Method of estimation and forecast of ageing processes (destruction) of polymer materials according to dynamics of total gas discharge and toxisity of volatile organic compounds (voc) migrating from polymer during ageing and detected by chromatography-mass spectrometry

G01N1/28 - INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (separating components of materials in general B01D, B01J, B03, B07; apparatus fully provided for in a single other subclass, see the relevant subclass, e.g. B01L; measuring or testing processes other than immunoassay, involving enzymes or micro-organisms C12M, C12Q; investigation of foundation soil in situE02D0001000000; monitoring or diagnostic devices for exhaust-gas treatment apparatus F01N0011000000; sensing humidity changes for compensating measurements of other variables or for compensating readings of instruments for variations in humidity, seeG01D; or the relevant subclass for the variable measuredtesting or determining the properties of structures G01M; measuring or investigating electric or magnetic properties of materials G01R; systems in general for determining distance, velocity or presence by use of propagation effects, e.g. Doppler effect, propagation time, of reflected or reradiated radio waves, analogous arrangements using other waves G01S; determining sensitivity, graininess, or density of photographic materials G03C0005020000; testing component parts of nuclear reactors G21C0017000000)

FIELD: instrumentation.

SUBSTANCE: invention relates to forecast of ageing processes of the synthetic polymer materials (SPM) depending on duration of their operation or storage. Analysis of the volatile organic compounds (VOC) migrating from SPM is performed by active sampling for sorbent, with further thermal desorption and gas chromatographic analysis. Forecast of the ageing processes of the material and estimation of toxicity of the gas discharge are performed as per dynamic of the qualitative and quantitative composition of gas discharge components in SPM initial state, and during artificial climatic thermal-humidity ageing. Dynamics analysis of the total gas discharge (ΣT) from each material is performed for all substances migrating from studied SPMs. Change of toxicity is estimated and forecast of the material ageing is performed as per developed indices of total gas discharge (ΣT) and as per hygienic index P=(ΣTinitial/ΣTn)/V, where Tinitial and Tn are indices of toxicity of gas discharge of each substance in initial state and after ageing, respectively, and ΣTinitial and ΣTn are total indices of toxicity of gas discharge of all components of SPM in initial state and after ageing, V is duration of ageing (year, month).

EFFECT: invention ensures high accuracy of the method of VOC qualitative and quantitative composition determination in gas discharge during materials ageing and the analysis results repeatability.

3 tbl

 

The invention is intended for assessment and prediction of aging (degradation) of synthetic polymeric materials (SCM) on the basis of detected changes of the total gas evolution and prediction of toxicity of chemical substances migrating from SPM in the process of their degradation, the detection method of gas chromatography / mass spectrometry after a given duration of climatic ageing at an accelerated climatic tests (IES).

The need for sanitary-hygienic and Toxicological evaluation of gas emission of SPM in the course of their operation are defined by the requirements of GOST R 50804-95, "Methodological guidelines for the sanitary-chemical and Toxicological study of polymeric materials for equipment inhabited hermetically closed compartments" Ratified. THE USSR MINISTRY OF HEALTH 1981, GOST 9.710-84, GOST 9.707-81. It is known that during storage and operation of polymers exposed to adverse factors, according to which there are basic types of degradation (aging): climate, radiation, ultrasound, under the influence of biological and mechanical factors, etc. GOST 9.710.-84, GOST 9.707-81), the effects of which leads to a decrease or irreversible (chemical destruction) changes the working characteristics of materials. Therefore, development of methods OTS�NCI and prediction of aging of non-metallic materials as well as establishing the actual terms of safe exploitation is of paramount importance in modern polymer science. After long-term use SPM in terms of tight spaces and manned spacecraft important to also assess the prediction of toxicity outgassing products in the aging process of the materials.

The need for sanitary-hygienic and Toxicological evaluation of gas emission of SPM in the course of their operation are defined by the requirements of GOST R 50804-95 and "guidance on sanitary-chemical and Toxicological study of polymeric materials for equipment inhabited hermetically closed compartments" Ratified. THE USSR MINISTRY OF HEALTH 1981, GOST 9.710-84, GOST 9.707-81.

Hygrothermal aging SPM was carried out in accordance with the recommendations of GOST 9.707-81 (method 1) in a sealed cells, precluding the possibility of mass transfer with the environment.

Preparation of polymeric materials for the tests were carried out in accordance with the requirements of GOST R ISO 14624-3:2010 "Safety and materials compatibility. Part 3. Definition of exhaust gases from materials and assembled products" and "Methodological guidelines for the sanitary-chemical and Toxicological study of polymeric materials for about�of adowania inhabited hermetically closed compartments" Ratified. The USSR Ministry of health 1981 and GOST R 50804-95. Synthetic polymeric materials were allowed to test no earlier than 6 months after their production and preparation in accordance with the requirements of GOST R ISO 14624-3:2010.

The technical result is achieved in that a method of preparing samples of synthetic polymeric materials to conduct temperature-humidity climatic ageing is carried out by method (GOST R ISO 14624-3:2010), excluding changes in the structure and chemical composition of the gas before the test.

Polymeric materials for testing should follow the recipe and the approved technical conditions agreed with the organs and institutions of state sanitary-epidemiological service of the Russian Federation. Imported products must be accompanied by documentation of its security (the security certificate of the country of manufacture, issued by the authorized bodies and/or certificate (confirmation) of the manufacturer, test reports indicating the standard indicators and test results).

In accordance with the provisions of GOST 9.710.-84 (the"common protection against corrosion and ageing. Aging of polymeric materials. Terms and definitions" clause 7") and GOST 9.707-81, allowing the use of any measure of the aging of polymeric�of material, us to identify and predict changes in properties of materials in the aging process was selected speaker of volatile organic compounds (VOCS) migrating from polymeric materials in the process of climatic ageing (degradation) of the detection of substances by the method of gas chromatography / mass spectrometry. Prediction of aging of polymeric materials is performed by changing concentrations of VOCS, characterizing the process of destruction of materials in the simulation the length of the temperature-humidity aging (from 1 to 33 years).

Accelerated climatic tests (IES) was carried out according to method 1 as recommended by GOST 9.707-81.

The analysis of the dynamics of the quantitative and qualitative composition of VOCS in the composition of outgassing from 35 polymeric materials representing the major classes of SPM, a method is developed for estimation and prediction of aging of polymeric materials on the dynamics of the developed index of total gas evolution (ΣT), as well as a method of assessment and prediction of toxicity (P) gassing from materials in the process hygrothermal climatic ageing.

The invention consists in the fact that as an indicator for the assessment and prediction of aging (degradation) of SMP and change of toxicity of outgassing of polymers used d�the dynamics of the composition and concentrations of chemicals migrating from materials, in the detection method of gas chromatography / mass spectrometry.

The prior art closest to the claimed invention is the method adopted for the evaluation of materials intended for use in GTO, GOST R ISO 14624-3:2010 "Safety and materials compatibility. Part 3. Definition of exhaust gases from materials and assembled products", in accordance with the requirements of "guidelines for the sanitary-chemical and Toxicological study of non-metallic materials for equipment inhabited sealed rooms", approved. The Ministry of health 03.09.1982 G., GOST R 50804-95 determining the methods of testing for emission of SPM.

The technical result achieved the claimed invention, is that when using the method of gas chromatography / mass spectrometry for the analysis of outgassing of polymers (GOST R ISO 16000, part 6) to achieve the high accuracy of quantitative analysis (10-12) volatile outgassing products, which is especially important for the prediction of the aging process and changes in the rate of change of material properties in time. A wide range of analytes allows to objectively evaluate the toxicity of the chemical composition of substances, which migrate into the air during long exploitation�AI polymers under conditions of tight spaces and long operating manned spacecraft.

Previously, such a comprehensive study has not been conducted, it should therefore be understood that the claimed method of evaluating and predicting the process of aging of polymeric materials and method of assessment and prediction of toxicity of gassing in the aging process is unique.

Assessment and forecasting of the process of destruction was carried out on the dynamics of the total gas evolution ΣT(T1+T2+...T3+Tn) of each polymeric material in the process of IPC. Assessment and prediction of the dynamics of the toxicity of the gassing process IES conducted on the dynamics of the index T, calculated with respect to the measured concentration of the substance SMG/m3/Pdmg/m3to its maximum permissible concentration (GOST R 50804-95, GN 2.2.5. 2895-11, GN 2.1.6.2897-11) for each substance migrating from investigated SPM in the process of IPC. Assessment and prediction of change process toxicity was performed according to the dynamics developed in hygienic measure P=(ΣT/ΣTn)/V, reflecting the dynamics of changes in the toxicity of gas emission of SPM in the process of aging where Tish and Tn - the toxicity of gas emission of each substance in the original and aged conditions, respectively, and Σ and ΣTn is a summary indicator of the toxicity of gassing all members of the sample of synthetic polymeric materials in the original and aged status�aniah, V - the duration of aging (year, month).

In the future, for each of the tested material specific set of allowable saturation - the ratio of the amount (weight, size, line size, etc.) of the material to the standard volume in terms of 1 m3.

Assessment of the hygienic characteristics of SPM was based on toxicity index of gas emission of each substance in the composition of the gas emission and the total gas evolution (ΣT) from each sample SPM, and the design of hygienic indicator (P=ΣT/ΣTn), reflecting the dynamics of changes in the toxicity of gas emission of SPM in the aging process.

Largest total score (ΣT) of gas emission, the value of which is below 1, all the tested materials can be operated for 33 years, subject to valid saturation, material composition and intensity of gas emission in the process of aging.

Based on the position of GOST 970781 (amended 1991), which States that the rate of degradation of materials under the action of climatic factors aging is and gassing, researched materials on the toxicity of gas emission (T criterion, ΣTi, hygiene index (P), were divided into 4 groups:

- 1 group (P<1) (T criterion from 0.003 to 0,043) SPM with the highest total value of gas emission (ΣT), save�nauseosa to 33 years IES and therefore, most susceptible to temperature and humidity climatic aging (degradation);

- 2 group (P from 1.2 to 10), (T criterion from 0.005 to 0,012) is characterized by greater total value of gas emission ΣT to 25 years IES compared with 3 and 4 groups;

- Group 3 (P from 11 to 30 (60) (T criterion from 0,0006 to 0,054) is characterized by larger values of the total gas evolution ΣT to 25 years IES compared with group 4 SPD;

Group 4 (P>60). Largest ΣT materials are characterized by reduced almost to a minimum of the index of total gas emission by increasing the length of the IES, indicating that the stability of these materials to a temperature-humidity climatic aging time up to 33 years.

Based on the experimental data to quantify the changes of the hygienic characteristics of SPM at various terms UKI proposed Settlement hygienic measure P=(ΣT/ΣTi)/V, which reflects the change in the toxicity of gas emission of SPM in the process of destruction (aging) and includes an assessment of the dynamics of the toxicity of each substance in the composition of the gas emission of SPM.

Examples.

The dynamics of the total (ΣT) gassing from materials in terms of ageing in the process of IPC.

0,014
Table 1
Name of materialInitial state10 years20 years25 years33
compound EDL-20M0,0250,0670,0130,0050,005
glue VK-TC0,0430,0040,0770,0200,012
primer AK-0700,1530,0060,0380,0130,001
varnish UR-2310,0460,0370,0330,0080,001
the insulating tape brand LESB0,0050,0130,045 0,0120,005
glue f-42L0,0140,0180,0250,0330,013
glue E-200,0340,0280,0490,0140,004
glass fiber SF-2-50G-0,80,0110,0270,0180,0120,003
cold cure glue ADV-50,3710,0110,0080,0260,002
fabric tech. Polyamide art. 560030,0470,0060.031 inch0,0000,000
film SCLF-4D0,0570,0100,0070,005
tape trick. Looped KTL-1000/60,0090,0130,0530,0200,002
polyamide 610 injection molding0,0370,0120,0260,0710,014
fibreglass CAST-IN-1,00,0770,0230,0380,0380,002
varnished cotton LSMS-105Of 0.0210,0100,1110,027
film of fluoroplastic f-4 MB0,0080,0020,0060,0130,002
tape tech. Aramina Lter-20-2000,0150,017 0,0120,1550,007
polycarbonate PC-LT-100,0220,0110,4270,0290,014
sealant 51-G-230,0260,0080,0130,0180,044
adhesive 88-SA0,0140,0040,0450,0200,004
fluoropolymer tape brand U-f-4 EA/180/KO0,0160,0110,0320,0060,001
the tube 305 TV-500,0230,0080,0450,0130,001
the rubberized fabric 918-90,0180,0220,013 0,0080,001
the adhesive tape LT-190,0360,0290,0480,016
putty EP-00100,0850,0020.076 mm0,0220,001
foam polystyrene tiled PS-1-1500,0380,0610,022Of 0.0210,006
the rigid polyurethane foam Mediart-13 (mark 5)0,0610,0290,0250,0110,015
the fabric is heat-resistant double-layered art. ND-250 Cu0,0350,0140,0020,0900,002
the technical fabric polyamide art. 56260 Cu IN0,190 0,3480,0450,1190,002
film brand Vitur T 0533-900,4110,1070,006Of 0.0210,006
sealant Humi Seal UY400,0070,006Of 0.0210,2470,002
polycarbonate glass-filled-grades PK-L-SV0,0360,0320,0030,305
heat resistant decorative finishing material "arlit" type "Talca-1"0,0910,0100,0130.031 inch0,004
(ΣT) together with the use of tested materials2,081,0061,431,450,18

�on the value of the total parameter ΣT gassing the value of which is below 1, all the tested materials can be operated for 33 years.

The table shows that by 25 and 33 years of age, the severity of destruction of materials in intensity and ΣT gassing was different.

The materials were divided into 4 groups (see Table 2) in its properties and aging resistance.

According to research results, materials were divided into 4 groups. Largest ΣT materials 4 most resilient to climate ageing and the level of outgassing of oxygen-containing compounds, and hence toxicity, decreases with increasing time of aging.

Table 2
Group 1
P is less than 1hygienic PInitial state10 years20 years25 years33
the insulating tape brand LESB0,90,0050,0130,0450,0120,00
sealant 51-G-230,60,0260,0080,0130,0180,044
glue f-42L0,40,0140,0180,0250,0330,013
polycarbonate PC-LT-100,80,0220,0110,4270,0290,014
tape technical Aramina Lter-20-2000,10,0150,0170,0120,1550,007
polycarbonate glass-filled-grades PK-L-SV0,10,0360,0320,0030,305
varnished cotton LSMS-1050,8Of 0.021 0,0100,1110,027
ΣT0,0200,0160,0910,0830,016
Group 2
P from 1 to 10hygienic indexInitial state10 years20 years25 years33
compound EDL-20M5,00,0250,0670,0130,0050,005
glue VK-TC3,60,0430,0040,0770,0200,012
glue E-208,40,0340,0280,0490,014 0,004
glass fiber SF-2-50G-0,83,70,0110,0270,0180,0120,003

fibreglass CAST-IN-1,0
ribbon knit stitch KTL-1000/64,90,0090,0130,0530,0200,002
polyamide 610 injection molding2,60,0370,0120,0260,0710,014
film of fluoroplastic f-4 MB4,90,0080,0020,0060,0130,002
adhesive 88-SA3,40,0140,0040,0450,0200,004
foam polystyrene tiled PS-1-150 6,30,0380,0610,022Of 0.0210,006
the rigid polyurethane foam Mediart-13 (mark 5)4,20,0610,0290,0250,0110,015
sealant Humi Seal UY403,20,0070,006Of 0.0210,2470,002
the adhesive tape LT-192,30,0360,0290,0480,016
ΣT0,0270,0230,0340,0390,006
Group 3
P from 10 to 30hygienic indexInitial state 10 years20 years25 years33
fluoropolymer tape brand U-f-EO/180/KO16,10,0160,0110,0320,0060,001
the tube 305 TV-5018,00,0230,0080,0450,0130,001
the rubberized fabric 918-930,00,0180,0220,0130,0080,001
the fabric is heat-resistant double-layered art.ND-250 CuA 20.70,0350,0140,0020,0900,002
"Arlit" type "Talca-1"26,00,0910,0100,0130.031 inch0,004
A 33.30,0770,0230,0380,0380,002
film SCLF-4D10,60,0570,0100,0140,0070,005
ΣT0,0370,013Of 0.0210,0290,002
Group 4
P over 30hygienic indexInitial state10 years20 years25 years33
cold cure glue ADV-5185,40,3710,0110,0080,0260,002
the technical fabric polyamide art. 56003 To 166.10,0470,0060.031 inch0,0000,000
the technical fabric polyamide art. 56260 Cu IN105,60,1900,3480,0450,1190,002

putty EP-001063,60,0850,0020.076 mm0,0220,001
primer AK-070RUB 252.80,1530,0060,0380,0130,001
varnish UR-23160,30,0460,0370,0330,0080,001
film brand Vitur T 0533-9072,50,4110,107 0,006Of 0.0210,006
ΣT0,1590,0610,0320,0280,002

To quantify the changes of the hygienic characteristics of the MTA, reflecting a predisposition JMP to the factors of temperature and humidity climatic ageing, defined by the dynamics of the total toxicity of the products of outgassing material, the offered rate P=(ΣTi/ΣTi)/V

where (ΣTi) - sum indices of toxicity detected compounds for materials in the initial state, (ΣTi) - sum indices of toxicity detected compounds for materials after aging, i is the sequence number of the identified compounds, V is the number of years of aging. The precise definition of this quantity will allow us to determine trends in levels of toxic hazard in time of materials with different chemical matrices. Since the basis is the total emission (ΣT), the accuracy of the estimate (P) depends on the accuracy of the method for measuring the concentrations of outgassing products.

Additionally, it is possible to calculate the hygienic index for the tested materials according to the formula: P=ΣT/ΣTi

Example�, T - test of the compound of EDL-20M in the initial state (Tish) equal to 0.025, and after 33 years UKI T-test was equal to 0.005, then in accordance with the presented formula we obtain that the hygienic value is equal to 5. That is, the Toxicological hazard of the material decreased in 5 times.

Comparative characteristic values T-test, and hygiene index (P) formed by the groups studied materials during the duration of the IES 33 years.

Table 3
Group 1
P is less than 1T-test (33)Hygienic P
the insulating tape brand LESB0,0050,9
sealant 51-G-230,0430,6
glue f-42L0,0120,4
polycarbonate PC-LT-100,0140,8
tape technical Aramina Lter-20-2000,007 0,1
polycarbonate glass-filled-grades PK-L-SV0,0030,1
varnished cotton LSMS-1050,0270,8
Group 2
R from 1 to 10T-criterion (33)Hygienic index
compound EDL-20M0,00505,0
glue VK-TC0,01203,6
glue E-200,00408,4
glass fiber SF-2-50G-0,80,00303,7
ribbon knit stitch KTL-1000/60,00184,9
polyamide 610 injection molding0,01432,6
film of fluoroplastic f-4 MBOf 0.00164,9
adhesive 88-SA 0,00423,4
foam polystyrene tiled PS-1-1500,00606,3
the rigid polyurethane foam Mediart-13 (mark 5)0,01454,2
sealant Humi Seal UY400,00223,2
the adhesive tape LT-190,01602,3
Group 3
R from 10 to 30 (60)T-test (33)Hygienic index
fluoropolymer tape brand U-f-4 EA/180/KOIs 0.001016,1
the tube 305 TV-50With 0.001318,0
the rubberized fabric 918-90,000630,0
the fabric is heat-resistant double-layered art. ND-250 Cu0,0017A 20.7
fibreglass CAST-IN-1,0 0,0023A 33.3
film SCLF-4D0,005410,6
"Arlit" type "Talca-1"0,003526,0
Group 4
P over 60T-test (33)Hygienic index
cold cure glue ADV-50,0020185,4
the technical fabric polyamide art. 560030,0003To 166.1
the technical fabric polyamide art. 56260 Cu IN0,0018105,6
putty EP-0010With 0.001363,6
primer AK-0700,0006RUB 252.8
varnish UR-2310,000860,3
film brand Vitur T 0533-900,005772,5

A comparative analysis of the distribution studied by SPM groups toxicity of gas emission in the process of the IES on T criterion, ΣT and P showed satisfactory convergence of the estimation and prediction of toxicity of outgassing of polymers in the aging process indicator P.

The results showed that the IES JMP modeling 20, 25 and 33 years of aging under heated storage, accompanied by the degradation of macromolecules of the polymer with the formation of low molecular weight olefins and oxygen-containing compounds: ketones, aldehydes, alcohols, aromatic hydrocarbons. The dynamics of the total outgassing of low molecular weight compounds is the nature of the phase.

Identification of the products of outgassing JMP (after 33 years IES) highly and extremely toxic monomer residues of macromolecules of polymers (methylisocyanate, toluenesulfonate, caprolactam, α-, ω-diolefin with a carbon number of 8-18, BPA, organophosphorus derivatives of naphthalene, terphenyl) that characterize the migration of substances from the inner layers JMP prognostically unfavorable for air quality long-term functioning of manned space stations.

Largest total score (ΣT) of gas emission, the value of which is below 1, all the tested materials can be used in �of Directors for 33 years, subject to the allowable saturation, material composition and intensity of gas emission in the process of aging.

Based on the position of GOST 970781 (amended 1991), which States that the rate of degradation of materials under the action of climatic factors aging is and gassing, researched materials on the toxicity of gas emission (T criterion, ΣTi, hygiene index (P) were divided into 4 groups:

- 1 group (P<1) (T criterion from 0.003 to 0,043) SPM with the highest total value of gas emission (ΣT), continuing up to 33 years IES and therefore the most susceptible to temperature and humidity climatic aging (degradation);

- 2 group (P from 1.2 to 10), (T criterion from 0.005 to 0,012) is characterized by greater total value of gas emission ΣT to 25 years IES compared with 3 and 4 groups;

- Group 3 (P from 11 to 30 (60) (T criterion from 0,0006 to 0,054) is characterized by larger values of the total gas evolution ΣT to 25 years IES compared with group 4 SPD;

- 4 group (P>60). Largest ΣT materials are characterized by reduced almost to a minimum of the index of total gas emission by increasing the length of the IES, indicating that the stability of these materials to a temperature-humidity climatic aging time up to 33 years.

On �the base of experimental data to quantify the changes of the hygienic characteristics of SPM at various terms UKI proposed Settlement hygienic measure P=(ΣT/ΣTi)/V, which reflects the change in the toxicity of gas emission of SPM in the process of destruction (aging) and includes an assessment of the dynamics of the toxicity of each substance in the composition of the gas emission of SPM.

Method of assessment and prediction of aging (degradation) of the polymer materials on the dynamics of the total gassing and toxicity of volatile organic compounds (VOCS) migrating from the polymer in the aging process, detected by the method of gas chromatography / mass spectrometry, includes the preparation of samples for artificial climate aging and the detection of volatile organic compounds (VOCS) by gas chromatography / mass spectrometry, the analysis of the qualitative and quantitative composition of gas samples from 35 of the main classes of polymeric materials in the original and aged conditions by measuring composition and concentration of components of gas evolution; the assessment of the toxicity of gas emission from each material in the aging process for each substance, migrating from investigated synthetic polymeric materials (SCM), assessment of changes to the toxicity of the total emission ΣT, developed by hygienic measure P=(ΣT/ΣTn)/V, reflecting the dynamics of changes in the toxicity of gas emission of SPM in the process of aging where Tish Tn and is an indicator of the toxicity of gassing everyone in�ety original and aged conditions, respectively, and Σ and ΣTn is a summary indicator of the toxicity of gassing all members of the sample of synthetic polymeric materials in the original and aged conditions, V is the duration of aging (year, month) and subsequent comparison of experimental and calculated values of hygiene.



 

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4 dwg, 1 tbl

FIELD: medicine.

SUBSTANCE: invention refers to medicine, namely to oncology, and can be used for recognising synchronous multifocal colorectal carcinoma. Substance of the invention consists in measuring preoperative blood follicle-stimulating hormone both in male and female patients suffering from colorectal carcinoma. If its concentration falls within the range of 26.01 to 60.91 IU/l in the females and of 2.71 to 5.67 IU/ml in the males, a single tumour is diagnosed in the patients, and if the hormone concentration is from 2.70 to 5.50 IU/ml in the females and from 12.88 to 52.04 IU/l in the males, the presence of synchronous colorectal new growths are stated. The method can be implemented at the preoperative stage; it is easily reproducible in the oncology hospital environment.

EFFECT: stating the presence of synchronous multifocal colorectal carcinoma.

6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to field of producing carbon-carbon composite materials for various purposes, and is intended for comparative characteristic of impregnation of carbon fibre (CF) braids with melts of pitches, and can be used in improvement of technologies of producing carbon-carbon composite materials, possessing various properties, by modification or replacement of pitch binder and/or carbon fibre, for instance, in research laboratories, in particular, in carrying out laboratory work. To determine degree of impregnation of carbon fibre braids with pitches, carbon fibre braid is placed into glass tube in such a way that the end of braid protrudes from glass tube, and carbon fibres in braid are oriented along glass tube axis, with braid thickness being selected in such a way that it tightly fits glass tube, protruding end of carbon fibre braid is brought in contact with melted pitch and keep in such position, after which carbon fibre braid is extracted from tube and height of impregnation of carbon fibre braid with pitch is determined.

EFFECT: simplification and acceleration of determination are achieved.

1 ex, 3 dwg

FIELD: chemistry.

SUBSTANCE: method involves cutting a sample for analysis and analysing its chemical composition, from which the rubber brand is determined. The sample is cut such that it has pre-decomposition zones. Chemical composition is analysed from a fracture in the sample by X-ray spectral technique on a scanning electron microscope with an energy-dispersive spectrometer. The obtained data on chemical composition of the sample are compared with chemical composition of a known rubber brand or a rubber brand used as a reference.

EFFECT: high accuracy and objectivity of determining a rubber brand.

3 ex, 1 tbl, 2 dwg

FIELD: chemistry.

SUBSTANCE: method involves titration of a suspension with a solvent which is soluble in water and dissolves the suspended resin-like substance until reducing light scattering, which is determined either visually or using optical devices which enable to measure the amount of light passing through the liquid.

EFFECT: rapid estimation of the amount of resin-like substance suspended in water.

3 dwg

FIELD: biotechnology.

SUBSTANCE: sample under study is placed in a sealed container of inert material, thermostated to the temperature above 25°C but below the destruction temperature of the biological object under study. From the thermostated sample the sampling of gas-vapour phase is carried out, which is examined by chromatography-mass spectrometry method by separation on the chromatographic column. Then the components of mixture of the gas-vapour phase are recorded as a series of chromatographic peaks in the chromatogram and are identified on time of their exit on the chromatogram and mass spectrum. Calculation of the concentration of alcohols is carried out in accordance with the obtained chromatogram according to the relevant peak areas of components of mixture of the gas-vapour phase.

EFFECT: increased sensitivity, accuracy and reliability of the identification and quantitative research, preservation of the object under study for possible repeat or additional studies.

1 tbl, 8 dwg

FIELD: chemistry.

SUBSTANCE: method of simultaneous determination of methanol and diethylene glycol in natural and sewage water by LC method with separation of said components in chromatographic column in flow of eluent, which represents sulphuric acid solution in deionised water with molar concentration 2.5 mmole/dm3; registering difference of indices of refraction of eluent solution and solutions, which contain target components and processing results of measurements by method of absolute calibration. Sample preparation does not require dilution of analysed water sample up to content of target components 10 g/dm3, more concentrated samples are diluted with deionised water.

EFFECT: quickness and simultaneousness of determination of diethylene glycol and methanol content.

FIELD: chemistry.

SUBSTANCE: described is an alcohol thermal hydration chamber and an apparatus for real-time determination of isotopic composition of non-exchangeable hydrogen and deuterium atoms in ethanol samples, comprising: A) an alcohol thermal dehydration chamber, B) an indicating device which has a pyrolysis reactor (26) and a continuous flow isotope spectrometer and is connected to the alcohol thermal dehydration chamber by C) a system of valves, connectors and capillary tubes which are used to transfer the analysed sample and clean the alcohol thermal dehydration chamber; the procedure for real-time determination of isotopic composition of non-exchangeable hydrogen and deuterium atoms in ethanol samples and the procedure for off-line preparation of ethene (ethylene) gas by means of the alcohol thermal dehydration chamber and for the identity and geographical origin of wines, alcoholic beverages, fruit juices, honey and etc.

EFFECT: high accuracy of determination.

9 cl, 3 dwg

FIELD: chemistry.

SUBSTANCE: invention can be used for simultaneous determination of content of ions of transition metals Fe(III), Fe(II), Cu, Pb, Zn, Ni, Co, Cd, Mn in natural, surface, waste, underground water and water extracts of saline soil. High-performance liquid chromatography is used for simultaneous determination of content of ions with separation of the ions in a chromatographic column in eluent flow. The eluent consists of a solution of sodium octane sulphonate, sodium hydrotartrate and acetonitrile in dionised water. Mixing is then carried out in a post-column reaction module with a reagent which is a solution of PAR ([4-(2-pyridylazo) resorcinol], glacial acetic acid and aqueous ammonia in deionised water. Further, the difference in optical absorption of the eluent and complexes of the determined ions with the added reagent is detected using spectrophotometric detector in the visible spectrum at 520 nm.

EFFECT: increased accuracy, faster simultaneous determination of content of transition metal ions in natural, surface, waste, underground water and water extracts of saline soil.

2 tbl

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

Gas analyzer // 2141656
The invention relates to devices for analytical instrumentation and can be used as a chromatographic device in the refining, petrochemical and other fields to measure the microtraces

FIELD: chemistry.

SUBSTANCE: method includes preparing a 1% solution of engine oil in hexane for full extraction of zinc dithiophosphates from engine oil and purity of the obtained samples; adding the obtained solution to an extraction cartridge filled with hydroxylated silica gel in amount of not more than 2 ml of the 1% solution of the oil in hexane per 1 g sorbent; successively passing a hexane:acetone mixture taken in volume ratio of 9:1, respectively; passing an isopropanol:water:phosphoric acid:acetonitrile mixture, taken in ratio of 4:2:0.4:1, respectively. Each mixture is taken in amount of not less than 1.5 times the volume of the oil solution in hexane. An aliquot of the obtained solution is analysed by RP HPLC.

EFFECT: high accuracy and reliability of determination.

1 tbl, 7 dwg

FIELD: chemistry.

SUBSTANCE: method involves extraction of drilling fluid in an extractor in order to continuously obtain a stream of extracted gases at the output of the extractor, containing the analysed hydrocarbons and at least one spurious compound which is not water and is more polar than the analysed hydrocarbons. The gas stream is then carried from the extractor over a transfer line into a separation column to separate the analysed hydrocarbons depending on their elution time in the separation column. Further, successive detection and/or determination of the amount of each analysed hydrocarbon is carried in a detector located at the output of the separation column. One or each spurious compound can have elution time in the separation column ranging from the elution time of the first analysed hydrocarbon in the separation column to the elution time of the last analysed hydrocarbon in the separation column. The method also involves passing the gas stream through a surface for chemical and/or physical interaction with the spurious compound which is in contact with gases between the output of the extractor and the input of the separation column, for selectively holding said spurious compounds without delaying the analysed hydrocarbons and so as to prevent washing-off of the spurious compounds in the separation column.

EFFECT: high accuracy of qualitative and quantitative evaluation of analysed hydrocarbons, and high rate of analysis.

FIELD: chemistry.

SUBSTANCE: invention refers to drinking, natural and waste water, precipitation sanitary-hygienic control and analysis for phenol content. Method includes chemical phenol modification in 2,4,6-tribromphenol, extraction concentration of 2,4,6- tribromphenol and gas chromatography testing. Herewith chemical modification is preceded with humic acid removal on aluminium oxide from aqueous medium sample with copper sulphate in amount 0.05-0.25% of aqueous medium sample weight.

EFFECT: higher analysis reliability.

7 ex, 2 tbl, 7 dwg

FIELD: silicon compounds technology.

SUBSTANCE: tetrafluorosilane production process comprises following stages: (1) hexafluorosilicate heating; (2-1) reaction of tetrafluorosilane gas containing hexafluorodisiloxane formed in stage (1) with fluorine gas; (2-2) reaction of tetrafluorosilane gas containing hexafluorodisiloxane formed in stage (1) with fluorine-polyvalent metal compound; (2-3) reaction of tetrafluorosilane gas obtained in stage (2-1) with fluorine-polyvalent metal compound. Finally, high-purity tetrafluorosilane with 0.1 ppm by volume of hexafluorodisiloxane is obtained, which is applicable in manufacture of optical fiber, semiconductors, and sun battery elements.

EFFECT: reduced content of impurities in product.

24 cl, 1 dwg, 1 tbl, 9 ex

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