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
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.
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 184.108.40.20697-11) 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.
The dynamics of the total (ΣT) gassing from materials in terms of ageing in the process of IPC.
|Table 1||Name of material||Initial state||10 years||20 years||25 years||33|
|the insulating tape brand LESB||0,005||0,013||0,045||0,012||0,005|
|glass fiber SF-2-50G-0,8||0,011||0,027||0,018||0,012||0,003|
|cold cure glue ADV-5||0,371||0,011||0,008||0,026||0,002|
|fabric tech. Polyamide art. 56003||0,047||0,006||0.031 inch||0,000||0,000|
|tape trick. Looped KTL-1000/6||0,009||0,013||0,053||0,020||0,002|
|polyamide 610 injection molding||0,037||0,012||0,026||0,071||0,014|
|varnished cotton LSMS-105||Of 0.021||0,010||0,111||0,027|
|film of fluoroplastic f-4 MB||0,008||0,002||0,006||0,013||0,002|
|tape tech. Aramina Lter-20-200||0,015||0,017||0,012||0,155||0,007|
|fluoropolymer tape brand U-f-4 EA/180/KO||0,016||0,011||0,032||0,006||0,001|
|the tube 305 TV-50||0,023||0,008||0,045||0,013||0,001|
|the rubberized fabric 918-9||0,018||0,022||0,013||0,008||0,001|
|the adhesive tape LT-19||0,036||0,029||0,048||0,016|
|putty EP-0010||0,085||0,002||0.076 mm||0,022||0,001|
|foam polystyrene tiled PS-1-150||0,038||0,061||0,022||Of 0.021||0,006|
|the rigid polyurethane foam Mediart-13 (mark 5)||0,061||0,029||0,025||0,011||0,015|
|the fabric is heat-resistant double-layered art. ND-250 Cu||0,035||0,014||0,002||0,090||0,002|
|the technical fabric polyamide art. 56260 Cu IN||0,190||0,348||0,045||0,119||0,002|
|film brand Vitur T 0533-90||0,411||0,107||0,006||Of 0.021||0,006|
|sealant Humi Seal UY40||0,007||0,006||Of 0.021||0,247||0,002|
|polycarbonate glass-filled-grades PK-L-SV||0,036||0,032||0,003||0,305|
|heat resistant decorative finishing material "arlit" type "Talca-1"||0,091||0,010||0,013||0.031 inch||0,004|
|(ΣT) together with the use of tested materials||2,08||1,006||1,43||1,45||0,18|
�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.
|P is less than 1||hygienic P||Initial state||10 years||20 years||25 years||33|
|the insulating tape brand LESB||0,9||0,005||0,013||0,045||0,012||0,00|
|tape technical Aramina Lter-20-200||0,1||0,015||0,017||0,012||0,155||0,007|
|polycarbonate glass-filled-grades PK-L-SV||0,1||0,036||0,032||0,003||0,305|
|varnished cotton LSMS-105||0,8||Of 0.021||0,010||0,111||0,027|
|P from 1 to 10||hygienic index||Initial state||10 years||20 years||25 years||33|
|glass fiber SF-2-50G-0,8||3,7||0,011||0,027||0,018||0,012||0,003|
|ribbon knit stitch KTL-1000/6||4,9||0,009||0,013||0,053||0,020||0,002|
|polyamide 610 injection molding||2,6||0,037||0,012||0,026||0,071||0,014|
|film of fluoroplastic f-4 MB||4,9||0,008||0,002||0,006||0,013||0,002|
|foam polystyrene tiled PS-1-150||6,3||0,038||0,061||0,022||Of 0.021||0,006|
|the rigid polyurethane foam Mediart-13 (mark 5)||4,2||0,061||0,029||0,025||0,011||0,015|
|sealant Humi Seal UY40||3,2||0,007||0,006||Of 0.021||0,247||0,002|
|the adhesive tape LT-19||2,3||0,036||0,029||0,048||0,016|
|P from 10 to 30||hygienic index||Initial state||10 years||20 years||25 years||33|
|fluoropolymer tape brand U-f-EO/180/KO||16,1||0,016||0,011||0,032||0,006||0,001|
|the tube 305 TV-50||18,0||0,023||0,008||0,045||0,013||0,001|
|the rubberized fabric 918-9||30,0||0,018||0,022||0,013||0,008||0,001|
|the fabric is heat-resistant double-layered art.ND-250 Cu||A 20.7||0,035||0,014||0,002||0,090||0,002|
|"Arlit" type "Talca-1"||26,0||0,091||0,010||0,013||0.031 inch||0,004|
|P over 30||hygienic index||Initial state||10 years||20 years||25 years||33|
|cold cure glue ADV-5||185,4||0,371||0,011||0,008||0,026||0,002|
|the technical fabric polyamide art. 56003||To 166.1||0,047||0,006||0.031 inch||0,000||0,000|
|the technical fabric polyamide art. 56260 Cu IN||105,6||0,190||0,348||0,045||0,119||0,002|
|putty EP-0010||63,6||0,085||0,002||0.076 mm||0,022||0,001|
|primer AK-070||RUB 252.8||0,153||0,006||0,038||0,013||0,001|
|film brand Vitur T 0533-90||72,5||0,411||0,107||0,006||Of 0.021||0,006|
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.
|P is less than 1||T-test (33)||Hygienic P|
|the insulating tape brand LESB||0,005||0,9|
|tape technical Aramina Lter-20-200||0,007||0,1|
|polycarbonate glass-filled-grades PK-L-SV||0,003||0,1|
|varnished cotton LSMS-105||0,027||0,8|
|R from 1 to 10||T-criterion (33)||Hygienic index|
|glass fiber SF-2-50G-0,8||0,0030||3,7|
|ribbon knit stitch KTL-1000/6||0,0018||4,9|
|polyamide 610 injection molding||0,0143||2,6|
|film of fluoroplastic f-4 MB||Of 0.0016||4,9|
|foam polystyrene tiled PS-1-150||0,0060||6,3|
|the rigid polyurethane foam Mediart-13 (mark 5)||0,0145||4,2|
|sealant Humi Seal UY40||0,0022||3,2|
|the adhesive tape LT-19||0,0160||2,3|
|R from 10 to 30 (60)||T-test (33)||Hygienic index|
|fluoropolymer tape brand U-f-4 EA/180/KO||Is 0.0010||16,1|
|the tube 305 TV-50||With 0.0013||18,0|
|the rubberized fabric 918-9||0,0006||30,0|
|the fabric is heat-resistant double-layered art. ND-250 Cu||0,0017||A 20.7|
|fibreglass CAST-IN-1,0||0,0023||A 33.3|
|"Arlit" type "Talca-1"||0,0035||26,0|
|P over 60||T-test (33)||Hygienic index|
|cold cure glue ADV-5||0,0020||185,4|
|the technical fabric polyamide art. 56003||0,0003||To 166.1|
|the technical fabric polyamide art. 56260 Cu IN||0,0018||105,6|
|putty EP-0010||With 0.0013||63,6|
|primer AK-070||0,0006||RUB 252.8|
|film brand Vitur T 0533-90||0,0057||72,5|
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.
FIELD: machine building.
SUBSTANCE: invention relates to devices and method of the vibration protection of vehicles, in particular to shock-absorbing gaskets under bases of rails or bars of the pointworks, as well as for vibration protection of the construction structures and industrial equipment. Method of shock-absorber stiffness regulation includes addition of the synthetic polypropylene fibre from 0.1 to 12 wt % to wet porous rubber mixture based on unsaturated rubber or mixture of rubbers, as calculated to weight of the rubber mixture with further creation and vulcanisation of the produced products. At that amount of the polypropylene fibre is calculated as per the preliminary obtained by tests relationship between the shock-absorber stiffness and content of fibre within the specified range and ensuring the required stiffness.
EFFECT: method produces the porous shock-absorber with set Young's modulus characterised, in principle, by the linear relationship of the Young's modulus and content of the specified polypropylene fibre.
18 cl, 1 dwg, 8 tbl
SUBSTANCE: marker used is a soluble form of adhesion molecules of the family ICAM - sICAM-1, sICAM-2, sICAM-3. If observing sICAM-1 decrease from 29-37.2 to 23-24, sICAM-2 decrease from 19.1-21.1 to 13-14, sICAM-3 decrease from 23-30.7 to 14-17, the nutritional support is considered to be effective.
EFFECT: method enables increasing the assessment accuracy of the efficacy of the nutritional support accompanying ulcerative colitis.
FIELD: measurement equipment.
SUBSTANCE: invention relates to analytical chemistry of food production facilities. The method to assess safety of packing polymer materials for thermal processing of vacuumised food products includes formation of a polymer material in the form of a packet, its vacuumising, sealing and thermal processing, after which the packet is thermostatted at room temperature, 5.0 cm3 of dried air is pierced into it with a syringe, and in 5 minutes, not taking the syringe out, they take 3.0 cm3 of air. The produced sample is introduced into a tight cell of detection in a "piezoelectronic nose" device, which comprises an array of seven mass-sensitive piezosensors. They record variation of signals of piezosensors in pairs of equilibrium gas phase of the sample for 60 s with the interval of 1 s, the highest responses of piezosensors are formed into a mass-aromogram of maxima, the area of the mass-aromogram is calculated. Under identical conditions they analyse the standard sample of the polymer material. Assessment of safety of the polymer material is carried out by comparison of the area of mass-aromograms of the analysed sample and the standard sample. Difference of the area of mass-aromograms by more than 30.0±1.0% certifies non-compliance of the sample with the standard of the polymer package.
EFFECT: invention makes it possible to assess the level of possible emission of highly volatile compounds from polymer materials in process of thermal processing with increased accuracy and reduction of analysis time.
2 dwg, 1 tbl
FIELD: test equipment.
SUBSTANCE: invention refers to material test methods. Essence of the invention: a sample is first strained to the maximum set deformation, held in this deformation for a given time, compressed to the initial unloaded state, left in it for a given time, with further cyclic deformation with delays in each deformation stage of compression and tension, where at each tension cycle the set deformation is less than at the previous cycle, and the set deformation at each unloading cycle is larger than in the previous cycle.
EFFECT: more information on material properties from a sample test, new information represented by equilibrium stress-strain curve, dissipation loss, material softening after each tension/compression cycle, and relaxation curves together with material structure recovery curves for various deformations.
2 cl, 1 dwg
FIELD: measurement equipment.
SUBSTANCE: invention relates to measurement equipment, in particular, to devices for measurement of profile of surfaces of low-modular viscoelastic sheet materials of light industry, namely, man-made and natural leathers, etc. A device to detect profile of materials in deformed condition, comprising a base, a counting unit, a locating element, installed as capable of rotation around its axis, differing by the fact that the locating element is made in the form of a semi-cylinder with a hollow semi-cone and two limiting plates to fix a sample; the device comprises an additional counting unit fixed on the semi-cylinder, to detect bending radius of the investigated sample, arranged in parallel to the semi-cone guide, at the same time the main counting unit is made as combined, capable of displacement along the axis of rotation of the locating element and comprises a strain gauge motion sensor and a digital optical microscope.
EFFECT: device makes it possible to study hidden defects of natural leather and man-made materials, to determine variation of material relief under bending deformation.
2 cl, 1 dwg
SUBSTANCE: disclosed is a method of determining the glass-transition point of tetrazole-based polymer composite materials based, according to which the glass-transition point is determined from the change of slope of a curve of temperature versus the inverse of dielectric constant 1/ε'=f(T).
EFFECT: high accuracy and reliability of determining the glass-transition point of tetrazole-based polymer composite materials.
4 dwg, 1 tbl
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.
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
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
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.
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
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.
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
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.
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
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
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.
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