CN102901764B - Method for testing trace moisture in dimethyl sulfoxide - Google Patents
Method for testing trace moisture in dimethyl sulfoxide Download PDFInfo
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- CN102901764B CN102901764B CN201210338717.8A CN201210338717A CN102901764B CN 102901764 B CN102901764 B CN 102901764B CN 201210338717 A CN201210338717 A CN 201210338717A CN 102901764 B CN102901764 B CN 102901764B
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Abstract
The invention provides a method for testing trace moisture in dimethyl sulfoxide. Prepared ethanol water is divided into two parts; a first part of the ethanol water is used for preparing a uniform transparent mixed system of dimethyl sulfoxide, hydroxylamine hydrochloride, the ethanol water and a Karl Fischer's reagent; and a second part of the ethanol water is used for comparison of moisture content with the uniform transparent mixed system of dimethyl sulfoxide, hydroxylamine hydrochloride, the ethanol water and the Karl Fischer's reagent. In the system where dimethyl sulfoxide and the Karl Fischer's reagent coexist, dimethyl sulfoxide has the capability of oxidizing I<-> ions and is reduced to be dimethyl thioether. According to the invention, since hydroxylamine hydrochloride in the Karl Fischer's reagent containing dimethyl sulfoxide is pre-oxidized by dimethyl sulfoxide, it is guaranteed that the I<-> ions are completely converted into I2 through an electrode, testing results are real, reliable and stable, and deficiency in testing of trace moisture in a dimethyl sulfoxide solution by using Karl Fischer coulometry is overcome.
Description
Technical field
The present invention relates to micro-moisture field tests, specifically a kind of method of testing micro-moisture in dimethyl sulfoxide (DMSO).
Background technology
Dimethyl sulfoxide (DMSO) is a kind of organic compounds containing sulfur, it under normal temperature, is the transparency liquid of no color or smell, it is a kind of hygroscopic flammable liquid, there is high polarity, higher boiling, Heat stability is good, non-proton, with the characteristic such as water is miscible, can be dissolved in ethanol, propyl alcohol, with most of organism such as chloroforms, be described as " alembroth ", be widely used as solvent and reaction reagent, in particular as process solvent and the solvent that reels off raw silk from cocoons, as polyurethane synthesizes and the solvent that reels off raw silk from cocoons, polyamide, the synthetic of polyimide and polysulfone resin, and aromatic hydrocarbons, the solvent of Butadiene Extraction solvent and synthetic cloflucarban etc.Outside, in medical industry, be also widely used.Dimethyl sulfoxide (DMSO) is very crucial to the requirement of moisture as the solvent in acrylonitrile polymerization reaction, and therefore analyzing and measuring micro-moisture content in dimethyl sulfoxide (DMSO) is the important means of controlling product quality.
In organism, the method for testing of moisture is a lot, gas chromatography, on August 29th, 2007 the disclosed patent No. be in CN101025407A, disclose and in the patent document that name is called " analytical approach that chromatography of gases is measured micro-moisture in cyclopropylamine ", overcome normalization method and need the long period to wait for that all components all goes out the shortcoming that just can draw measurement result behind peak, adopt internal standard method to carry out quantitative test, offset stability of instrument poor, the quantitative test error that the reason such as sample size is not accurate enough is brought.But internal standard method also exist internal standard compound and reference material selection and processing, determine the stability of chromatographic condition, the calculating of correction factor, the defect such as expend time in long.Classical KF volumetric method, advantage be to improve and reagent automatically with addition of, the improvement of terminal and reagent.But KF volumetric method also exists the shortcoming that need frequently measure titer due to reagent imperfect stability, makes test process loaded down with trivial details, and at the bottom of test result degree of accuracy, work efficiency can not significantly improve.Karl Fischer coulomb method, the elemental iodine producing by electrolysis be called " electronics dropper " can high precision carry out with addition of, utilize electric charge and I-to generate quantitative relationship strict between elemental iodine simultaneously and calculate moisture.Karl Fischer coulomb method is absolute determination, without measuring titer.The current efficiency that only need guarantee I-generation elemental iodine is 100%, and present reagent can reach this requirement.
It is a kind of electrochemical method that karl Fischer coulomb method is measured moisture, its principle is that the Ka Shi reagent in the electrolytic cell of instrument injects moisture sample while reaching balance, water participates in the redox reaction of iodine, sulphuric dioxide, the in the situation that of pyridine and methyl alcohol existence, generate hydroiodic acid pyridine and methylsulfuric acid pyridine, the iodine having consumed produces at anode electrolysis, thereby redox reaction is constantly carried out, until moisture all exhausts, according to Faraday's laws of electrolysis, the electric weight relation in direct ratio that electrolysis generation iodine consumes while being same electrolysis, its reaction is as follows:
H
2O+I
2+SO
2+3C
5H
5N→2C
5H
5N·HI+C
5H
5N·SO
3
C
5H
5N·SO
3+CH
3OH→C
5H
5N·HSO
4CH
3
In electrolytic process, electrode reaction is as follows:
Anode: 2I
--2e
-→ I
2
Negative electrode: 2H
++ 2e
-→ H
2↑
From above reaction, can find out, i.e. the sulphuric dioxide of the elemental iodine of 1mol oxidation 1mol, needs the water of 1mol, so be that 1mol iodine reacts with the equivalent of 1mol water, the electric weight of electrolysis iodine is equivalent to the electric weight of brine electrolysis.Because its method of testing is easy, quick, accurate, in measuring, the analysis of organism micro-moisture obtains general application.
Xian Kangben Material Co., Ltd. mainly utilizes karl Fischer coulomb Moisture Meter test production PAN-based carbon fiber starting material used as vinyl cyanide, methyl acrylate, moisture in the solution such as solvent dimethyl sulfoxide (DMSO), secondly also comprises for technological experiment needs and now configures the moisture in solution.A large amount of experimental results show, Ka Feixiu coulomb method is measured the data stabilization of liquid water content in solution, reliable results, but when test dimethyl sulphoxide solution liquid water content, but occurred along with the prolongation test result of test duration is unstable, and existed integrated testability result lower than this problem of actual value; While finding again that karl Fischer coulomb method is measured in certain solution liquid water content, data are reliable and stable, if add after a certain amount of dimethyl sulfoxide (DMSO) in the Ka Shi reagent in titration cup, while again testing the water cut of this solution, appearance overall data sharply declines and is unstable, illustrate when dimethyl sulfoxide (DMSO) exists in Ka Shi reagent, can the result of test be produced and be disturbed.
Summary of the invention
Occur that test result is unstable when overcoming in Ka Erbenfeixiu coulomb method test dimethyl sulphoxide solution micro-moisture, eliminate while being mixed with dimethyl sulphoxide solution in the Ka Shi reagent in titration cup simultaneously, to the interference of other solution water cut test result, occur that test result is unstable, along with the prolongation integrated testability result of test duration is lower than the deficiency of actual value, the present invention proposes a kind of method of testing micro-moisture in dimethyl sulfoxide (DMSO).
Detailed process of the present invention comprises the following steps:
Step 1, preparation ethanol water.Described ethanol water is formulated by ethanol and pure water.In ethanol water, the massfraction of pure water is 0.9～1.2%.Absolute ethyl alcohol is mixed with pure water, obtain ethanol water.Prepared ethanol water is divided into 2 parts, and it is for subsequent use that first part of ethanol water is used as new Ka Shi reagent for the preparation of the mixed liquor that has Ka Shi reagent.Second part of ethanol water is used for the contrast of its water cut test result under different condition.
Step 2, the water cut of second part of ethanol water that test obtains for the first time.By coulomb Moisture Meter, the water cut of described second part of ethanol water is carried out to repeatedly parallel testing, and get its mean value as test result.
Step 3 adds dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup.In described coulomb of Moisture Meter titration cup, pack 100～150mL Ka Shi reagent into.To the dimethyl sulfoxide (DMSO) 5mL that adds water cut ﹤ 0.1% in the Ka Shi reagent in described coulomb Moisture Meter titration cup, obtain the Ka Shi reagent that contains dimethyl sulfoxide (DMSO).
Step 4, the water cut of second part of ethanol water that test obtains for the second time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Concrete test process is, in the water cut of the described second part of ethanol water of the ready rear test of coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, repeatedly the mean value of parallel testing result is 0.801%.The comparison of test result for the first time of this second part of ethanol water water cut that described test result and step 2 are obtained.While proving to have dimethyl sulfoxide (DMSO) in Ka Shi reagent, dimethyl sulfoxide (DMSO) has obvious impact to the test result of ethanol water water cut, and test result is obviously on the low side and unstable, and between data, deviation is large, and data are unreliable.
Step 5, prepares oxammonium hydrochloride solution.Concrete preparation process is, taking ethanol water as solvent, sour azanol is dissolved as to oxammonium hydrochloride solution, the proportioning of oxammonium hydrochloride and described first part of ethanol water is to add 30mL ethanol water in every 1g oxammonium hydrochloride, and put into 30～40 DEG C of water-baths and fully dissolve after mixing, obtain 1 part of oxammonium hydrochloride solution.
Step 6, the mixed liquor of the sour hydroxylamine solution that preparation contains dimethyl sulfoxide (DMSO).In described sour hydroxylamine solution, add dimethyl sulfoxide (DMSO), in every 1 part of oxammonium hydrochloride solution, add the dimethyl sulfoxide (DMSO) of 5mL water cut ﹤ 0.1% and leave standstill 0.5h, dimethyl sulfoxide (DMSO) and oxammonium hydrochloride solution are fully mixed, obtain the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO) of 1 part of homogeneous transparent.
Step 7, is prepared with the mixed liquor of Ka Shi reagent.Concrete preparation process is, in the mixed liquor of the described sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), add 100～120mL Ka Shi reagent, and place 20～24h under the water-bath of 30～35 DEG C, the Ka Shi reagent adding is fully mixed with the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), obtain the mixed liquor of Ka Shi reagent.
Step 8, changes the former Ka Shi reagent that is mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup.Concrete Renewal process is, remove the Ka Shi reagent that has been mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup, in the mixed liquor that has Ka Shi reagent obtaining in step 7 is poured coulomb Moisture Meter titration cup into as new Ka Shi reagent, in order to the water cut of second part of ethanol water obtaining of test.
Step 9, the water cut of second part of ethanol water that test obtains for the third time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Concrete test process is, in the water cut of the described second part of ethanol water of the ready rear test of coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, repeatedly the mean value of parallel testing result is 1.034%, compared with step 2 test result, test result data is stable, and deviation is in controlled range, and data are reliable.
In step 3, in the Ka Shi reagent in described coulomb of Moisture Meter titration cup, add described 5mL dimethyl sulfoxide (DMSO) points for ten times, and until before Ka Shi reagent complete reaction, a coulomb Moisture Meter in the dimethyl sulfoxide (DMSO) and the titration cup that once add after automatically entering equilibrium state, again in coulomb Moisture Meter titration cup, add dimethyl sulfoxide (DMSO) next time; Circulation according to this, until be all added to 5mL dimethyl sulfoxide (DMSO) in the Ka Shi reagent in coulomb Moisture Meter titration cup.
From reaction principle, the I of 1moL
2the SO of oxidation 1moL
2, need the water of 1moL, there is 2moL I in reaction product
-, backward reaction 2moL I simultaneously
-change and produce 1moLI by electrode again
2.The moisture of detected solution and SO
2after complete reaction, backward reaction I-is changed produced I completely by electrode
2, a coulomb Moisture Meter enters balance and stability state automatically, and the quantity that coulomb Moisture Meter calculates electric charge transfer by self record instrument is simultaneously calculated the water cut in solution.Through conscientious research and analysis, consult relative literature simultaneously, discovery coexists in system dimethyl sulfoxide (DMSO) and Ka Shi reagent, and dimethyl sulfoxide (DMSO) has oxidation I
-ability, by the I in system
-be oxidized to I
2, self is reduced to dimethyl sulfide, this part of I
-with I
2between conversion realize by redox reaction, electric weight that this part should have been changed by electrode is calculated and is not counted by the registering instrument of coulomb Moisture Meter, make test result lower than actual value.Utilize this strong reducing property reagent of oxammonium hydrochloride, in the Ka Shi reagent that contains dimethyl sulfoxide (DMSO), dimethyl sulfoxide (DMSO) is preoxidized is oxammonium hydrochloride, thereby has ensured that I-is converted to I by electrode completely
2, make test result true, reliable, stable, problem is solved.
Embodiment
Embodiment mono-
The present embodiment is the method for micro-moisture in a kind of karl Fischer coulomb method test dimethyl sulfoxide (DMSO), and its detailed process comprises the following steps:
Step 1, preparation ethanol water.Described ethanol water is formulated by ethanol and pure water.In ethanol water, the massfraction of pure water is 0.9～1.2%, and in the present embodiment, in ethanol water, the massfraction of pure water is 1.2%.Concrete configuration process is, absolute ethyl alcohol is mixed with pure water, obtains ethanol water.Prepared ethanol water is divided into 2 parts, and it is for subsequent use that first part of ethanol water is used as new Ka Shi reagent for the preparation of the mixed liquor that has Ka Shi reagent; Second part of ethanol water is used for the contrast of its water cut test result under different condition.
Step 2, the water cut of second part of ethanol water that test obtains for the first time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Concrete test process is, in the water cut of the described second part of ethanol water of the ready rear test of coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of 5 parallel testing results is 1.185%.The test result of coulomb Moisture Meter is as follows:
The result of second part of ethanol water of coulomb Moisture Meter test is stable, and data deviation is in claimed range, and data are reliable, illustrates that coulomb Moisture Meter test ethanol water test result is normal;
Step 3 adds dimethyl sulfoxide (DMSO) in the titration cup of coulomb Moisture Meter.In described coulomb of Moisture Meter titration cup, pack 100～150mL Ka Shi reagent into, in the present embodiment, in described coulomb of Moisture Meter titration cup, packed 120mL Ka Shi reagent into.Specifically add the process of dimethyl sulfoxide (DMSO) to be, the syringe that is 1mL by specification is to the dimethyl sulfoxide (DMSO) 0.5mL that adds water cut ﹤ 0.1% in the Ka Shi reagent in titration cup, wait for that, after the Ka Shi reagent in titration cup and the moisture complete reaction in dimethyl sulfoxide (DMSO), a coulomb Moisture Meter enters equilibrium state automatically; Again to the dimethyl sulfoxide (DMSO) 0.5mL that adds water cut ﹤ 0.1% in titration cup, wait for that after Ka Shi reagent in titration cup and moisture complete reaction in dimethyl sulfoxide (DMSO), a coulomb Moisture Meter enters equilibrium state automatically; Cycling ten times according to this, accumulative total, to the dimethyl sulfoxide (DMSO) 5mL that adds water cut ﹤ 0.1% in titration cup, obtains being mixed with the Ka Shi reagent of dimethyl sulfoxide (DMSO);
Step 4, the water cut of second part of ethanol water that test obtains for the second time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Specifically test process is, the water cut of testing described second part of ethanol water by coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of 5 parallel testing results is 0.928%.The test result of coulomb Moisture Meter is as follows:
The comparison of test result for the first time of this second part of ethanol water water cut that described test result and step 2 are obtained; While proving to have dimethyl sulfoxide (DMSO) in Ka Shi reagent, dimethyl sulfoxide (DMSO) has obvious impact to the test result of ethanol water water cut, and test result is obviously on the low side and unstable, and between data, deviation is large, and data are unreliable;
Step 5, prepares oxammonium hydrochloride solution.Concrete preparation process is, taking ethanol water as solvent, sour azanol is dissolved as to oxammonium hydrochloride solution, the proportioning of oxammonium hydrochloride and described first part of ethanol water is to add 30mL ethanol water in every 1g oxammonium hydrochloride, and put into 30～40 DEG C of water-baths and fully dissolve after mixing, obtain 1 part of oxammonium hydrochloride solution.In the present embodiment, the temperature of water-bath is 35 DEG C;
Step 6, the mixed liquor of the sour hydroxylamine solution that preparation contains dimethyl sulfoxide (DMSO).Concrete preparation process is to add dimethyl sulfoxide (DMSO) in described sour hydroxylamine solution; In every 1 part of oxammonium hydrochloride solution, add the dimethyl sulfoxide (DMSO) of 5mL water cut ﹤ 0.1% and leave standstill 0.5h, dimethyl sulfoxide (DMSO) and oxammonium hydrochloride solution are fully mixed, obtaining the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO) of 1 part of homogeneous transparent;
Step 7, is prepared with the mixed liquor of Ka Shi reagent.Concrete preparation process is, in the mixed liquor of the described sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), add 100～120mL Ka Shi reagent, and place 20～24h under the water-bath of 30～35 DEG C, the Ka Shi reagent adding is fully mixed with the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), obtain the mixed liquor of Ka Shi reagent.If the mixed liquor that has Ka Shi reagent obtaining described exceedes 24h and there will be not clear crystal standing time, thereby affects measuring accuracy.In the present embodiment, the addition of described Ka Shi reagent is to add 110mL Ka Shi reagent in the mixed liquor of every part of sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), and the temperature of water-bath is 31 DEG C, and the water-bath time is 21h;
Step 8, changes the former Ka Shi reagent that is mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup.Concrete Renewal process is, remove the Ka Shi reagent that has been mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup, in the mixed liquor that has Ka Shi reagent obtaining in step 7 is poured coulomb Moisture Meter titration cup into as new Ka Shi reagent, in order to the water cut of second part of ethanol water obtaining of test;
Step 9, the water cut of second part of ethanol water that test obtains for the third time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Specifically test process is, the water cut of testing described second part of ethanol water by coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of more than 5 parallel testing result is 1.189%.The test result of coulomb Moisture Meter is as follows:
Compared with step 2 test result, test result data is stable, and deviation is in controlled range, and data are reliable, oxammonium hydrochloride can well be revised the interference of dimethyl sulfoxide (DMSO) to ethanol water liquid water content test result as can be seen here, has ensured the accuracy of test result.
Embodiment bis-
The present embodiment is the method for micro-moisture in a kind of karl Fischer coulomb method test dimethyl sulfoxide (DMSO), and its detailed process comprises the following steps:
Step 1, preparation ethanol water.Described ethanol water is formulated by ethanol and pure water.In ethanol water, the massfraction of pure water is 0.9～1.2%, and in the present embodiment, in ethanol water, the massfraction of pure water is 1.1%.Concrete configuration process is, absolute ethyl alcohol is mixed with pure water, obtains ethanol water.Prepared ethanol water is divided into 2 parts, and it is for subsequent use that first part of ethanol water is used as new Ka Shi reagent for the preparation of the mixed liquor that has Ka Shi reagent; Second part of ethanol water is used for the contrast of its water cut test result under different condition;
Step 2, the water cut of second part of ethanol water that test obtains for the first time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Concrete test process is, in the water cut of the described second part of ethanol water of the ready rear test of coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of 5 parallel testing results is 1.187%.The test result of coulomb Moisture Meter is as follows:
The result that coulomb Moisture Meter is tested this ethanol water is stable, and data deviation is in claimed range, and data are reliable, illustrates that coulomb Moisture Meter test ethanol water test result is normal.
Step 3 adds dimethyl sulfoxide (DMSO) in the titration cup of coulomb Moisture Meter.In described coulomb of Moisture Meter titration cup, pack 100～150mL Ka Shi reagent into, in the present embodiment, in described coulomb of Moisture Meter titration cup, packed 130mL Ka Shi reagent into.Specifically add the process of dimethyl sulfoxide (DMSO) to be, the syringe that is 1mL by specification is to the dimethyl sulfoxide (DMSO) 0.5mL that adds water cut ﹤ 0.1% in the Ka Shi reagent in titration cup, wait for that, after the Ka Shi reagent in titration cup and the moisture complete reaction in dimethyl sulfoxide (DMSO), a coulomb Moisture Meter enters equilibrium state automatically; Again to the dimethyl sulfoxide (DMSO) 0.5mL that adds water cut ﹤ 0.1% in titration cup, wait for that after Ka Shi reagent in titration cup and moisture complete reaction in dimethyl sulfoxide (DMSO), a coulomb Moisture Meter enters equilibrium state automatically; Cycling ten times according to this, accumulative total is to the dimethyl sulfoxide (DMSO) 5mL that adds water cut ﹤ 0.1% in titration cup; Obtain being mixed with the Ka Shi reagent of dimethyl sulfoxide (DMSO);
Step 4, the water cut of second part of ethanol water that test obtains for the second time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Specifically test process is, the water cut of testing described second part of ethanol water by coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of 5 parallel testing results is 0.925%.The test result of coulomb Moisture Meter as:
The comparison of test result for the first time of this second part of ethanol water water cut that described test result and step 2 are obtained; While proving to have dimethyl sulfoxide (DMSO) in Ka Shi reagent, dimethyl sulfoxide (DMSO) has obvious impact to the test result of ethanol water water cut, and test result is obviously on the low side and unstable, and between data, deviation is large, and data are unreliable;
Step 5, prepares oxammonium hydrochloride solution.Concrete preparation process is, taking ethanol water as solvent, sour azanol is dissolved as to oxammonium hydrochloride solution, the proportioning of oxammonium hydrochloride and described first part of ethanol water is to add 30mL ethanol water in every 1g oxammonium hydrochloride, and put into 30～40 DEG C of water-baths and fully dissolve after mixing, obtain 1 part of oxammonium hydrochloride solution.In the present embodiment, the temperature of water-bath is 38 DEG C;
Step 6, the mixed liquor of the sour hydroxylamine solution that preparation contains dimethyl sulfoxide (DMSO).Concrete preparation process is to add dimethyl sulfoxide (DMSO) in described sour hydroxylamine solution; In every 1 part of oxammonium hydrochloride solution, add the dimethyl sulfoxide (DMSO) of 5mL water cut ﹤ 0.1% and leave standstill 0.5h, dimethyl sulfoxide (DMSO) and oxammonium hydrochloride solution are fully mixed, obtaining the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO) of 1 part of homogeneous transparent;
Step 7, is prepared with the mixed liquor of Ka Shi reagent.Concrete preparation process is, in the mixed liquor of the described sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), add 100～120mL Ka Shi reagent, and place 20～24h under the water-bath of 30～35 DEG C, the Ka Shi reagent adding is fully mixed with the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), obtain the mixed liquor of Ka Shi reagent.If the mixed liquor that has Ka Shi reagent obtaining described exceedes 24h and there will be not clear crystal standing time, thereby affects measuring accuracy.In the present embodiment, the addition of described Ka Shi reagent is to add 100mL Ka Shi reagent in the mixed liquor of every part of sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), and the temperature of water-bath is 33 DEG C, and the water-bath time is 23h;
Step 8, changes the former Ka Shi reagent that contains dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup.Concrete Renewal process is to remove the Ka Shi reagent that has been mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup; In the mixed liquor that has Ka Shi reagent obtaining in step 7 is poured coulomb Moisture Meter titration cup into as new Ka Shi reagent, in order to the water cut of second part of ethanol water obtaining of test;
Step 9, the water cut of second part of ethanol water that test obtains for the third time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Specifically test process is, the water cut of testing described second part of ethanol water by coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of more than 5 parallel testing result is 1.187%.The test result of coulomb Moisture Meter is as follows:
Compared with step 2 test result, test result data is stable, and deviation is in controlled range, and data are reliable, oxammonium hydrochloride can well be revised the interference of dimethyl sulfoxide (DMSO) to ethanol water liquid water content test result as can be seen here, has ensured the accuracy of test result.
Embodiment tri-
The present embodiment is the method for micro-moisture in a kind of karl Fischer coulomb method test dimethyl sulfoxide (DMSO), and its detailed process comprises the following steps:
Step 1, preparation ethanol water.Described ethanol water is formulated by ethanol and pure water.In ethanol water, the massfraction of pure water is 0.9～1.1.2%, and in the present embodiment, in ethanol water, the massfraction of pure water is 1.0%.Concrete configuration process is, absolute ethyl alcohol is mixed with pure water, obtains ethanol water.Prepared ethanol water is divided into 2 parts, and it is for subsequent use that first part of ethanol water is used as new Ka Shi reagent for the preparation of the mixed liquor that has Ka Shi reagent; Second part of ethanol water is used for the contrast of its water cut test result under different condition;
Step 2, the water cut of second part of ethanol water that test obtains for the first time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Concrete test process is, in the water cut of the described second part of ethanol water of the ready rear test of coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of 5 parallel testing results is 1.185%.The test result of coulomb Moisture Meter is as follows:
The result that coulomb Moisture Meter is tested this ethanol water is stable, and data deviation is in claimed range, and data are reliable, illustrates that coulomb Moisture Meter test ethanol water test result is normal.
Step 3 adds dimethyl sulfoxide (DMSO) in the titration cup of coulomb Moisture Meter.In described coulomb of Moisture Meter titration cup, pack 100～150mL Ka Shi reagent into, in the present embodiment, in described coulomb of Moisture Meter titration cup, packed 140mL Ka Shi reagent into.Specifically add the process of dimethyl sulfoxide (DMSO) to be, the syringe that is 1mL by specification is to the dimethyl sulfoxide (DMSO) 0.5mL that adds water cut ﹤ 0.1% in the Ka Shi reagent in titration cup, wait for that, after the Ka Shi reagent in titration cup and the moisture complete reaction in dimethyl sulfoxide (DMSO), a coulomb Moisture Meter enters equilibrium state automatically; Again to the dimethyl sulfoxide (DMSO) 0.5mL that adds water cut ﹤ 0.1% in titration cup, wait for that after Ka Shi reagent in titration cup and moisture complete reaction in dimethyl sulfoxide (DMSO), a coulomb Moisture Meter enters equilibrium state automatically; Cycling ten times according to this, accumulative total is to the dimethyl sulfoxide (DMSO) 5mL that adds water cut ﹤ 0.1% in titration cup; Obtain being mixed with the Ka Shi reagent of dimethyl sulfoxide (DMSO);
Step 4, the water cut of second part of ethanol water that test obtains for the second time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Specifically test process is, the water cut of testing described second part of ethanol water by coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of 5 parallel testing results is 0.925%.The test result of coulomb Moisture Meter as:
The comparison of test result for the first time of this second part of ethanol water water cut that described test result and step 2 are obtained; While proving to have dimethyl sulfoxide (DMSO) in Ka Shi reagent, dimethyl sulfoxide (DMSO) has obvious impact to the test result of ethanol water water cut, and test result is obviously on the low side and unstable, and between data, deviation is large, and data are unreliable;
Step 5, prepares oxammonium hydrochloride solution.Concrete preparation process is, taking ethanol water as solvent, sour azanol is dissolved as to oxammonium hydrochloride solution, the proportioning of oxammonium hydrochloride and described first part of ethanol water is to add 30mL ethanol water in every 1g oxammonium hydrochloride, and put into 30～40 DEG C of water-baths and fully dissolve after mixing, obtain 1 part of oxammonium hydrochloride solution.In the present embodiment, the temperature of water-bath is 33 DEG C;
Step 6, the mixed liquor of the sour hydroxylamine solution that preparation contains dimethyl sulfoxide (DMSO).Concrete preparation process is to add dimethyl sulfoxide (DMSO) in described sour hydroxylamine solution; In every 1 part of oxammonium hydrochloride solution, add the dimethyl sulfoxide (DMSO) of 5mL water cut ﹤ 0.1% and leave standstill 0.5h, dimethyl sulfoxide (DMSO) and oxammonium hydrochloride solution are fully mixed, obtaining the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO) of 1 part of homogeneous transparent;
Step 7, is prepared with the mixed liquor of Ka Shi reagent.Concrete preparation process is, in the mixed liquor of the described sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), add 100～120mL Ka Shi reagent, and place 20～24h under the water-bath of 30～35 DEG C, the Ka Shi reagent adding is fully mixed with the mixed liquor of the sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), obtain the mixed liquor of Ka Shi reagent.If the mixed liquor that has Ka Shi reagent obtaining described exceedes 24h and there will be not clear crystal standing time, thereby affects measuring accuracy.In the present embodiment, the addition of described Ka Shi reagent is to add 120mL Ka Shi reagent in the mixed liquor of every part of sour hydroxylamine solution that contains dimethyl sulfoxide (DMSO), and the temperature of water-bath is 35 DEG C, and the water-bath time is 22h;
Step 8, changes the former Ka Shi reagent that contains dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup.Concrete Renewal process is to remove the Ka Shi reagent that has been mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup; In the mixed liquor that has Ka Shi reagent obtaining in step 7 is poured coulomb Moisture Meter titration cup into as new Ka Shi reagent, in order to the water cut of second part of ethanol water obtaining of test;
Step 9, the water cut of second part of ethanol water that test obtains for the third time.Adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method.Specifically test process is, the water cut of testing described second part of ethanol water by coulomb Moisture Meter.For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, and get its mean value as test result.In the present embodiment, the mean value of more than 5 parallel testing result is 1.186%.The test result of coulomb Moisture Meter is as follows:
Compared with step 2 test result, test result data is stable, and deviation is in controlled range, and data are reliable, oxammonium hydrochloride can well be revised the interference of dimethyl sulfoxide (DMSO) to ethanol water liquid water content test result as can be seen here, has ensured the accuracy of test result.
Claims (2)
1. a method of testing micro-moisture in dimethyl sulfoxide (DMSO), is characterized in that, detailed process is:
Step 1, preparation ethanol water: described ethanol water is formulated by ethanol and pure water; In ethanol water, the massfraction of pure water is 0.9～1.2%; Absolute ethyl alcohol is mixed with pure water, obtain ethanol water; Prepared ethanol water is divided into 2 parts, and first part of ethanol water is for the preparation of the mixed liquor that has Ka Shi reagent; Second part of ethanol water is used for the contrast of water cut test result under different condition;
Step 2, the water cut of second part of ethanol water that test obtains for the first time: by coulomb Moisture Meter, the water cut of described second part of ethanol water is carried out to repeatedly parallel testing, and the water cut mean value of getting described second part of ethanol water is as test result;
Step 3 adds dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup: in described coulomb of Moisture Meter titration cup, pack 100～150mL Ka Shi reagent into; To the dimethyl sulfoxide (DMSO) 5mL that adds water cut ﹤ 0.1% in the Ka Shi reagent in described coulomb Moisture Meter titration cup, obtain the Ka Shi reagent that contains dimethyl sulfoxide (DMSO);
Step 4, the water cut of second part of ethanol water that test obtains for the second time: adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method; Concrete test process is, in the water cut of the described second part of ethanol water of the ready rear test of coulomb Moisture Meter; For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, repeatedly the mean value of parallel testing result is 0.801%; The comparison of test result for the first time of this second part of ethanol water water cut that described test result and step 2 are obtained; While proving to have dimethyl sulfoxide (DMSO) in Ka Shi reagent, dimethyl sulfoxide (DMSO) has obvious impact to the test result of ethanol water water cut, and test result is obviously on the low side and unstable, and between data, deviation is large, and data are unreliable;
Step 5, prepare oxammonium hydrochloride solution: concrete preparation process is, taking ethanol water as solvent, oxammonium hydrochloride is dissolved as to oxammonium hydrochloride solution, the proportioning of oxammonium hydrochloride and described first part of ethanol water is to add 30mL ethanol water in every 1g oxammonium hydrochloride, and put into 30～40 DEG C of water-baths and fully dissolve after mixing, obtain 1 part of oxammonium hydrochloride solution;
Step 6, the mixed liquor of the oxammonium hydrochloride solution that preparation contains dimethyl sulfoxide (DMSO): add dimethyl sulfoxide (DMSO) in described oxammonium hydrochloride solution, in every 1 part of oxammonium hydrochloride solution, add the dimethyl sulfoxide (DMSO) of 5mL water cut ﹤ 0.1% and leave standstill 0.5h, dimethyl sulfoxide (DMSO) and oxammonium hydrochloride solution are fully mixed, obtain the mixed liquor of the oxammonium hydrochloride solution that contains dimethyl sulfoxide (DMSO) of 1 part of homogeneous transparent;
Step 7, be prepared with the mixed liquor of Ka Shi reagent: concrete preparation process is, in the mixed liquor of the described oxammonium hydrochloride solution that contains dimethyl sulfoxide (DMSO), add 100～120mL Ka Shi reagent, and place 20～24h under the water-bath of 30～35 DEG C, the Ka Shi reagent adding is fully mixed with the mixed liquor of the oxammonium hydrochloride solution that contains dimethyl sulfoxide (DMSO), obtain the mixed liquor of Ka Shi reagent;
Step 8, change the former Ka Shi reagent that is mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup: remove the Ka Shi reagent that has been mixed with dimethyl sulfoxide (DMSO) in coulomb Moisture Meter titration cup, in the mixed liquor that has Ka Shi reagent obtaining in step 7 is poured coulomb Moisture Meter titration cup into as new Ka Shi reagent, in order to the water cut of second part of ethanol water obtaining of test;
Step 9, the water cut of second part of ethanol water that test obtains for the third time: adopt coulomb Moisture Meter by the water cut of second part of ethanol water of sample injection method test of decrement method; Concrete test process is, in the water cut of the described second part of ethanol water of the ready rear test of coulomb Moisture Meter; For obtaining test result accurately, need carry out repeatedly parallel testing to the water cut of second part of ethanol water, repeatedly the mean value of parallel testing result is 1.034%, compared with step 2 test result, test result data is stable, and deviation is in controlled range, and data are reliable.
2. a kind of method of testing micro-moisture in dimethyl sulfoxide (DMSO) as claimed in claim 1, it is characterized in that, in step 3, in the Ka Shi reagent in described coulomb of Moisture Meter titration cup, add dimethyl sulfoxide (DMSO) points for ten times, and until before Ka Shi reagent complete reaction, a coulomb Moisture Meter in the dimethyl sulfoxide (DMSO) and the titration cup that once add after automatically entering equilibrium state, again in coulomb Moisture Meter titration cup, add dimethyl sulfoxide (DMSO) next time; Circulation according to this, until be all added to 5mL dimethyl sulfoxide (DMSO) in the Ka Shi reagent in coulomb Moisture Meter titration cup.
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| US3656907A (en) * | 1969-07-14 | 1972-04-18 | Clive Stephen Delmonte | Modified karl fischer reagent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3656907A (en) * | 1969-07-14 | 1972-04-18 | Clive Stephen Delmonte | Modified karl fischer reagent |
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