CN106370778A - Method for determining humus and component contents thereof in sludge compost - Google Patents

Method for determining humus and component contents thereof in sludge compost Download PDF

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CN106370778A
CN106370778A CN201610885346.3A CN201610885346A CN106370778A CN 106370778 A CN106370778 A CN 106370778A CN 201610885346 A CN201610885346 A CN 201610885346A CN 106370778 A CN106370778 A CN 106370778A
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李国学
李恕艳
李丹阳
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China Agricultural University
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    • 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
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    • 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
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators

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Abstract

The invention relates to a method for determining humus and component contents thereof in sludge compost. The method comprises the following steps: determining the water content of a sludge compost sample, adding a leaching solution, treating in a water bath, centrifugating to obtain a clear solution, and taking out a first humus solution and a second humus solution from the clear solution; regulating the pH value of the second humus solution to 1-2, centrifugating to separate the precipitate out, washing with water, adding sodium hydroxide, completely dissolving the sodium hydroxide to obtain a humic acid solution, taking out a first humic acid solution from the humic acid solution, respectively adding a potassium dichromate solution and concentrated sulfuric acid into the first humus solution and first humic acid solution to respectively obtain a first sample and a second sample, respectively adding an isometric indicator to respectively obtain a first titrating sample and a second titrating sample, sequentially titrating to the preset color by using a ferrous sulfate standard solution, and calculating the component contents according to the preset formula. The method overcomes the effects of incomplete extraction and long extraction period in the traditional process, and has high accuracy of determination results.

Description

A kind of method of humus and its constituent content in mensure sludge composting
Technical field
The present invention relates to humus determination techniques field is and in particular to a kind of measure humus and its component in sludge composting The method of content.
Background technology
High temperature aerobic composting be process mud, the solid waste such as feces of livestock and poultry so as to innoxious and resource effective Approach, is progressively degraded by unstable organic substance in composted solids garbage, generates stable Humus thing simultaneously Matter.Compost humus material is to evaluate the important indicator of rotten degree.Humus fertilizer can improve Soil structure, improve fertilizer The utilization rate of material, reduces the pollution to environment, adjusts plant physiology function, impact enzymatic activity and microbial activity simultaneously.
According to its different solubility in soda acid, humus can be divided into humic acid, fulvic acid, humin.Humic acid, Fulvic acid is larger to the activity influence of humus, and humin is the inert substance in humus.Therefore, research humic acid, Fu Li Acid content affects larger on Humus fertilizer agricultural effect.The mensure of humus is affected by many factors, as exchanger Property, concentration of salt solution, ph, ELUTION METHOD and measured matter mineral species and quantity, the content of organic matter etc..Measure humic at present The extractant of matter has highly basic or some inorganic salt (naoh, koh, na2co3、na4p2o7Deng) and organic base (ethylenediaminetetraacetic acid Sodium salt edta, ethylenediamine eda, dimethylformamide dmf, dimethyl sulfoxide emso etc.).But this several extractant all exists at present Extract not exclusively, the shortcoming of extracting cycle length.Extraction and determination with regard to humus lacks standard criterion at present both at home and abroad.
Content of the invention
For solving above-mentioned technical problem, the invention provides a kind of measure humus and its constituent content in sludge composting Method, it comprises the steps:
S1, will sludge composting air-dry after obtain sludge composting sample, measure and obtain the aqueous of described sludge composting sample Rate ω；
S2, the described sludge composting sample taking quality to be m, are added thereto to the extraction containing sodium hydroxide and sodium pyrophosphate Liquid, carries out boiling water bath to humus extraction completely, is centrifuged, gained supernatant is humus solution, volume after cooling after mixing For v2, it is taken out volume and be respectively v3And v4The first humus solution and the second humus solution；Separately take equivalent (i.e. with institute State in sludge composting sample add lixiviating solution equivalent) described lixiviating solution carry out described boiling water bath, be then taken out volume It is respectively v3And v4The first blank sample and the second blank sample；
S3, the ph value of described second humus solution is adjusted to 1～2, is centrifuged after standing, by gained precipitate and separate out, Then described precipitation is added sodium hydroxide solution to be completely dissolved to precipitation after washing, obtaining volume is v5Humic acid molten Liquid；Separately the ph value of described second blank sample is adjusted to 1～2, and is taken out volume for v5The 3rd blank sample；
S4, from described Humic Acid Solution take out volume be v3' the first Humic Acid Solution, from described 3rd blank sample Middle taking-up volume is v3' the 4th blank sample, molten to described first humus solution, the first blank sample, the first humic acid Each add the mixed liquor of potassium bichromate solution and concentrated sulphuric acid in liquid and the 4th blank sample, carry out boiling water bath after mixing extremely described First humus solution, the first Humic Acid Solution reaction completely, respectively obtain the first sample, blank sample one, second after cooling Sample and blank sample two；
S5, the respective instruction adding equivalent in described first sample, blank sample one, the second sample and blank sample two Agent, respectively obtains the first titration sample, blank titration sample one, second titration sample and blank titration sample two, is c with concentration The first titration sample, blank titration sample one, second titration sample and blank described in ferrous sulfate standard solution stepwise titration Titration sample two starts the predetermined color being presented during excess to described ferrous sulfate standard solution, then according to the following formula The content of the humus united hs-c in described sludge composting sample, humic acid carbon ha-c and fulvic acid carbon fa-c:
h s - c = c ( v 0 - v 1 ) × m m × ( 1 - ω ) × v 2 v 3 × 1000 h a - c = c ( v 0 - v 1 ′ ) × m m × ( 1 - ω ) × v 2 v 3 × v 5 v 3 ′ × 1000 f a - c = ( h s - c ) - ( h a - c ) ,
In formula,
Hs-c: humus united, unit g/kg (the i.e. quality g) of the humus united contained by sludge composting sample described in every kg；
Ha-c: humic acid carbon, unit g/kg (the i.e. quality g) of the humic acid carbon contained by sludge composting sample described in every kg；
Fa-c: fulvic acid carbon, unit g/kg (the i.e. quality g) of the fulvic acid carbon contained by sludge composting sample described in every kg；
v0: the volume of the ferrous sulfate standard solution that titration blank titration sample one is consumed, units/ml；
v0': the volume of the ferrous sulfate standard solution that titration blank titration sample two is consumed, units/ml；
v1: the volume of the ferrous sulfate standard solution that titration the first titration sample is consumed, units/ml；
v1': the volume of the ferrous sulfate standard solution that titration the second titration sample is consumed, units/ml；
M: the quality of sludge composting sample, unit g described in step s2；
C: the concentration of ferrous sulfate standard solution, unit mol/l；
The molal weight of m:1/4 carbon atom, i.e. 3g/mol.
Sludge composting of the present invention is conventional sludge composting.Humus in the present invention, Humic acids and fulvic acids It is all to be carried out quantitative with its carbon content, in described humus united, humic acid carbon and fulvic acid carbon content and its saline solution, carbon contains Amount is equivalent, and therefore term humus solution, Humic Acid Solution and fulvic acid solution are to define for the sake of describing simplicity , they refer to the saline solution of humus, Humic acids and fulvic acids respectively, that is, described humus solution, Humic Acid Solution and In fulvic acid solution, humus, Humic acids and fulvic acids are deposited respectively in the form of humus salt, humic acid salt and fulvate ?.
Compared with traditional sodium hydroxide concussion extracting method, the method for the invention significantly increases the extraction of humus Amount, overcomes the incomplete shortcoming of extraction of traditional extraction process presence.Due to significantly increasing the extracted amount of humus, thus The humus content recording more presses close to actual humus content in compost；Accordingly, with respect to existing determination techniques, the present invention Method improve the accuracy of measurement of humus in compost.Extraction process is simple and efficient, and digestion agent species used is few, cost Low, and without poisonous or severe corrosive organic base, extraction process safety.The computing formula providing, has filled up and has existed both at home and abroad The blank in this field；Assay method is simple and efficient, and the requirement to instrument and equipment for the whole measurement process is low, and agents useful for same species Few, low cost.
The method of the invention, in described lixiviating solution, the molar concentration of sodium hydroxide and sodium pyrophosphate is equal.
Preferably, in described lixiviating solution, the molar concentration of sodium hydroxide and sodium pyrophosphate is 0.1mol/l.
Further, in step s2, the amount adding described lixiviating solution in sludge composting sample described in every 1g is 10～14ml. Sludge composting under this proportioning and lixiviating solution, so that the extraction of humus optimizes further, further increase the product of humus Amount.
The method of the invention, the time of boiling water bath described in step s2 is 20～35min, preferably 25～30min.At this Under the conditions of boiling water bath, the extraction of humus is more complete.
The method of the invention, step s3 adopts hydrochloric acid to adjust the ph of described second humus solution and the second blank sample Value, hydrochloric acid preferred concentration used is the hydrochloric acid solution of 6mol/l.
The method of the invention, the concentration of sodium hydroxide solution described in step s3 is 0.1～0.15mol/l；And/or, institute The concentration stating ferrous sulfate standard solution is 0.15～0.25mol/l.
As a kind of preferred version, the method for the invention comprises the steps:
S1, sludge composting is air-dried and after pulverizing, obtains sludge composting sample, measure and obtain described sludge composting sample Moisture content ω；
S2, take sludge composting sample described in 5g, add the leaching that 50～70ml contains sodium hydroxide and sodium pyrophosphate wherein Extract, carries out boiling water bath to humus extraction completely, adds deionized water and be settled to 200ml, be then centrifuged for, institute after cooling after mixing Obtain supernatant and be humus solution, volume is v2, it is taken out volume and be respectively v3And v4The first humus solution and second Humus solution, in described lixiviating solution, the molar concentration of sodium hydroxide and sodium pyrophosphate is 0.1mol/l；Separately take the institute of equivalent State lixiviating solution and carry out described boiling water bath, be then taken out volume and be respectively v3And v4The first blank sample and the second blank examination Sample；
S3, with hydrochloric acid, the ph value of described second humus solution is adjusted to 1～2, is centrifuged after standing 10～12h, will Described precipitation out, is then added sodium hydroxide solution to be completely dissolved to precipitation, obtains by centrifugation gained precipitate and separate after washing It is v to volume5Humic Acid Solution；Separately the ph value of described second blank sample is adjusted to 1～2, and is taken out volume for v5 The 3rd blank sample；
S4, from described Humic Acid Solution take out volume be v3' the first Humic Acid Solution, from described 3rd blank sample Middle taking-up volume is v3' the 4th blank sample, molten to described first humus solution, the first blank sample, the first humic acid Each add the mixed liquor of potassium bichromate solution and concentrated sulphuric acid in liquid and the 4th blank sample, carry out boiling water bath after mixing extremely described First humus solution, the first Humic Acid Solution reaction completely, respectively obtain the first sample, blank sample one, second after cooling Sample and blank sample two；
S5, the respective instruction adding equivalent in described first sample, blank sample one, the second sample and blank sample two Agent, respectively obtains the first titration sample, blank titration sample one, second titration sample and blank titration sample two, with concentration is First titration sample, blank titration sample one, second titration examination described in the ferrous sulfate standard solution stepwise titration of 0.2mol/l Sample and blank titration sample two start the predetermined color being presented during excess to described ferrous sulfate standard solution, then press described Formula calculates the content of the humus united hs-c, humic acid carbon ha-c and fulvic acid carbon fa-c in described sludge composting sample.
The method of the invention, described in step s2, the mode of centrifugation is preferably: under the centrifugal rotational speed of 4000r/min, from Heart 10min.
The method of the invention, the concentration of described potassium bichromate solution is 0.1～0.15mol/l.
The method of the invention, described indicator is mixed by ferrous sulfate and 1,10- phenanthroline；With or, described pre- It is brick-red for determining color；Preferably, described indicator is by 0.695g ferrous sulfate and 1.485g1, and 10- phenanthroline is dissolved in Prepare in 100ml deionized water.
The technique scheme of the present invention has the advantages that
1st, the method for the invention significantly increases the extracted amount of humus, and humus units increased in production reaches on 40%, overcomes What traditional extraction process existed extract not exclusively and extracting cycle length shortcoming, extraction process is simple and efficient, digestion agent used Species is few, low cost, extraction process safety.
2nd, the method for the invention is due to significantly increasing the extracted amount of humus, thus the humus content recording is more Press close to actual humus content in compost；Accordingly, with respect to existing determination techniques, the method for the present invention improves rotten in compost Grow the accuracy of measurement of matter, the selection hence for compost and using having important indicative significance.
3rd, the computing formula measuring for humus that the method for the invention provides, has filled up both at home and abroad in this field Blank；Assay method is simple and efficient, and in whole measurement process, the requirement to instrument and equipment is low, and agents useful for same species is few, becomes This is low.
Specific embodiment
With reference to embodiment, embodiments of the present invention are described in further detail.Following examples are used for illustrating this Invention, but can not be used for limiting the scope of the present invention.Described in following examples and comparative example, sludge composting is both from Sewage Mud is formed with carbon-nitrogen ratio 15:1 mixed stack with straw；Other reagent be city available from；Lixiviating solution described in following examples It is the aqueous solution of sodium hydroxide and sodium pyrophosphate, and the molar concentration of wherein sodium hydroxide and sodium pyrophosphate is 0.1mol/ l.
Embodiment 1
Present embodiments provide a kind of method measuring humus and its constituent content in sludge composting, it includes following step Rapid:
S1, sludge composting is air-dried and pulverizes, after crossing 100 mesh sieves, obtain sludge composting sample, then measure described mud The moisture content ω of compost sample；
S2, take sludge composting sample described in 5g step s1, add 50ml lixiviating solution wherein, after mixing, carry out 30min's Boiling water bath, adds deionized water and is settled to 200ml after cooling, be then centrifuged 10min, gained under the centrifugal rotational speed of 4000r/min Supernatant is humus solution, and volume is v2, it is taken out volume and be respectively v3And v4The first humus solution and second rotten Grow matter solution；The described lixiviating solution separately taking equivalent carries out described boiling water bath, is then taken out volume and is respectively v3And v4First Blank sample and the second blank sample；
S3, with hydrochloric acid, the ph value of described second humus solution is adjusted to 1, is centrifuged after standing 10～12h, will be centrifuged Gained precipitation (predominantly humic acid) is separated, and then described precipitation is added sodium hydroxide solution after washing to having precipitated CL, obtains volume and is v5Humic Acid Solution；Separately the ph value of described second blank sample is adjusted to 1～2, and therefrom take Going out volume is v5The 3rd blank sample；
S4, from described Humic Acid Solution take out volume be v3' the first Humic Acid Solution, from described 3rd blank sample Middle taking-up volume is v3' the 4th blank sample, molten to described first humus solution, the first blank sample, the first humic acid Each add, in liquid and the 4th blank sample, the potassium bichromate solution 10ml and concentrated sulphuric acid 15ml that concentration is 0.13mol/l, mix Carry out boiling water bath afterwards respectively to react completely to described first humus solution and the first Humic Acid Solution, after cooling, respectively obtain the One sample blank sample one, the second sample and blank sample two；
S5, the respective instruction adding equivalent in described first sample, blank sample one, the second sample and blank sample two (this indicator is to be dissolved in 100ml deionized water by 0.695g ferrous sulfate and 1.485g1,10- phenanthroline preparing for agent ), respectively obtain the first titration sample, blank titration sample one, second titration sample and blank titration sample two, with concentration be First titration sample, blank titration sample one, second titration examination described in the ferrous sulfate standard solution stepwise titration of 0.2mol/l Sample and blank titration sample two start the predetermined color being presented during excess to described ferrous sulfate standard solution, then press following The content of humus united hs-c, humic acid carbon ha-c and fulvic acid carbon fa-c in the formula described sludge composting sample of calculating:
h s - c = c ( v 0 - v 1 ) × m m × ( 1 - ω ) × v 2 v 3 × 1000 h a - c = c ( v 0 - v 1 ′ ) × m m × ( 1 - ω ) × v 2 v 3 × v 5 v 3 ′ × 1000 f a - c = ( h s - c ) - ( h a - c ) ,
In formula,
Hs-c: humus united, unit g/kg (the i.e. quality g) of the humus united contained by sludge composting sample described in every kg；
Ha-c: humic acid carbon, unit g/kg (the i.e. quality g) of the humic acid carbon contained by sludge composting sample described in every kg；
Fa-c: fulvic acid carbon, unit g/kg (the i.e. quality g) of the fulvic acid carbon contained by sludge composting sample described in every kg；
v0: the volume of the ferrous sulfate standard solution that titration blank titration sample one is consumed, units/ml；
v0': the volume of the ferrous sulfate standard solution that titration blank titration sample two is consumed, units/ml；
v1: the volume of the ferrous sulfate standard solution that titration the first titration sample is consumed, units/ml；
v1': the volume of the ferrous sulfate standard solution that titration the second titration sample is consumed, units/ml；
M: the quality of sludge composting sample, unit g described in step s2；
C: the concentration of ferrous sulfate standard solution, unit mol/l；
The molal weight of m:1/4 carbon atom, i.e. 3g/mol.
In the present embodiment, c is 0.20mol/l, v0For 39.78ml, v1For 19.65ml, m is 5.00g, and ω is 16.44%, v2For 200.00ml, v3For 5.00ml, v0' it is 39.73ml, v1' it is 14.38ml, v4For 50ml, v5For 50ml, v3' it is 10ml, Above-mentioned parameter substitution formula is obtained final product the content of humus united hs-c, fulvic acid carbon fa-c and humic acid carbon ha-c.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, differs only in:
The time of boiling water bath described in step s2 is 25min；
The volume of described first humus solution is 8ml；
In step s3, the ph value of described second humus solution is adjusted to 2.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, differs only in:
The time of boiling water bath described in step s2 is 20min；
The volume of described first humus solution is 8ml；
The volume of described first Humic Acid Solution is 15ml.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, differs only in:
The amount of described lixiviating solution is 70ml；
The time of boiling water bath described in step s2 is 25min；
In step s3, the ph value of described first humus solution is adjusted to 2；
The volume of described first Humic Acid Solution is 15ml.
Embodiment 5
The present embodiment is substantially the same manner as Example 1, differs only in:
The amount of described lixiviating solution is 80ml；
The time of boiling water bath described in step s2 is 35min；
The volume of described first Humic Acid Solution is 15ml.
Embodiment 6
The present embodiment is substantially the same manner as Example 1, differs only in:
The amount of described lixiviating solution is 70ml；
The volume of described first humus solution is 8ml；
The volume of described first Humic Acid Solution is 15ml；
In step s3, the ph value of described first humus solution is adjusted to 3.
Comparative example
This comparative example is substantially the same manner as Example 1, differs only in step s2:
Step s2 of this comparative example, particularly as follows: taking sludge composting sample described in 5g step s1, adds 70ml concentration wherein Sodium hydroxide solution for 0.1mol/l, stirs, and adds deionized water and be settled to 200ml, Ran Hou after vibration 2h under room temperature It is centrifuged 10min, gained supernatant is humus solution, volume is v under the centrifugal rotational speed of 4000r/min2, it is taken out volume It is respectively v3And v4The first humus solution and the second humus solution；The described lixiviating solution separately taking equivalent carries out described boiling water Bath, is then taken out volume and is respectively v3And v4The first blank sample and the second blank sample.
The result that above example and comparative example are measured is as shown in table 1:
Table 1: the content of humus and its component in sludge composting
Table 1 shows, compared with traditional sodium hydroxide mechanical shaking extraction method, humus contain embodiment of the present invention methods described Amount improves 27.9%～44.8%, obvious effect of increasing production, thus the humus content recording is closer to actual corruption in compost Grow matter content, this also indirect proof embodiment of the present invention methods described improve the accuracy of measurement of humus in compost, from And the selection for compost and using having important directive significance.
With reference to embodiment 7, Accuracy Verification is carried out to the computing formula of the present invention.
Embodiment 7
Present embodiments provide the assay method of humus and its constituent content in a kind of sludge composting, it includes walking as follows Rapid:
S1 is identical with the s1 of the embodiment of the present invention 1；
S2 is identical with the s2 of the embodiment of the present invention 1；
S3 is identical with the s3 of the embodiment of the present invention 1；
S4, using U.S.'s sievers innovox total organic carbon analyzer molten to the first humus solution, the first humic acid Organic carbon content in liquid is measured.
After measured, humus united content is 117.9g/kg, and humic acid carbon content is 72.92g/kg.With survey of the present invention The method of determining is compared, and two methods gained humus and its constituent content are more or less the same.Therefore, assay method of the present invention is basic On can accurately reflect humus and its constituent content.Meanwhile, sievers innovox total organic carbon analyzer measures required one-tenth This is higher, and often one sample of mensure is (parallel containing 3) needs 240 yuan.Therefore, the assay method of the present invention be a kind of economical, effectively, Accurately assay method.
Embodiments of the invention in order to example and description for the sake of and be given, and be not exhaustively or by this Bright it is limited to disclosed form.A lot of modification changes are obvious for the ordinary skill in the art.Select It is in order to the principle of the present invention and practical application are more preferably described with description embodiment, and enable those of ordinary skill in the art Enough understand the present invention thus design is suitable to the various embodiments with various modifications of special-purpose.

Claims (10)

1. a kind of method measuring humus and its constituent content in sludge composting is it is characterised in that comprise the steps:
S1, will sludge composting air-dry after obtain sludge composting sample, measure and obtain the moisture content ω of described sludge composting sample；
S2, the described sludge composting sample taking quality to be m, are added thereto to the lixiviating solution containing sodium hydroxide and sodium pyrophosphate, Carry out boiling water bath after mixing to humus extraction completely, be centrifuged after cooling, gained supernatant is humus solution, volume is v2, it is taken out volume and be respectively v3And v4The first humus solution and the second humus solution；Separately take the described extraction of equivalent Liquid carries out described boiling water bath, is then taken out volume and is respectively v3And v4The first blank sample and the second blank sample；
S3, the ph value of described second humus solution is adjusted to 1～2, is centrifuged after standing, by gained precipitate and separate out, then Described precipitation is added sodium hydroxide solution to be completely dissolved to precipitation after washing, obtaining volume is v5Humic Acid Solution；Separately The ph value of described second blank sample is adjusted to 1～2, and is taken out volume for v5The 3rd blank sample；
S4, from described Humic Acid Solution take out volume be v3' the first Humic Acid Solution, take from described 3rd blank sample Going out volume is v3' the 4th blank sample, to described first humus solution, the first blank sample, the first Humic Acid Solution and Each add the mixed liquor of potassium bichromate solution and concentrated sulphuric acid in 4th blank sample, after mixing, carry out boiling water bath extremely described first Humus solution, the first Humic Acid Solution reaction completely, respectively obtain the first sample, blank sample one, the second sample after cooling With blank sample two；
S5, each add the indicator of equivalent in described first sample, blank sample one, the second sample and blank sample two, Respectively obtain the first titration sample, blank titration sample one, second titration sample and blank titration sample two, be c's with concentration First titration sample, blank titration sample one, second titration sample and blank described in ferrous sulfate standard solution stepwise titration Determine the predetermined color that sample two starts to be presented during excess to described ferrous sulfate standard solution, then institute according to the following formula State the content of the humus united hs-c, humic acid carbon ha-c and fulvic acid carbon fa-c in sludge composting sample:
h s - c = c ( v 0 - v 1 ) × m m × ( 1 - ω ) × v 2 v 3 × 1000
h a - c = c ( v 0 - v 1 ′ ) × m m × ( 1 - ω ) × v 2 v 4 × v 5 v 3 ′ × 1000 ,
Fa-c=(hs-c)-(ha-c)
In formula,
Hs-c: humus united, unit g/kg；
Ha-c: humic acid carbon, unit g/kg；
Fa-c: fulvic acid carbon, unit g/kg；
v0: the volume of the ferrous sulfate standard solution that titration blank titration sample one is consumed, units/ml；
v0': the volume of the ferrous sulfate standard solution that titration blank titration sample two is consumed, units/ml；
v1: the volume of the ferrous sulfate standard solution that titration the first titration sample is consumed, units/ml；
v1': the volume of the ferrous sulfate standard solution that titration the second titration sample is consumed, units/ml；
M: the quality of sludge composting sample, unit g described in step s2；
C: the concentration of ferrous sulfate standard solution, unit mol/l；
The molal weight of m:1/4 carbon atom.
2. according to claim 1 method it is characterised in that in described lixiviating solution sodium hydroxide and sodium pyrophosphate mole dense Degree is equal.
3. according to claim 2 method it is characterised in that in described lixiviating solution sodium hydroxide and sodium pyrophosphate mole dense Degree is 0.1mol/l.
4. method it is characterised in that in step s2, adds institute in sludge composting sample described in every 1g according to claim 3 The amount stating lixiviating solution is 10～14ml.
5. according to Claims 1 to 4 any one methods described it is characterised in that step s3 adopts hydrochloric acid to adjust described second corruption Grow the ph value of matter solution and the second blank sample.
6. according to Claims 1 to 5 any one methods described it is characterised in that the concentration of sodium hydroxide solution described in step s3 For 0.1～0.15mol/l；And/or, the concentration of described ferrous sulfate standard solution is 0.15～0.25mol/l.
7. according to claim 1～6 any one methods described it is characterised in that comprising the steps:
S1, sludge composting is air-dried and after pulverizing, obtains sludge composting sample, measure and obtain containing of described sludge composting sample Water rate ω；
S2, take sludge composting sample described in 5g, add the lixiviating solution that 50～70ml contains sodium hydroxide and sodium pyrophosphate wherein, Carry out boiling water bath after mixing to humus extraction completely, add deionized water after cooling and be settled to 200ml, be then centrifuged for, on gained Clear liquid is humus solution, and volume is v2, it is taken out volume and be respectively v3And v4The first humus solution and the second humic Matter solution, in described lixiviating solution, the molar concentration of sodium hydroxide and sodium pyrophosphate is 0.1mol/l；Separately take the described leaching of equivalent Extract carries out described boiling water bath, is then taken out volume and is respectively v3And v4The first blank sample and the second blank sample；
S3, with hydrochloric acid, the ph value of described second humus solution is adjusted to 1～2, is centrifuged after standing 10～12h, will be centrifuged Described precipitation out, is then added sodium hydroxide solution to be completely dissolved to precipitation, obtains body by gained precipitate and separate after washing Amass and be v5Humic Acid Solution；Separately the ph value of described second blank sample is adjusted to 1～2, and is taken out volume for v5? Three blank samples；
S4, from described Humic Acid Solution take out volume be v3' the first Humic Acid Solution, take from described 3rd blank sample Going out volume is v3' the 4th blank sample, to described first humus solution, the first blank sample, the first Humic Acid Solution and Each add the mixed liquor of potassium bichromate solution and concentrated sulphuric acid in 4th blank sample, after mixing, carry out boiling water bath extremely described first Humus solution, the first Humic Acid Solution reaction completely, respectively obtain the first sample, blank sample one, the second sample after cooling With blank sample two；
S5, each add the indicator of equivalent in described first sample, blank sample one, the second sample and blank sample two, Respectively obtain the first titration sample, blank titration sample one, second titration sample and blank titration sample two, with concentration be First titration sample, blank titration sample one, second titration examination described in the ferrous sulfate standard solution stepwise titration of 0.2mol/l Sample and blank titration sample two start the predetermined color being presented during excess to described ferrous sulfate standard solution, then press described Formula calculates the content of the humus united hs-c, humic acid carbon ha-c and fulvic acid carbon fa-c in described sludge composting sample.
8. according to claim 1～7 any one methods described it is characterised in that the concentration of described potassium bichromate solution be 0.1～ 0.15mol/l.
9. according to claim 1～8 any one methods described it is characterised in that described indicator is luxuriant and rich with fragrance by ferrous sulfate and 1,10- Sieve quinoline mixes；With or, described predetermined color be brick-red.
10. according to claim 9 method it is characterised in that described indicator be by 0.695g ferrous sulfate and 1.485g1,10- phenanthroline is dissolved in and preparing in 100ml deionized water.
CN201610885346.3A 2016-10-10 2016-10-10 Method for determining humus and component contents thereof in sludge compost Pending CN106370778A (en)

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