CN110618227B - Method for detecting dicyandiamide content in cyanamide solution by using HPLC method - Google Patents
Method for detecting dicyandiamide content in cyanamide solution by using HPLC method Download PDFInfo
- Publication number
- CN110618227B CN110618227B CN201910985947.5A CN201910985947A CN110618227B CN 110618227 B CN110618227 B CN 110618227B CN 201910985947 A CN201910985947 A CN 201910985947A CN 110618227 B CN110618227 B CN 110618227B
- Authority
- CN
- China
- Prior art keywords
- dicyandiamide
- solution
- cyanamide
- sample
- content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention discloses a method for detecting dicyandiamide content in a cyanamide solution by using an HPLC method, which comprises the following steps in sequence: (1) preparing a standard solution; (2) detecting the standard solution and drawing a standard curve; (3) and (5) measuring the sample solution and calculating the content of the sample. The method has the advantages of high precision, high accuracy, good repeatability, capability of realizing direct detection of the sample and greatly reducing analysis time, simplicity, practicability, convenience and reliability.
Description
Technical Field
The invention belongs to the technical field of analysis, relates to a quantitative analysis method of dicyandiamide in a cyanamide solution, and particularly relates to a method for detecting the content of dicyandiamide in the cyanamide solution by using an HPLC (high performance liquid chromatography) method.
Background
Cyanamide (CN)2H2) Usually in the form of aqueous solution, pure cyanamide is crystal, and is rhombic, colorless, deliquescent and has a melting point of 46 ℃. Cyanamide has high solubility in water and is weakly alkaline, and is completely mutually soluble with water at the temperature of 43 ℃. Cyanamide is very polar, contains cyano and amino, is an active group, is easy to generate addition, substitution, condensation and other reactions, is decomposed by alkali to generate dicyandiamide and a polymer, is decomposed by acid to generate urea, and is heated to 180 ℃ for decomposition.
Dicyandiamide, also known as dicyanodiamide (cyanouanidine, C)2H4N4) DICY or DCD, abbreviated as DICY, is a white prismatic crystalline powder, a dimer of cyanamide and also a cyano derivative of guanidine, soluble in water, alcohols, glycols and dimethylformamide, practically insoluble in ethers and benzene, non-flammable and stable on drying.
The industrial production of cyanamide started from the end of the last 30 th century and began from the reaction of lime nitrogen with sulfuric acid, followed by a gradual evolution with calcium cyanamide, CO2The raw material process route is adopted for the production of the cyanamide in modern industry by using water and the like as raw materials, but the dicyandiamide and other byproducts are generated in the production process, so that the dicyandiamide and other byproducts need to be quantitatively detected.
At present, the detection methods of dicyandiamide substances mainly include a chemical analysis method, a potentiometric titration method, a liquid chromatography tandem mass spectrometry method and the like. Among them, the chemical analysis method and the potentiometric titration method, although relatively simple, are time-consuming, have large human error, and the mass spectrometer is expensive and is rarely equipped in a laboratory. In addition, the literature reports that the detection method of dicyandiamide is to concentrate and extract a sample and then use a high performance liquid chromatograph for detection, and the method is time-consuming and expensive. Therefore, a method for detecting the content of dicyandiamide, which is simple to operate, high in accuracy and low in cost, is urgently needed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting the content of dicyandiamide in a cyanamide solution by using an HPLC method. The method has the advantages of high precision, high accuracy and good repeatability, can realize direct detection of the sample, greatly reduces the analysis time, and is simple, feasible, convenient and reliable.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for detecting the content of dicyandiamide in a cyanamide solution by using an HPLC method comprises the following steps of:
(1) preparing a dicyandiamide standard stock solution; diluting the prepared dicyandiamide standard stock solution to obtain dicyandiamide standard solutions A, B, C, D, E with different concentrations;
(2) carrying out sample injection analysis on dicyandiamide standard solutions A, B, C, D, E with different concentrations by using a high performance liquid chromatograph, recording peak areas of dicyandiamide, and drawing a concentration-peak area standard curve of dicyandiamide by using an external standard method to obtain a regression equation of the standard curve;
(3) preparing a cyanamide sample solution, carrying out sample injection analysis by using a high performance liquid chromatograph, recording the peak area, and calculating the content of dicyandiamide in the cyanamide solution according to the standard curve regression equation in the step (2).
In the above method, preferably, the hplc is agilent hplc 1260.
In the above method, preferably, the separation chromatographic column is a Dionex IonPacTMCS16 cation exchange column, the column length was 250mm, and the column inner diameter was 5 μm.
In the method, the preferable column temperature in the chromatographic condition is 20-45 ℃.
In the method, preferably, a variable wavelength ultraviolet absorption detector is adopted in the chromatographic condition, the detection wavelength is 195-215 nm,
in the above method, preferably, the chromatographic conditions are performed with 10 to 25 mmol of methanesulfonic acid aqueous solution as a mobile phase.
In the method, preferably, the flow rate of the mobile phase in the chromatographic condition is 0.6-1.0 mL/min, and the sample injection volume is 2-20 muL.
In the above method, preferably, the solvent used for preparing the dicyandiamide standard stock solution is water.
The invention provides the optimal chromatographic conditions from the aspects of separation effect, simple operation, time saving and cost saving: the chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm; the detector is a variable ultraviolet absorption detector, and the detection wavelength is 205 nm; the column temperature was 35 ℃; the mobile phase is 18 mmol methanesulfonic acid aqueous solution; the flow rate is 1.0 mL/min; the dicyandiamide is detected under the chromatographic conditions, so that the cost is minimum, the time is saved most, and the separation effect is best. The column temperature of 35 ℃ is preferred because the sample injection under the same conditions has less influence on the separation degree, peak shape, symmetry and the like of the sample, and the dicyandiamide sample can be well separated. The flow rate of 1 mL/min is preferred because the sample is injected under the same conditions, the influence on the aspects of the separation degree, the peak shape, the symmetry degree and the like of the sample is small, the separation time is short, and the dicyandiamide sample can be well separated.
Compared with the prior art, the invention has the advantages that:
the method for detecting the content of dicyandiamide in the cyanamide solution by using the HPLC method has the advantages of high precision, high accuracy and good repeatability, can realize direct detection of the sample, greatly reduces the analysis time, and is simple, feasible, convenient and reliable.
Drawings
FIG. 1 is a liquid chromatogram of a sample of test solution (i) in example 1;
FIG. 2 is a liquid chromatogram of sample of test solution II in example 2;
FIG. 3 is a liquid chromatogram of a sample from sample 3;
FIG. 4 is a liquid chromatogram of a sample of test solution (R) in example 4;
FIG. 5 is a liquid chromatogram of a sample of test solution (i) in example 5;
FIG. 6 is a liquid chromatogram of a sample (first sample) in the test solution of example 6.
The abscissa of the graph represents retention time and the ordinate represents voltage value.
Detailed Description
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative only and not limiting.
Example 1:
100 kilograms of a cyanamide solution with the content of 30 percent of cyanamide and the content of less than 5 percent of dicyandiamide needs to be detected.
The adopted high performance liquid chromatography conditions are as follows: the chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 205 nm; the column temperature was 35 ℃; the mobile phase is 18 mmol methanesulfonic acid aqueous solution; the flow rate is 1.0 mL/min; the injection volume is 10. mu.L.
A method for detecting the content of dicyandiamide in a cyanamide solution by using an HPLC method adopts a high performance liquid chromatograph to carry out detection and external standard quantitative analysis, and specifically comprises the following steps of:
(1) preparing dicyandiamide standard stock solution
Accurately weighing 0.1000 g of dicyandiamide standard substance (with the purity of 99%) in a 500 ml volumetric flask, and preparing 198 ppm dicyandiamide standard stock solution by using water to fix the volume to a scale.
(2) Preparing dicyandiamide standard solution
1 ml, 2.5 ml, 5 ml, 10 ml and 25 ml of dicyandiamide stock solutions are accurately transferred into a 100 ml volumetric flask and are made to volume to the scale with water to obtain a standard solution A, B, C, D, E (wherein the concentration of dicyandiamide is 1.98 ppm, 4.95 ppm, 9.90 ppm, 19.80 ppm and 49.50 ppm respectively).
(3) Drawing a standard curve
Shaking the standard solution A, B, C, D, E uniformly, analyzing by using a high performance liquid chromatograph, and simultaneously recording the peak area; drawing a standard curve of dicyandiamide concentration-peak area to obtain a regression equation of the standard curve: y =65.4894x-0.8533, R2And =1, wherein y is the peak area of dicyandiamide, x is the concentration of dicyandiamide, and R is a linear correlation coefficient.
(4) Preparing a cyanamide sample solution.
Precisely weighing 5.0035 gW) A sample of cyanamide solution is made up to 100 ml with water (V 2) The sample cyanamide stock solution is obtained by a volumetric flask, and four parts of 10 ml are precisely transferred respectivelyV 3) Stock solutions of sample cyanamide in 50 ml of (C: (A))V 1) In the volumetric flask, water is used for fixing the volume to obtain sample solutions I, II, III and IV; adopting the same chromatographic conditions to perform sample injection analysis on a high performance liquid chromatograph, and simultaneously recording peak areas (table 1), wherein a liquid chromatogram of a sample of a test solution I is shown in figure 1;
(5) calculating the content of dicyandiamide
In the formula:
w is the mass fraction of dicyandiamide,%;
y is the area of the peak of the dicyandiamide;
V 1the volume is determined as mL of sample solution;
V 2the volume is determined by the volume of the sample mother liquor;
V 3the volume of the sample mother liquor to be transferred is mL;
Wmass of the cyanamide sample, g;
table 1 content of dicyandiamide in example 1
As can be seen from table 1, the dicyandiamide content in the cyanamide solution was 2.02%.
Example 2:
100 kilograms of a cyanamide solution with the content of 30 percent of cyanamide and the content of less than 5 percent of dicyandiamide needs to be detected.
The adopted high performance liquid chromatography conditions are as follows: the chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 205 nm; the column temperature was 35 ℃; the mobile phase is 18 mmol methanesulfonic acid aqueous solution; the flow rate is 1.0 mL/min; the injection volume is 10. mu.L.
A method for detecting the content of dicyandiamide in a cyanamide solution by using an HPLC method adopts a high performance liquid chromatograph to carry out detection and external standard quantitative analysis, and specifically comprises the following steps of:
(1) preparing dicyandiamide standard stock solution
The procedure is as in example 1.
(2) Preparing dicyandiamide standard solution
The procedure for preparing a dicyandiamide standard solution is the same as in example 1.
(3) Drawing a standard curve
The procedure is as in example 1, to obtain the regression equation of the standard curve: y =64.9493x +1.8112, R2=0.9999, wherein y is the peak area of dicyandiamide, x is the concentration of dicyandiamide, and R is the linear correlation coefficient.
(4) Preparing a cyanamide sample solution.
Precisely weighing 5.0015 gW) A sample of cyanamide solution is made up to 100 ml with water (V 2) The sample cyanamide stock solution is obtained by a volumetric flask, and four parts of 10 ml are precisely transferred respectivelyV 3) Stock solutions of sample cyanamide in 50 ml of (C: (A))V 1) In the volumetric flask, water is used for fixing the volume to obtain sample solutions I, II, III and IV; performing sample injection analysis on high performance liquid chromatograph under the same chromatographic conditionsRecording peak area (table 2), wherein the liquid chromatogram of the sample solution (II) is shown in figure 2;
(5) calculating the content of dicyandiamide
In the formula:
w is the mass fraction of dicyandiamide,%;
y is the area of the peak of the dicyandiamide;
V 1the volume is determined as mL of sample solution;
V 2the volume is determined by the volume of the sample mother liquor;
V 3the volume of the sample mother liquor to be transferred is mL;
Wmass of the cyanamide sample, g;
table 2 dicyandiamide content in example 2
As can be seen from table 2, the dicyandiamide content in the cyanamide solution was 1.55%.
Example 3:
100 kilograms of a cyanamide solution with the content of 30 percent of cyanamide and the content of less than 5 percent of dicyandiamide needs to be detected.
The adopted high performance liquid chromatography conditions are as follows: the chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 205 nm; the column temperature was 35 ℃; the mobile phase is 18 mmol methanesulfonic acid aqueous solution; the flow rate is 1.0 mL/min; the injection volume is 10. mu.L.
A method for detecting the content of dicyandiamide in a cyanamide solution by using an HPLC method adopts a high performance liquid chromatograph to carry out detection and external standard quantitative analysis, and specifically comprises the following steps of:
(1) preparing dicyandiamide standard stock solution
The procedure is as in example 1.
(2) Preparing dicyandiamide standard solution
The procedure is as in example 1.
(3) Drawing a standard curve
The procedure is as in example 1, to obtain the regression equation of the standard curve: y =68.8153x +1.5127, R2And =1, wherein y is the peak area of dicyandiamide, x is the concentration of dicyandiamide, and R is a linear correlation coefficient.
(4) Preparing a cyanamide sample solution.
Precisely weighing 4.8005 gW) A sample of cyanamide solution is made up to 100 ml with water (V 2) The sample cyanamide stock solution is obtained by a volumetric flask, and four parts of 10 ml are precisely transferred respectivelyV 3) Stock solutions of sample cyanamide in 50 ml of (C: (A))V 1) In the volumetric flask, water is used for fixing the volume to obtain sample solutions I, II, III and IV; adopting the same chromatographic condition to perform sample injection analysis on a high performance liquid chromatograph, and simultaneously recording peak areas (table 3), wherein a liquid chromatogram of a sample of the test solution and the sample is shown in figure 3;
(5) calculating the content of dicyandiamide
In the formula:
w is the mass fraction of dicyandiamide,%;
y is the area of the peak of the dicyandiamide;
V 1the volume is determined as mL of sample solution;
V 2the volume is determined by the volume of the sample mother liquor;
V 3the volume of the sample mother liquor to be transferred is mL;
Wmass of the cyanamide sample, g;
table 3 dicyandiamide content in example 3
As can be seen from table 3, the dicyandiamide content in the cyanamide solution was 1.24%.
Example 4:
100 kilograms of a cyanamide solution with the content of 30 percent of cyanamide and the content of less than 5 percent of dicyandiamide needs to be detected.
The adopted high performance liquid chromatography conditions are as follows: the chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 195 nm; the column temperature was 45 ℃; the mobile phase is 10 mmol methanesulfonic acid aqueous solution; the flow rate is 0.7 mL/min; the injection volume is 10. mu.L.
The method adopts a high performance liquid chromatograph to carry out detection and external standard quantitative analysis, and specifically comprises the following steps in sequence:
(1) preparing dicyandiamide standard stock solution
The procedure is as in example 1.
(2) Preparing dicyandiamide standard solution
The procedure is as in example 1.
(3) Drawing a standard curve
The procedure is as in example 1, to obtain the regression equation of the standard curve: y =51.4792x-8.4438, R2=0.9991, wherein y is the peak area of dicyandiamide, x is the concentration of dicyandiamide, and R is the linear correlation coefficient.
(4) Preparing a cyanamide sample solution.
Precisely weighing 4.9805 gW) A sample of cyanamide solution is made up to 100 ml with water (V 2) The sample cyanamide stock solution is obtained by a volumetric flask, and four parts of 10 ml are precisely transferred respectivelyV 3) Stock solutions of sample cyanamide in 50 ml of (C: (A))V 1) In the volumetric flask, water is used for fixing the volume to obtain sample solutions I, II, III and IV; adopting the chromatographic conditions on a high performance liquid chromatographAnalyzing the sample injection, and simultaneously recording the peak area (table 4), wherein the liquid chromatogram of the sample of the test solution (R) is shown in figure 4;
(5) calculating the content of dicyandiamide
In the formula:
w is the mass fraction of dicyandiamide,%;
y is the area of the peak of the dicyandiamide;
V 1the volume is determined as mL of sample solution;
V 2the volume is determined by the volume of the sample mother liquor;
V 3the volume of the sample mother liquor to be transferred is mL;
Wmass of the cyanamide sample, g;
table 4 dicyandiamide content in example 4
As can be seen from table 4, the dicyandiamide content in the cyanamide solution was 1.63%.
According to chromatogram, the detection is unstable and the peak shape is poor due to the higher column temperature and the lower detection wavelength; while lower concentrations of the mobile phase also result in a later time to peak.
Example 5:
100 kilograms of a cyanamide solution with the content of 30 percent of cyanamide and the content of less than 5 percent of dicyandiamide needs to be detected.
The adopted high performance liquid chromatography conditions are as follows: the chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 215 nm; the column temperature is 20 ℃; the mobile phase is 25 mmol of methanesulfonic acid aqueous solution; the flow rate was 0.6 mL/min; the sample injection volume is 2 mu L;
the method adopts a high performance liquid chromatograph to carry out detection and external standard quantitative analysis, and specifically comprises the following steps in sequence:
(1) preparing dicyandiamide standard stock solution
The procedure is as in example 1.
(2) Preparing dicyandiamide standard solution
The procedure is as in example 1.
(3) Drawing a standard curve
The procedure is as in example 1, to obtain the regression equation of the standard curve: y =12.2974x +0.1954, R2=0.9997, wherein y is the peak area of dicyandiamide, x is the concentration of dicyandiamide, and R is the linear correlation coefficient.
(4) Preparing a cyanamide sample solution.
Precisely weighing 5.0105 gW) A sample of cyanamide solution is made up to 100 ml with water (V 2) The sample cyanamide stock solution is obtained by a volumetric flask, and four parts of 10 ml are precisely transferred respectivelyV 3) Stock solutions of sample cyanamide in 50 ml of (C: (A))V 1) In the volumetric flask, water is used for fixing the volume to obtain sample solutions I, II, III and IV; analyzing sample introduction on a high performance liquid chromatograph under the chromatographic conditions, and simultaneously recording peak areas (table 5), wherein a liquid chromatogram of a sample of a test solution I is shown in fig. 5;
(5) calculating the content of dicyandiamide
In the formula:
w is the mass fraction of dicyandiamide,%;
y is the area of the peak of the dicyandiamide;
V 1the volume is determined as mL of sample solution;
V 2the volume is determined by the volume of the sample mother liquor;
V 3volume of sample mother liquor removed，mL；
WMass of the cyanamide sample, g;
table 5 dicyandiamide content in example 5
As can be seen from table 5, the dicyandiamide content in the cyanamide solution was 1.29%.
According to chromatogram, the peak shape is poor due to low column temperature; although the concentration of the mobile phase is higher, the flow rate is lower, resulting in a later time to peak.
Example 6:
100 kilograms of a cyanamide solution with the content of 30 percent of cyanamide and the content of less than 5 percent of dicyandiamide needs to be detected.
The adopted high performance liquid chromatography conditions are as follows: the chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm; the detector is a variable wavelength ultraviolet absorption detector, and the detection wavelength is 200 nm; the column temperature was 25 ℃; the mobile phase is 15mmol methanesulfonic acid aqueous solution; the flow rate is 0.8 mL/min; the injection volume was 20. mu.L.
The method adopts a high performance liquid chromatograph to carry out detection and external standard quantitative analysis, and specifically comprises the following steps in sequence:
(1) preparing dicyandiamide standard stock solution
The procedure is as in example 1.
(2) Preparing dicyandiamide standard solution
The procedure is as in example 1.
(3) Drawing a standard curve
The procedure is as in example 1, to obtain the regression equation of the standard curve: y =127.3404x +10.6223, R2=0.9996, wherein y is the peak area of dicyandiamide, x is the concentration of dicyandiamide, and R is the linear correlation coefficient.
(4) Preparing a cyanamide sample solution.
Precisely weighing 4.9850 gW) Cyanamide solventThe liquid sample is made up to 100 ml with water (V 2) The sample cyanamide stock solution is obtained by a volumetric flask, and four parts of 10 ml are precisely transferred respectivelyV 3) Stock solutions of sample cyanamide in 50 ml of (C: (A))V 1) In the volumetric flask, water is used for fixing the volume to obtain sample solutions I, II, III and IV; analyzing sample introduction on a high performance liquid chromatograph under the chromatographic conditions, and simultaneously recording peak areas (table 6), wherein a liquid chromatogram of a sample of a test solution I is shown in fig. 6;
(5) calculating the content of dicyandiamide
In the formula:
w is the mass fraction of dicyandiamide,%;
y is the area of the peak of the dicyandiamide;
V 1the volume is determined as mL of sample solution;
V 2the volume is determined by the volume of the sample mother liquor;
V 3the volume of the sample mother liquor to be transferred is mL;
Wmass of the cyanamide sample, g;
table 6 dicyandiamide content in example 6
As can be seen from table 6, the dicyandiamide content in the cyanamide solution was 1.26%.
According to the chromatogram, the peak shape is better under the condition, but the peak appearance time is later.
Example 7: method performance test
1. Precision test
The test solution (i) in example 1 was used as an object to be examined, after shaking up, the sample was injected 6 times by using a high performance liquid chromatograph, and the peak areas (table 7) were recorded at the same time, and the RSD of the sample was less than 1% by comparing the peak areas, indicating that the detection method of the present invention has good precision.
TABLE 7 results of precision test
2. Accuracy test
Taking example 2 as a subject to be examined, placing the test solution at 4 ℃, injecting samples at 0h, 6h, 12h, 24h, 48h and 72h respectively, recording peak areas (table 8), and comparing the peak areas to obtain the RSD of less than 1%, which indicates that the stability of the sample solution is good, so the detection method of the invention has high accuracy.
TABLE 8 accuracy test results
3. Repeatability test
Taking the third step in the embodiment 3 as a study object, sampling for 6 times on the same type instrument by different testers at different times, recording peak areas (table 9), and comparing the peak areas to obtain the RSD less than 1%, which shows that the detection method of the invention has good repeatability.
TABLE 9 results of the repeatability tests
4. Spiked recovery test
1.0000 g of dicyandiamide standard substance (purity 99%) is precisely weighed in a 100 ml volumetric flask, and water is added to the volumetric flask to fix the volume to the scale to prepare a dicyandiamide standard stock solution A with the concentration of 0.99%. Accurately transferring 0 ml, 5 ml, 10 ml and 25 ml of solution A into a 50 ml volumetric flask, fixing the volume to a scale by using a cyanamide solution (the content of the cyanamide is 30 percent and the content of the dicyandiamide is less than 5 percent), respectively marking the volume as firstly, secondly, thirdly and fourthly, accurately transferring 2.5 ml of the solution to the volume of 500 ml, shaking uniformly, injecting by using a high performance liquid chromatograph, simultaneously recording the peak area (table 10) of a sample, and calculating the standard recovery rate according to the peak area.
TABLE 10 results of the normalized recovery test
As can be seen from the above tests of precision, accuracy, repeatability and standard recovery, the method for detecting the content of dicyandiamide in the cyanamide solution by using the HPLC method is convenient and feasible, has high precision, high accuracy and good repeatability, can realize direct detection of a sample, does not need to perform any pretreatment on the sample, and greatly reduces the analysis time.
Claims (5)
1. A method for detecting the content of dicyandiamide in a cyanamide solution by using an HPLC method is characterized by comprising the following steps: comprises the following steps which are carried out in sequence:
(1) preparing a dicyandiamide standard stock solution: diluting the prepared dicyandiamide standard stock solution to obtain dicyandiamide standard solutions A, B, C, D, E with different concentrations;
(2) carrying out sample injection analysis on dicyandiamide standard solutions A, B, C, D, E with different concentrations by using a high performance liquid chromatograph, recording peak areas of dicyandiamide, and drawing a concentration-peak area standard curve of dicyandiamide by using an external standard method to obtain a regression equation of the standard curve;
(3) preparing a cyanamide sample solution, carrying out sample injection analysis by using a high performance liquid chromatograph, recording peak area, and calculating to obtain the content of dicyandiamide in the cyanamide solution according to the standard curve regression equation in the step (2);
the high performance liquid chromatograph is an Agilent high performance liquid chromatograph 1260;
in the step (3), the high performance liquid chromatography conditions adopted for sample injection analysis are as follows: separating chromatographic column is Dionex IonPacTMCS16 cation exchange column with length of 250mm and inner diameter of 5 μm;
in the condition of the high performance liquid chromatography, 10-25 mmol of methanesulfonic acid aqueous solution is used as a mobile phase.
2. The method for detecting the dicyandiamide content in the cyanamide solution by the HPLC method according to claim 1, wherein: the column temperature in the high performance liquid chromatography is 20-45 ℃.
3. The method for detecting the dicyandiamide content in the cyanamide solution by the HPLC method according to claim 1, wherein: the high performance liquid chromatography adopts a variable wavelength ultraviolet absorption detector, and the detection wavelength is 195-215 nm.
4. The method for detecting the dicyandiamide content in the cyanamide solution by the HPLC method according to claim 1, wherein: the flow rate of the mobile phase is 0.6-1.0 mL/min, and the sample injection volume is 2-20 mu L.
5. The method for detecting the dicyandiamide content in the cyanamide solution by the HPLC method according to claim 1, wherein: the solvent used for preparing the dicyandiamide standard stock solution is water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910985947.5A CN110618227B (en) | 2019-10-17 | 2019-10-17 | Method for detecting dicyandiamide content in cyanamide solution by using HPLC method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910985947.5A CN110618227B (en) | 2019-10-17 | 2019-10-17 | Method for detecting dicyandiamide content in cyanamide solution by using HPLC method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110618227A CN110618227A (en) | 2019-12-27 |
| CN110618227B true CN110618227B (en) | 2021-07-23 |
Family
ID=68925995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910985947.5A Active CN110618227B (en) | 2019-10-17 | 2019-10-17 | Method for detecting dicyandiamide content in cyanamide solution by using HPLC method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110618227B (en) |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101339178B (en) * | 2008-08-07 | 2013-05-01 | 贵州天安药业股份有限公司 | Metformin hydrochloride enteric-coated tablets quality control method |
| CN101576543A (en) * | 2009-04-21 | 2009-11-11 | 新疆出入境检验检疫局检验检疫技术中心 | Method for fast detecting melamine in dry milk |
| CN102384948A (en) * | 2011-07-28 | 2012-03-21 | 福建省农业科学院土壤肥料研究所 | Method for measuring dicyandiamide in fertilizer and fertilizer additives |
| CN103181923B (en) * | 2011-12-29 | 2017-10-27 | 北京韩美药品有限公司 | Pharmaceutical preparation comprising Repaglinide and preparation method thereof |
| CN104502473B (en) * | 2014-12-10 | 2016-07-20 | 黄河三角洲京博化工研究院有限公司 | A kind of quantitative approach utilizing HPLC method detection cyanamide |
| CN105021737B (en) * | 2015-08-10 | 2017-04-05 | 云南省食品药品检验所 | It is a kind of at the same detect milk product in dicyandiamide and content of melamine method |
| CN109387586B (en) * | 2018-12-14 | 2021-07-20 | 宁夏瑞泰科技股份有限公司 | Method for measuring content of sodium cyanamide |
| CN110013836B (en) * | 2019-03-27 | 2021-11-05 | 天津大学 | Reversed phase/ion exchange mixed mode chromatographic stationary phase, preparation method and application |
-
2019
- 2019-10-17 CN CN201910985947.5A patent/CN110618227B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110618227A (en) | 2019-12-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103454367B (en) | A kind of method utilizing sulfate by ion chromatography monomethyl amine | |
| CN107247103B (en) | A method of utilizing thiocarbamide content in the synthesis of HPLC external standard method thiocarbamide | |
| CN111537657A (en) | Method for detecting content of trace metal ions in high-purity thiourea by ion chromatography | |
| CN108802256A (en) | A kind of detection method of monoethanolamine content | |
| CN101354349A (en) | Method for measuring protein nitrogen content in tobacco | |
| CN113295805B (en) | Method for detecting hydrazine hydrate in medicine | |
| CN108195986B (en) | A kind of method that LC-MS analyzes urea, dicyandiamide, content of melamine in guanidine hydrochloride and its three wastes | |
| CN110618227B (en) | Method for detecting dicyandiamide content in cyanamide solution by using HPLC method | |
| CN111189956B (en) | H 2 O 2 Method for detecting content of nitrite in sodium chloride sample by using oxidized ion chromatography | |
| CN108414647B (en) | High performance liquid chromatography analysis and detection method for purple uric acid and related substances thereof | |
| CN104502473B (en) | A kind of quantitative approach utilizing HPLC method detection cyanamide | |
| CN106338559A (en) | Gas chromatography detection method of chlorination by-product dichloroacetamide | |
| CN109030653A (en) | Detection method in relation to substance in a kind of l-leucovorin | |
| CN114200062A (en) | Method for detecting tetraethylene glycol dimethyl ether in leather | |
| CN114280191A (en) | Method for detecting related substances in bis-cysteine and preparation thereof | |
| CN103048407A (en) | Content detection method for lysine of compound ketoacid tablet | |
| CN112578037A (en) | Method for detecting content of hexaketal in ulipristal acetate intermediate I | |
| CN111830185A (en) | Ultra-high performance liquid chromatography tandem mass spectrometry detection method of quinclorac | |
| CN110646531A (en) | Ion chromatography quantitative analysis method for raw material diethanolamine in reaction liquid for synthesizing iminodiacetic acid by dehydrogenation of diethanolamine | |
| CN104280470B (en) | The method of intermediate in liquid chromatogram measuring LLM-105 production waste water | |
| CN111220761A (en) | High performance liquid chromatography analysis method for determining imidazole content in alkaline reaction solution | |
| CN110967425A (en) | Determination of N-alkyl imidazole impurity in imidazole type ionic liquid | |
| CN114280179B (en) | Pretreatment of exenatide and detection method of isomer in His amino acid eluent obtained by pretreatment | |
| CN109324139A (en) | Ribosylzeatin liquid-liquid extraction-liquid chromatography-tandem mass spectrometry measuring method in a kind of tobacco leaf | |
| CN112730689B (en) | Liquid chromatography analysis method of 2-amino-5, 8-dimethoxy [1,2,4] triazolo [1,5-c ] pyrimidine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20211221 Address after: 065500 South District of Gu'an County Industrial Park, Langfang City, Hebei Province Patentee after: GUAN JUNDE TONGCHUANG BIOLOG ENGINEERING Co.,Ltd. Address before: 100085 room B601, block B, No.9, Shangdi 3rd Street, Haidian District, Beijing Patentee before: Beijing Junde Tongchuang Biotechnology Co.,Ltd. |