Method of quantitative determination of manganese, lead and nickel in bile by method of atomic-absorption analysis with atomisation in flame

FIELD: chemistry.

SUBSTANCE: invention relates to laboratory methods of analysis and deals with method of quantitative determination of manganese, lead and nickel in bile by method of atomic-absorption analysis with atomisation in flame. Essence of method lies in the following: sampling of bile is carried out during duodenal probing, after that it is frozen, and unfrozen at room temperature, homogenisation of bile by mixing being performed already at partial soft unfreezing. After that, sampling of homogenised bile is carried out for preparation for analysis, concentrated nitric acid is introduced into it with volume ratio 1:1, mixture is kept at room temperature, then heated and further mixture is kept for not less than 2.5 hours at room temperature. In order to obtain analyte, to obtained mixture added is concentrated hydrogen peroxide in volume ratio 1:1 to volume of bile sample volume, analyte is heated, after that cooled to room temperature. After that by method of atomic-absorption spectrometry, using graduated diagram, quantitative content of particular type of metal: manganese, lead and nickel is determined in analyte.

EFFECT: invention allows increasing accuracy of quantitative determination of manganese, lead and nickel in bile.

6 tb

 

The invention relates to the field of medical chemistry, in particular to health Toxicological research, and can be used in the diagnosis of environment-related pathologies caused by the presence of heavy metals in the human body.

The invention can find application in the laboratories of biochemistry, the specialized agencies and clinical diagnostic laboratories medical centers.

In the result of increasing anthropogenic impact is observed progressive pollution of geochemical elements, including heavy metals. The accumulation of various pollutants in the atmosphere, soil and water contribute to the emissions from industrial, domestic and agricultural wastes. These pollutants have a toxic effect on living organisms. So the accumulation of heavy metals (e.g. lead, manganese, Nickel, zinc, cadmium, cobalt, chromium and the like) in the body can lead to Central nervous and cardiovascular systems, to contribute to the emergence of chronic diseases of the gastrointestinal tract, etc. On the content of heavy metals in biological media (e.g., bile), you can identify the symptoms of various functional disorders hepatobiliary system and stomach of a man living the conditions of exposure to high anthropogenic load.

Currently known a number of methods for detecting specific types of heavy metals in biological media by atomic-absorption analysis, namely:

- RF patent №2342659 known "Method of determining the content of cadmium in organs and muscle tissue of pigs", according to which the level of manganese and potassium in kopitam the horn and the corresponding regression equations establish the content of cadmium;

- RF patent №2009484 known "Method of determination of cobalt in biological material", which produce a salinity sample of the biomaterial, the processing of picric acid, extraction of the chloroform solution - methylcyclohexene 1,1 - dicarboxylic acid, treatment of the extract with ethyl alcohol followed by atomic absorption analysis;

- RF patent №1257520 known "Method of determination of heavy metals in ectodermal tissues, whereby a sample of hair or nails is shredded, add to them a 30%solution of Tetramethylammonium, heated, then diluted with bidistilled water, centrifuged, separating the solution 1, and nerastvorim sediment transfer in soluble form nitric acid and perhydrol with obtaining a solution of 2, then the above solutions by atomic absorption analysis to determine cobalt, Nickel, copper, manganese, zinc.

However, all these known what local methods are complex, characterized by long time of determination and cannot be used as a biomaterial bile.

Closest to the proposed technical solution to the technical essence is a Method of determining the content of iron, zinc, Nickel in the bile by the method of atomic absorption, see 4.1 guidelines MUK 4.1.775-99 approved 06.07.1999, and was developed by the Department of state sanitary and epidemiological surveillance Ministry of health of Russia.

According to the method produces a sampling of bile in duodenal intubation of 5 cm3and with the help of atomic absorption analysis by direct determination measure metal concentrations, with the results of the measurements recorded on the readings with a digital indexing calibrated according to the working standard solutions of defined metal and are in the form: Xcf.±0,25·XWed,ág/cm3where Xcf. - the average value of the measured concentrations.

The disadvantage of this method is the instability of the results of the analysis in the study of samples of bile nonuniform viscosity and composition, however, we cannot exclude the influence of the organic component. In cases of heterogeneity of bile reliability of the results of research more than the allowable value of such the s operational control accuracy, stated in the mentioned known method.

The technical result achieved by the invention, is to improve the accuracy of quantitative determination of manganese, lead and Nickel in bile due to the transfer of samples of bile in the homogeneous condition, the decomposition of the organic component and, thereby, reduce its impact while saving used biomaterial.

The specified technical result is achieved by the proposed method for quantitative determination of manganese, lead and Nickel in bile by atomic-absorption analysis with atomization in flame, including the selection of bile and defining the quantitative content of heavy metals by the method of atomic absorption spectrometry, after selection bile produce freezing, then thawing, which at the same time, starting with partial soft defrost, carry out the homogenization of bile through mixing, then produce a selection of homogeneous samples of bile to prepare for the analysis, then the resulting sample is injected concentrated nitric acid in a volume ratio of 1:1, respectively, the mixture incubated at room temperature for 15-20 minutes, then heated for 5-10 minutes at a temperature of 120±5°C, then stand at least 2.5 hours at room temperature the round, then, to obtain the analyte to the resulting mixture concentrated hydrogen peroxide in a volume ratio of 1:1 to a sample volume of bile, the analyte is heated for 5-10 minutes at a temperature of 120±5°C, cooled to room temperature and then using the method of atomic absorption spectrometry and using the calibration curve, make a determination in the quantitative analyte content of a certain kind of metal is manganese, lead and Nickel, with concentrated nitric acid and concentrated hydrogen peroxide charge in a volume ratio of 1:1.

This technical result in the implementation of the proposed method for quantitative determination of manganese, lead and Nickel in bile by atomic-absorption analysis with atomization in flame, is achieved by the next.

It is necessary to clarify that the bile is often a heterogeneous biological environment. It contains a liquid phase, mucus, various clots include sediment, preventing analysis. Therefore, using natural, i.e. pre-unprepared, biological media studies there are large variations in the definitions, often clogged capillary spectrometer.

Due to the fact that prior studies of bile frozen, and then thawed, starting her already stirring when partially the om soft release (already in the presence of ice "porridge"), is the homogenization of the sample, decreases its viscosity, as ice "mess" crushed clots, large inclusions of mucus and mixed with the liquid phase. After that, possible sampling pipette or dispenser to further prepare it for analysis.

To achieve homogeneity of the sample and the destruction of the organic matrix in it successively added concentrated nitric acid and concentrated hydrogen peroxide with heating after the introduction of each of the specified reagent for 5-10 minutes at a temperature of 120±5°C for dissolving residual precipitate forms.

The addition of bile specified reagents (concentrated nitric acid and concentrated hydrogen peroxide) consistently in their declared the quantitative relationship between themselves and with the sample volume, is provided by chemical modification of the analyzed material with the formation of soluble compounds and quantitative translation of the studied metals in the solution, transfer the sample into a form suitable for analysis.

Heating and curing the mixture of bile samples with concentrated nitric acid at room temperature for at least 2.5 hours provides the decomposition (mineralization) of organic components of bile, helps to remove the formed gases.

Sample preparation in the proposed method is virtually in one ol the tag, that reduces the risk of sample contamination from utensils and possible losses if necessary, transfer the sample.

Through the above operations, their sequence and the declared modes, ensures the solution of the analyte from the sample of bile, which can already be used to conduct several studies, the results of which will be guaranteed to be stable and accurate, and that was proven by experiment.

The experiments showed that the deviation in the lower side of the declared volume ratios of samples of bile and entered in her volumes of concentrated nitric acid and concentrated hydrogen peroxide, may result in incomplete oxidation of the organic component and inflated results, apparently, against the background of the matrix effect, and when deviations in a big way - increase the dilution of the sample, which may lead to the exit of the range of sensitivity of the method, in addition, the acidity of the analyte should not exceed the limits specified in the operating instructions of the spectrophotometer.

Heating a mixture of bile samples with concentrated nitric acid and then with concentrated hydrogen peroxide less than 5 minutes at a temperature of 120±5°C can lead to incomplete mineralization and insufficient degassing of the analyte, and heated at over 10 min is too violent boiling, razbryzgivaya the s and significant evaporation of the sample, which leads to a distortion of results.

Maintaining a mixture of bile samples with concentrated nitric acid after said heating of at least 2.5 hours at room temperature ensures the destruction of the organic matrix. The decrease in this stage of preparation often leads to incomplete mineralization that does not warrant a quantitative translation of the examined element in the solution.

Sampling of bile to prepare one portion of the analyte is carried out in a volume of 1 cm3but not more than 2 cm3because the reaction can be carried out quite rapidly and you must find other conditions for mineralization.

In the implementation of the proposed method carry out the following operations in the following sequence:

produce selection bile in duodenal intubation of approximately 5 cm3(minimum volume of 2 cm3);

after selection bile produce freezing, i.e. get a solid phase;

- then start it defrost at room temperature;

- when defrosting is already in partial soft defrost simultaneously carry out the homogenization of bile by mixing (mixing should start already during the formation of ice "porridge", i.e. it characterizes partial, soft defrost, and continue to stir until complete razmara the air traffic management);

next make a selection of a homogenized sample of bile into a clean tube, preferably of 1 cm3to prepare for analysis;

- then enter it in a volume ratio of 1:1, i.e. in the order of 1 cm3, concentrated nitric acid with a concentration of 70%;

the mixture was kept at room temperature for 15-20 min, then heated for 5-10 min in vitro heater, for example, the brand HACH COD REACTOR, at a temperature of 120±5°C;

- and then the mixture stand at least 2.5 hours in an advantageous variant of 2.5-3 hours) at room temperature,

- then, to obtain the analyte to the resulting mixture concentrated hydrogen peroxide with a concentration of 33%; in a volume ratio of 1:1 (i.e. 1 cm3) for a sample volume of bile (it should be stated that to obtain the analyte concentrated nitric acid and concentrated hydrogen peroxide charge in a volume ratio of 1:1, i.e. in this example, 1 cm3);

- Analyt again heated in vitro heater 5-10 minutes at a temperature of 120±5°C,

is cooled to room temperature,

for each series of experiments put 2 blank sample, repeating the procedure for the preparation of the analyte, replacing the bile of treated bidistilled water. The dimension of the blank samples together with the real samples;

- the volume of the received analyte and idle about the s register, if evaporation is brought up to 3 cm3(respectively the initial total sample volume of bile and added reagents) purified bidistilled water,

and then by the method of atomic absorption spectrometry (using, for example, atomic absorption spectrophotometer brand Perkin Elmer 3110 or other), using a calibration curve, constructed by the method of absolute calibration certified mixtures of solutions of metals, produce a definition in quantitative analyte content of a particular type of metal: lead, manganese and Nickel.

Determination of the atomic absorption spectrophotometer begin with installation in the instrument spectral lamp corresponding to the designated metal, and warm up at least 20 minutes (according to instructions). To measure the used absorption with wavelength equal to the maximum absorption of the designated metal when passing through the containing pairs of atoms of the metal layer air: manganese - 248,3 nm; lead - is 283.3 nm; Nickel - 232,2 nm. The monochromator set at the desired wavelength, choose the width of the spectral gap, put on spraying purified bidistilled water, pick up the necessary ratio of gases (acetylene - air to support combustion and ignite the flame. Capillary feeding the solution into the flame, dipped in a 1%solution of nitric acid and predelut the zero line. Sprayed into the flame of a certified mixture of the analyzed metal to construct the calibration curve, then injected sample and record the concentrations of the investigated samples. Precision instrument settings, check the introduction of certified mixture set concentration every five samples, if necessary recalibrates. The high content of the designated metal analyte and a blank sample was diluted with 1%nitric acid solution, the dilution factor into account when calculating the result of the analysis. Calculation of the content (X) of metals in bile is carried out by the formula:

where C is the concentration, determined by a calibration curve, constructed by the method of absolute calibration certified mixtures of solutions of metals, mg/cm3;

With' - value of the blank sample concentration, mg/cm3;

V is the total volume of the analyte, cm3;

V' is the volume of bile samples taken for analysis, cm3.

For the measurement arithmetic mean of the value oftwo parallel definitions of XmaxXmin, the difference between which r must not exceed the limit of repeatability rn:

The result of quantitative analysis in the documents providing for its use, performance, which is in the form: ( ±Δ), µ g/cm3at a confidence level (maximum error for a given reliability) P=0,95, where

- the average result analysis, ug/cm3,

;

Δ is the characteristic error µg/cm3when P=0,95

,

where δ is the relative importance of the error characteristics, %.

The proposed method was tested in laboratory conditions. For its implementation we used the following reagents and solutions:

The nitric acid concentrated, GOST 4461-77, OFS.;

Acetylene, GOST 5457-75;

Hydrogen peroxide, GOST 177-88, 33%;

Nitric acid (HNO3), 1%;

Purified bidistilled water;

Nitric acid (HNO3), 1%;

Hydrogen peroxide, 6%.

Studies of bile on the subject of quantitative determination of Nickel, manganese and lead were carried out by implementation of the above operations and modes.

Data for the quantitative content of Nickel in bile obtained during the implementation of the proposed method are shown in table 1, for the quantitative content of manganese in table 2, for the quantitative content of the lead - in table 3.

Further, by calculations on the basis of these data determined the parameters of repeatability, reproducibility and accuracy of the proposed method. Below PR who entered the order of the calculations on the example of the quantitative content of Nickel, defined in the sample of bile proposed method.

1. The index of the repeatability of the proposed method

1.1. The arithmetic mean of parallel definitionscalculated according to the formula (data for the calculation are taken from table 1):

1.2. The sample variance of the results of a single analysis of the content of Nickel, obtained in conditions of repeatability (parallel detection),calculated according to the formula (table 1):

1.3. To test the hypothesis, the General equality of variances. The value of Gl(max) calculated by the formula:

G1(max)=0,120, Gtable=0,602 (at a confidence level of P=0,95). The homogeneous dispersion (G1<Gtable).

1.4. The calculation of the mean-square deviation (RMS) Srperform according to the formula:

,

1.5. The measure of repeatability σrthe proposed method in the form of the mean-square deviation:

The measure of the repeatability of the proposed method in the limit of repeatability rncalculated by the formula:

rn=Q(P,n)·σrwhere n is the number of parallel measurements, provided the proposed method to obtain the analysis result

Q(P,n)=2,77 when n=2, P=0,95

rn=2,77·1,94·10-3=are 5.36·10-3

1.6. The mean value of the analysis results obtained under repeatability:

1.7. The measure of repeatability σr≈Srin relative units:

The limit of repeatability of the proposed method r in relative units:

2. The index of the repeatability of the proposed method

2.1. Calculate the variance that characterizes the dispersion of arithmetic mean of the results of parallel measurements (Xl) relative to the overall averageaccording to the formula:

2.2. A measure of the reproducibility of the proposed method in terms of RMSE when the experiment in the same laboratory are calculated according to the formula:

A measure of the reproducibility of the proposed method in relative units:

A measure of the reproducibility of the proposed method in the limit of reproducibilitycalculated by the formula:

for P=0,95

2.3. The limit of reproducibilityin relative units:

3. The index of the accuracy of the methods

Get the L series results-defined metal - Nickel in the sample without additives (working sample) -and the sample with the additive (sample with the addition of the designated metal) -(see table 4).

The amount of the additive to the working sample=0,100 mg/cm3error preparing certified mixtures ±Δco=±0,001 mg/cm3(1%) (for the calibration curve prepare a certified mixture with specified concentrations of Nickel in 1%nitric acid solution).

3.1. The average value of the sample without additives (working sample):

The standard deviation characterizing the random scatter of results of analysis of the sample without additives:

3.2. The average value of the sample with the additive (see tablicu):

The standard deviation characterizing the random scatter of results of analysis of samples with the addition of:

,

3.3. The value of the experimentally found values of the additive:

3.4. Systematic progressmonitordialog ways θ m:

3.5. Examine the significance of the calculated values of θmthe student test (t):

Calculate the value t:

where S1and S2The standard deviation characterizing the random scatter of results of analysis of the sample without additives and samples with the additive;

Δco- uncertainty of the certified values of the additive in the sample.

The value t is compared with ttable.When the number of degrees of freedom f=L-1 for a confidence probability P=0.95 to ttable.=of 2.26.

As t<ttable.(0,27<and 2.26), the estimation bias is equal to zero, θm=0.

3.6. The indicator of the correctness of the proposed method are calculated according to the formula:

3.7. Upper (ΔST) and lower (ΔCH) border non-excluded systematic error with the accepted probability P=0,95 found by the formula:

In relative units:

4. Evaluation of the accuracy rate of the proposed method.

4.1. The standard deviation σ(Δ) error analysis is:

The upper and lower bounds (ΔIn, ΔN), in which the accuracy of any of the aggregate results analysands adopted with probability P=0.95, and calculated by the formula:

In relative units:

The calculation of repeatability, reproducibility and accuracy of the proposed method for manganese and lead is the same way.

Data measuring range in bile Nickel, lead and manganese proposed method, and the values of repeatability, reproducibility and accuracy are shown in tables 5 and 6.

Known prototype-based method for direct determination of metals in bile allows measurements with the total error of the up to 25%, while the proposed method can reduce the error in the determination of Nickel up to 5%, lead up to 10%, of manganese to 14.85% (see table 5).

Thanks for the specified sequence of operations and use of certain modes, the proposed method can improve the accuracy of determination of Nickel, manganese and lead in a sample of bile.

Table 1
Data for the quantitative content of Nickel in the sample of bile obtained during the implementation of the proposed method, ug/cm3
L, result, l=1,LN, the number of parallel about what medeleni, n=1,NXnthe result of parallel detection,the arithmetic mean of parallel measurements, N=2the values of the sample variance
110,1500,14854,5·10-6
20,147
210,1510,15202,0·10-6
20,153
310,1490,14754,5·10-6
20,146
410,1550,15402,0·10-6
20,153
510,1480,14954,5·10-6
20,151
610,1490,14754,5·10-6
20,146
710,1530,15402,0·10-6
20,155
810,1530,15454,5·10-6
20,156
910,1500,14854,5·10-6
20,147
1010,152 0,15354,5·10-6
20,155

Table 2
Data for the quantitative content of manganese in the sample of bile obtained during the implementation of the proposed method, ug/cm3
L, result, l=1,LN, the number of parallel measurements, n=1,NXnthe result of parallel detection,the arithmetic mean of parallel measurements, N=2the values of the sample variance
110,0520,05250,50·10-6
20,053
210,0460,04702,0·10-6
20,048
310,0490,05002,0·10-6
20,051
410,0470,04602,0·10-6
20,045
510,0440,04554,5·10-6
20,047
610,0550,05354,5·10-6
20,052
710,0480,05008,0·10-6
20,052
810,051 0,05450.5 to 10-6
20,050
910,0460,04408,0·10-6
20,050
1010,0470,04554,5·10-6
20,044

Table 3
Data for the quantitative content of lead in a sample of bile obtained during the implementation of the proposed method, ug/cm3
L, result, l=1,LN, the number of parallel measurements, n=1,NXnthe result
parallel definitions
,the arithmetic mean of parallel measurements, N=2the values of the sample variance
110,1560,1525at 2.45·10-5
20,149
210,1410,14351,25·10-5
20,146
31is 0.1350,1385at 2.45·10-5
20,142
410,1370,13951,25·10-5
20,142
510,1520,14901,8·10-5
20,146
610,134 0,13600,8·10-5
2was 0.138
710,1420,14501,8·10-5
20,148
810,1540,15101,8·10-5
20,148
91was 0.1380,14101,8·10-5
20,144
1010,1510,14851,25·10-5
20,146

Table 5
Data about the range of Areni in bile Nickel, lead and manganese proposed method, and the values of the indicators of its repeatability, reproducibility and accuracy
The name of the component to be determined and the measurement range, µg/cm3The measure of repeatability (relative standard deviation repeatability) σr, %The measure of reproducibility (relative standard deviation of reproducibility)σR, %Accuracy rate (bounds the relative error with probability P=0,95),±δ, %
Nickel,
from 0.10 to 1.00 incl.
1,282,324,94
Lead,
from 0.10 to 1.00 incl.
2,824,71there is a 10.03
Manganese,
from 0.025 to 0.250 on.
3,917,1014,85

Table 6
The limits of repeatability and reproducibility of the proposed method when the Trustee verojatnost is P=0,95
The name of the component to be determined and the measurement range, µg/cm3The limit of repeatability (relative value allowable discrepancies between the two results of parallel measurements), rn%Limit intralaboratory reproducibility (relative value allowable discrepancies between the two measurement results obtained in one laboratory, but in different conditions),, %
Nickel,
from 0.10 to 1.00 incl.
3,556.42 per
Lead,
from 0.10 to 1.00 incl.
7,8213,04
Manganese,
from 0.025 to 0.250 on.
10,8319,68

The method of quantitative determination of manganese, lead and Nickel in bile by atomic-absorption analysis with atomization in flame, including the selection of bile and defining the quantitative content of heavy metals by the method of atomic absorption spectrometry, wherein upon selection of the bile produce freezing, then thawing, which at the same time, starting with partial soft is asparagine, carry out the homogenization of bile through mixing, then produce a selection of homogeneous samples of bile to prepare for the analysis, then the resulting sample is injected concentrated nitric acid in a volume ratio of 1:1, respectively, the mixture was kept at room temperature for 15-20 min, then heated for 5-10 minutes at a temperature of 120±5°C, then stand at least 2.5 h at room temperature, then, to obtain the analyte to the resulting mixture concentrated hydrogen peroxide in a volume ratio of 1:1 to a sample volume of bile, the analyte is heated for 5-10 minutes at a temperature of 120±5°C, cooled to room temperature and then using the method of atomic absorption spectrometry, using a calibration curve, make a determination in the quantitative analyte content of a certain kind of metal is manganese, lead and Nickel, with concentrated nitric acid and concentrated hydrogen peroxide charge in a volume ratio of 1:1.



 

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11 cl, 2 dwg

FIELD: instrument engineering.

SUBSTANCE: invention is designed for calibrating gas analyser detectors, according to which there prepared is calibration substance solution with concentration A=By/k (%) as per Henry constant value k (mg/m %) at calibration temperature and as per the specified value of calibration substance mass concentration in calibration steam/gas mixture By (mg/m). After the solution has been introduced into the vessel in quantity enough for fully saturated equilibrium calibration steam/gas mixture to appear above the solution surface, the sensor calibration is carried out by means of mixture; at that, mixture concentration is changed by means of direct proportional change of solution concentration by diluting concentrated reference solution of calibration substance with analytical accuracy up to the specified concentration value A (%). There also proposed is the device for realising this method, which includes a solution point for preparing calibration solution with analytical accuracy, vessel with thermostatic device for obtaining steam/gas mixture with constant concentration corresponding to Henry law; at that, solution point includes graduated dose metre, graduated diluter, mixer with a reducer, capacity with solvent, and reference container with reference solution, which is stabilised with a gate valve meant for multiple use of container, and vessel with thermostatic device consists of thermometre and heat-insulating cover plate with an inlet branch pipe containing a normally closed return valve and a pusher for valve opening.

EFFECT: decrease of calibration substance losses; accuracy and reproducibility of metrological performance, and meeting requirements of industrial and ecological safety.

6 cl, 2 dwg

FIELD: instrument engineering.

SUBSTANCE: device for generating flow of vapor-gas mixture with preset concentration of vapor has vessel partially filled with fluid, second vessel provided with branch pipes for supply and removal of gas, and vapors of fluid pipeline-leak. One of vessels is connected with gas discharge forcer; fluid vapors pipeline-leak connects both vessels. Vessel, partially filled with fluid, is mounted inside second vessel. Pipeline-line, connecting both vessels, is totally placed inside second vessel. Device is also provided with additional discharge forcer for adjusting concentration of fluid vapor in second vessel. Granulated filler is introduced into vessel partially filled with fluid. Device is also provided with gas analyzer for providing gas concentration in space of second vessel.

EFFECT: higher precision of keeping of preset concentration of vapor; improved efficiency of vapor concentration control and adjustment.

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for synthesis of ester perfluorinated derivative by using a chemical reaction. This reaction represents the fluorination reaction of the parent compound as a raw, the reaction of chemical conversion of fragment of ester perfluorinated derivative to yield another ester perfluorinated derivative or the interaction reaction of carboxylic acid with alcohol under condition that at least one or reagent, i. e. carboxylic acid or alcohol, represents a perfluorinated compound wherein indicated perfluorinated derivative of ester represents a compound comprising a fragment of the formula (1):

with a boiling point 400°C, not above. The reaction time for carrying out abovementioned chemical reaction is sufficient to provide the required yield of ester perfluorinated derivative and wherein this yield of ester perfluorinated compound is determined by the gas chromatography method by using a nonpolar column. Also, invention relates to a method for pyrolysis of ester perfluorinated derivative with a boiling point 400°C, not above, to yield the dissociation product wherein this product represents a derivative of acyl fluoride or ketone and wherein pyrolysis time is sufficient to provide the required degree of conversion of ester perfluorinated derivative and wherein the indicated conversion degree of ester perfluorinated derivative is determined by gas chromatography method by using a nonpolar column. Also, invention relates to a method for analysis of ester perfluorinated derivative with a boiling point 400°C, not above, that involves analysis of ester perfluorinated derivative in a sample containing ester perfluorinated derivative by gas chromatography method by using a nonpolar column wherein ester perfluorinated derivative represents compound comprising a fragment of above given formula (1).

EFFECT: improved method of synthesis.

8 cl, 1 dwg, 2 ex

The invention relates to the field of analytical chemistry of organic compounds, namely, the field determination of organic compounds in their joint presence using gas-liquid column chromatography, and can be used for the separate determination of phenols in liquid environments, mainly in industrial effluents, as well as the analysis of natural waters

The invention relates to the field of gas analysis and can be used for calibration of gas analysis equipment

The invention relates to the field of analytical instrumentation, in particular, to devices for preparation of calibration gas mixtures used in the calibration and verification of gas analyzers

The invention relates to the field of analytical instrumentation and can be used in the calibration and verification of gas analyzers

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for synthesis of ester perfluorinated derivative by using a chemical reaction. This reaction represents the fluorination reaction of the parent compound as a raw, the reaction of chemical conversion of fragment of ester perfluorinated derivative to yield another ester perfluorinated derivative or the interaction reaction of carboxylic acid with alcohol under condition that at least one or reagent, i. e. carboxylic acid or alcohol, represents a perfluorinated compound wherein indicated perfluorinated derivative of ester represents a compound comprising a fragment of the formula (1):

with a boiling point 400°C, not above. The reaction time for carrying out abovementioned chemical reaction is sufficient to provide the required yield of ester perfluorinated derivative and wherein this yield of ester perfluorinated compound is determined by the gas chromatography method by using a nonpolar column. Also, invention relates to a method for pyrolysis of ester perfluorinated derivative with a boiling point 400°C, not above, to yield the dissociation product wherein this product represents a derivative of acyl fluoride or ketone and wherein pyrolysis time is sufficient to provide the required degree of conversion of ester perfluorinated derivative and wherein the indicated conversion degree of ester perfluorinated derivative is determined by gas chromatography method by using a nonpolar column. Also, invention relates to a method for analysis of ester perfluorinated derivative with a boiling point 400°C, not above, that involves analysis of ester perfluorinated derivative in a sample containing ester perfluorinated derivative by gas chromatography method by using a nonpolar column wherein ester perfluorinated derivative represents compound comprising a fragment of above given formula (1).

EFFECT: improved method of synthesis.

8 cl, 1 dwg, 2 ex

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