CN106680265A - Method for measuring concentration of hydrochloric acid generated in trichloromethane under ultrasonic wave condition - Google Patents

Method for measuring concentration of hydrochloric acid generated in trichloromethane under ultrasonic wave condition Download PDF

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CN106680265A
CN106680265A CN201611235886.3A CN201611235886A CN106680265A CN 106680265 A CN106680265 A CN 106680265A CN 201611235886 A CN201611235886 A CN 201611235886A CN 106680265 A CN106680265 A CN 106680265A
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concentration
polymer
hydrochloric acid
mol
acid
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希尔艾力·买买提依明
茹科亚·麦提斯迪克
布海丽且姆·伊马木
司玛依·努尔拉
萨拉麦提·拜科日
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Xinjiang University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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Abstract

The invention relates to a method for measuring the concentration of hydrochloric acid generated in trichloromethane under the ultrasonic wave condition. The method is characterized in that the concentration of the generated hydrochloric acid is detected when ultrasonic time is 0-640 seconds. By measuring the ultraviolet-visible absorption spectra of a polymer/trichloromethane solution under the ultrasound condition and a polymer/trichloromethane/hydrochloric acid solution under the non-ultrasound condition, a linear relation is made according to the data, and accordingly the concentration of the hydrochloric acid generated in a trichloromethane solution under the ultrasound condition can be calculated. The method is easy to operate and implement, high in measuring speed and high in accuracy.

Description

A kind of assay method of the concentration of hydrochloric acid produced in chloroform under Ultrasonic Conditions
Technical field
The present invention relates to a kind of assay method of the concentration of hydrochloric acid produced in chloroform under Ultrasonic Conditions, with it The polymer of performance is offered reference for the application in the field such as pH or sensor.
Background technology
Concentration of hydrochloric acid measure is significant with industrial in scientific research, mainly uses sour when determining the PH of solution at present Alkali titration, acid base neutralization titration is carried out with standard solution of sodium hydroxide and determines concentration of hydrochloric acid, but utilizes this in the industrial production Method runs into many difficulties, and acid-base titrations are widely used in domain of inorganic chemistry. it is because the hydrochloric acid generated in Organic substance Concentration can not be measured in this way, why we using ultrasonic method to determine Organic substance in acid concentration. the present invention By different time ultrasound polymerization thing chloroformic solution, with time chloroform lowering of concentration, ultrasonic time can be found out according to this feature With the linear relationship of concentration so as to calculating acid concentration.
The eighties in 20th century, sonochemistry (Sonochemistry) or title sonochemistry rise as a frontier branch of science, profit Accelerate chemical reaction with ultrasound wave, the attention of countries in the world researcher has been caused at present, and have in difficult degradation Organic pollutants improvement aspect achieve gratifying effect. ultrasound wave be to the degraded Basic Ways of water body organism cavitation and Radical reaction.In the presence of ultrasound wave, the small complex in liquid is intensified, show as the concussion of complex, growth, A series of dynamic processes such as contraction or even collapse, this process is to concentrate sound field energy, and the adiabatic mistake for discharging rapidly Journey. with high temperature, the high pressure for occurring during ultrasonic cavitation, make the hydrone entered in microvesicle rupture, produce H and OH .OH and H are the free radicals of high response, and property is active, and with very strong oxidability, it is difficult under normal condition to make The organic matter degradation of decomposition.Ultrasonic degradation Organic substance is simple to operate with low cost compared with additive method, pollution-free Advantage, there is significant superiority in terms of hardly degraded organic substance is processed, at the water factory that has a good application prospect is conventional , for the dissolved organic matter in water, especially disinfection byproduct (DBP) clearance is not high for science and engineering skill, must carry out advanced treating. each In Advanced Treatment of Drinking Water, ultrasonic Treatment becomes a kind of very promising technology with its above-mentioned advantage. at present for The research of ultrasonic Treatment sewage or Micropolluted watD is more.Ultrasound is used for the report of organic chemical reactionses, first appeared in 1938, main research water was made under conditions of cosolvent, the hydrolysis of esters and acetal；Carbon-carbon bond, the fracture of carbon-halogen bond and The reaction such as oxidation.
Generally, it is considered that ultrasonic effect is relevant with the appearance of following several phenomenons：During sound pressure variations, solvent is subject to compression and sparse work With making fluid produce motion drastically；Under conditions of air pocket and temperature rise very little is produced, a large amount of vibrational energies are input into into micro volume When microjet effect. it is wherein relatively more directly perceived, it has been generally acknowledged that most important phenomenon is the appearance of air pocket. and think those sizes The shock wave that unstable microbubble is produced when growing up so that bursting suddenly is ultrasound to the main of chemical reaction generation effect Reason. in above process, not only sometimes it is observed that luminescence phenomenon, and root is it is estimated that when microvesicle bursts, Ke Yi The pressure for being up to 1011Pa is produced in local space, up to 104-106K. at present, external force field is to chemical reaction for central temperature Impact has become a focus in chemical research problem. and it is not only that chemist has opened up promotion and changed chemical reaction course New technique, and be that traditional chemical thermodynamicses without external force field action and chemical kineticses absorb in theory Contemporary Physics Achievement is accumulated experience and factual materials and important channel. importantly, they will provide new technique for commercial Application Approach. the Prior efforts of application ultrasound, carry out in water phase mostly. ultrasound can make to produce hydrogen peroxide and hydrogen in water phase, Oxidation primary chemical effect with it under irradiation of some solutes under ultrasonication be similar, it was demonstrated that under ultrasonication, Water decomposition becomes hydroxyl free radical and hydrogen atom. it is interesting that the saturated aqueous solution of methane and ethane is under ultrasonication, can be with The presence of formaldehyde and acetic acid is detected, but yield is very low.
Organohalogen compounds, for example：CH2Cl2, CHCl3And CCl4In aqueous medium, receive ultrasonication.Generate the bond fission of carbon chlorine The complexity of free radical and the stability order of free radical are identical with the photodissociation result of these compounds. because water is life Immanent medium in system, this is probably that water cross-talk chemical developer is much ahead of the acoustochemical important original of non-aqueous liquid phase Cause. the sonochemistry research as biomolecule such as protein, enzymes is shown, it is to cause many simple products that sound causes redox Main mechanism. for example：Pyrimidine, purine, pyrroles and porphyrin equimolecular are carried out after supersound process, it can be clearly observed purple The change of outer absorption spectrum, illustrates to generate sonochemical effect.
The present invention is coupled polycondensation reaction and is prepared for the polymer with preferable solubility property and it is surpassed by Sonogashira Changing color resulting from acid performance under the conditions of sound is inquired into.
Polymer synthesized by the present invention has certain dissolubility in conventional organic solvent. and Polymer optical performance test is tied Fruit shows：There is maximum absorption band at 423 nm in uv-visible absorption spectra of the polymer in chloroformic solution. polymer Chloroformic solution there is changing color resulting from acid phenomenon. with the increase of concentration of hydrochloric acid, on the intensity of the original absworption peak of copolymer is continuous Rise, and occur in that a new absworption peak, UV-Vis absworption peaks occur red shift.
The content of the invention
The present invention 3- dodecylthiophenes and 2- aminopyrimidines are that raw material passes through sonogashira coupling reaction successes Synthetic polymer is simultaneously adopted1 H-NMR、13 The means of testing such as CNMR, infrared spectrum, uv-visible absorption spectra, fluorescence spectrum, Its structure is characterized, the changing color resulting from acid performance under its unique ultrasound condition is inquired into. the main polymer solution that determines is super Ultraviolet-visible spectrum absorbance under the conditions of sound wave is over time. by constantly changing polymer-chloroform hydrochloric acid mixed solution Middle concentration of hydrochloric acid, is successfully prepared the polymer solution with variable concentrations, and polymer solution is tested：By ultraviolet suction Receive spectrum to test polymer-chloroform mixed liquor, determine polymeric acid mutagens color range and minimum response acid concentration.
As a result the conjugated polymer prepared in the present invention is shown, it has certain dissolubility in conventional organic solvent and has Changing color resulting from acid phenomenon, adds after hydrochloric acid in its chloroformic solution, and the absorption peak strength at 504 nm constantly rises.
Ultraviolet-visible spectrum can be obtained herein by the chloroformic solution supersound process of polymer, the chloroformic solution correspondence of polymer is not UV, visible light fluorescence spectrum can be drawn with the impact of acid concentration, then carries out supersound process by tetrahydrofuran solution and can see to calculate Error k.The actual concentrations in 32s-640s can be calculated by the relation of absorbance between the two and error again. it is dense during 32s Spend for 0.000139（1±0.045）Concentration when mol/L, 640s is 0.004621（10±.045）mol/L.
The purpose of the present invention：
An object of the present invention is to provide a kind of polymer with ultrasound wave discoloration in chloroformic solution.
The second object of the present invention ten is provided under ultrasound condition, the detection method of the concentration of hydrochloric acid produced in chloroform.
Description of the drawings
Fig. 1：The synthetic route of copolymer；
Fig. 2：Polymer solution UV-visible spectrum over time under Ultrasonic Conditions；
Fig. 3：UV-visible spectrum during polymer solution correspondence difference acid concentration；
Fig. 4：Polymer solution under uviol lamp ultrasound and heating after color change figure；
Fig. 5：Error Graph of the polymer solution in Ultrasonic Conditions；
Fig. 6：Polymer solution ultraviolet-visible light over time in the range of absorbance 0.06-0.12 under Ultrasonic Conditions Spectrum linear relationship chart.
Embodiment：
（1）Synthetic polymer：Room temperature, lucifuge, 2.44 mmol, 1g 2,5- are accurately weighed under nitrogen protection in 50ml there-necked flasks Two bromo- 3- dodecylthiophenes, 23mg Cu I, 86mg Pd (PPh3)2 Cl2, then inject eliminating water deoxygenation with syringe Diisopropylamine 30ml, after stirring 30 minutes, is gradually added dropwise to 0.8ml trimethylsilyl acetylenes, is gradually heating to 80 DEG C and returns Stream 3.5 hours, now, solution is in brown, after being cooled to room temperature, is filtered, and with a small amount of petroleum ether filter cake, decompression steams molten Agent, uses 4cm silica gel column chromatographies（Eluent petroleum ether）It is quick to cross post, remove de- liquid under reduced pressure（Time control 10min it It is interior）, obtain yellow liquid 1.02g（Thick yield may have part to be the petroleum ether being evaporated more than 100%）Directly taken off Silicon is tested, and pours 42 ml THF in product into, and 21 ml methanol, the KOH of 0.45 ml 20% are stirred at room temperature 8h, is stopped, sucking filtration, Decompression steams solvent（Within 10 min）, petroleum ether crosses column chromatography（Plus post is pressed through, within 30min）, Bluepoint is collected, steam molten Agent（Within 10 min, completed before solution colour becomes redness from yellow）Crude product is collected, copolymerization is directly carried out anti- Should.Estimate 2,5-diacetylene-3- dodecylthiophene percentage compositions are about 50%, take 0.4g crude products（Estimation contains 0.67 mmol, 0.2g, 2,5-diacetylene-3- dodecylthiophenes）, 0.67 mmol, 0.234g, 2- amino -4,6- diiodo-s Pyrimidine, 47 mg Pd4(PPh3), 13mg Cu I under nitrogen protection, together with 12 ml diisopropylamine and 30 ml toluene In being added to reactor, mixture heats 30 min at 80 DEG C, generates yellowish-brown polymer. and reactant mixture is cooled to After room temperature, it is added dropwise in the acetone in quick stirring and has precipitation to be formed. filter, collect filter cake and use acetone, hot second Alcohol and hot methanol repeated washing；
（2）The chloroformic solution of prepared polymer:5 mg polymer are taken, in being dissolved in 550 ml chloroform solvents, prepared polymer Chloroformic solution；
（3）The hydrochloric acid solution of configuration variable concentrations：Using the hydrochloric acid solution that concentration is 12.6 mol/L, constantly dilution configuration is different The hydrochloric acid solution of concentration. concentration is respectively 1.26 mol/L, 0.126 mol/L, 0.0126 mol/L, 0.00126 mol/L, 0.000126 mol/L.
（4）Prepared polymer-chloroform hydrochloric acid mixed solution：Constantly change concentration of hydrochloric acid in polymer-chloroform hydrochloric acid mixed solution, into The polymer solution of the preparation with variable concentrations of work(, determines change of the UV intensity with concentration, A concentration：5670*10-6mol/ L, B concentration：3025.26*10-6 mol/L, C concentration：1135.26*10-6mol/L, D concentration：505.26*10-6mol/L, E is dense Degree：253.26*10-6mol/L, F concentration：20.16*10-6mol/L, C straight polymer solution concentration：9*10-6mol/L. determine Fluorescence intensity with concentration change, 0mol/L, A concentration：20.79*10-6mol/L, B concentration：140.49*10-6mol/L, C is dense Degree：266*10-6mol/L, D concentration：581*10-6mol/L, E concentration：644*10-6mol/L.
（5）Polymer solution is tested：By ultra-violet absorption spectrum, the chloroform of Study Polymer Melts is molten under Ultrasonic Conditions Liquid changing color resulting from acid performance. the solution to having configured carries out ultrasound, with the difference of ultrasonic time, determines corresponding ultraviolet-visible Spectrum.
（6）Changing color resulting from acid recovers Journal of Sex Research：Absorbance is significantly improved after the chloroformic solution ultrasound of polymer, and it is heated Absorbance and fluorescence intensity return to original state. and color of the chloroformic solution of polymer under uviol lamp is blueness, after ultrasound Become yellow green, liquid color is gradually restored to original state under solution uviol lamp after heating.

Claims (5)

1. the present invention is a kind of assay method of the concentration of hydrochloric acid produced in chloroform under Ultrasonic Conditions, including following tool Body step：
（1）Synthesize the polymer to ultrasound wave colour developing（Fig. 1）.
（2）Configuration polymer/chloroform mixed solution simultaneously carries out ultrasound wave discoloration experiment.
Polymer solution concentration is：9*10-6 mol/L.
Under ultrasound condition, the pass between the absorbance at ultrasonic time and 504 nm is detected by uv-visible absorption spectra System.
Ultrasonic time is：0,32s, 40s, 80s, 160s, 320s, 480s, 640s. obtain ultraviolet-visible light spectral curve（Fig. 2）.
（3）Configuration polymer/chloroform/hydrochloric acid mixed solution simultaneously determines ultraviolet-visible spectrum（Fig. 3）. the purple of this mixed solution The establishment of spectrum relation obtained under outward-visible spectrum and Ultrasonic Conditions, obtains the sour concentration produced in chloroformic solution. polymerization The concentration of thing/chloroform/hydrochloric acid solution is：a）5670*10-6mol/L, b）3025.26*10-6mol/L, c）1135.26*10- 6mol/L, d）505.26*10-6mol/L, e）253.26*10-6mol/L, f）20.16*10-6mol/L, polymer solution concentration As the solution under ultrasound condition, it is：9*10-6mol/L.
（4）Changing color resulting from acid recovery technology：Polymer chloroformic solution ultrasound after, the absorbance at 504 nm significantly improve with it is glimmering Light intensity is reduced, and it is heated（70 degree, 30 minutes, then cool down）Absorbance and fluorescence intensity return to original state （Fig. 4）.
2. the measure side of the concentration of hydrochloric acid that a kind of according to claims 1 produces under Ultrasonic Conditions in chloroform Method, it is typically characterized by：When being prepared for the ultrasound in chloroformic solution by Sonogashira coupling polycondensation reactions, possesses acid The polymer of mutagens color property and by 1HNMR, IR proves the structure of compound.
3. the measure side of the concentration of hydrochloric acid that a kind of according to claims 1 produces under Ultrasonic Conditions in chloroform Method, it is typically characterized by：Opening relationships between spectrum is obtained under the conditions of the spectrum for obtaining and the acid adding set up under ultrasound condition, Computing formula is obtained, formula is as follows：
C=C0 exp-kt k= - 0.00951,C0=0.000203 0 < t < 32
k= - 0.00951, C0=0.000203 32 < t < 160
k= - 0.00386, C0=0.000493 160 < t < 640
C is concentration, and unit is mol/L, and C0 is initial concentration, and unit is mol/L, and t is
Time, unit is the second（second）.
4. the measure side of the concentration of hydrochloric acid that a kind of according to claims 1 produces under Ultrasonic Conditions in chloroform Method, it is typically characterized by：Uv-visible absorption spectra is carried out to polymer/chloroform/hydrochloric acid mixed solution, has successfully been determined The changing color resulting from acid sensitive volume of polymer and minimum response acid concentration.
5. the measure side of the concentration of hydrochloric acid that a kind of according to claims 1 produces under Ultrasonic Conditions in chloroform Method, it is typically characterized by：By the tetrahydrofuran solution Deca acid under Ultrasonic Conditions, drawn according to variable concentrations Absorbance data calculates error k=0.045（Fig. 5）. again linear relationship chart is made with the data obtained, needed for so as to obtain us Concentration（Fig. 6）；
Corresponding acid concentration=0.000139 of 32s（1±0.045）mol / L
Corresponding acid concentration=0.000188 of 40s（1±0.045）mol / L
Corresponding acid concentration=0.000433 of 80s（1±0.045）mol / L
Corresponding acid concentration=0.00092 of 160s（1±0.045）mol / L
Corresponding acid concentration=0.001697 of 320s（1±0.045）mol / L
Corresponding acid concentration=0.003159 of 480s（1±0.045）mol / L
Corresponding acid concentration=0.004621 of 640s（1±0.045）mol / L.
CN201611235886.3A 2016-12-28 2016-12-28 Method for measuring concentration of hydrochloric acid generated in trichloromethane under ultrasonic wave condition Pending CN106680265A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111122766A (en) * 2018-10-31 2020-05-08 Tcl集团股份有限公司 Method for detecting chloroform in sulfur-containing quantum dot solution

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CN105445210A (en) * 2015-11-12 2016-03-30 新疆大学 Method for detecting concentration of trifluoroacetic acid with polymer in acidichromism performance

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Publication number Priority date Publication date Assignee Title
CN105445210A (en) * 2015-11-12 2016-03-30 新疆大学 Method for detecting concentration of trifluoroacetic acid with polymer in acidichromism performance

Non-Patent Citations (4)

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XIRALI MAMTIMIN ET AL: "Acidochromicity of a Low-Molecular-Weight Pyrimidine-Based Copolymer", 《J. APPL. POLYM. SCI》 *
XIRALI MAMTIMIN ET AL: "New soluble rigid rod copolymers comprising alternating 2-amino-pyrimidine and phenylene repeat units: Syntheses, characterization, optical and electrochemical properties", 《POLYMER》 *
XIRALI MAMTIMIN ET AL: "Synthesis, characterization and acidochromism of Poly (2-N,N–dimethylamino-4,6-Bis (2-thienyl)-pyrimidine)", 《J POLYM RES》 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111122766A (en) * 2018-10-31 2020-05-08 Tcl集团股份有限公司 Method for detecting chloroform in sulfur-containing quantum dot solution

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Application publication date: 20170517