green to dark green, and then dropwise adding the ferrous sulfate standard solution until brick red is generated;
and 4, step 4: simultaneously weighing 0.2g of silicon dioxide instead of a sample, and carrying out a blank test by using the same reagent according to the same analysis steps of the steps 1 to 3;
and 5: the dry-basis organic matter content omega in the sample is expressed by mass fraction and calculated according to the formula:
secondly, measuring the content of the activated brown black humic acid;
step 1: weighing 1.0g to 3.0g of a sample from the sample, adding 100mL of citric acid-sodium citrate extraction solution into a 250mL conical flask, shaking to wet the sample, placing the conical flask in a small funnel at the opening of the conical flask, placing the conical flask in a boiling water bath, heating and extracting for 60min, wherein the amplitude is 20r/min to 30r/min, and uniformly extracting the sample;
step 2: taking out the conical flask, cooling to room temperature, transferring all the extract and residues into a 200mL volumetric flask, diluting to a scale with water, and shaking up to obtain solution A; dry-filtering with medium-speed qualitative filter paper, discarding the initial solution of about 5mL, and filtering to obtain filtrate of 150-180 mL to obtain solution B, and performing blank test;
and step 3: accurately sucking 100mL of the B solution by using a 50mL pipette, slowly adding a sulfuric acid solution into a centrifuge cup to adjust the pH value of the solution to 2.00, centrifuging the suspension at 3000r/min for 30min, decanting the supernatant, collecting, washing the centrifugation residue for 3 times by using a sulfuric acid washing solution, wherein the dosage of the supernatant and the washing solution is 20mL each time, and combining the supernatant and the washing solution to obtain a C solution;
and 4, step 4: dissolving the precipitate in the centrifuge cup with 50mL of sodium hydroxide solution, transferring the precipitate to a 200mL volumetric flask, washing the centrifuge cup with 20mL of water each time, repeating the washing for 3-4 times, transferring the washing liquid into the volumetric flask, and fixing the volume to obtain solution D;
and 5: accurately sucking 10mL of D liquid into a 250mL conical flask, accurately adding 5mL of 0.4mol/L potassium dichromate solution and 15mL of sulfuric acid by using a pipette, placing the solution in a boiling water bath, oxidizing for 30min, and carrying out amplitude of 20r/min-30r/min, then taking down the solution, cooling to room temperature, diluting to about 100mL by using water, adding 3-inch phenanthroline indicator after cooling, and titrating to brick red by using a ferrous ammonium sulfate standard solution; simultaneously, measuring a blank value according to the steps;
step 6: the content of active brown black humic acid BHAad is calculated according to the formula, wherein the numerical value is expressed by percent:
thirdly, measuring active humic acid;
step 1: weighing 0.3g-0.5g of an analysis sample in a 250mL conical flask, adding 100mL of water, shaking to wet the sample, placing the sample in a water bath at 100 ℃ in a small funnel at the opening of the conical flask, heating and extracting for 1h, and shaking once every 20min to uniformly extract the sample; simultaneously, performing a blank experiment;
step 2: taking out the conical flask, cooling to room temperature, transferring the extract to a 200mL volumetric flask, washing with water to constant volume, and shaking up; filtering with slow-speed fixed filter paper, discarding the initial 10mL of filtrate, accurately transferring 100mL of filtrate into a 250mL beaker, placing the beaker on an electromagnetic stirrer, regulating the pH to 1 with 2mol/L hydrochloric acid solution under stirring, stabilizing for 5min, placing the solution into a centrifuge cup, centrifuging for 30min at 3000r/min, transferring the centrifuged clear solution onto the filter paper which is dried at 105-110 ℃ in advance and has constant weight and slow fixed amount, adding 50mL of 2mol/L hydrochloric acid solution into the centrifuged residue, stirring uniformly, centrifuging for 30min at 3000r/min, transferring the acid-washed clear solution onto the filter paper, repeating acid washing for three times, transferring the residue onto the filter paper, and washing with acid until the color is formed;
and step 3: transferring the precipitate and filter paper into a weighing bottle, drying in a drying oven at 105-110 ℃ for 2h, taking a certain amount of sample, putting the sample into a dryer, cooling to room temperature, and weighing; performing checking drying until the difference value of two continuous times is not more than 0.001g, calculating the mass, and weighing the mass of the blank sample;
and 4, step 4: transferring the dried precipitate with constant weight and filter paper into a constant-weight and weighed net bottom ceramic crucible, placing the crucible into a muffle furnace, leaving a gap of 15-20 mm on a furnace door, slowly ashing the dried precipitate and the filter paper from room temperature to 250-300 ℃, closing the furnace door after ashing, burning for 1h at 815 +10 ℃, taking the crucible out of the muffle furnace, cooling the crucible in the air for 5min, placing the crucible into a drier, cooling to room temperature (about 20min), weighing, performing inspection burning until the difference value of two continuous times is not more than 0.001g, and calculating the quality of the burned residues of humic acid and the weight of blank burned residues;
2. the method for inspecting active humic acid organic fertilizer product according to claim 1, wherein in step 1 of organic matter content determination, the potassium dichromate solution is prepared as follows: weighing 39.2g of potassium dichromate, dissolving with a small amount of water, transferring into a 1L volumetric flask, diluting to a scale, and shaking up.
3. The method for inspecting active humic acid organic fertilizer product according to claim 1, wherein in step 3 of measuring organic content, the preparation method of ferrous sulfate standard solution is as follows: weighing 55.6g of ferrous sulfate heptahydrate, dissolving in 900mL of water, adding 20mL of sulfuric acid for dissolving, diluting to a constant volume of 1L, and shaking up for later use; the preparation method of the o-phenanthroline indicator is as follows: weighing 0.695g of ferrous sulfate and 1.485g of o-phenanthroline, dissolving in 100mL of water, and shaking uniformly.
4. The method for inspecting active humic acid organic fertilizer product of claim 1, wherein in step 5 of organic matter content determination, ω is dry basis organic matter content; c is the molar concentration of the ferrous sulfate standard solution, and the unit is mol/L; v. of0When the test is a blank test, the volume of the ferrous sulfate standard solution is consumed, and the unit is mL; v is the volume of the ferrous sulfate standard solution consumed in the sample determination, and the unit is mL; 0.003 is the molar mass of a quarter of a carbon atom in g/mmol; 1.724 is a coefficient converted from organic carbon to organic matter; m is the mass of the air-dried sample, and the unit is g; mad is the moisture of the analysis sample; d is the volume multiple of the volume to be measured/volume to be measured, 250/50; and taking the arithmetic mean of the parallel analysis results as a determination result, and keeping four significant digits of the analysis results.
5. The method for testing the active humic acid organic fertilizer product as claimed in claim 1, wherein in the step 1 of testing the content of the activated brown black humic acid, the citric acid-sodium citrate extract is prepared by mixing 70mL of citric acid solution with 930mL of sodium citrate solution and shaking up, and the concentration of the citric acid-sodium citrate extract is 0.1mol/L and the pH value is 6-7.
6. The method for inspecting active humic acid organic fertilizer product according to claim 1, wherein in the step 3 of measuring the content of the activated brown black humic acid, the preparation method of the sulfuric acid solution is as follows: diluting 28ml of 98% sulfuric acid with water, metering to 1000ml volumetric flask, and shaking up; the sulfuric acid washing liquor is prepared by mixing and shaking up sulfuric acid solution and water according to the volume ratio of 1: 9.
7. The method for inspecting active humic acid organic fertilizer product according to claim 1, characterized in that in the step 5 of the determination of the content of the activated brown black humic acid, the sulfuric acid is concentrated sulfuric acid with the concentration of 98%; the preparation method of the potassium dichromate solution comprises the following steps: weighing 20g of potassium dichromate, dissolving in a proper amount of water, fixing the volume to a volumetric flask of 1000ml, and shaking up; the standard solution of ferrous ammonium sulfate is prepared by the following steps: weighing 40g of ferrous ammonium sulfate, dissolving the ferrous ammonium sulfate in water, adding 20mL of sulfuric acid with the concentration of 98%, metering the volume to a 1000mL brown volumetric flask, and shaking up.
8. The method for inspecting active humic acid organic fertilizer product of claim 1, wherein in step 6 of the determination of the content of activated humic acid with brown black color, v is0The volume of the blank consumed ammonium ferrous sulfate standard solution is titrated, and the unit is mL; v. of1The volume of the standard solution of ferrous ammonium sulfate consumed by the titration test solution is a numerical value, and the unit is milliliter (mL); c is an accurate value of the concentration of the ammonium ferrous sulfate standard solution, and the unit is mol/L; r is the carbon content of humic acid, and the value is 0.58; m is the numerical value of the mass of the sample, and the unit is g; a is the numerical value of the total volume of the extract after constant volume, the unit is mL, and a is 200 in the method; d is the numerical value of the total volume of the acid precipitate after alkali dissolution and volume fixing, the unit is mL, and d is 200 in the method; b is the numerical value of the volume of the test solution taken in the acidification, the unit is mL, and b is 100 in the method; e is the volume value of the test solution taken in the oxidation measurement, the unit is mL, and e is 10 in the method; 0.003 is a number corresponding to a mass of carbon in g for 1.00mL of a 1.000mol/L solution of ferrous ammonium sulfate C (Fe2 +); 1.05 is an oxidation correction factor.
9. The method for inspecting active humic acid organic fertilizer product according to claim 1, wherein in the step 2 of active humic acid determination, the hydrochloric acid solution is prepared in the following way: 166mL of concentrated hydrochloric acid was accurately transferred and slowly placed in a 1L beaker into which 600mL of distilled water had been added, stirred uniformly, cooled, and transferred to a 1000mL volumetric flask.
10. The method for inspecting active humic acid organic fertilizer product of claim 1, wherein in step 5 of active humic acid determination, formulaIn the formula, omega is the content of dry-base active humic acid, m is the mass of a sample, and the unit is g; m is1The unit is the dry mass of humic acid, and is g; m is2The dry mass of blank filter paper is gram; m is3The unit is g of the quality of residue burned by humic acid; m is4The mass of the residue after blank filter paper firing is given in gram; d is the volume multiple of the volume to be measured/volume to be measured, 200/100; madTo analyze the moisture content of a sample; and during calculation, the arithmetic mean value of the parallel measurement results is taken as the measurement result, and the result is reserved to one digit behind the decimal point.
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