CN104020169A - Chemical detection method for dissolved organic matters in organic fertilizer - Google Patents
Chemical detection method for dissolved organic matters in organic fertilizer Download PDFInfo
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Abstract
The invention discloses a chemical detection method for dissolved organic matters in organic fertilizer. The method comprises the following steps: adding appropriate amount of water in samples to be detected, uniformly shaking, carrying out ultrasonic treatment by an ultrasonic cleaning instrument, metering the volume in an appropriate volumetric flask and standing; taking out supernatant, centrifuging, and oxidizing certain amount of centrifugate with excess potassium dichromate standard testing solution-concentrated sulfuric acid; with phenanthroline as an indicator, titrating non-consumed potassium dichromate with a ferrous sulfate solution and recording the volume of the consumed ferrous sulfate; and with water of the same volume as blank control experiment, recording the volume of the consumed ferrous sulfate and calculating the content of the dissolved organic matters in the samples. Compared with a conventional detection method for the dissolved organic matters in soil, the chemical detection method for the dissolved organic matters in organic fertilizer is simple and rapid, is targeted, has strong operability, and is beneficial to determination of the content of dissolved organic matters in organic fertilizer, and the detection result has good reproducibility and is accurate and reliable.
Description
Technical field
The present invention relates to chemical detection technique field, relate in particular to the chemical detection method of Dissolved Organic Matter (DOM) content in a kind of organic fertilizer.
Background technology
Serious along with inorganic fertilizer is large to soil harm, fertility runs off, large etc. not enough in cognitive widely to environmental impact, organic fertilizer starts more and more by public acceptance as a kind of new-type fertilizer; Inorganic fertilizer relatively, the organic matter in organic fertilizer is the material that soil improvement is played a decisive role; Therefore organic detection be organic fertilizer one to important indicator, national standard NY-525-2012 to organic fertilizer in the content of organic matter measure and also made corresponding specification.Its control criterion is the butt meter content of organic matter >=45%.
Water-soluble organic matter (DOM) refers to by 0.45 μ m sieve aperture and can be dissolved in water, acid, alkali or salt solusion, the organic molecule mixture of different size structures, in soil, water-soluble organic matter has very strong reactivity, for the improvement of soil texture, soil environment balance has significant role; And organic as the indissoluble such as cellulose, grease thing with respect to slightly solubility, Dissolved Organic Matter (DOM) is more easily degraded by microorganisms and changes into the absorbent element of plant, also can improve microbial activity simultaneously, accelerates the carrying out of microbial degradation reaction.Therefore the height of Dissolved Organic Matter (DOM) content, is reacting the height of organic fertilizer fertilizer efficiency to a certain extent.And by measuring the content of Dissolved Organic Matter (DOM) in organic fertilizer raw material, also can provide an important theoretical foundation for the production fermentation period assessment of organic fertilizer.
A quality control foundation using Dissolved Organic Matter (DOM) assay as organic fertilizer not yet due to China, therefore, at present for the measurement of Dissolved Organic Matter (DOM) in organic fertilizer, not yet puts into effect concerned countries standard method.The content of organic matter is measured relatively, and the sample pre-treatments before Dissolved Organic Matter (DOM) is measured is extremely important.Conventionally in organic fertilizer (natural base), Dissolved Organic Matter (DOM) is 3% left and right only, and therefore, in the time measuring, in GB, the assay method of the content of organic matter cannot be used in resolvability content of organic matter mensuration.
Dissolved Organic Matter (DOM) content assaying method mainly contains Dissolved Organic Matter (DOM) content determination in soil at present.In soil, the measuring method of Dissolved Organic Matter (DOM) mainly contains at present: 1. many water and soil reference method, and as reference method, this method can only determine the Dissolved Organic Matter (DOM) content in soil by comparison, because sample object is different, cannot be applicable in organic fertilizer; 2. potassium bichromate titrimetric method, by pertinent literature, this method in sampling amount and sample preparation in the low content of organic matter of more applicable soil water-soluble organic matter measure; And particle is generally less than normal in soil, soil particle density is greater than water.Containing the particularly organic fertilizer process sample of organic fertilizer of the complicated ingredients such as more cellulose, lignin, humic acid, this method, in sampling amount, sample preparation way, all needs to improve relatively.Therefore need to improve by experiment and formulate one and there is reference significance, strong operability the authentic and valid detection method of measuring Dissolved Organic Matter (DOM) in organic fertilizer of energy.
Summary of the invention
Technical matters solved by the invention is to provide the chemical detection method of Dissolved Organic Matter (DOM) content in a kind of organic fertilizer, thereby solves the problem in above-mentioned background technology.
Technical matters solved by the invention realizes by the following technical solutions:
The inventive method is in the component of organic fertilizer complexity, leach and process at sample, method by ultrasonic resonance fast and effectively water leaches its water-soluble organic matter component, the ultrasonic oscillation method using can shorten extraction time greatly, and the shatter large-scale crumb structure of ultrasonic oscillation energy is more conducive to the leaching of Dissolved Organic Matter (DOM).
More can make Separation of Solid and Liquid come by the ultracentrifugal method of hydro-extractor compared with Filter paper filtering method; Prove after centrifugal to get supernatant within the scope of this concentration Dissolved Organic Matter (DOM) by orthogonal experiment, differ very little (irregularities deviation) with crossing 0.45 μ m filter membrane result, can reduce filtration step, be conducive to improve conventional efficient.
In the time of Organic oxidation, compared with 170 DEG C of bath oilings, be oxidized little molecule Dissolved Organic Matter (DOM) energy-saving safety with 105 DEG C of water-baths, have more specific aim.
In computing method, determine that by control experiment water-soluble organic matter is by the oxidation correction coefficient of potassium dichromate oxidation, blindly quote in the organic assay method of GB 1.5 oxidation correction coefficient with a high credibility, result is convergence actual value more, on result is calculated, adopt the blank comparison of primary standard substance potassium dichromate, reduce National Standard Method and surveyed operation steps and the experimentation cumulative errors while demarcating ferrous ion solubility with 0.1mol/L1/6 potassium dichromate when organic, can measure quickly and accurately the content of water-soluble organic matter in organic fertilizer.
Due to experiment condition restriction, when the oxidation of potassium dichromate for the inventive method-concentrated sulphuric acid is organic, adopt 100 ± 5 DEG C of water bath heatings, in oxidation correction coefficient, 1.1 the oxidation correction coefficient that cannot use with reference to 170 DEG C of bath oilings in Dissolved Organic Matter (DOM) assay method in soil, Dissolved Organic Matter (DOM) content is lower, molecular activity is high, therefore also cannot, with reference to the oxidation correction coefficient that adopts 1.5 in content of organic matter assay method in fertilizer, therefore must determine oxidation correction coefficient by confirmatory experiment.
In organic fertilizer, a chemical detection method for Dissolved Organic Matter (DOM) content, specifically comprises the steps:
(1) get testing sample (m), add suitable quantity of water and shake up, be placed in ultrasonic washing instrument ultrasonic after, constant volume is to leaving standstill in suitable volumetric flask (V);
(2) adopt hydro-extractor ultracentrifugal method to separate, get upper strata liquid centrifugal after, with excessive potassium dichromate (V
c) (concentration is that c) concentrated sulphuric acid is oxidized a certain amount of centrifugate (V to benchmark test solution
x);
(3) taking Phen as indicator, the potassium dichromate not being consumed with copperas solution titration, the volume that record consumes ferrous sulphate is V
1;
(4) do blank experiment with the water of same volume, the volume that record consumes ferrous sulphate is V
0;
(5) in organic fertilizer, the computing formula of Dissolved Organic Matter (DOM) content is:
By the concentration of potassium dichromate with 1/6 potassium dichromate concentration (c
0) calculate meter constant volume: centrifugate volume (V:V
x)=D, after simplifying, formula is:
V, V in formula
0, V
cunit is ml; c
0=6c, is 1/6 potassium bichromate solution solubility, and unit is mol/L; M is the quality that takes sample, and unit is g; 1.724 are converted into organic reduction coefficient for organic carbon; A is oxidation correction coefficient.
In described step (3), when contiguous titration end-point, solution becomes sapphirine, wait becoming when brick-red, arrives titration end-point.
In described step (3), the chemical equation relating to is as follows:
Organic carbon is oxidized:
Potassium dichromate is reduced:
In described step (5), oxidation correction coefficient confirmatory experiment method is: take a certain amount of glucose (A.R.) water-bath oxidation in 100 DEG C of water-baths, calculate A.R. level under the condition that is not multiplied by oxidation correction coefficient in, in glucose, organic carbon content is 36.78%, theoretical value is 40%, be oxidized correction coefficient A=40 ÷ 36.78=1.09 ≈ 1.1, finally selected computing formula is:
。
The present invention has following beneficial effect:
Raw material, the reagent of the inventive method are easy to get, and instrument application is extensive, and detection method is with strong points, and testing result accuracy is high.In the time not formulating the detection method of respective country standard, can be used as a kind of monitoring mode and detection method and be applied to the each side such as the raw material detection of organic fertilizer field, process monitoring, product inspection.
Embodiment
For technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1:
Get organic fertilizer semi-manufacture in production run and detect its Dissolved Organic Matter (DOM) content, specifically comprise the steps:
(1) take 4.994g sample and add about 50ml distilled water in 250ml conical flask, be placed in ultrasonic washing instrument each concussion 10 minutes under high power and weak power, be settled to standing about 30min in 100ml volumetric flask;
(2) get upper strata liquid and pour (liquid level can not exceed centrifuge tube 2/3) in 30ml centrifuge tube into, be placed in hydro-extractor (centrifuge tube is placed and should be noted ensureing hydro-extractor pallet balance), power-on, by slow extremely fast, slowly adjusting rotary speed, to 3000r/min, centrifugal 20 minutes, takes out stand-by;
(3) pipette 10ml centrifugate in 250ml conical flask, pipette the 1/6 potassium bichromate solution 10ml of 0.4000mol/L with transfer pipet, slowly add the 10ml concentrated sulphuric acid, conical flask is placed in to water-bath, be placed in water-bath at 100 DEG C, water-bath 30min, takes out cooling;
(4) add 2 ~ 3 Phen indicator, adding distil water to about 80ml, with the titration of ferrous sulphate ammonia solution, when solution gradually becomes sapphirine, starts dropwise to add mark liquid, until record consumes the volume (14.76ml) of ferrous sulphate when brick-red;
(5) do blank assay with 10ml water, record consumes ferrous sulphate mark liquid long-pending (25.23ml); Calculate the content (in natural base) of Dissolved Organic Matter (DOM) according to formula:
By same sample is measured to control experiment repeatedly, measurement result is respectively 1.92%, 1.88%; Data stabilization is reliable, favorable reproducibility, can reflect comparatively really the Dissolved Organic Matter (DOM) content of sample in the production of organic fertilizer process.
Embodiment 2:
Get the content that finished product organic fertilizer detects its water-soluble organic matter, specifically comprise the steps:
(1) take 4.833g sample and add about 50ml distilled water in 250ml conical flask, be placed in ultrasonic washing instrument each concussion 10 minutes under high power and weak power, be settled to standing about 30min in 100ml volumetric flask;
(2) get upper strata liquid and pour in 30ml centrifuge tube, be placed in hydro-extractor, power-on, by slow, to fast, slowly adjusting rotary speed, to 3000r/min, centrifugal 20 minutes, takes out stand-by;
(3) pipette 10ml centrifugate in 250ml conical flask, pipette the 1/6 potassium bichromate solution 10ml of 0.8000mol/L with transfer pipet, slowly add the 10ml concentrated sulphuric acid, conical flask is placed in to water-bath, be placed in water-bath at 100 DEG C, water-bath 30min, takes out cooling;
(4) add 2 ~ 3 Phen indicator, adding distil water to about 80ml, with the titration of ferrous sulphate ammonia solution, when solution gradually becomes sapphirine, starts dropwise to add mark liquid, until record consumes the volume (30.95ml) of ferrous sulphate when brick-red;
(5) do blank assay with 10ml water, record consumes ferrous sulphate mark liquid long-pending (50.52ml), calculates the content (in natural base) of Dissolved Organic Matter (DOM) according to formula:
By same sample is measured to control experiment repeatedly, measurement result is respectively 3.52%, 3.56%; Data stabilization is reliable, favorable reproducibility, can reflect comparatively really the Dissolved Organic Matter (DOM) content of sample in the production of organic fertilizer process.
Embodiment 3:
Mark approximately 1% Dissolved Organic Matter (DOM) glucose in organic fertilizer, detects total Dissolved Organic Matter (DOM) in test sample product, carries out interior mark experiment, and confirmatory experiment accuracy, specifically comprises the steps:
(1) in embodiment 2 samples, take 99.00g organic fertilizer, add A.R. level glucose 1.00g, the meter glucose content of organic matter is 100%, and, in this sample, interior mark Dissolved Organic Matter (DOM) content is 1%;
(2) take 4.287g sample and add about 50ml distilled water in 250ml conical flask, be placed in ultrasonic washing instrument each concussion 10 minutes under high power and weak power, be settled to standing about 30min in 100ml volumetric flask;
(3) get upper strata liquid and pour in 30ml centrifuge tube, be placed in hydro-extractor, power-on, by slow, to fast, slowly adjusting rotary speed, to 3000r/min, centrifugal 20 minutes, takes out stand-by;
(4) pipette 10ml centrifugate in 250ml conical flask, pipette the 1/6 potassium bichromate solution 10ml of 0.8000mol/L with transfer pipet, slowly add the 10ml concentrated sulphuric acid, conical flask is placed in to water-bath, be placed in water-bath at 100 DEG C, water-bath 30min, takes out cooling;
(5) add 2 ~ 3 Phen indicator, adding distil water to about 80ml, with the titration of ferrous sulphate ammonia solution, when solution gradually becomes sapphirine, starts dropwise to add mark liquid, until record consumes the volume (30.16ml) of ferrous sulphate when brick-red;
(6) do blank assay with 10ml water, record consumes ferrous sulphate mark liquid long-pending (50.52ml), calculates the content (in natural base) of Dissolved Organic Matter (DOM) according to formula:
Same sample is carried out after parallel laboratory test, record Dissolved Organic Matter (DOM) content in this sample and be respectively 4.32%, 4.38%, after the Dissolved Organic Matter (DOM) of interior mark 1%, in embodiment 2, detection level has improved 0.7% relatively, there is 0.3% error, analyze by certification, obtain a result as follows:
Interior its molecular formula of mark glucose is
, its organic carbon content is 40%, thus after interior mark 1% glucose, in organic fertilizer in target organic carbon be 0.4%, be multiplied by after correction coefficient 1.724, be converted into the interior mark content of organic matter and be:
0.4%×1.724=0.6896%
Coincide with measurement result, fixed by interior mapping, show that this method is detecting Dissolved Organic Matter (DOM) result accurately and reliably.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and instructions, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (4)
1. a chemical detection method for Dissolved Organic Matter (DOM) content in organic fertilizer, is characterized in that: specifically comprise the steps:
(1) get testing sample (m), add suitable quantity of water and shake up, be placed in ultrasonic washing instrument ultrasonic after, constant volume is to leaving standstill in suitable volumetric flask (V);
(2) adopt hydro-extractor ultracentrifugal method to separate, get upper strata liquid centrifugal after, with excessive potassium dichromate (V
c) (concentration is that c) concentrated sulphuric acid is oxidized a certain amount of centrifugate (V to benchmark test solution
x);
(3) taking Phen as indicator, the potassium dichromate not being consumed with copperas solution titration, the volume that record consumes ferrous sulphate is V
1;
(4) do blank experiment with the water of same volume, the volume that record consumes ferrous sulphate is V
0;
(5) in organic fertilizer, the computing formula of Dissolved Organic Matter (DOM) content is:
By the concentration of potassium dichromate with 1/6 potassium dichromate concentration (c
0) calculate meter constant volume: centrifugate volume (V:V
x)=D, after simplifying, formula is:
V, V in formula
0, V
cunit is ml; c
0=6c, is 1/6 potassium bichromate solution solubility, and unit is mol/L; M is the quality that takes sample, and unit is g; 1.724 are converted into organic reduction coefficient for organic carbon; A is oxidation correction coefficient.
2. a kind of chemical detection method of Dissolved Organic Matter (DOM) content in organic fertilizer according to claim 1, is characterized in that: in described step (3), when contiguous titration end-point, solution becomes sapphirine, wait becoming when brick-red, arrives titration end-point.
3. the chemical detection method of Dissolved Organic Matter (DOM) content in a kind of organic fertilizer according to claim 1, is characterized in that: in described step (3), the chemical equation relating to is as follows:
Organic carbon is oxidized:
Potassium dichromate is reduced:
。
4. a kind of chemical detection method of Dissolved Organic Matter (DOM) content in organic fertilizer according to claim 1, it is characterized in that: in described step (5), oxidation correction coefficient confirmatory experiment method is: take a certain amount of glucose (A.R.) water-bath oxidation in 100 DEG C of water-baths, calculate A.R. level under the condition that is not multiplied by oxidation correction coefficient in, in glucose, organic carbon content is 32.28%, theoretical value is 36.37%, be oxidized correction coefficient A=33.37 ÷ 32.28=1.09 ≈ 1.1, finally selected computing formula is:
。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110018272A (en) * | 2019-04-19 | 2019-07-16 | 四川省劲腾环保建材有限公司 | A method of preparing detection content of organics in extruding dregs porcelain granule |
| CN112285272A (en) * | 2020-10-26 | 2021-01-29 | 广西北海巨丰农牧科技有限公司 | Method for determining nutrient substances in commercial wormcast organic fertilizer |
| CN113933451A (en) * | 2020-06-29 | 2022-01-14 | 红河锦东化工股份有限公司 | Method for inspecting active humic acid organic fertilizer product |
| WO2023005026A1 (en) * | 2021-07-29 | 2023-02-02 | 上海城市水资源开发利用国家工程中心有限公司 | New method for determining degradable organic carbon (doc) indexes of sludge |
-
2014
- 2014-06-25 CN CN201410287887.7A patent/CN104020169A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 郝汉舟: "《土壤地理学与生物地理学实习实践教程》", 1 June 2013 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110018272A (en) * | 2019-04-19 | 2019-07-16 | 四川省劲腾环保建材有限公司 | A method of preparing detection content of organics in extruding dregs porcelain granule |
| CN113933451A (en) * | 2020-06-29 | 2022-01-14 | 红河锦东化工股份有限公司 | Method for inspecting active humic acid organic fertilizer product |
| CN112285272A (en) * | 2020-10-26 | 2021-01-29 | 广西北海巨丰农牧科技有限公司 | Method for determining nutrient substances in commercial wormcast organic fertilizer |
| WO2023005026A1 (en) * | 2021-07-29 | 2023-02-02 | 上海城市水资源开发利用国家工程中心有限公司 | New method for determining degradable organic carbon (doc) indexes of sludge |
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Application publication date: 20140903 |