CN114184512A - Method for measuring nitrogen content in piperazine diphosphate - Google Patents
Method for measuring nitrogen content in piperazine diphosphate Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 69
- MWFNQNPDUTULBC-UHFFFAOYSA-N phosphono dihydrogen phosphate;piperazine Chemical compound C1CNCCN1.OP(O)(=O)OP(O)(O)=O MWFNQNPDUTULBC-UHFFFAOYSA-N 0.000 title claims abstract description 57
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 46
- 238000005303 weighing Methods 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001816 cooling Methods 0.000 claims abstract description 37
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 239000011521 glass Substances 0.000 claims abstract description 31
- 238000009835 boiling Methods 0.000 claims abstract description 27
- 239000002244 precipitate Substances 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 238000004364 calculation method Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 230000029087 digestion Effects 0.000 claims description 56
- 150000002576 ketones Chemical class 0.000 claims description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 36
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 36
- 239000011574 phosphorus Substances 0.000 abstract description 36
- 238000004458 analytical method Methods 0.000 abstract description 13
- 238000001556 precipitation Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 70
- 239000012153 distilled water Substances 0.000 description 33
- 239000011259 mixed solution Substances 0.000 description 12
- 238000005485 electric heating Methods 0.000 description 11
- NQQWFVUVBGSGQN-UHFFFAOYSA-N phosphoric acid;piperazine Chemical compound OP(O)(O)=O.C1CNCCN1 NQQWFVUVBGSGQN-UHFFFAOYSA-N 0.000 description 11
- 229960001954 piperazine phosphate Drugs 0.000 description 11
- 239000012716 precipitator Substances 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- TVBSSDNEJWXWFP-UHFFFAOYSA-N nitric acid perchloric acid Chemical compound O[N+]([O-])=O.OCl(=O)(=O)=O TVBSSDNEJWXWFP-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- HSNVNALJRSJDHT-UHFFFAOYSA-N P(=O)(=O)[Mo] Chemical compound P(=O)(=O)[Mo] HSNVNALJRSJDHT-UHFFFAOYSA-N 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction 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
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention belongs to the field of chemical detection and analysis, and particularly relates to a method for determining nitrogen content in piperazine diphosphate. Weighing a piperazine diphosphate sample m, adding water, dissolving, and fixing the volume to 500mL to obtain a solution A; weighing potassium persulfate, adding into water, adding a certain amount of concentrated nitric acid, transferring 10mL of solution A, uniformly mixing, digesting at 110-120 ℃ for 30-40min, and cooling; adding concentrated nitric acid into the cooled solution, heating to boiling state, adding quinomolybdenyl citraconic precipitant, heating to slightly boil for 1-3min, cooling, and filtering and washing with glass sand core crucible of mass m 1; filtering and washing to obtain a glass sand core crucible with precipitates, placing the glass sand core crucible in a constant temperature drying box at 180 ℃ for 45min, taking out the crucible, cooling and weighing m2, and calculating the nitrogen content% = (m2-m 1). times.0.014X 100/(m X10/500) by adopting a calculation formula. Meanwhile, the method for measuring the phosphorus content by the precipitation method has the characteristics of good stability and high accuracy.
Description
Technical Field
The invention relates to the field of chemical detection and analysis, and particularly relates to a digestion method of methyl silicone oil and a method for determining nitrogen content of piperazine diphosphate by a quinomolybdenyl citranone precipitation method.
Background
Piperazine diphosphate is white uniform powder, is a nitrogen-phosphorus synergistic halogen-free high-efficiency flame retardant, has excellent flame retardant performance, can also be used as an intermediate raw material, and is widely used for the production of piperazine pyrophosphate.
Piperazine diphosphate and phosphoric acid raw materials are used in the synthesis, and a product contains nitrogen elements after the reaction is finished, so that the purity and the reaction degree of the product can be reflected by detecting the nitrogen content and the phosphorus content in the piperazine diphosphate, a basis is provided for improving the quality of the product, and data is provided for the reaction process and the proportion adjustment of the product.
The method for measuring the phosphorus content comprises the methods of a phosphomolybdenum blue spectrophotometry method, a quinomolybdenyl citranone precipitation method, an ion chromatography method and the like. The phosphomolybdic blue spectrophotometry and the ion chromatography are suitable for samples with low phosphorus content, the quinomolybdic citraconic precipitation method is suitable for samples with normal light phosphorus content, and the samples with 10 percent of phosphorus content, such as piperazine diphosphate, are only suitable for being measured by the quinomolybdic citraconic weight method.
Disclosure of Invention
The invention provides a method for digesting piperazine diphosphate by an electric hot plate and determining the phosphorus content by a gravimetric method.
In order to solve the defects of the prior art, the technical scheme adopted by the invention is as follows: a method for digesting piperazine diphosphate by heating a potassium persulfate and nitric acid mixed solution through an electric hot plate and measuring the content of phosphorus by a gravimetric method comprises the following steps:
(1) weighing a piperazine diphosphate sample m, adding water, dissolving and fixing the volume to obtain a solution A;
(2) weighing potassium persulfate, adding into water, adding a certain amount of concentrated nitric acid, transferring 10mL of solution A, uniformly mixing, digesting at 110-120 ℃ for 30-40min, and cooling;
(3) adding concentrated nitric acid into the cooled solution, heating to boiling state, adding quinomolybdenyl citraconic precipitant, heating to slightly boil for 1-3min, cooling, and filtering and washing with glass sand core crucible of mass m 1;
(4) and filtering and washing to obtain a glass sand core crucible with precipitates, placing the glass sand core crucible in a constant-temperature drying oven at the temperature of 175-180 ℃ for 35-45min, taking out the crucible, cooling and weighing m2, and calculating the nitrogen content as (m2-m 1). times.0.014 × 100/(m × 10/500) by using a calculation formula.
In the step (2), the mass fraction of the potassium persulfate is 99 percent or more; the mass fraction of the concentrated nitric acid is 68 percent or more.
In the step (2), the amount of the added digestion solution potassium persulfate is 0.8-1.2 g and 10-20mL of concentrated nitric acid for every 10mL of the solution A.
The amount of the digestion solution potassium persulfate added is 1.0g and 10mL of concentrated nitric acid for every 10mL of the solution A.
The volume ratio of the solution cooled in the step (3) to the concentrated nitric acid is 1: 1-2, the addition amount of the quinomolybdenyl citraconic ketone is at least 3 times of the volume of the solution after cooling.
Because piperazine diphosphate has the characteristics of large viscosity and good chemical stability, no effective digestion method is available for piperazine diphosphate, and the invention provides a new idea for the digestion and detection of piperazine diphosphate.
The digestion of organic compounds is decomposed by nitric acid or nitric acid-perchloric acid, or by potassium persulfate microwave digestion and potassium persulfate autoclave digestion. According to the invention, the nitric acid-perchlorate cannot be completely digested by the method, and the content of phosphorus in the measured solution is low. The potassium persulfate pressure cooker has long digestion time, and the pressure cooker can be opened only by cooling, so the time is long and unsafe. The potassium persulfate and the nitric acid are mixed and digested directly on the electric hot plate, and the method has the advantages of simple equipment, easy operation and good digestion effect. Meanwhile, experiments prove that when the usage amount of the sample and potassium persulfate is 10mL of solution A (1g/500mL of piperazine diphosphate), 0.8g-1.2g of potassium persulfate and 10mL of concentrated nitric acid are needed.
Detailed Description
The invention is further illustrated by the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1
The digestion solution is pure potassium persulfate and concentrated nitric acid, and the mass-volume ratio of the digestion solution to the concentrated nitric acid is 1g:10 mL.
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 10mL of concentrated nitric acid were added, then 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and left to cool.
3) Washing the digestion solution with distilled water, and adding 10mL of nitric acid solution (volume ratio of 1: 1) heating on an electric heating plate to boil, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuing heating and slightly boiling for 1min, standing, cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed constantly.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The formula of the calculation is that the phosphorus content is (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 1 analysis results of phosphorus content in piperazine phosphate
Example 2
The method and conditions were the same as example 1, except that the digestion solution was 1g of pure potassium persulfate
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) Weighing 1.0g of potassium persulfate, adding 100mL of distilled water, then transferring 10mL of solution A into the mixed solution, heating and boiling on an electric hot plate for 30-40 minutes, digesting until the volume of the solution is 20-30mL, and cooling.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 2 analysis of the phosphorus content in piperazine phosphate shows a slightly lower phosphorus content of 1.3, but with good precision
Example 3
The method and the conditions are the same as those of the example 1, only the digestion solution is pure potassium persulfate and the mass-to-volume ratio of the concentrated nitric acid is 1g:8mL
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 8mL of concentrated nitric acid were added, 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and allowed to cool.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
Table 3 analysis results of phosphorus content in piperazine phosphate show that the phosphorus content is lower than 0.7%, and the precision is better
Example 4
The method and conditions are the same as example 1, only the digestion solution is pure potassium persulfate and concentrated nitric acid, and the mass-to-volume ratio is 1:12
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 12mL of concentrated nitric acid were added, 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and allowed to cool.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 4 analysis of the phosphorus content in piperazine phosphate results, which are normal, but according to the saving principle, the amount of nitric acid should be reduced
Example 5
The method and conditions are the same as example 1, only the digestion solution is pure potassium persulfate and concentrated nitric acid, and the mass-to-volume ratio is 1:6
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 6mL of concentrated nitric acid were added, 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and allowed to cool.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
Table 5 analysis of phosphorus content in piperazine phosphate shows that the phosphorus content is 0.6% lower and the precision is better
Example 6
The method and conditions are the same as example 1, only the digestion solution is pure potassium persulfate and concentrated nitric acid, and the mass-to-volume ratio is 1:16
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 16mL of concentrated nitric acid were added, 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and allowed to cool.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
Table 6 analysis results of phosphorus content in piperazine phosphate, the results are similar to those of example 1, but the use amount of nitric acid is large, which has an influence on environmental protection
Example 7
The method and conditions are the same as example 1, only the digestion solution is concentrated nitric acid
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) Adding 100mL of distilled water and 10mL of concentrated nitric acid, then transferring 10mL of the solution A into the mixed solution, heating and boiling the solution on a hot plate for 30-40 minutes, digesting the solution until the volume of the solution is 20-30mL, and cooling the solution.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 7 analysis of the phosphorus content in piperazine phosphate results, which are 6% lower and unstable
Example 8
The method and conditions are the same as example 1, only the digestion solution is pure potassium persulfate and perchloric acid, and the mass-volume ratio is 1g:10
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 10mL of perchloric acid were added, and then 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and allowed to cool.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 8 analysis of the phosphorus content in piperazine phosphate shows a 3% reduction and is unstable
Example 9
The method and conditions are the same as example 1, only the digestion solution is pure potassium persulfate and concentrated sulfuric acid with the mass-to-volume ratio of 1:10
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 10mL of concentrated sulfuric acid were added, and then 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and allowed to cool.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 9 analysis of the phosphorus content in piperazine phosphate results, low precision
Example 10
The method and conditions are the same as example 1, and the mass volume ratio of the digestion solution to the pure potassium persulfate to the concentrated hydrochloric acid is 1:10
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) 1.0g of potassium persulfate was weighed, 100mL of distilled water and 10mL of concentrated hydrochloric acid were added, and then 10mL of solution A was transferred to the mixed solution, heated and boiled on a hot plate for 30 to 40 minutes, digested to a solution volume of 20 to 30mL, and allowed to cool.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 10 analysis of the phosphorus content in piperazine phosphate, results are lower
Example 11
The method and conditions are the same as example 1, only the digestion solution is concentrated nitric acid and concentrated hydrochloric acid with the mass-volume ratio of 10:1
A digestion method of piperazine diphosphate and a method for measuring the phosphorus content in the piperazine diphosphate based on the digestion method comprise the following steps:
1) weighing two parallel samples by a ten-thousandth balance, weighing 1g (m) piperazine diphosphate sample, putting the sample into a beaker, adding distilled water for dissolving, and metering to 500mL after uniformly mixing.
2) Transferring 10mL of concentrated nitric acid, adding 100mL of distilled water and 1mL of concentrated hydrochloric acid, then transferring 10mL of solution A into the mixed solution, heating and boiling on a hot plate for 30-40 minutes, digesting until the volume of the solution is 20-30mL, and cooling.
3) The digestion solution was washed with distilled water, and 10mL of a nitric acid solution (1: 1) heating and boiling on an electric heating plate, taking down and adding 30mL of the quinomolybdenyl citraconic ketone precipitator, continuously heating and slightly boiling for 1min, standing and cooling, and filtering and washing the precipitate by using a glass sand core crucible m1 which is weighed by constant weight.
4) And (3) placing the filtered glass sand core crucible with the precipitate in a constant-temperature drying box at 180 ℃ for 45min, taking out, cooling, weighing m2, and calculating.
5) The calculation formula is that x% ═ (m2-m1) × 0.014 × 100/(m × 10/500)
TABLE 11 analysis of the phosphorus content in piperazine phosphate shows a 8% reduction and is very unstable
As can be seen from the table, the method can quickly and accurately measure the content of phosphorus in piperazine diphosphate, and the measurement result has better repeatability and precision.
The above-mentioned embodiments are merely examples for clarity and should not be construed as limitations of the present embodiments, and other variations and modifications may be made on the basis of the above description. The scope of the present invention is defined by the claims, and other modifications, including equivalents of the features of the claims, are intended to be included within the scope of the present invention. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (5)
1. A method for measuring the nitrogen content in piperazine diphosphate is characterized by comprising the following steps:
(1) weighing a piperazine diphosphate sample m, adding water, dissolving and fixing the volume to obtain a solution A;
(2) weighing potassium persulfate, adding into water, adding a certain amount of concentrated nitric acid, transferring 10mL of solution A, uniformly mixing, digesting at 110-120 ℃ for 30-40min, and cooling;
(3) adding concentrated nitric acid into the cooled solution, heating to boiling state, adding quinomolybdenyl citraconic precipitant, heating to slightly boil for 1-3min, cooling, and filtering and washing with glass sand core crucible of mass m 1;
(4) filtering and washing to obtain a glass sand core crucible with precipitates, placing the glass sand core crucible in a constant temperature drying oven at the temperature of 175-180 ℃ for 35-45min, taking out the crucible, cooling and weighing m2, and calculating the nitrogen content by adopting a calculation formula to be% = (m2-m 1). times.0.014 × 100/(m × 10/500).
2. The method for measuring the nitrogen content in piperazine diphosphate according to claim 1, wherein the mass fraction of potassium persulfate in step (2) is 99% or more; the mass fraction of the concentrated nitric acid is 68 percent or more.
3. The method for determining the nitrogen content in piperazine diphosphate according to claim 2, wherein the amount of potassium persulfate added as the digestion solution per 10mL of solution A in step (2) is 0.8-1.2 g and 10-20mL of concentrated nitric acid.
4. The method for measuring nitrogen content in piperazine diphosphate according to claim 3, wherein the amount of potassium persulfate added as the digestion solution per 10mL of solution A is 1.0g and 10mL of concentrated nitric acid.
5. The method for determining the nitrogen content in piperazine diphosphate according to claim 1, wherein the volume ratio of the solution cooled in step (3) to concentrated nitric acid is 1: 1-2, the addition amount of the quinomolybdenyl citraconic ketone is at least 3 times of the volume of the solution after cooling.
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