CN102830118B - Method for determining mass fraction of triazole in industrial sodium triazole - Google Patents
Method for determining mass fraction of triazole in industrial sodium triazole Download PDFInfo
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- CN102830118B CN102830118B CN201110448364.2A CN201110448364A CN102830118B CN 102830118 B CN102830118 B CN 102830118B CN 201110448364 A CN201110448364 A CN 201110448364A CN 102830118 B CN102830118 B CN 102830118B
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Abstract
A method for determining the mass fraction of triazole in industrial sodium triazole is characterized in that the method comprises the following steps: separating triazole from a sodium triazole sample, dissolving the triazole in glacial acetic acid which is a solvent, titrating with a perchloric acid standard titration solution, and obtaining the mass fraction of the triazole in the sodium triazole sample through calculating according to the concentration and the application amount of the perchloric acid standard titration solution and the mass of the sodium triazole sample. In the invention, acetone is adopted as a solvent to separate the triazole from the industrial sodium triazole sample, the glacial acetic acid is adopted as the solvent to dissolve the triazole, and then a process for adopting the perchloric acid standard titration solution to tiltrate the obtained triazole glacial acetic acid solution to determine the mass fraction of the triazole in the industrial sodium triazole, so the method has the advantages of high accuracy, good precision, simple operation, high purity and reuse realization of recovered acetone, and environmental protection benefiting. The method has an important meaning for improving the conversion rate of the triazole raw material in the chemical engineering production and improving the sodium triazole product quality.
Description
Technical field
The present invention relates to a kind of assay method of triazole massfraction, relate in particular to the assay method of triazole massfraction in a kind of industrial triazole sodium.
Background technology
Triazole sodium also claims 1,2,4-triazole sodium or 1-sodium-1, and 2,4-triazole is widely used in synthetic medicine, agricultural chemicals and auxiliary chemicals, is important organic synthesis intermediate.Industrial common first synthesizing triazazole, then taking triazole as raw material synthesizing triazazole sodium, therefore, in triazole sodium, often contain the complete triazole of unreacted.Measure the massfraction of triazole in industrial triazole sodium, to improve triazole raw material conversion ratio, improve triazole sodium product quality significant.
When triazole individualism, its massfraction is measured available chromatography or chemical analysis method, but it be present in triazole sodium sample measure just more difficult, so far there are no report.
Summary of the invention
The object of the present invention is to provide the assay method of triazole massfraction in a kind of industrial triazole sodium accurately and rapidly.
The object of the present invention is achieved like this, the assay method of triazole massfraction in a kind of industrial triazole sodium, it is characterized in that: first triazole is separated from triazole sodium sample, again taking glacial acetic acid as triazole described in dissolution with solvents, then use the titration of perchloric acid standard titration solution, can calculate the massfraction of triazole according to the quality of the concentration of described perchloric acid standard titration solution, consumption and described triazole sodium sample.
In said determination method, select taking acetone as solvent, triazole to be separated from triazole sodium sample.
Said determination method comprises the following steps:
1) preparation perchloric acid standard titration solution, and demarcate perchloric acid standard titration solution by national standard;
2) triazole sodium sample is ground, add acetone, sonic oscillation, filters, and the acetone evaporated in filtrate is reclaimed, and obtains triazole, is then dissolved taking glacial acetic acid as solvent, obtains triazole glacial acetic acid solution;
3) by triazole glacial acetic acid solution described in the titration of described perchloric acid standard titration solution, with crystal violet instruction, solution turned blue green is terminal, does blank test simultaneously, and result is calculated as follows
In formula:
The consumption of the perchloric acid standard titration solution that V---titration triazole glacial acetic acid solution consumes, unit is mL;
V
0---the consumption of the perchloric acid standard titration solution that blank test consumes, unit is mL;
---the actual concentrations of perchloric acid standard titration solution, unit is mol/L;
The accurate numerical value of the quality of m---triazole sodium sample, unit is g;
0.06907---with 1mL perchloric acid standard titration solution
Suitable triazole quality numerical value, the g of unit.
Because industrial triazole sodium is generally 16 order～250 object particles, and triazole sodium is insoluble to acetone, in order to ensure that the triazole in sample is fully dissolved in acetone as soon as possible, need first sample to be ground, add sonic oscillation after acetone, duration of oscillation must not be less than 10min.
Indicate titration end-point by crystal violet, and contrast by current potential instruction titration end-point, when potential change is maximum, solution just becomes blue-green from blueness, therefore definite taking blue-green as titration end-point.
Preparation, demarcation and the density calculating method of above-mentioned perchloric acid standard titration solution are all carried out by national standard.
Triazole is because there being lone pair electrons to be alkalescence on nitrogen-atoms in molecule, but very weak at aqueous solution neutral and alkali, cannot use its massfraction of determination of acid-basetitration.But, triazole is dissolved in glacial acetic acid, its alkalescence strengthens, and therefore, it is that titrant carries out nonaquepous tration to triazole with perchloric acid standard titration solution that the present invention adopts in glacial acetic acid.
In order to verify the accuracy of triazole assay method in the present invention, applicant carries out control test with triazole standard items:
Accurately take triazole standard items (indicating massfraction > 99%), claim standard to 0.0001g, ice acetic acid 20mL dissolves, and adds 1 of crystal violet indicator solution, being titrated to blue-green with perchloric acid standard titration solution is terminal, does blank test simultaneously.Sample quality 0.2016g, perchloric acid standard titration solution concentration 0.1040mol/L, consumes perchloric acid standard titration solution 28.05mL when titration sample solution, and blank test consumes 0.10mL.Calculating triazole standard items quality mark is 99.59%.
Control test shows, with triazole assay method in the inventive method, triazole standard items is measured, and the massfraction that its massfraction and standard items indicate is consistent, illustrate the method for measuring triazole massfraction in the inventive method be accurately, reliable.
In order further to verify the accuracy of assay method of the present invention, applicant adopts mark-on recovery test to measure the recovery of triazole in industrial triazole sodium sample.First adopt the application's assay method to measure the triazole massfraction in industrial triazole sodium sample, then in industrial triazole sodium sample, add triazole standard items, measure wherein triazole gross mass by assay method of the present invention again, calculate the triazole recovery.Experimental data is in table 1.
Table 1 triazole recovery experimental data
In industrial triazole sodium sample, triazole average recovery rate is 95.7%, shows that the inventive method accurately, reliably.
Applicant measures in the quality that separates front and back triazole sodium in sample, tests and also shows, the triazole sodium in sample is uniform quality before and after separating, and proves that separation method of the present invention is effective.
The acetone of recovery is carried out to gas chromatography separation, its spectrogram and analysis pure acetone gas chromatogram no significant difference; Recovery acetone is continued on for to the separating experiment of sample, after separation, measure respectively triazole and triazole sodium quality, consistent with the result of measuring after the separation of use analysis pure acetone.
In order to verify separating effect and to detect the quality that reclaims acetone, carry out following experiment:
(1) getting massfraction is 99.1% industrial triazole sodium sample, grinds, and accurately takes 2.0162g, adds acetone solution, in 250mL triangular flask, washs solid filter paper on acetone with dry Filter paper filtering, and filtrate is stand-by.Volatilize the acetone on filter paper, by the solid transfer on filter paper to the beaker of 250mL, wash filter paper with water, till not making phenolphthalein redden to wash water, wash water is incorporated in beaker, adds water the solid in beaker is dissolved completely, be transferred in the volumetric flask of 250mL, and be diluted with water to scale, and accurately draw 25mL, recording triazole sodium quality is 0.2015g.
(2) by filtrate water bath method, and reclaim acetone.To ice acetic acid 20mL in the residue after evaporate to dryness, shake up and make to dissolve, add 1 of crystal violet, be titrated to blue-green with perchloric acid standard titration solution, recording triazole quality is 0.01g.
(3) will reclaim acetone for gas chromatographic analysis, the pure spectrogram no significant difference of its spectrogram and former analysis.
(4) taking above-mentioned recovery acetone with analyze pure acetone as solvent, measure with the triazole massfraction in a collection of industrial triazole sodium product by assay method of the present invention, the results are shown in Table 2.
Table 2 is respectively to reclaim acetone and to analyze pure acetone as solvent mensuration is with the measurement result of triazole massfraction in a collection of industrial triazole sodium product
Above-mentioned experimental result shows, in assay method of the present invention, is that separated from solvent is effective with acetone, and the acetone purity of recovery is high, can Reusability.
The present invention has following beneficial effect; the present invention first separates triazole taking acetone as solvent from triazole sodium sample; taking glacial acetic acid as triazole described in dissolution with solvents, then measure the massfraction of triazole in industrial triazole sodium by the method for perchloric acid standard titration solution titration triazole glacial acetic acid solution again, not only accuracy is high; precision is good; and easy and simple to handle, the acetone purity of recovery is very high, can recycle; avoid discharge, be conducive to environmental protection.The present invention is significant to the conversion ratio of triazole raw material and the quality of triazole sodium product in raising Chemical Manufacture.
Embodiment
Embodiment 1, in a kind of industrial triazole sodium, the assay method of triazole massfraction, comprises the following steps,
1) preparation perchloric acid standard titration solution and crystal violet indicator solution;
Perchloric acid standard titration solution: get glacial acetic acid 750mL, add perchloric acid 8.5mL, shake up, drip 23mL acetic anhydride in the situation that stirring, limit edged shakes, and after adding, jolting is even again, lets cool, and ice acetic acid is to 1000mL;
Crystal violet indicator solution: take 0.50g crystal violet, be dissolved in glacial acetic acid, be diluted to 100mL with glacial acetic acid.
2) demarcate perchloric acid standard titration solution: be taken at 105 DEG C of benchmark Potassium Hydrogen Phthalates that are dried to constant weight, accurately weighed, ice acetic acid 20mL makes to dissolve, and adds 1 of crystal violet indicator solution, slowly be titrated to blueness with the perchloric acid standard titration solution preparing, then do blank test.
Calculate the concentration of perchloric acid standard titration solution.Related data sees table 3.
The preparation of table 3 embodiment of the present invention 1 perchloric acid standard titration solution and demarcation related data
3) measure the massfraction of triazole in industrial triazole sodium:
A, instrument and reagent
Glacial acetic acid (analyzing pure); Acetone (analyzing pure); Perchloric acid standard titration solution (0.1055mol/L); Liquor argenti nitratis ophthalmicus (0.1mol/L); Crystal violet indicator solution 5g/L; The general glass apparatus in laboratory;
B, determination step
Get industrial triazole sodium sample in mortar, grind, take 2g, be accurate to 0.0002g, be placed in 50mL dried and clean triangular flask, add acetone 25mL, sonic oscillation 10min, filter with dry filter paper, filtrate is placed in dry 250mL tool plug triangular flask, with the filter residue on triangular flask and the filter paper of acetone gradation washing 50mL, meeting liquor argenti nitratis ophthalmicus to filtrate only generates without white precipitate, (get 5 of filtrates, add 1 inspection of 0.1mol/L liquor argenti nitratis ophthalmicus), cleansing solution is incorporated in 250mL tool plug triangular flask, take off the tool plug triangular flask of containing filtrate, water bath method also reclaims acetone, add glacial acetic acid 20mL dissolved residue, add 1 of crystal violet indicator solution, be titrated to firm change blue-green with perchloric acid standard titration solution.Do blank test simultaneously.
Triazole sodium sample quality is 2.2136g, consumes the perchloric acid standard titration solution 1.38mL of 0.1055mol/L when titration triazole glacial acetic acid solution, and blank test consumes perchloric acid standard titration solution 0.08mL.
C, result are calculated
In triazole sodium sample, the massfraction of triazole (w) represents with (%):
In formula,
V---when titration sample, consume the consumption of perchloric acid standard titration solution, Unit/mL;
V
0---when blank test, consume the consumption of perchloric acid standard titration solution, Unit/mL;
---the actual concentrations of perchloric acid standard titration solution, the mol/L of unit;
The accurate numerical value of m---sample quality, the g of unit;
0.06907---with 1mL perchloric acid standard titration solution
Suitable triazole quality numerical value, the g of unit.
Embodiment 2, the assay method of triazole massfraction in a kind of industrial triazole sodium, experimental procedure is referring to embodiment 1, industrial triazole sodium sample amount 2.2102g, sonic oscillation time 12min, perchloric acid standard titration solution actual concentrations 0.1040mol/L, the perchloric acid standard titration solution 1.34mL consuming when titration triazole glacial acetic acid solution, blank test consumes perchloric acid standard titration solution 0.07mL.
Result of calculation: triazole massfraction w=0.41% in sample
Embodiment 3, the assay method of the massfraction of triazole in a kind of industrial triazole sodium, experimental procedure is referring to embodiment 1, industrial triazole sodium sample amount 2.0086g, sonic oscillation time 15min, perchloric acid standard titration solution actual concentrations 0.1040mol/L, the perchloric acid standard titration solution 1.18mL consuming when titration triazole glacial acetic acid solution, blank test consumes perchloric acid standard titration solution 0.08mL.
Result of calculation: triazole massfraction w=0.39% in sample
Embodiment 4, the assay method of the massfraction of triazole in a kind of industrial triazole sodium, experimental procedure, referring to embodiment 1, repeats to test 5 times, and experimental data is in table 4.
Table 4 reappearance test determination result
As can be seen from Table 4, the measurement result favorable reproducibility of the embodiment of the present invention, precision is high.
Claims (2)
1. an assay method for triazole massfraction in industrial triazole sodium, is characterized in that: comprises the following steps,
(1). preparation perchloric acid standard titration solution, and demarcate perchloric acid standard titration solution by national standard;
(2). triazole sodium sample is ground, add acetone, sonic oscillation, filters, and the acetone evaporated in filtrate is reclaimed, and obtains triazole, is then dissolved taking glacial acetic acid as solvent, obtains triazole glacial acetic acid solution;
(3). by triazole glacial acetic acid solution described in the titration of described perchloric acid standard titration solution, with crystal violet instruction, solution turned blue green is terminal, makes blank assay simultaneously, and result is calculated as follows
In formula:
The consumption of the perchloric acid standard titration solution that V---titration triazole glacial acetic acid solution consumes, unit is mL;
V
0---the consumption of the perchloric acid standard titration solution that blank test consumes, unit is mL;
---the actual concentrations of perchloric acid standard titration solution, unit is mol/L;
The accurate numerical value of the quality of m---triazole sodium sample, unit is g;
0.06907---with 1mL perchloric acid standard titration solution (
=1.000mol/L) suitable triazole quality numerical value, the g of unit.
2. the assay method of triazole massfraction in industrial triazole sodium as claimed in claim 1, is characterized in that: the described sonic oscillation time is no less than 10 minutes.
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| CN108627611A (en) * | 2017-03-24 | 2018-10-09 | 衡阳师范学院 | A kind of assay method of triazole sodium purity salt |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1622368A1 (en) * | 1989-02-10 | 1991-01-23 | Всесоюзный Научно-Исследовательский Институт Химических Реактивов И Особо Чистых Химических Веществ | 2,7-bis-(2-aminophenyl)-2,7-dihydro-4-methylbenzo/1,2-,3,4-/bistriazol as agent for spectrometry analysis of selenium (iv) |
| CN1539829A (en) * | 2003-04-25 | 2004-10-27 | 上海应用技术学院 | Method for synthesizing 1H-1, 2,3 triazole |
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- 2011-12-26 CN CN201110448364.2A patent/CN102830118B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1622368A1 (en) * | 1989-02-10 | 1991-01-23 | Всесоюзный Научно-Исследовательский Институт Химических Реактивов И Особо Чистых Химических Веществ | 2,7-bis-(2-aminophenyl)-2,7-dihydro-4-methylbenzo/1,2-,3,4-/bistriazol as agent for spectrometry analysis of selenium (iv) |
| CN1539829A (en) * | 2003-04-25 | 2004-10-27 | 上海应用技术学院 | Method for synthesizing 1H-1, 2,3 triazole |
Non-Patent Citations (2)
| Title |
|---|
| 《1H-1,2,4三氮唑的气相色谱分析》;徐发菊;《浙江化工》;CNKI;19921231;第23卷(第2期);60 * |
| 徐发菊.《1H-1,2,4三氮唑的气相色谱分析》.《浙江化工》.CNKI,1992,第23卷(第2期),60. |
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