CN103115922B - Method for determining content of triethylamine salt - Google Patents
Method for determining content of triethylamine salt Download PDFInfo
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- CN103115922B CN103115922B CN201310067401.4A CN201310067401A CN103115922B CN 103115922 B CN103115922 B CN 103115922B CN 201310067401 A CN201310067401 A CN 201310067401A CN 103115922 B CN103115922 B CN 103115922B
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Abstract
The invention relates to a method for determining content of triethylamine salt. The method is processed according to the following steps of: 1) accurately weighing a sample containing triethylamine salt, evenly shaking in a separating funnel containing water, adding methyl red indicating liquid; 2) dropwise adding a sodium hydroxide solution while adding until a proper amount of solution is dropwise added after the solution becomes yellow; 3) adding an organic solvent to vibrate and deflate; 4) standing and layering, and then separating liquid and collecting extract solution; 5) accurately absorbing a part of collected extract solution, adding to a triangular flask containing a polar solvent, and then adding the methyl red indicating liquid; 6) adding standard acid liquid into the solution to perform titration operation until the solution becomes orange red from yellow; and 7) calculating the content of the triethylamine salt in the sample. By adopting the method, the content of the triethylamine salt in the sample can be rapidly detected in real time, and the method has the advantages of being simple and convenient to operate, high in accuracy, good in precision, low in analysis cost and the like.
Description
Technical field
The present invention relates to triethylamine and triethylamine salt, particularly relate to a kind of assay method of triethylamine salt content.
Background technology
Triethylamine, another name N, N-diethyl ethanamine, fusing point-115 DEG C, boiling point 90 DEG C, density 0.7g/cm
3, moderate toxicity, is slightly soluble in water, is dissolved in the organic solvent such as ethanol, chloroform, meets acid reaction and generates triethylamine salt, is solvent, catalyzer and reaction raw materials conventional in organic synthesis industry.In Chemical Manufacture, triethylamine is often present in reactant liquor, mother liquor, intermediate product and industrial residue and waste water in a salt form.Therefore, measure the content of triethylamine salt and triethylamine accurately and rapidly, all significant to the recycling of the monitoring of the chemical reaction process that triethylamine is correlated with, triethylamine, waste residue and wastewater treatment etc.
In prior art, triethylamine detects containing quantitative analysis vapor-phase chromatography, bromophenol blue spectrophotometric method, the chromatography of ions etc. usually.With gas chromatography determination industry triethylamine product content, the triethylamine using trace in bromophenol blue spectrophotometry waste water in national standard.Survey triethylamine step by vapor-phase chromatography and the chromatography of ions all comparatively loaded down with trivial details, sense cycle is long, and needs to use valuable detecting instrument, and analysis cost is high; Bromophenol blue spectrophotometric method is applicable to measure micro-triethylamine.And the detection of triethylamine salt content is not reported so far.
Summary of the invention
The object of the present invention is to provide a kind of assay method of triethylamine salt content, the method can easy, the content that measures triethylamine salt quickly and accurately, is applicable to macro-analysis.
Object of the present invention realizes like this:
An assay method for triethylamine salt content, is characterized in that, it is undertaken by the following stated step:
1), accurately take the sample containing triethylamine salt, in the separating funnel filling water, shake up, add methyl red indicator solution;
2), drip sodium hydroxide solution, limit edged shakes, and it is suitably excessive again after yellow for dropping to solution;
3), add organic solvent, jolting, and note venting;
4), after stratification, separatory, collects extract;
5), accurately draw the extract collected by part, add and fill in the triangular flask of polar solvent, then add methyl red indicator solution;
6), use sour standard titration solution, be titrated to solution orange red by xanthochromia;
7) content of triethylamine salt in sample, is calculated.
Above-mentioned steps 3) in, because triethylamine is slightly soluble in water, but can the organic solvents such as chloroform be dissolved in, wherein chloroform and water immiscible, and comparatively large with the density variation of water, be convenient to separatory, therefore select chloroform to be extraction solvent during extraction.
When extraction selects chloroform to be extraction solvent, above-mentioned steps 5) in, because acid base indicator variable color in chloroform is failed to understand, if take only chloroform as solvent, terminal cannot judge.Test shows, add ethanol in proper amount polar solvent in the chloroformic solution of triethylamine after, during titration end-point, indicator discoloration is comparatively obvious, can carry out accurate titration.If add suitable quantity of water wherein again, during terminal, the change of indicator color will be more obvious.In order to easy to operate, the final aqueous solution preferably directly adding ethanol.
Above-mentioned steps 5) in, the ratio of chloroform, second alcohol and water directly affects endpoint observation.Test shows, when chloroform: ethanol: during the volume ratio=10:20:5 of water, terminal clearly, and the constant muddiness of solution in titration process.And reduce the ratio of ethanol or increase the ratio of water, solution all may be caused to become solution in muddy or titration process and to become muddy, thus affect endpoint observation; The ratio of suitable increase ethanol or the ratio of minimizing water, and the amount simultaneously increasing second alcohol and water is according to the above ratio not fairly obvious on terminal impact.In order to both be convenient to titration operation, making again terminal sharp, and considering saving reagent simultaneously, the solvent of this drop reaction is defined as the agent of every 10mL chloroform extraction and adds ethanolic solution (80+20) 30mL.
Above-mentioned steps 2) in, be add sodium hydroxide solution in sample, triethylamine salt in sample is converted into triethylamine.Find after deliberation: when pH equals 5.2, in sample, triethylamine salt just transforms completely, and add suitably excessive sodium hydroxide solution, both ensure that triethylamine salt transformed completely, improve conversion rate again simultaneously, so, after measuring 2mL ~ 3mL after sodium hydroxide solution addition is defined as methyl red flavescence look.
Above-mentioned steps 6) in, the standard titration solutions such as available hydrochloric acid or sulfuric acid are to the triethylamine direct titration in chloroform, ethanol and water mixed solution.
More specifically, the assay method of triethylamine salt content of the present invention, is undertaken by the following stated step:
1), take sample 1 ~ 5g containing triethylamine salt, claim accurate to 0.0002g, be placed in the separating funnel filling 20mL water, shake up, add the methyl red indicator solution 1 ~ 2 of 1g/L;
2), drip the sodium hydroxide solution of 100g/L, limit edged shakes, to solution in time yellow after amount 2mL ~ 3mL;
3), again methenyl choloride 20mL is accurately added, jolting 1 minute, about jolting 140 ~ 160 times;
4), leave standstill, after layering, slowly open funnel stopcock, discard the chloroform extraction liquid about 2 ~ 3mL flowed down at first, then residue extract is collected in the container of dried and clean;
5) the extract 10mL collected by, accurately drawing adds in the triangular flask filling 30mL ethanolic solution (80+20), adds the methyl red indicator solution 1 of 1g/L;
6), with the Hydrochloric Standard Titration of 0.1 mol/L, solution is titrated to orange red by xanthochromia;
7), result calculates
In sample, triethylamine salt content is in triethylamine, its massfraction with
(%) represent, result is calculated as follows:
In formula,
---the actual concentrations of Hydrochloric Standard Titration, unit is mole often liter (mol/L);
---the consumption of Hydrochloric Standard Titration during titration, unit is milliliter (mL);
---the volume of the extract of absorption, unit is milliliter (mL);
v 0 ---the methenyl choloride volume added, unit is milliliter (mL);
---the exact value of sample mass, unit is gram (g);
0.1012---with 1mL Hydrochloric Standard Titration [
=1.000mol/L] suitable for a gram quality for the triethylamine represented.
A kind of Lewis alkali according to triethylamine, be alkaline in aqueous solution because there is dissociation reaction, the character that its alkalescence is stronger than ammonia, selects with sour standard titration solution direct titration triethylamine, records the content of triethylamine salt in sample by measuring the amount of triethylamine that transformed by triethylamine salt.The triethylamine measured in sample by this method also will be simultaneously determined.
The inventive method has following beneficial effect:
The invention discloses a kind of assay method of triethylamine salt content, the method can be fast, the content of triethylamine salt in real-time test samples, and have easy and simple to handle, accuracy is high, the plurality of advantages such as precision is good, with by after in sample, triethylamine salt is converted into triethylamine, compare more fast easy again with gas chromatography determination, and do not need with valuable instrument, easy to implement, analysis cost is low, be suitable for the reactant liquor of organic chemical industry's production run, mother liquor, triethylamine salt assay contained in intermediate and waste residue and waste liquid, the chemical reaction process monitoring relevant to triethylamine, the recycling of triethylamine, waste residue and wastewater treatment are all significant.The relative standard deviation RSD=0.59%(n=6 of its sample determination is shown through experimental test data result), recovery of standard addition 96.87% ~ 99.36%.
Embodiment
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is; following examples are only for being further detailed the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to foregoing invention content to the present invention.
Embodiment 1
Accurately take the sample 1.0086g containing triethylamine hydrochloride, be placed in the separating funnel filling 20mL water, add the methyl red indicator solution 1 of 1g/L after shaking up, drip the sodium hydroxide solution of 100g/L, limit edged shakes, after amount 2mL when being yellow to solution; Accurately add methenyl choloride 20mL, jolting 1 minute (about jolting 140 ~ 160 times), and note venting; After stratification, with clean absorbent cotton dry filler neck part with micro-moisture, slowly open funnel stopcock afterwards, discard the chloroform extraction liquid 3mL flowed down at first, then remaining extract is collected in the container of dried and clean; The extract 10mL that accurate absorption is collected is in the triangular flask filling 30mL ethanolic solution (80+20), add the methyl red indicator solution 1 of 1g/L, be titrated to solution with the Hydrochloric Standard Titration that concentration is 0.1003mol/L and be terminal by xanthochromia is orange red, now consume Hydrochloric Standard Titration 12.63mL altogether;
Result calculates
In selected sample, the content of triethylamine hydrochloride is in triethylamine, its massfraction with
(%) represent, be calculated as follows:
=
In formula,
---the actual concentrations of Hydrochloric Standard Titration, unit is mole often liter (mol/L);
---the consumption of Hydrochloric Standard Titration during titration, unit is milliliter (mL);
---the volume of the extract of absorption, unit is milliliter (mL);
v 0 ---the volume of the methenyl choloride added, unit is milliliter (mL);
---the exact value of sample mass, unit is gram (g);
0.1012---with 1mL Hydrochloric Standard Titration [
=1.000mol/L] suitable for a gram quality for the triethylamine represented.
Embodiment 2(Accuracy Verification: with national standard method results contrast)
Accurately taking triethylamine reagent 2.5128g(according to relevant national standard mensuration content is 99.1%), add in the volumetric flask of the 100mL filling about 60mL water, be diluted with water to scale, shake up, make triethylamine standard solution.This solution of accurate absorption 10mL is contained in separating funnel, adds hydrochloric acid solution (1+3) 5mL, shakes up, it is made to generate triethylamine hydrochloride completely, add the methyl red indicator solution 1 of 1g/L, start from " dripping the sodium hydroxide solution of 100g/L " according to embodiment 1, proceed to measure.Consume the Hydrochloric Standard Titration 12.30 milliliters of 0.1003mol/L when titration is complete, result of calculation, recording triethylamine is 0.2497g.
And predicted according to relevant national standard determination method the triethylamine reagent 2.5128g that content is 99.1% in example, through get its 1/10th that is triethylamine quality be 0.2490g.
More than experiment is after the triethylamine of known content is quantitatively made triethylamine hydrochloride, then measures by this law, and the relative deviation of the triethylamine quality 0.2497g measured, the quality 0.2490g recorded with standard method is 0.14%.
Conclusion: this method measurement result is consistent with standard method result.
Embodiment 3-7(Accuracy Verification: recovery testu)
In order to the accuracy of further check analysis method, using standard samples recovery is additionally used: the triethylamine reagent adopting known content in above-described embodiment 2 is standard items in this example, the each 5mL of triethylamine standard solution made in accurate extraction embodiment 2, be placed in 5 separating funnels respectively, respectively add hydrochloric acid solution (1+3) 5mL.Take each about 1g of various sample of 5 known triethylamine hydrochloride content again, claim accurate to 0.0002g, be placed in this 5 separating funnels respectively, shake up, add the methyl red indicator solution 1 of 1g/L, start from " dripping the sodium hydroxide solution of 100g/L " according to embodiment 1, proceed measurement and calculation, its specific experiment and calculating data see the following form 1.
Table 1
As seen from Table 1, the triethylamine hydrochloride recovery is between 96.87% ~ 99.36%, and average recovery rate is 98.15%, illustrates that this assay method is accurate.
For the sample of recovery testu, be respectively the reactant liquor in organic chemical industry's production run, mother liquor, intermediate product, waste residue and waste liquid.
Although mark-on experiment is for triethylamine hydrochloride, but due to the measuring principle of this law be with alkali, triethylamine salt is converted into triethylamine after, carry out extracting, separatory, titration, other inorganic acid salts that therefore this law measures triethylamine or triethylamine also have the effect identical with its hydrochloride.
Embodiment 8(Precision Experiment)
Select same sample, take after six parts respectively, according to the step described in embodiment 1, carry out triethylamine hydrochloride assay and calculating, the average content recording triethylamine hydrochloride in this sample is 31.38%, RSD=0.59%, and its concrete data see the following form 2.
Table 2
Embodiment 9
Selected sample (waste liquid containing triethylamine hydrochloride) quality is 4.2946g, consume the Hydrochloric Standard Titration 4.60mL that concentration is 0.1003mol/L, other specific experiment steps and parameter see embodiment 1, result of calculation: in sample, the content of triethylamine salt is in triethylamine, its massfraction
(%)=2.17.
Claims (7)
1. an assay method for triethylamine salt content, is characterized in that, it is undertaken by the following stated step:
1), take sample containing triethylamine salt, in the separating funnel filling water, shake up, add methyl red indicator solution;
2), drip sodium hydroxide solution, limit edged shakes, and it is suitably excessive again after yellow for dropping to solution;
3), add chloroform, jolting, and note venting;
4), after stratification, separatory, collects extract;
5), draw extract collected by part, add and fill in the triangular flask of polar solvent, then add methyl red indicator solution;
6), with Hydrochloric Standard Titration, solution is titrated to orange red by xanthochromia;
7) content of triethylamine salt in sample, is calculated
In sample, triethylamine salt content is in triethylamine, its massfraction with
(%) represent, result is calculated as follows:
In formula,
---the actual concentrations of Hydrochloric Standard Titration, unit is mole often liter (mol/L);
---the consumption of Hydrochloric Standard Titration during titration, unit is milliliter (mL);
---the volume of the extract of absorption, unit is milliliter (mL);
v 0 ---the methenyl choloride volume added, unit is milliliter (mL);
---the exact value of sample mass, unit is gram (g);
0.1012---with 1mL Hydrochloric Standard Titration [
=1.000mol/L] suitable for a gram quality for the triethylamine represented.
2. the assay method of triethylamine salt content according to claim 1, it is characterized in that: in described step 5), ethanol elected as by described polar solvent.
3. the assay method of triethylamine salt content according to claim 1, it is characterized in that: in described step 5), the aqueous solution of ethanol elected as by described polar solvent.
4. the assay method of triethylamine salt content according to claim 3, is characterized in that: the ratio of described chloroform, second alcohol and water is according to volume ratio=10:20:5 proportioning.
5. the assay method of triethylamine salt content according to claim 3, is characterized in that: the ratio-dependent of described chloroform, second alcohol and water is the ethanolic solution 30mL that the agent of every 10mL chloroform extraction adds that concentration is 80+20.
6., according to the assay method of the arbitrary described triethylamine salt content of claim 1-5, it is characterized in that: described step 2) in, after measuring 2mL ~ 3mL after sodium hydroxide solution addition is defined as methyl red flavescence look.
7. the assay method of triethylamine salt content according to claim 1, is characterized in that, specifically, the inventive method is undertaken by the following stated step:
1), take sample 1 ~ 5g containing triethylamine salt, claim accurate to 0.0002g, be placed in the separating funnel filling 20mL water, shake up, add the methyl red indicator solution 1 ~ 2 of 1g/L;
2), drip the sodium hydroxide solution of 100g/L, limit edged shakes, to solution in time yellow after amount 2mL ~ 3mL;
3), more accurately add methenyl choloride 20mL, jolting 1 minute, jolting 140 ~ 160 times, and note venting;
4), leave standstill, after layering, slowly open funnel stopcock, discard the chloroform extraction liquid 2 ~ 3mL flowed down at first, then residue extract is collected in the container of dried and clean;
5) the extract 10mL collected by, accurately drawing adds in the triangular flask filling 30mL ethanolic solution (80+20), adds the methyl red indicator solution 1 of 1g/L;
6), with the Hydrochloric Standard Titration of 0.1 mol/L, solution is titrated to orange red by xanthochromia;
7), result calculates
In sample, triethylamine salt content is in triethylamine, its massfraction with
(%) represent, result is calculated as follows:
In formula,
---the actual concentrations of Hydrochloric Standard Titration, unit is mole often liter (mol/L);
---the consumption of Hydrochloric Standard Titration during titration, unit is milliliter (mL);
---the volume of the extract of absorption, unit is milliliter (mL);
v 0 ---the methenyl choloride volume added, unit is milliliter (mL);
---the exact value of sample mass, unit is gram (g);
0.1012---with 1mL Hydrochloric Standard Titration [
=1.000mol/L] suitable for a gram quality for the triethylamine represented.
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| CN102040522A (en) * | 2010-12-14 | 2011-05-04 | 青岛瀚生生物科技股份有限公司 | Method for recycling triethylamine from production of propargite |
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| RU2011970C1 (en) * | 1991-07-08 | 1994-04-30 | Научно-производственное объединение "Государственный институт прикладной химии" | Method for determining triethylamine |
| CN101307002A (en) * | 2008-06-24 | 2008-11-19 | 山东潍坊润丰化工有限公司 | Recovery method of triethylamine in glyphosate mother liquid |
| CN102153479A (en) * | 2011-02-24 | 2011-08-17 | 浙江新华制药有限公司 | Recovering and applying method of triethylamine in acylation liquid for preparing levofloxacin 1 |
| CN202221411U (en) * | 2011-09-09 | 2012-05-16 | 苏州浩波科技股份有限公司 | Triethylamine gas detection device |
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Address after: 401220 No. 3, Huabei Road, economic and Technological Development Zone, Changshou District, Chongqing Patentee after: CHONGQING UNISPLENDOUR INTERNATIONAL CHEMICAL Co.,Ltd. Address before: 401220 North District of Huabei Road, Changshou District (Changshou) chemical industry park, Chongqing Patentee before: CHONGQING UNISPLENDOUR INTERNATIONAL CHEMICAL Co.,Ltd. |