Method of determining brand of vulcanised rubber

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

 

The invention relates to a method of determining brand vulcanized rubber and can be used in mechanical engineering.

Known way to determine the grade of vulcanized rubber, taken by the authors for similar, comprising heating the analyzed sample in an oven to a temperature of degradation and the study of the products formed spectral method Spectral analysis of technical rubbers. The index of domestic and foreign materials in aviation technology. NIAT, 1988, vol. No. 11, cep.VIII, c.11). Then, given the color of the rubber and the non-combustible residue, as well as its chemical composition, installed brand rubber. The data obtained are compared with the parameters specified in the control table. One of the main disadvantages of this method is that not all elements are determined by the spectral method, for example CL. In addition, the low precision of the analysis results and subjectivity in their decoding are one of the major disadvantages of this method.

The closest to the technical nature of the claimed method is to determine the grade of vulcanized rubber, comprising the cutting of the sample for the study and analysis of its chemical composition, on the basis of which is determined by the brand of vulcanized rubber, prototype (patent RF №2053512, 27.01.1996, G01N 33/44). The essence of this method consists that what is compiled directory curves derivation for well-known brands of vulcanized rubbers. A sample cut from an unknown brand rubber is heated to a temperature of destruction and record the signal with differentsialnoi thermocouple. The obtained curves are compared with the curves of well-known brands of rubber and the results of the analysis of the curves define the brand of vulcanized rubber.

The disadvantage of this method is the low precision of the results: firstly, because of the limited possibilities of spectral analysis (as was mentioned above, CL, and are not defined), second - aging rubber leads to a significant change in the progress curves of derivatograph, and hence to a large degree of error.

The technical result of the claimed method is to improve the accuracy and objectivity determine the grade of rubber.

This technical result is achieved that the way to determine the grade of vulcanized rubber, comprising the cutting of the sample for the study and analysis of its chemical composition, on the basis of which the judge rubber stamp, a sample cut out taking into account the presence of zones of zaratracheny, and chemical composition analysis is carried out with a fracture of the sample x-ray method for scanning electron microscope with energy dispersive spectrometer, comparing the obtained data khimicheskogo the composition of the sample with the chemical composition of a famous brand of rubber or rubber stamps, adopted as the standard.

Cutting the sample with regard to the presence of zones of zaratracheny (Dol) allows to exclude in the survey area ingress of foreign particles, distorting the results (chemical analysis). The analysis of the chemical composition of the fracture of the sample x-ray method for scanning electron microscope with energy dispersive spectrometer allows to obtain high precision results due to the possibility of defining a larger number of chemical elements (such as CL, s, and O) of the sample, to exclude the impact of the aging of rubber on the research results. All this, consequently, increases the accuracy and objectivity determine the grade of rubber.

The essence of the claimed invention is illustrated in the following materials:

table 1 - the data directory of the chemical composition of well-known brands of vulcanized rubbers;

figure 1 shows the derivation sample vulcanized rubber obtained by the method of derivatographic analysis;

figure 2 shows a graph of curves derivation of famous brands vulcanized rubber obtained by the method of derivatographic analysis.

The claimed method to determine the grade of vulcanized rubber is defined as follows.

Sample cut out from the workpiece or goto the CSOs products (unknown brand rubber) with the obligatory presence of a zone of zaratracheny (Dol) 2,0 x 3,0 mm It is necessary to exclude in the survey area sample hit a large number of particles, distorting the results of the study. Next, the sample is placed in a sample holder and placed in a column of a scanning electron microscope, for example EVO-50-taken from, with attachment for x-ray microanalysis by energy dispersive spectrometer INCAx-act. The results of the analysis of the chemical composition of the investigated sample is compared with the result of the chemical composition of well-known brands of rubber or rubber grade adopted as the standard. The results of the analysis determine the brand of the investigated vulcanized rubber.

The chemical composition of the known brands of vulcanized rubber or brand of vulcanized rubber, adopted as the standard is determined in advance (prior to the analysis of the chemical composition of the sample rubber grade) is similar to the claimed method of the image and catalog parameters of their chemical composition.

A catalogue of the chemical composition of the famous brands of rubber (or rubber stamps, accepted for standard) allows you to accelerate the analysis and the procedure to determine the grade of the investigated rubber.

Further, as examples of the results determine the grade of vulcanized rubber by known methods and the claimed method.

In the present who's following examples, it was necessary to match the sample rubber stamp BUT-68-1.

Example 1

To match the sample rubber stamp BUT-68-1 was used in the claimed method to determine the grade of vulcanized rubber.

Of the finished product was cut sample with the presence of a zone of zaratracheny (Dol) and carried out x-ray microanalysis in the scanning electron microscope EVO-50-taken from energy dispersive spectrometer.

The results of x-ray microanalysis of the sample was obtained following chemical composition:

C=86,47%, O=Is 3.08%, S=0,41%, Cl=7,03%, Zn=1,58%, Mg=0,62% (hydrogen by this method is not defined).

Next, we compared the obtained results with the data directory (see table 1). From table 1 it is seen that the analyzed sample can be attributed only to the brand with the rubber BUT-68-1.

The above example shows that the claimed method to determine the grade of vulcanized rubber enables high accuracy (about 100%) to establish the brand of the investigated rubber based on the obtained data of the chemical composition of the sample.

Example 2

To match the sample rubber stamp BUT-68-1 was used known way to determine the grade of vulcanized rubber with the help of spectral analysis, which was carried out heating the sample in an oven up to temp the atmospheric temperature degradation and study the resulting products of the spectral method.

The results of the analysis the following data were obtained in the chemical composition of the investigated sample:

Mg=2.6%, and Zn=5,6%, S=2.6% Of (C, O and Cl - is not defined). Color rubber black. Color of dry residue light gray.

The results show that the sample of rubber can be attributed to several brands - possible brand rubber:

BUT-68-1, B14 or B14-1.

From this example it follows that there is a method to determine the grade of vulcanized rubber with the help of spectral analysis is not possible from the data of the chemical composition of the sample to accurately establish the brand of the investigated rubber. The accuracy of this method is 58-60%.

Example 3

To match the sample rubber stamp BUT-68-1 was used known way to determine the grade of vulcanized rubber using the method derivatographic analysis of rubber, whereby the sample was heated to the temperature of decomposition and the recorded signals with a differential thermocouple. According to the obtained data was constructed derivation of thermocouple signal from the temperature of the furnace (curve derivation).

The comparative analysis of the obtained curve derivation sample (see figure 1) with the curves of the derivations of well-known brands of vulcanized rubber (see figure 2). Comparative analysis showed that the sample of rubber can be attributed to the following grades of rubber:

BUT-68-1, B14 or B14-1.

From the above example it follows that there is a method to determine the grade of vulcanized rubber by the method derivatographic analysis does not allow to determine precisely mark the investigated rubber. The accuracy of this method is 59-61%.

Thus, from the above examples it is seen that in comparison with the known proposed method provides higher accuracy and objectivity of the analysis and can be used for rapid analysis of rubber during conduct of examination rubber products.

Table 1
Brand rubberThe content of chemical elements in %
OSSiClCaZnMgNa
BUT-68-183,53-90,76and 2.26-5,030,39-0,79-6,70 to 10.7-1,06-2,65 0,44-0,91-
In-14-190,96-98,251,74-3,521,21-3,06--0,07-0,201,58-2,820,08-0,120,18-0,22
B-1492,67-97,312,67-2,741,88-2,67--0,07-0,171,78-2,49-0,31
382673,44-84,399,99-17,090,90-1,420,13-0,14-4,06-7,710,45-1,49--
Ypres 107871,88-78,21scored 8.38-17,580,51 was 1.432,67-6,250,230,15-1,102,55-of 10.58-0,19
3508-N-174,81-78,996,92-8,54about 0.53-0.540,09-0,1011,32-15,00-2,11-2,310,70-1,17-

The way to determine the grade of vulcanized rubber, comprising the cutting of the sample for the study and analysis of its chemical composition, on the basis of which the judge rubber stamp, characterized in that the sample cut out taking into account the presence of zones of zaratracheny, and chemical composition analysis is carried out with a fracture of the sample x-ray method for scanning electron microscope with energy dispersive spectrometer, comparing the obtained data of the chemical composition of the sample with the chemical composition of a famous brand of rubber or rubber grade adopted as the standard.



 

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