CN112326874A - Method for analyzing mixed alkali in hydrazine hydrate by hydrogen peroxide oxidation method - Google Patents
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000003513 alkali Substances 0.000 title claims abstract description 41
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 title claims abstract description 36
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 230000003647 oxidation Effects 0.000 title claims abstract description 15
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 15
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000243 solution Substances 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 81
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 54
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 27
- 235000017550 sodium carbonate Nutrition 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000004448 titration Methods 0.000 abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 10
- 239000002253 acid Substances 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
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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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- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the technical field of analysis of mixed alkali in hydrazine hydrate, and discloses a method for analyzing the mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method, which comprises the following steps: preparing a sample with known hydrazine content and the content of each component of the mixed alkali; respectively taking 25mL of the mixed solution as an experimental sample, and adding corresponding hydrogen peroxide into the experimental sample according to different hydrazine contents. According to the method for analyzing the mixed alkali in the hydrazine hydrate by using the hydrogen peroxide oxidation method, the hydrazine hydrate in the hydrogen peroxide oxidation solution is added, the interference of the hydrazine hydrate on the titration of the mixed alkali is eliminated, then a double-indicator method is adopted, the standard hydrochloric acid solution is used for titration, and the content of each component of the mixed alkali is calculated according to the consumption of acid under two different indicators.
Description
Technical Field
The invention relates to the technical field of analysis of mixed alkali in hydrazine hydrate, in particular to a method for analyzing the mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method.
Background
The method mainly comprises sodium chloride, sodium carbonate and sodium hydroxide in a crude hydrazine hydrate solution prepared by a urea method, and no report about a method for analyzing the content of mixed alkali in hydrazine hydrate is found at present for the mixed alkali of sodium carbonate and sodium hydroxide, while the method for analyzing pure mixed alkali is more, the analysis method commonly adopted by laboratories is a double-indicator method for measuring the content of each component, the double-indicator method is that a phenolphthalein indicator is added into a mixed alkali test solution, the solution is titrated to be colorless by using a hydrochloric acid standard solution, the titration volume is V1mL, a methyl orange indicator is added, the titration is continued by using the hydrochloric acid standard solution until the solution is changed from yellow to orange, the titration volume is V2mL, and the content of each component of the mixed alkali can be calculated according to V1 and V2.
The traditional double-indicator method is not completely suitable for measuring the content of the mixed alkali in the hydrazine hydrate, the hydrazine hydrate is an alkaline solution, acid is used for titration, and part of acid reacts with the hydrazine hydrate, so that the final result of the mixed alkali is higher, and the accuracy of the experimental result is influenced.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for analyzing mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method, which has the advantages of accurately analyzing the content of each component of the mixed alkali in a crude hydrazine hydrate solution and the like, and solves the problems that the traditional double-indicator method is not completely suitable for measuring the content of the mixed alkali in the hydrazine hydrate, the hydrazine hydrate is an alkaline solution, and the final result of the mixed alkali is higher and the accuracy of the experimental result is influenced because a part of acid reacts with the hydrazine hydrate by acid titration.
(II) technical scheme
In order to realize the purpose of accurately analyzing the content of each component of the mixed alkali in the crude hydrazine solution, the invention provides the following technical scheme:
a method for analyzing mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method comprises the following steps:
1) preparing a sample with known hydrazine content and the content of each component of mixed alkali, and respectively and sequentially preparing a mixed solution with the hydrazine concentration of 30-80 g/L, the sodium carbonate concentration of 137g/L and the sodium hydroxide concentration of 12 g/L;
firstly, respectively sucking 821g/L hydrazine solution 36.5mL, 48.7mL, 60.9mL, 73.1mL, 85.3mL and 97.4mL by using a syringe, and respectively injecting into a volumetric flask of 1000 mL;
adding 137g of sodium carbonate and 12g of sodium hydroxide into each volumetric flask in turn;
③ adding water to dilute to scale, thus preparing the compound with Na2CO3 of 137g/L, NaOH of 12g/L and hydrazine concentration of respectively: mixed solutions of 30g/L, 40g/L, 50g/L, 60g/L, 70g/L and 80g/L hydrazine;
2) respectively taking 25mL of the mixed solution in the step 1) as an experimental sample, and according to the weight ratio of hydrazine to hydrogen peroxide reaction substances of 1: 2, adding corresponding hydrogen peroxide (30%) into the experimental sample according to different hydrazine contents;
adding 3.4-9.1 g of hydrogen peroxide into an experimental sample respectively, and uniformly shaking;
secondly, heating and boiling the uniformly shaken experimental sample on a stove to dry, removing gas generated by the reaction, and naturally cooling to room temperature;
thirdly, adding a proper amount of water, obtaining the contents of Na2CO3 and NaOH in the solution by a double-indicator method, and analyzing the result to show whether the contents of Na2CO3 and NaOH in the solution are consistent with the prepared result.
(III) advantageous effects
Compared with the prior art, the invention provides a method for analyzing mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method, which has the following beneficial effects:
according to the method for analyzing the mixed alkali in the hydrazine hydrate by using the hydrogen peroxide oxidation method, the hydrazine hydrate in the hydrogen peroxide oxidation solution is added, the interference of the hydrazine hydrate on the titration of the mixed alkali is eliminated, then a double-indicator method is adopted, the standard hydrochloric acid solution is used for titration, and the content of each component of the mixed alkali is calculated according to the consumption of acid under two different indicators.
Drawings
FIG. 1 is a chart of experimental data according to an embodiment of the present invention;
FIG. 2 is a graph of experimental data for a second embodiment of the present invention;
FIG. 3 is a chart of data from three experiments in accordance with the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows: a method for analyzing mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method comprises the following steps:
1) preparing a sample with known hydrazine content and the content of each component of mixed alkali, and respectively and sequentially preparing a mixed solution with the hydrazine concentration of 30-80 g/L, the sodium carbonate concentration of 137g/L and the sodium hydroxide concentration of 12 g/L;
firstly, respectively sucking 821g/L hydrazine solution 36.5mL, 48.7mL, 60.9mL, 73.1mL, 85.3mL and 97.4mL by using a syringe, and respectively injecting into a volumetric flask of 1000 mL;
adding 137g of sodium carbonate and 12g of sodium hydroxide into each volumetric flask in turn;
③ adding water to dilute to scale, thus preparing the compound with Na2CO3 of 137g/L, NaOH of 12g/L and hydrazine concentration of respectively: mixed solutions of 30g/L, 40g/L, 50g/L, 60g/L, 70g/L and 80g/L hydrazine;
2) respectively taking 25mL of the mixed solution in the step 1) as an experimental sample, and according to the weight ratio of hydrazine to hydrogen peroxide reaction substances of 1: 2, adding corresponding hydrogen peroxide (30%) into the experimental sample according to different hydrazine contents;
adding 3.4g, 4.5g, 5.7g, 6.8g, 7.9g and 9.1g of hydrogen peroxide into an experimental sample respectively, and shaking uniformly;
secondly, heating and boiling the uniformly shaken experimental sample on a stove to dry, removing gas generated by the reaction, and naturally cooling to room temperature;
thirdly, adding a proper amount of water, calculating the content of Na2CO3 and NaOH in the solution by a double-indicator method, and analyzing to find that the content of NaOH and Na2CO3 in hydrazine hydrate is close to an actual value, wherein the result of experimental data is shown in figure 1.
Example two: a method for analyzing mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method comprises the following steps:
1) preparing a sample with known hydrazine content and the content of each component of mixed alkali, and respectively and sequentially preparing a mixed solution with the hydrazine concentration of 30-80 g/L, the sodium carbonate concentration of 137g/L and the sodium hydroxide concentration of 12 g/L;
firstly, respectively sucking 821g/L hydrazine solution 36.5mL, 48.7mL, 60.9mL, 73.1mL, 85.3mL and 97.4mL by using a syringe, and respectively injecting into a volumetric flask of 1000 mL;
adding 137g of sodium carbonate and 12g of sodium hydroxide into each volumetric flask in turn;
③ adding water to dilute to scale, thus preparing the compound with Na2CO3 of 137g/L, NaOH of 12g/L and hydrazine concentration of respectively: mixed solutions of 30g/L, 40g/L, 50g/L, 60g/L, 70g/L and 80g/L hydrazine;
2) respectively taking 25mL of the mixed solution in the step 1) as an experimental sample, and according to the weight ratio of hydrazine to hydrogen peroxide reaction substances of 1: 1, adding corresponding hydrogen peroxide (30%) into the experimental sample according to different hydrazine contents;
adding 1.7g, 2.3g, 2.8g, 3.3g, 4.0g and 4.7g of hydrogen peroxide into an experimental sample respectively, and uniformly shaking;
secondly, heating and boiling the uniformly shaken experimental sample on a stove to dry, removing gas generated by the reaction, and naturally cooling to room temperature;
thirdly, adding a proper amount of water, obtaining the content of Na2CO3 and NaOH in the solution by a double-indicator method, analyzing and finding that the content of NaOH in hydrazine hydrate is 0.3-1 g/L larger than the actual value, the content of Na2CO3 is increased along with the increase of the content of hydrazine and is far larger than the actual value, and the experimental data result is shown in figure 2.
Example three: a method for analyzing mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method comprises the following steps:
1) preparing a sample with known hydrazine content and the content of each component of mixed alkali, and respectively and sequentially preparing a mixed solution with the hydrazine concentration of 30-80 g/L, the sodium carbonate concentration of 137g/L and the sodium hydroxide concentration of 12 g/L;
firstly, respectively sucking 821g/L hydrazine solution 36.5mL, 48.7mL, 60.9mL, 73.1mL, 85.3mL and 97.4mL by using a syringe, and respectively injecting into a volumetric flask of 1000 mL;
adding 137g of sodium carbonate and 12g of sodium hydroxide into each volumetric flask in turn;
③ adding water to dilute to scale, thus preparing the compound with Na2CO3 of 137g/L, NaOH of 12g/L and hydrazine concentration of respectively: mixed solutions of 30g/L, 40g/L, 50g/L, 60g/L, 70g/L and 80g/L hydrazine;
2) respectively taking 25mL of the mixed solution in the step 1) as an experimental sample, and according to the weight ratio of hydrazine to hydrogen peroxide reaction substances of 1: 3, adding corresponding hydrogen peroxide (30%) into the experimental sample according to different hydrazine contents;
adding 5.1g, 6.8g, 8.5g, 10.2g, 11.9g and 13.6g of hydrogen peroxide into an experimental sample respectively, and uniformly shaking;
secondly, heating and boiling the uniformly shaken experimental sample on a stove to dry, removing gas generated by the reaction, and naturally cooling to room temperature;
thirdly, adding a proper amount of water, calculating the content of Na2CO3 and NaOH in the solution by using a double-indicator method, and analyzing to find that the content of Na2CO3 in hydrazine hydrate is slightly lower than the actual value by about 1-2 g/L and the content of NaOH is slightly lower than the actual value by about 1g/L, wherein the reason is that the color of the indicator is oxidized and removed by hydrogen peroxide when the indicating end point is not reached, the reaction end point is mistakenly considered, the result is lower, and the result of experimental data is shown in FIG. 3.
The invention has the beneficial effects that: the method has the advantages that the hydrazine hydrate in the hydrogen peroxide oxidizing solution is added, the interference of the hydrazine hydrate on the titration of the mixed alkali is eliminated, then a double-indicator method is adopted, the standard hydrochloric acid solution is used for titration, the content of each component of the mixed alkali is calculated according to the amount of consumed acid under two different indicators, the method not only improves the accuracy of the content determination of the mixed alkali in the hydrazine hydrate, but also makes up the determination vacancy of the mixed alkali in the hydrazine hydrate industry, and the effect of efficiently and accurately detecting the content of each component of the mixed alkali in the hydrazine hydrate is achieved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. A method for analyzing mixed alkali in hydrazine hydrate by a hydrogen peroxide oxidation method is characterized by comprising the following steps:
1) preparing a sample with known hydrazine content and the content of each component of mixed alkali, and respectively and sequentially preparing a mixed solution with the hydrazine concentration of 30-80 g/L, the sodium carbonate concentration of 137g/L and the sodium hydroxide concentration of 12 g/L;
firstly, respectively sucking 821g/L hydrazine solution 36.5mL, 48.7mL, 60.9mL, 73.1mL, 85.3mL and 97.4mL by using a syringe, and respectively injecting into a volumetric flask of 1000 mL;
adding 137g of sodium carbonate and 12g of sodium hydroxide into each volumetric flask in turn;
③ adding water to dilute to scale, thus preparing the compound with Na2CO3 of 137g/L, NaOH of 12g/L and hydrazine concentration of respectively: mixed solutions of 30g/L, 40g/L, 50g/L, 60g/L, 70g/L and 80g/L hydrazine;
2) respectively taking 25mL of the mixed solution in the step 1) as an experimental sample, and according to the weight ratio of hydrazine to hydrogen peroxide reaction substances of 1: 2, adding corresponding hydrogen peroxide (30%) into the experimental sample according to different hydrazine contents;
adding 3.4g, 4.5g, 5.7g, 6.8g, 7.9g and 9.1g of hydrogen peroxide into an experimental sample respectively, and shaking uniformly;
secondly, heating and boiling the uniformly shaken experimental sample on a stove to dry, removing gas generated by the reaction, and naturally cooling to room temperature;
thirdly, adding a proper amount of water, obtaining the contents of Na2CO3 and NaOH in the solution by a double-indicator method, and analyzing the result to show whether the contents of Na2CO3 and NaOH in the solution are consistent with the prepared result.
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