CN106248467A - A kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea - Google Patents
A kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea Download PDFInfo
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- CN106248467A CN106248467A CN201610809397.8A CN201610809397A CN106248467A CN 106248467 A CN106248467 A CN 106248467A CN 201610809397 A CN201610809397 A CN 201610809397A CN 106248467 A CN106248467 A CN 106248467A
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- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 238000000108 ultra-filtration Methods 0.000 title claims abstract description 62
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000004202 carbamide Substances 0.000 title claims abstract description 25
- 239000004021 humic acid Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 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 18
- 238000002203 pretreatment Methods 0.000 title claims abstract description 17
- 239000000706 filtrate Substances 0.000 claims abstract description 47
- 238000002835 absorbance Methods 0.000 claims abstract description 33
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 claims abstract description 17
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 claims abstract description 17
- PUKLDDOGISCFCP-JSQCKWNTSA-N 21-Deoxycortisone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)C)(O)[C@@]1(C)CC2=O PUKLDDOGISCFCP-JSQCKWNTSA-N 0.000 claims abstract description 16
- FCYKAQOGGFGCMD-UHFFFAOYSA-N Fulvic acid Natural products O1C2=CC(O)=C(O)C(C(O)=O)=C2C(=O)C2=C1CC(C)(O)OC2 FCYKAQOGGFGCMD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012670 alkaline solution Substances 0.000 claims abstract description 16
- 239000002509 fulvic acid Substances 0.000 claims abstract description 16
- 229940095100 fulvic acid Drugs 0.000 claims abstract description 16
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 10
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 238000011088 calibration curve Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000012417 linear regression Methods 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000012086 standard solution Substances 0.000 claims description 12
- 238000004090 dissolution Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000012088 reference solution Substances 0.000 claims description 6
- 238000002798 spectrophotometry method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 239000010949 copper Substances 0.000 claims 1
- 239000011593 sulfur Substances 0.000 claims 1
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 8
- 230000004044 response Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 235000013877 carbamide Nutrition 0.000 description 21
- 239000003337 fertilizer Substances 0.000 description 6
- 238000007654 immersion Methods 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 238000012271 agricultural production Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- VZOPRCCTKLAGPN-UHFFFAOYSA-L potassium;sodium;2,3-dihydroxybutanedioate;tetrahydrate Chemical class O.O.O.O.[Na+].[K+].[O-]C(=O)C(O)C(O)C([O-])=O VZOPRCCTKLAGPN-UHFFFAOYSA-L 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- -1 copper complex salt Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to a kind of ultrafiltration pre-treatment and measure the method for Biuret Content in humic acid urea；Use ultrafiltration pre-treatment sample, fulvic acid be trapped in ultrafiltration cup, collect filtrate, utilize biuret copper sulfate, sodium potassium tartrate tetrahydrate alkaline solution in generate purple coordination compound, calculate the content of biuret finally according to the size of absorbance and Working calibration curve；There is the advantage that method is simple, testing cost is low, the cycle is short, precision is high, the response rate is good.
Description
Technical field
The invention belongs to measure Biuret Content technical field, be specifically related to a kind of ultrafiltration pre-treatment and measure humic acid urea
The method of middle Biuret Content.
Background technology
Along with industrialization and the change of Fertilization Structure of agricultural production, in soil, organic content is in reducing trend,
Soil quality declines year by year, and the method the most easily changing this situation generally acknowledged is to be directly added into corruption in the chemical fertilizer used to plant
Acid, humic acids has the effect of improvement soil quality, the most also has promotion crop growth, improves the work of crop yield
With.Humic acids is according to its physicochemical characteristics and has divided the big I of amount to be divided into humic acid, ulmic acid and fulvic acid.Humic acid was both
Being also insoluble in alkali insoluble in acid, molecular weight is maximum, and character is close to coal dust, and it is to agricultural production and the improvement to soil quality
Act on minimum；Fulvic acid molecular weight minimum is not only dissolved in acid but also be dissolved in alkali, and it is to the facilitation of crop growth and to soil
Improving effect is best；Ulmic acid is the most therebetween.
Humic acids adding the method in carbamide and divides two kinds, one is by finished urea and humic acids premixing in proportion
After, reheating and dissolve pelletize again, another kind is to be sprayed by humic acids in vacuum evaporation drying process in urea production process
Enter direct pelletize.Former is owing to again dissolving carbamide, and carbamide can generate substantial amounts of biuret in the blown state；And latter
Method is without re-melting, and its Biuret Content is low.Due to biuret crops can be damaged when concentration height, the underproduction even
Total crop failure, so one of biuret topmost quality control index that is chemical fertilizer.
Do not retrieve at present about containing the assay method of Biuret Content in humic acid urea and national and foreign standards, retrieving
Relevant criterion mainly have: " the assay method part 2 of carbamide: Biuret Content spectrophotography " (GB/T2441.2-
2010)；" mensuration of Biuret Content in complex fertilizer (compound fertilizer) " (GB/T22924-2008)；" import chemical fertilizer inspection party
The mensuration of method Biuret Content ".
The method of biuret in chemical fertilizer that measures in relevant criterion has two kinds, and the first is high performance liquid chromatography, the second
It it is copper complex salt light photometry.The first instrument is expensive, is desirable that equipment configuration, reagent, consumptive material and operator very
Sternly；The second is due to the fulvic acid severe jamming measurement result in humic acid urea, it is impossible to meet testing requirement.The most at home
Foreign language is presented and also be can not find out about containing the detection method of Biuret Content in humic acid urea.
Summary of the invention
It is an object of the invention to overcome defect of the prior art, and provide that a kind of method is simple, testing cost is low, all
A kind of ultrafiltration pre-treatment that phase is short, precision is high, the response rate is good measures the method for Biuret Content in humic acid urea.
The object of the present invention is achieved like this: use ultrafiltration pre-treatment sample, fulvic acid is trapped in ultrafiltration cup,
Collect filtrate, utilize biuret copper sulfate, sodium potassium tartrate tetrahydrate alkaline solution in generate purple coordination compound, finally according to extinction
The size of degree and Working calibration curve calculate the content of biuret；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 200mL volumetric flasks add concentration be the biuret standard solution 0mL of 4mg/mL, 2.5mL,
5mL, 10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 20mg, 40mg, 80mg, 120mg,
160mg、200mg、240mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 20 |
| 3 | 5.00 | 40 |
| 4 | 10.0 | 80 |
| 5 | 15.0 | 120 |
| 6 | 20.0 | 160 |
| 7 | 25.0 | 200 |
| 8 | 30.0 | 240 |
(1.2) in 8 volumetric flasks described in step (1.1), it is separately added into fulvic acid aqueous solution 10～30mL, and uses
1mol/L sulfuric acid solution regulation solution pH value to 4.5, shake up after being diluted with water to 200mL graduation mark, put it into complete from
The dynamic vertical autoclave sterilizer of digital display keeps at a temperature of 110 DEG C～120 DEG C 3min～7min, takes out and be cooled to room temperature,
Pour into the most successively in the ultrafiltration cup having installed 3000Da ultrafilter membrane；
(1.3) being passed through nitrogen in the ultrafiltration cup of step (1.2), regulation ultrafiltration cup pressure is to open after 0.2MPa～0.4MPa
Begin to collect in the conical flask that filtrate is dried to 100mL, discard initial filtrate 20mL, pipette 50.00mL filtrate the most respectively and place
In 8 volumetric flasks, the most backward 8 volumetric flasks are sequentially added into 15～25mL sodium potassium tartrate tetrahydrate alkaline solutions and 15～
25mL copper-bath, carries out constant volume；
(1.4) fully shake up after constant volume, 8 volumetric flasks described in above-mentioned steps (1.3) are immersed the constant temperature of 30 ± 5 DEG C
The heating 10～30min when shake in water-bath；
(1.5) using solution that biuret is zero as reference solution, at wavelength 550nm, spectrophotometric determination mark is used
The accurate absorbance than solution, and record data；
(1.6) with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate draws standard curve, and
Obtaining equation of linear regression, equation is: y=0.0028x+0.0029, coefficient R2=0.9995；
(2) mensuration of Biuret Content
(2.1) sample 15g～25g is weighed, in 200mL volumetric flask, accurately to 0.0002g；(with biuret-containing 80mg～
200mg is advisable)
(2.2) with after water dissolution shake well, adjust the pH to 4.5 of solution with sulfuric acid solution, and be diluted with water to 200mL
Shake up after graduation mark；Pour in ready 3000Da ultrafilter membrane ultrafiltration cup；
(2.3) be passed through in the ultrafiltration cup described in step (2.2) nitrogen regulation ultrafiltration cup pressure be 0.2MPa～
Start after 0.4MPa to collect filtrate, in the conical flask that filtrate collection to 100mL is dried, discard initial filtrate 20mL, accurately move
Take 50.00mL filtrate in 100mL volumetric flask, in volumetric flask, be then sequentially added into 15～25mL sodium potassium tartrate tetrahydrates alkalescence
Solution and 15～25mL copper-baths, shake up；
(2.4) shake up, then appearance after being diluted with water to 100mL graduation mark in the volumetric flask described in step (2.3)
The heating 10～30min when shake in the water bath with thermostatic control of measuring bottle immersion 30 ± 5 DEG C；With spectrophotometer at wavelength
Survey its absorbance at 550nm, and record data；
(2.5) standard curve that the absorbance data of record in above-mentioned steps (2.4) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or by equation of linear regression is obtained the quality of biuret, i.e. can get the contracting two in sample
Urea content.
In described step (2.1) interior 15g～25g sample, the content of biuret is 80mg～200mg.
The present invention has the advantage that method is simple, testing cost is low, the cycle is short, precision is high, the response rate is good.
Accompanying drawing explanation
Fig. 1 is the standard working curve of the biuret of the embodiment of the present invention one.
Fig. 2 is the standard working curve of the biuret of the embodiment of the present invention two.
Fig. 3 is the standard working curve of the biuret of the embodiment of the present invention three.
Detailed description of the invention
The present invention is that a kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea, uses ultrafiltration pre-treatment
Sample, is trapped in fulvic acid in ultrafiltration cup, collects filtrate, utilizes biuret at copper sulfate, the alkaline solution of sodium potassium tartrate tetrahydrate
Middle generation purple coordination compound, finally according to size and the content of Working calibration curve calculating biuret of absorbance；Concrete steps
As follows:
(1) drafting of standard curve:
(1.1) in 8 200mL volumetric flasks add concentration be the biuret standard solution 0mL of 4mg/mL, 2.5mL,
5mL, 10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 20mg, 40mg, 80mg, 120mg,
160mg、200mg、240mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 20 |
| 3 | 5.00 | 40 |
| 4 | 10.0 | 80 |
| 5 | 15.0 | 120 |
| 6 | 20.0 | 160 |
| 7 | 25.0 | 200 |
| 8 | 30.0 | 240 |
(1.2) in 8 volumetric flasks described in step (1.1), it is separately added into fulvic acid aqueous solution 10～30mL, and uses
1mol/L sulfuric acid solution regulation solution pH value to 4.5, shake up after being diluted with water to 200mL graduation mark, put it into complete from
The dynamic vertical autoclave sterilizer of digital display keeps at a temperature of 110 DEG C～120 DEG C 3min～7min, takes out and be cooled to room temperature,
Pour into the most successively in the ultrafiltration cup having installed 3000Da ultrafilter membrane；
(1.3) being passed through nitrogen in the ultrafiltration cup of step (1.2), regulation ultrafiltration cup pressure is to open after 0.2MPa～0.4MPa
Begin to collect in the conical flask that filtrate is dried to 100mL, discard initial filtrate 20mL, pipette 50.00mL filtrate the most respectively and place
In 8 volumetric flasks, the most backward 8 volumetric flasks are sequentially added into 15～25mL sodium potassium tartrate tetrahydrate alkaline solutions and 15～
25mL copper-bath, carries out constant volume；
(1.4) fully shake up after constant volume, 8 volumetric flasks described in above-mentioned steps (1.3) are immersed the constant temperature of 30 ± 5 DEG C
The heating 10～30min when shake in water-bath；
(1.5) using solution that biuret is zero as reference solution, at wavelength 550nm, spectrophotometric determination mark is used
The accurate absorbance than solution, and record data；
(1.6) with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate draws standard curve, and
Obtaining equation of linear regression, equation is: y=0.0028x+0.0029, coefficient R2=0.9995；
(2) mensuration of Biuret Content
(2.1) sample 15g～25g is weighed, in 200mL volumetric flask, accurately to 0.0002g；(with biuret-containing 80mg～
200mg is advisable)
(2.2) with after water dissolution shake well, adjust the pH to 4.5 of solution with sulfuric acid solution, and be diluted with water to 200mL
Shake up after graduation mark；Pour in ready 3000Da ultrafilter membrane ultrafiltration cup；
(2.3) be passed through in the ultrafiltration cup described in step (2.2) nitrogen regulation ultrafiltration cup pressure be 0.2MPa～
Start after 0.4MPa to collect filtrate, in the conical flask that filtrate collection to 100mL is dried, discard initial filtrate 20mL, accurately move
Take 50.00mL filtrate in 100mL volumetric flask, in volumetric flask, be then sequentially added into 15～25mL sodium potassium tartrate tetrahydrates alkalescence
Solution and 15～25mL copper-baths, shake up；
(2.4) shake up, then appearance after being diluted with water to 100mL graduation mark in the volumetric flask described in step (2.3)
The heating 10～30min when shake in the water bath with thermostatic control of measuring bottle immersion 30 ± 5 DEG C；With spectrophotometer at wavelength
Survey its absorbance at 550nm, and record data；
(2.5) standard curve that the absorbance data of record in above-mentioned steps (2.4) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or by equation of linear regression is obtained the quality of biuret, i.e. can get the contracting two in sample
Urea content.
In described step (2.1) interior 15g～25g sample, the content of biuret is 80mg～200mg.
For the more detailed explanation present invention, in conjunction with embodiment, the present invention is further elaborated.Specific embodiment
As follows:
Embodiment one:
A kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea, uses ultrafiltration pre-treatment sample, will
Fulvic acid is trapped in ultrafiltration cup, collect filtrate, utilize biuret copper sulfate, sodium potassium tartrate tetrahydrate alkaline solution in generate purple
Color coordination compound, finally according to size and the content of Working calibration curve calculating biuret of absorbance；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 200mL volumetric flasks add concentration be the biuret standard solution 0mL of 4mg/mL, 2.5mL,
5mL, 10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 20mg, 40mg, 80mg, 120mg,
160mg、200mg、240mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 20 |
| 3 | 5.00 | 40 |
| 4 | 10.0 | 80 |
| 5 | 15.0 | 120 |
| 6 | 20.0 | 160 |
| 7 | 25.0 | 200 |
| 8 | 30.0 | 240 |
(1.2) in 8 volumetric flasks described in step (1.1), it is separately added into fulvic acid aqueous solution 10mL, and uses 1mol/
The pH value of the sulfuric acid solution regulation solution of L, to 4.5, shakes up after being diluted with water to 200mL graduation mark, puts it into full-automatic digital display
Vertical autoclave sterilizer keeps at a temperature of 110 DEG C 3min, takes out and be cooled to room temperature, pour into the most successively and install
In the ultrafiltration cup of 3000Da ultrafilter membrane；
(1.3) in the ultrafiltration cup of step (1.2), be passed through nitrogen, regulation ultrafiltration cup pressure be 0.2Mpa, after start collect
In the conical flask that filtrate is dried to 100mL, discard initial filtrate 20mL, pipette 50.00mL filtrate the most respectively and be positioned over 8 appearances
In measuring bottle, the most backward 8 volumetric flasks are sequentially added into 15mL sodium potassium tartrate tetrahydrate alkaline solution and 15mL copper-bath, enter
Row constant volume；
(1.4) fully shake up after constant volume, 8 volumetric flasks described in above-mentioned steps (1.3) are immersed the thermostatted water of 25 DEG C
Bath heats 10min when shake；
(1.5) using solution that biuret is zero as reference solution, at wavelength 550nm, spectrophotometric determination mark is used
The accurate absorbance than solution, and record data；
| Corresponding amount/the mg of biuret | Absorbance/A |
| 0 | 0.000 |
| 20 | 0.052 |
| 40 | 0.115 |
| 80 | 0.227 |
| 120 | 0.324 |
| 160 | 0.446 |
| 200 | 0.548 |
| 240 | 0.660 |
(1.6) with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate draws standard curve, and
Obtaining equation of linear regression, equation is: y=0.0027x+0.0013, coefficient R2=0.9996；
(2) mensuration of Biuret Content
(2.1) sample 15.0001g is weighed, in 200mL volumetric flask；
(2.2) with after water dissolution shake well, adjust the pH to 4.5 of solution with sulfuric acid solution, and be diluted with water to 200mL
Shake up after graduation mark；Pour in ready 3000Da ultrafilter membrane ultrafiltration cup；
(2.3) being passed through nitrogen regulation ultrafiltration cup pressure in the ultrafiltration cup described in step (2.2) is beginning after 0.2MPa
Collect filtrate, in the conical flask that filtrate collection to 100mL is dried, discard initial filtrate 20mL, accurately pipette 50.00mL filtrate
In 100mL volumetric flask, in volumetric flask, then it is sequentially added into 15mL sodium potassium tartrate tetrahydrate alkaline solution and 15mL copper sulfate
Solution, shakes up；
(2.4) shake up, then appearance after being diluted with water to 100mL graduation mark in the volumetric flask described in step (2.3)
The water bath with thermostatic control of measuring bottle immersion 25 DEG C heats 10min when shake；At wavelength 550nm, it is surveyed with spectrophotometer
Absorbance is 0.508；
(2.5) standard curve that the absorbance data of record in above-mentioned steps (2.4) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or by equation of linear regression is obtained quality 188mg of biuret, i.e. can get in sample
Biuret Content 1.25%.
Embodiment two
A kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea, uses ultrafiltration pre-treatment sample, will
Fulvic acid is trapped in ultrafiltration cup, collect filtrate, utilize biuret copper sulfate, sodium potassium tartrate tetrahydrate alkaline solution in generate purple
Color coordination compound, finally according to size and the content of Working calibration curve calculating biuret of absorbance；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 200mL volumetric flasks add concentration be the biuret standard solution 0mL of 4mg/mL, 2.5mL,
5mL, 10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 20mg, 40mg, 80mg, 120mg,
160mg、200mg、240mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 20 |
| 3 | 5.00 | 40 |
| 4 | 10.0 | 80 |
| 5 | 15.0 | 120 |
| 6 | 20.0 | 160 |
| 7 | 25.0 | 200 |
| 8 | 30.0 | 240 |
(1.2) in 8 volumetric flasks described in step (1.1), it is separately added into fulvic acid aqueous solution 20mL, and uses 1mol/
The pH value of the sulfuric acid solution regulation solution of L, to 4.5, shakes up after being diluted with water to 200mL graduation mark, puts it into full-automatic digital display
Vertical autoclave sterilizer keeps at a temperature of 115 DEG C 5min, takes out and be cooled to room temperature, pour into the most successively and install
In the ultrafiltration cup of 3000Da ultrafilter membrane；
(1.3) being passed through nitrogen in the ultrafiltration cup of step (1.2), regulation ultrafiltration cup pressure is to start after 0.3MPa to collect filter
In the conical flask that liquid is dried to 100mL, discard initial filtrate 20mL, pipette 50.00mL filtrate the most respectively and be positioned over 8 capacity
In Ping, the most backward 8 volumetric flasks are sequentially added into 20mL sodium potassium tartrate tetrahydrate alkaline solution and 20mL copper-bath, carry out
Constant volume；
(1.4) fully shake up after constant volume, 8 volumetric flasks described in above-mentioned steps (1.3) are immersed the thermostatted water of 30 DEG C
Bath heats 20min when shake；
(1.5) using solution that biuret is zero as reference solution, at wavelength 550nm, spectrophotometric determination mark is used
The accurate absorbance than solution, and record data；
| Corresponding amount/the mg of biuret | Absorbance/A |
| 0 | 0.000 |
| 20 | 0.053 |
| 40 | 0.117 |
| 80 | 0.235 |
| 120 | 0.332 |
| 160 | 0.447 |
| 200 | 0.551 |
| 240 | 0.669 |
(1.6) with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate draws standard curve, and
Obtaining equation of linear regression, equation is: y=0.0028x+0.0029, coefficient R2=0.9995；
(2) mensuration of Biuret Content
(2.1) sample 20.0002g is weighed, in 200mL volumetric flask；
(2.2) with after water dissolution shake well, adjust the pH to 4.5 of solution with sulfuric acid solution, and be diluted with water to 200mL
Shake up after graduation mark；Pour in ready 3000Da ultrafilter membrane ultrafiltration cup；
(2.3) being passed through nitrogen regulation ultrafiltration cup pressure in the ultrafiltration cup described in step (2.2) is beginning after 0.3MPa
Collect filtrate, in the conical flask that filtrate collection to 100mL is dried, discard initial filtrate 20mL, accurately pipette 50.00mL filtrate
In 100mL volumetric flask, in volumetric flask, then it is sequentially added into 20mL sodium potassium tartrate tetrahydrate alkaline solution and 20mL copper sulfate
Solution, shakes up；
(2.4) shake up, then appearance after being diluted with water to 100mL graduation mark in the volumetric flask described in step (2.3)
The water bath with thermostatic control of measuring bottle immersion 30 DEG C heats 20min when shake；At wavelength 550nm, it is surveyed with spectrophotometer
Absorbance is 0.452；
(2.5) standard curve that the absorbance data of record in above-mentioned steps (2.4) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or be 160mg by the quality obtaining biuret in equation of linear regression, i.e. can get sample
In Biuret Content be 0.80%.
Embodiment three
A kind of ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea, uses ultrafiltration pre-treatment sample, will
Fulvic acid is trapped in ultrafiltration cup, collect filtrate, utilize biuret copper sulfate, sodium potassium tartrate tetrahydrate alkaline solution in generate purple
Color coordination compound, finally according to size and the content of Working calibration curve calculating biuret of absorbance；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 200mL volumetric flasks add concentration be the biuret standard solution 0mL of 4mg/mL, 2.5mL,
5mL, 10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 20mg, 40mg, 80mg, 120mg,
160mg、200mg、240mg；
(1.2) in 8 volumetric flasks described in step (1.1), it is separately added into fulvic acid aqueous solution 30mL, and uses 1mol/
The pH value of the sulfuric acid solution regulation solution of L, to 4.5, shakes up after being diluted with water to 200mL graduation mark, puts it into full-automatic digital display
Vertical autoclave sterilizer keeps at a temperature of 120 DEG C 7min, takes out and be cooled to room temperature, pour into the most successively and install
In the ultrafiltration cup of 3000Da ultrafilter membrane；
(1.3) being passed through nitrogen in the ultrafiltration cup of step (1.2), regulation ultrafiltration cup pressure is to start after 0.4MPa to collect filter
In the conical flask that liquid is dried to 100mL, discard initial filtrate 20mL, pipette 50.00mL filtrate the most respectively and be positioned over 8 capacity
In Ping, the most backward 8 volumetric flasks are sequentially added into 25mL sodium potassium tartrate tetrahydrate alkaline solution and 25mL copper-bath, carry out
Constant volume；
(1.4) fully shake up after constant volume, 8 volumetric flasks described in above-mentioned steps (1.3) are immersed the thermostatted water of 35 DEG C
Bath heats 30min when shake；
(1.5) using solution that biuret is zero as reference solution, at wavelength 550nm, spectrophotometric determination mark is used
The accurate absorbance than solution, and record data；
| Corresponding amount/the mg of biuret | Absorbance/A |
| 0 | 0.000 |
| 20 | 0.050 |
| 40 | 0.115 |
| 80 | 0.233 |
| 120 | 0.326 |
| 160 | 0.445 |
| 200 | 0.549 |
| 240 | 0.658 |
(1.6) with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate draws standard curve, and
Obtaining equation of linear regression, equation is: y=0.0027x+0.0022, coefficient R2=0.9994；
(2) mensuration of Biuret Content
(2.1) sample 25.0002g is weighed, in 200mL volumetric flask；
(2.2) with after water dissolution shake well, adjust the pH to 4.5 of solution with sulfuric acid solution, and be diluted with water to 200mL
Shake up after graduation mark；Pour in ready 3000Da ultrafilter membrane ultrafiltration cup；
(2.3) being passed through nitrogen regulation ultrafiltration cup pressure in the ultrafiltration cup described in step (2.2) is beginning after 0.4MPa
Collect filtrate, in the conical flask that filtrate collection to 100mL is dried, discard initial filtrate 20mL, accurately pipette 50.00mL filtrate
In 100mL volumetric flask, in volumetric flask, then it is sequentially added into 25mL sodium potassium tartrate tetrahydrate alkaline solution and 25mL copper sulfate
Solution, shakes up；
(2.4) shake up, then appearance after being diluted with water to 100mL graduation mark in the volumetric flask described in step (2.3)
The water bath with thermostatic control of measuring bottle immersion 35 DEG C heats 30min when shake；At wavelength 550nm, it is surveyed with spectrophotometer
Absorbance is 0.272；
(2.5) standard curve that the absorbance data of record in above-mentioned steps (2.4) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or by equation of linear regression is obtained quality 100mg of biuret, i.e. can get in sample
Biuret Content be 0.40%.
Experimental example one
Recovery test
Weigh humic acid urea 20g (accurately to 0.0002g) that the Biuret Content in embodiment two is 0.80% in
In 200mL volumetric flask, with accurately adding 4g/L biuret standard solution 5.00mL after water dissolution, dilute, with 1mol/L's
Sulfuric acid solution adjust solution pH value to 4.5, be diluted with water to scale, shake up, ultrafiltration, after in the identical survey of 1.3.2.2 step its contracting
Two urea content, the results are shown in Table 5.
Recovery test result
Recovery of standard addition is between 99.5%～100.5%.
Experimental example two
Precision test:
To the same sample replication in embodiment two 10 times, measurement result see table:
Containing humic acid urea testing result
Precision extreme difference, average deviation and standard deviation represent, in this test method:
R=Xmax-Xmin=0.03%
The a series of detailed description of those listed above is only for the feasibility embodiment of the present invention specifically
Bright, they also are not used to limit the scope of the invention, all equivalent implementations made without departing from skill of the present invention spirit
Or change should be included within the scope of the present invention.
Claims (2)
1. a ultrafiltration pre-treatment measures the method for Biuret Content in humic acid urea, it is characterised in that: locate before using ultrafiltration
Reason sample, is trapped in fulvic acid in ultrafiltration cup, collects filtrate, utilizes biuret molten in the alkalescence of copper sulfate, sodium potassium tartrate tetrahydrate
Liquid generates purple coordination compound, finally according to size and the content of Working calibration curve calculating biuret of absorbance；Concrete step
Rapid as follows:
(1) drafting of standard curve:
(1.1) in 8 200mL volumetric flasks add concentration be the biuret standard solution 0mL of 4mg/mL, 2.5mL, 5mL,
10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 20mg, 40mg, 80mg, 120mg,
160mg、200mg、240mg；
(1.2) in 8 volumetric flasks described in step (1.1), it is separately added into fulvic acid aqueous solution 10～30mL, and uses 1mol/
The pH value of the sulfuric acid solution regulation solution of L, to 4.5, shakes up after being diluted with water to 200mL graduation mark, puts it into full-automatic digital display
Vertical autoclave sterilizer keeps at a temperature of 110 DEG C～120 DEG C 3min～7min, takes out and be cooled to room temperature, then depend on
Secondary pour in the ultrafiltration cup installing 3000Da ultrafilter membrane；
(1.3) being passed through nitrogen in the ultrafiltration cup of step (1.2), regulation ultrafiltration cup pressure is to start after 0.2MPa～0.4MPa to receive
In the conical flask that collection filtrate is dried to 100mL, discard initial filtrate 20mL, pipette 50.00mL filtrate the most respectively and be positioned over 8
In volumetric flask, the most backward 8 volumetric flasks are sequentially added into 15～25mL sodium potassium tartrate tetrahydrate alkaline solutions and 15～25mL sulfur
Acid copper solution, carries out constant volume；
(1.4) fully shake up after constant volume, 8 volumetric flasks described in above-mentioned steps (1.3) are immersed the water bath with thermostatic control of 30 ± 5 DEG C
In when shake heating 10～30min；
(1.5) using solution that biuret is zero as reference solution, at wavelength 550nm, with spectrophotometric determination standard ratio
The absorbance of solution, and record data；
(1.6) with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate draws standard curve, and obtains
Equation of linear regression, equation is: y=0.0028x+0.0029, coefficient R2=0.9995；
(2) mensuration of Biuret Content
(2.1) sample 15g～25g is weighed, in 200mL volumetric flask, accurately to 0.0002g；
(2.2) with after water dissolution shake well, adjust the pH to 4.5 of solution with sulfuric acid solution, and be diluted with water to 200mL scale
Shake up after line；Pour in ready 3000Da ultrafilter membrane ultrafiltration cup；
(2.3) after being passed through nitrogen regulation in the ultrafiltration cup described in step (2.2) ultrafiltration cup pressure being 0.2MPa～0.4MPa
Start to collect filtrate, in the conical flask that filtrate collection to 100mL is dried, discard initial filtrate 20mL, accurately pipette 50.00mL
Filtrate, in 100mL volumetric flask, is then sequentially added into 15～25mL sodium potassium tartrate tetrahydrate alkaline solutions and 15 in volumetric flask
～25mL copper-bath, shake up；
(2.4) shake up, then volumetric flask after being diluted with water to 100mL graduation mark in the volumetric flask described in step (2.3)
Immerse the heating 10～30min when shake in the water bath with thermostatic control of 30 ± 5 DEG C；With spectrophotometer at wavelength 550nm
Survey its absorbance, and record data；
(2.5) standard curve that the absorbance data of record in above-mentioned steps (2.4) is put in above-mentioned steps (1.5) is checked in phase
The quality of corresponding biuret or by obtaining the quality of biuret in equation of linear regression, the biuret that i.e. can get in sample contains
Amount.
A kind of ultrafiltration pre-treatment the most according to claim 1 measures the method for Biuret Content in humic acid urea, and it is special
Levy and be: in described step (2.1) interior 15g～25g sample, the content of biuret is 80mg～200mg.
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