CN106290198A - A kind of sodium carbonate Precipitation Determination is containing the method for Biuret Content in manganese carbamide - Google Patents
A kind of sodium carbonate Precipitation Determination is containing the method for Biuret Content in manganese carbamide Download PDFInfo
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- CN106290198A CN106290198A CN201610809396.3A CN201610809396A CN106290198A CN 106290198 A CN106290198 A CN 106290198A CN 201610809396 A CN201610809396 A CN 201610809396A CN 106290198 A CN106290198 A CN 106290198A
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- 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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- 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
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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
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention belongs to a kind of sodium carbonate Precipitation Determination containing the method for Biuret Content in manganese carbamide；After sample dissolution, add sodium carbonate liquor, the manganese sulfate in sample is precipitated under conditions of heating, then filter, in filtrate, copper sulfate and sodium potassium tartrate tetrahydrate is added after again, the biuret in filtrate is made to generate purplish red coordination compound in alkaline solution, finally according to size and the content of Working calibration curve calculating biuret of absorbance；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 sodium carbonate Precipitation Determination carbamide in manganese
The method of middle Biuret Content.
Background technology
Manganese is one of necessary element of crop growth, is to constitute the important element of multiple enzyme in plant, has promotion
Germination, taking root, grow, strengthen photosynthesis, Accelerate bloom increase is spent number, is strengthened disease resistance ability, production-increasing function.At me
State-owned many manganese deficiency plot, use the fertilizer containing manganese has significantly volume increase and quality raising effect to specific crop.At extensive urine
During element produces, manganese sulfate can be configured to aqueous solution, join in urine evaporation system by dosing pump, through evaporation prilling
Obtaining containing manganese carbamide, the mensuration (copper complex salt light photometry) of the important indicator biuret of carbamide is existed serious dry by manganese ion
Disturb, suitable pre-treatment must be carried out.
Do not retrieve at present about containing the assay method of Biuret Content in manganese carbamide and national and foreign standards, the phase retrieved
Pass standard mainly has: " 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 method of inspection contracting two
The mensuration of urea 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 containing the manganese ion severe jamming measurement result in manganese carbamide, it is impossible to meet testing requirement.The most at home and abroad
Also can not find out on document about containing the detection method of Biuret Content in manganese carbamide.
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 sodium carbonate Precipitation Determination that phase is short, precision is high, the response rate is good is containing the method for Biuret Content in manganese carbamide.
The object of the present invention is achieved like this: after sample dissolution, adds sodium carbonate liquor, under conditions of heating
Manganese sulfate in precipitation sample, then filters, then after in filtrate, add copper sulfate and sodium potassium tartrate tetrahydrate, make in filtrate
Biuret generates purplish red coordination compound in alkaline solution, and size and Working calibration curve finally according to absorbance calculate biuret
Content；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 conical flasks add concentration be the biuret standard solution 0mL of 2mg/mL, 2.5mL, 5mL,
10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 5mg, 10mg, 20mg, 30mg, 40mg,
50mg、60mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 5 |
| 3 | 5.00 | 10 |
| 4 | 10.0 | 20 |
| 5 | 15.0 | 30 |
| 6 | 20.0 | 40 |
| 7 | 25.0 | 50 |
| 8 | 30.0 | 60 |
(1.2) in 8 conical flasks described in step (1.1), it is sequentially added into manganese sulfate standard solution 3～8mL and carbonic acid
Sodium solution 3～8mL, is placed in heated and boiled 5min on the electric hot plate of 500W～1000W, is cooled to room temperature, with Medium speed filter paper by upper
State the solution in 8 conical flasks and filter respectively in 8 volumetric flasks, rinse precipitation 2～5 times and collect washing liquid in volumetric flask,
Then in 8 volumetric flasks, it is sequentially added into 10～30mL sodium potassium tartrate tetrahydrate alkaline solutions and 10～30mL copper-baths；
(1.3) fully shake up after constant volume, above-mentioned 8 volumetric flasks are immersed the shape in shake in the water bath with thermostatic control of 30 ± 5 DEG C
10～30min are heated under state；
(1.4) 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；
(1.5) 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=0.0069x+0.0019, coefficient R2=0.9997；
(2) mensuration of Biuret Content
(2.1) sample 3g～7g is weighed in 100mL conical flask, accurately to 0.0002g；
(2.2) add 20～after 30mL water dissolution, add sodium carbonate liquor 3～8mL, be placed on the electric hot plate of 500W～1000W
Heated and boiled 5～10min, is cooled to room temperature, by Medium speed filter paper filtered sample in volumetric flask, rinses precipitation 2～5 times and collects
Washing liquid, in volumetric flask, is then sequentially added into 10.0～30.0mL sodium potassium tartrate tetrahydrate alkaline solutions and 10.0～30.0mL copper sulfate
Solution, shakes up；
(2.3) it is diluted to scale shake up, above-mentioned 8 volumetric flasks is immersed the shape in shake in the water bath with thermostatic control of 30 ± 5 DEG C
10～30min are heated under state；At wavelength 550nm, survey its absorbance with spectrophotometer, and record data；
(2.4) standard curve that the absorbance data of record in above-mentioned steps (2.3) 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), in the sample of 3g～7g, the content of biuret is 20mg～50mg.
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 sodium carbonate Precipitation Determination contains the method for Biuret Content in manganese carbamide, after sample dissolution,
Add sodium carbonate liquor, under conditions of heating, precipitate the manganese sulfate in sample, then filter, then after add in filtrate
Copper sulfate and sodium potassium tartrate tetrahydrate, make the biuret in filtrate generate purplish red coordination compound in alkaline solution, finally according to absorbance
Size and Working calibration curve calculate biuret content；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 conical flasks add concentration be the biuret standard solution 0mL of 2mg/mL, 2.5mL, 5mL,
10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 5mg, 10mg, 20mg, 30mg, 40mg,
50mg、60mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 5 |
| 3 | 5.00 | 10 |
| 4 | 10.0 | 20 |
| 5 | 15.0 | 30 |
| 6 | 20.0 | 40 |
| 7 | 25.0 | 50 |
| 8 | 30.0 | 60 |
(1.2) in 8 conical flasks described in step (1.1), it is sequentially added into manganese sulfate standard solution 3～8mL and carbonic acid
Sodium solution 3～8mL, is placed in heated and boiled 5min on the electric hot plate of 500W～1000W, is cooled to room temperature, with Medium speed filter paper by upper
State the solution in 8 conical flasks and filter respectively in 8 volumetric flasks, rinse precipitation 2～5 times and collect washing liquid in volumetric flask,
Then in 8 volumetric flasks, it is sequentially added into 10～30mL sodium potassium tartrate tetrahydrate alkaline solutions and 10～30mL copper-baths；
(1.3) fully shake up after constant volume, above-mentioned 8 volumetric flasks are immersed the shape in shake in the water bath with thermostatic control of 30 ± 5 DEG C
10～30min are heated under state；
(1.4) 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；
(1.5) 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=0.0069x+0.0019, coefficient R2=0.9997；
(2) mensuration of Biuret Content
(2.1) sample 3g～7g is weighed in 100mL conical flask, accurately to 0.0002g；
(2.2) add 20～after 30mL water dissolution, add sodium carbonate liquor 3～8mL, be placed on the electric hot plate of 500W～1000W
Heated and boiled 5～10min, is cooled to room temperature, by Medium speed filter paper filtered sample in volumetric flask, rinses precipitation 2～5 times and collects
Washing liquid, in volumetric flask, is then sequentially added into 10.0～30.0mL sodium potassium tartrate tetrahydrate alkaline solutions and 10.0～30.0mL copper sulfate
Solution, shakes up；
(2.3) it is diluted to scale shake up, above-mentioned 8 volumetric flasks is immersed the shape in shake in the water bath with thermostatic control of 30 ± 5 DEG C
10～30min are heated under state；At wavelength 550nm, survey its absorbance with spectrophotometer, and record data；
(2.4) standard curve that the absorbance data of record in above-mentioned steps (2.3) 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), in the sample of 3g～7g, the content of biuret is 20mg～50mg.
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 sodium carbonate Precipitation Determination is containing the method for Biuret Content in manganese carbamide, after sample dissolution, adds carbonic acid
Sodium solution, precipitates the manganese sulfate in sample under conditions of heating, then filters, then after add in filtrate copper sulfate and
Sodium potassium tartrate tetrahydrate, makes the biuret in filtrate generate purplish red coordination compound in alkaline solution, finally according to absorbance size and
Working calibration curve calculates the content of biuret；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 conical flasks add concentration be the biuret standard solution 0mL of 2mg/mL, 2.5mL, 5mL,
10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 5mg, 10mg, 20mg, 30mg, 40mg,
50mg、60mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 5 |
| 3 | 5.00 | 10 |
| 4 | 10.0 | 20 |
| 5 | 15.0 | 30 |
| 6 | 20.0 | 40 |
| 7 | 25.0 | 50 |
| 8 | 30.0 | 60 |
(1.2) in 8 conical flasks described in step (1.1), it is sequentially added into manganese sulfate standard solution 3mL and sodium carbonate
Solution 3mL, is placed in heated and boiled 5min on the electric hot plate of 500W, is cooled to room temperature, with Medium speed filter paper by above-mentioned 8 conical flasks
Solution filter respectively in 8 volumetric flasks, rinse precipitation 2 times and collect washing liquid in volumetric flask, then in 8 volumetric flasks
It is sequentially added into 10.0mL sodium potassium tartrate tetrahydrate alkaline solution and 10.0mL copper-bath；
(1.3) fully shake up after constant volume, above-mentioned 8 volumetric flasks are immersed in the water bath with thermostatic control of 30 DEG C ± 5 DEG C in shake
10min is heated under state；
(1.4) 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 |
| 5 | 0.035 |
| 10 | 0.072 |
| 20 | 0.143 |
| 30 | 0.211 |
| 40 | 0.280 |
| 50 | 0.350 |
| 60 | 0.418 |
(1.5) as it is shown in figure 1, with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate is drawn
Standard curve, and obtain equation of linear regression, equation is: y=0.0069x+0.0036, coefficient R2=0.9998；
(2) mensuration of Biuret Content
(2.1) sample 3.0381g is weighed in 100mL conical flask；
(2.2) after adding 20mL water dissolution, add sodium carbonate liquor 3mL, be placed in heated and boiled 5min on the electric hot plate of 500W, cold
But, to room temperature, by Medium speed filter paper filtered sample in volumetric flask, rinse precipitation 2 times and collect washing liquid in volumetric flask, then depending on
Secondary addition 10.0mL sodium potassium tartrate tetrahydrate alkaline solution and 10.0mL copper-bath, shake up；
(2.3) it is diluted to scale shake up, above-mentioned 8 volumetric flasks is immersed the shape in shake in the water bath with thermostatic control of 30 ± 5 DEG C
10min is heated under state；Surveying its absorbance at wavelength 550nm with spectrophotometer is 0.230；
(2.4) standard curve that the absorbance data of record in above-mentioned steps (2.3) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or by equation of linear regression is obtained quality 32.8mg of biuret, i.e. can get in sample
Biuret Content be 1.08%.
Embodiment two
A kind of sodium carbonate Precipitation Determination is containing the method for Biuret Content in manganese carbamide, after sample dissolution, adds carbonic acid
Sodium solution, precipitates the manganese sulfate in sample under conditions of heating, then filters, then after add in filtrate copper sulfate and
Sodium potassium tartrate tetrahydrate, makes the biuret in filtrate generate purplish red coordination compound in alkaline solution, finally according to absorbance size and
Working calibration curve calculates the content of biuret；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 conical flasks add concentration be the biuret standard solution 0mL of 2mg/mL, 2.5mL, 5mL,
10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 5mg, 10mg, 20mg, 30mg, 40mg,
50mg、60mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 5 |
| 3 | 5.00 | 10 |
| 4 | 10.0 | 20 |
| 5 | 15.0 | 30 |
| 6 | 20.0 | 40 |
| 7 | 25.0 | 50 |
| 8 | 30.0 | 60 |
(1.2) in 8 conical flasks described in step (1.1), it is sequentially added into manganese sulfate standard solution 5mL and sodium carbonate
Solution 5mL, is placed in heated and boiled 8min on the electric hot plate of 750W, is cooled to room temperature, with Medium speed filter paper by above-mentioned 8 conical flasks
Solution filter respectively in 8 volumetric flasks, rinse precipitation 3 times and collect washing liquid in volumetric flask, then in 8 volumetric flasks
It is sequentially added into 20.0mL sodium potassium tartrate tetrahydrate alkaline solution and 20.0mL copper-bath；
(1.3) fully shake up after constant volume, above-mentioned 8 volumetric flasks are immersed in the water bath with thermostatic control of 30 DEG C ± 5 DEG C in shake
20min is heated under state；
(1.4) 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 |
| 5 | 0.036 |
| 10 | 0.074 |
| 20 | 0.142 |
| 30 | 0.210 |
| 40 | 0.277 |
| 50 | 0.345 |
| 60 | 0.408 |
(1.5) as in figure 2 it is shown, with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate is drawn
Standard curve, and obtain equation of linear regression, equation is: y=0.0069x+0.0019, coefficient R2=0.9997；
(2) mensuration of Biuret Content
(2.1) sample 5.0028g is weighed in 100mL conical flask；
(2.2) after adding 25mL water dissolution, add sodium carbonate liquor 5mL, be placed in heated and boiled 8min on the electric hot plate of 750W, cold
But, to room temperature, by Medium speed filter paper filtered sample in volumetric flask, rinse precipitation 3 times and collect washing liquid in volumetric flask, then depending on
Secondary addition 20.0mL sodium potassium tartrate tetrahydrate alkaline solution and 20.0mL copper-bath, shake up；
(2.3) it is diluted to scale shake up, above-mentioned 8 volumetric flasks is immersed the shape in shake in the water bath with thermostatic control of 30 ± 5 DEG C
20min is heated under state；Surveying its absorbance at wavelength 550nm with spectrophotometer is 0.257；
(2.4) standard curve that the absorbance data of record in above-mentioned steps (2.3) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or by equation of linear regression is obtained quality 37.0mg of biuret, i.e. can get in sample
Biuret Content be 0.74%.
Embodiment three
A kind of sodium carbonate Precipitation Determination is containing the method for Biuret Content in manganese carbamide, after sample dissolution, adds carbonic acid
Sodium solution, precipitates the manganese sulfate in sample under conditions of heating, then filters, then after add in filtrate copper sulfate and
Sodium potassium tartrate tetrahydrate, makes the biuret in filtrate generate purplish red coordination compound in alkaline solution, finally according to absorbance size and
Working calibration curve calculates the content of biuret；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 conical flasks add concentration be the biuret standard solution 0mL of 2mg/mL, 2.5mL, 5mL,
10mL, 15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 5mg, 10mg, 20mg, 30mg, 40mg,
50mg、60mg；
| Bottle number | Biuret standard solution volume/mL | Corresponding amount/the mg of biuret |
| 1 | 0 | 0 |
| 2 | 2.50 | 5 |
| 3 | 5.00 | 10 |
| 4 | 10.0 | 20 |
| 5 | 15.0 | 30 |
| 6 | 20.0 | 40 |
| 7 | 25.0 | 50 |
| 8 | 30.0 | 60 |
(1.2) in 8 conical flasks described in step (1.1), it is sequentially added into manganese sulfate standard solution 8mL and sodium carbonate
Solution 8mL, is placed in heated and boiled 10min on the electric hot plate of 1000W, is cooled to room temperature, with Medium speed filter paper by above-mentioned 8 conical flasks
In solution filter respectively in 8 volumetric flasks, rinse precipitation 5 times and collect washing liquid in volumetric flask, then to 8 volumetric flasks
In be sequentially added into 30.0mL sodium potassium tartrate tetrahydrate alkaline solution and 30.0mL copper-bath；
(1.3) fully shake up after constant volume, above-mentioned 8 volumetric flasks are immersed in the water bath with thermostatic control of 30 DEG C ± 5 DEG C in shake
30min is heated under state；
(1.4) 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 |
| 5 | 0.034 |
| 10 | 0.076 |
| 20 | 0.146 |
| 30 | 0.209 |
| 40 | 0.277 |
| 50 | 0.348 |
| 60 | 0.417 |
(1.5) as it is shown on figure 3, with the quality (mg) of biuret-containing as abscissa, corresponding absorbance is that vertical coordinate is drawn
Standard curve, and obtain equation of linear regression, equation is: y=0.0069x+0.0048, coefficient R2=0.9996；
(2) mensuration of Biuret Content
(2.1) sample 7.0998g is weighed in 100mL conical flask；
(2.2) after adding 20mL water dissolution, add sodium carbonate liquor 8mL, be placed in heated and boiled 10min on the electric hot plate of 1000W,
It is cooled to room temperature, by Medium speed filter paper filtered sample in volumetric flask, rinses precipitation 5 times and collect washing liquid in volumetric flask, then
It is sequentially added into 30.0mL sodium potassium tartrate tetrahydrate alkaline solution and 30.0mL copper-bath, shakes up；
(2.3) it is diluted to scale shake up, above-mentioned 8 volumetric flasks is immersed the shape in shake in the water bath with thermostatic control of 30 ± 5 DEG C
30min is heated under state；Surveying its absorbance at wavelength 550nm with spectrophotometer is 0.203；
(2.4) standard curve that the absorbance data of record in above-mentioned steps (2.3) is put in above-mentioned steps (1.5) is looked into
Corresponding biuret quality or by equation of linear regression is obtained quality 28.7mg of biuret, i.e. can get in sample
Biuret Content be 0.40%.
Experimental example one
Recovery test
Weigh manganese addition carbamide 5g (accurately to 0.0002g) that the Biuret Content in embodiment two is 0.74% in 100mL
In conical flask, with accurately adding 2g/L biuret standard solution 5mL after water dissolution, add sodium carbonate liquor 5mL, be slowly heated and boil
5min, is cooled to room temperature, by Medium speed filter paper filtered sample in 100mL volumetric flask, rinses precipitation 3 times, is then sequentially added into
20.0mL sodium potassium tartrate tetrahydrate alkaline solution and 20.0mL copper-bath, shake up, be diluted to scale, and volumetric flask is immersed 30 ± 5
DEG C water-bath in about 20min frequently shaking, at wavelength 550nm, survey its absorbance with spectrophotometer, and calculate in sample
Biuret Content, result see table:
Recovery test result
Recovery of standard addition is between 99.2%～100.4%.
Experimental example two
Precision test:
To the same sample replication in embodiment two 10 times, measurement result see table:
Manganese addition carbamide 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 sodium carbonate Precipitation Determination is containing the method for Biuret Content in manganese carbamide, it is characterised in that: after sample dissolution,
Add sodium carbonate liquor, under conditions of heating, precipitate the manganese sulfate in sample, then filter, then after add in filtrate
Copper sulfate and sodium potassium tartrate tetrahydrate, make the biuret in filtrate generate purplish red coordination compound in alkaline solution, finally according to absorbance
Size and Working calibration curve calculate biuret content；Specifically comprise the following steps that
(1) drafting of standard curve:
(1.1) in 8 conical flasks add concentration be the biuret standard solution 0mL of 2mg/mL, 2.5mL, 5mL, 10mL,
15mL, 20mL, 25mL, 30mL, to make biuret corresponding amount in solution be 0mg, 5mg, 10mg, 20mg, 30mg, 40mg, 50mg,
60mg；
(1.2) in 8 conical flasks described in step (1.1), it is sequentially added into manganese sulfate standard solution 3～8mL and sodium carbonate is molten
Liquid 3～8mL, is placed in heated and boiled 5min～10min on the electric hot plate of 500W～1000W, is cooled to room temperature, will with Medium speed filter paper
Solution in above-mentioned 8 conical flasks filters respectively in 8 volumetric flasks, rinses precipitation 2～5 times and collects washing liquid in volumetric flask
In, in 8 volumetric flasks, then it is sequentially added into 10～30mL sodium potassium tartrate tetrahydrate alkaline solutions and 10～30mL copper sulfate are molten
Liquid；
(1.3) fully shake up after constant volume, above-mentioned 8 volumetric flasks are immersed in the water bath with thermostatic control of 30 ± 5 DEG C when shake
Heating 10～30min；
(1.4) using solution that biuret is zero as reference solution, at wavelength 550nm, with spectrophotometric determination standard ratio
The absorbance of solution, and record data；
(1.5) 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=0.0069x+0.0019, coefficient R2=0.9997；
(2) mensuration of Biuret Content
(2.1) sample 3g～7g is weighed in 100mL conical flask, accurately to 0.0002g；
(2.2) add 20～after 30mL water dissolution, add sodium carbonate liquor 3～8mL, being placed on the electric hot plate of 500W～1000W heating
Boil 5～10min, be cooled to room temperature, by Medium speed filter paper filtered sample in volumetric flask, rinse precipitation 2～5 times and collect washing liquid
In volumetric flask, then it is sequentially added into 10.0～30.0mL sodium potassium tartrate tetrahydrate alkaline solutions and 10.0～30.0mL copper sulfate are molten
Liquid, shakes up；
(2.3) it is diluted to scale shake up, above-mentioned 8 volumetric flasks is immersed in the water bath with thermostatic control of 30 ± 5 DEG C when shake
Heating 10～30min；At wavelength 550nm, survey its absorbance with spectrophotometer, and record data；
(2.4) standard curve that the absorbance data of record in above-mentioned steps (2.3) 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 sodium carbonate Precipitation Determination the most according to claim 1 is containing the method for Biuret Content in manganese carbamide, and it is special
Levy and be: in described step (2.1), in the sample of 3g～7g, the content of biuret is 20mg～50mg.
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| CN110057763A (en) * | 2019-04-25 | 2019-07-26 | 唐山三友化工股份有限公司 | With the method for the content of sulfate in spectrophotometry measurement sodium carbonate |
| CN110806392A (en) * | 2019-11-22 | 2020-02-18 | 段毅平 | Method for measuring content of biuret in urea humate |
| CN111487209A (en) * | 2020-04-06 | 2020-08-04 | 浙江信捷检测技术有限公司 | Method for measuring concentration of urea in swimming pool water |
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