Method for determining content of sulphurated hydrogen and light mercaptans in gas condensate and oils

FIELD: oil and gas industry.

SUBSTANCE: method involves sampling and preparation of sample with thermostatting at temperature of 50-70°C with simultaneous extrusion of sulphurated hydrogen and light mercaptans with inert gas or air to in-series located absorbing solutions; at that, as absorbing solution for determining sulphurated hydrogen, there used is sodium carbonate solution, and as absorbing solution for determining light mercaptans there used is sodium hydrate solution, quantitative estimation of sulphurated hydrogen and light mercaptans by method of iodimetric titration. At that, before mixture of vapours of light hydrocarbons with sulphurated hydrogen and light mercaptans, which is extruded from the sample with air or inert gas, enters in-series located absorbing solutions, it is cooled to the temperature of more than 15°C to 20°C.

EFFECT: improving accuracy and reliability, and speeding-up the analysis.

5 ex, 3 tbl, 1 dwg

 

The proposal relates to methods of analytical quality control of oil and gas condensate and can be used in oil and gas refining industries.

There is a method of determining the content of hydrogen sulfide and light mercaptans (methyl - and ethyl mercaptan) in oil by gas chromatography, based on the evaporation and the displacement of the volatile components of the oil with an inert carrier gas in the evaporator at a temperature of 70°C, the separation of crude oil components on the chromatographic column at a temperature of 35 to 60°C, the Desk emerging from the chromatographic column of hydrogen sulfide and light mercaptans flame photometric detector and calculating the results of determination by the method of absolute calibration (GOST R 50802-95). This method is set as a standard test method in accordance with GOST R 51858-2002 Oil. General technical conditions" to determine the facilities of oil to a certain type when delivered to consumers.

The disadvantages of this method are the necessity of using complex and expensive equipment, failure analysis is stationary laboratory, a large error and the scatter of the measurements associated with too small a volume of the analyzed sample, and limitation of range of the analyzed products are virtually the only ski oils product quality.

There is a method of determining the content of hydrogen sulfide and mercaptans in petroleum products, based on potentiometric titration (GOST 17323-71 "Fuel for engines"). This method involves sampling, diluting it with a solvent and further potentiometric titration and the construction of titration curve, which represents the dependence of the values of the electrode potential from the volume of titrant, finding the equivalence point on the graph, allowing to calculate the concentration of mercaptans in the sample. The hydrogen sulfide content is determined by difference of the volume of titrant used for titration before and after the removal of hydrogen sulfide from oil.

The disadvantages of this method are the duration of the analysis and the high cost of silver nitrate used for titration, involvement in the analysis not only of light mercaptans, but heavy mercaptans and sulfur compounds from other classes, which leads to the gentle curves of potentiometric titration and related error in the determination of the equivalence point, and to an overestimation of the results of the analysis of the mercaptans. High accuracy determination of hydrogen sulfide on the difference between the results of the two analyses in connection with the imprecision of the definitions and loss of light mercaptans in the process of binding the Oia of hydrogen sulfide. These shortcomings lead to a narrowing of the range of the analyzed products almost exclusively petroleum products, namely fuels for engines.

There is a method of determining the content of hydrogen sulfide in fuel oils (petroleum product), including the selection and preparation of samples, the displacement of the hydrogen sulfide from the resulting mass of inert gas in the absorbing solution, the quantitative determination of hydrogen sulfide by the method iodometric titration. (U.S. Pat. No. 2155960, IPC G01 No. 33/22, publ. 10.09.2000). According to the method take a sample of fuel oil 20-50 g and diluted in the ratio 1:1 with an organic solvent, stir until smooth, then replacing hydrogen with an inert gas within 1-2 h in the adsorption solution (30%solution of cadmium chloride) and produce quantitative determination of hydrogen sulfide content method iodometric titration.

The disadvantages of this method are: the need for dilution and mixing of oil in the process of sample preparation, which leads to the loss of hydrogen sulfide and inaccuracies of the analysis; the relatively large size of the sample and the associated duration of the purging of the oil with an inert gas. The method does not provide simultaneous determination of hydrogen sulfide and light mercaptans in oil and gas condensate and light mercaptans in oil is Ah.

The closest in technical essence to the present invention is a method of determining the content of hydrogen sulfide and light mercaptans in oil, oil products and gas condensate (U.S. Pat. No. 2285917 IPC G01N 33/22, 33/26, SW 17/16, SS 321/04 published. 20.10.2006, including the selection and preparation of samples, the displacement of hydrogen sulfide and light mercaptans with an inert gas or air in the absorbing solutions and quantitative determination of hydrogen sulfide and mercaptans method iodometric titration.

The disadvantage of this method is that the Stripping of hydrogen sulfide and light mercaptans is made by bubbling the sample air or inert gas at a temperature of 60±5°C. the composition of the gas condensates is from 50 to 95% of light hydrocarbons and oil composition is from 3 to 15% and when the blow-off portion of the hydrocarbon condensate accumulates in the absorption bottle, which leads to an overestimation of the results of determination of hydrogen sulfide content.

The technical objective of the proposed method is an extension of functionality by increasing the accuracy of determining the content of hydrogen sulfide and light mercaptans from gas condensate and crude oil.

The result is achieved by the method of determination of hydrogen sulfide and light mercaptans from gas condensate and oil, including the selection and preparation of samples with the temperature at which the temperature of 50-70°C with simultaneous displacement of hydrogen sulfide and light mercaptans with an inert gas or air in consistently located absorbing solutions, and as an absorbing solution for hydrogen sulfide using a solution of carbonate of sodium, and as an absorbing solution for determining the light mercaptans use a solution of sodium hydroxide, quantitative determination of hydrogen sulfide and mercaptans method iodometric titration.

What's new is that to prevent condensation of vapors of the hydrocarbons in the flask with the absorption solution and to resolve the error when iodometric titration before admission to consistently located absorbing solutions displaced from the sample air or inert gas mixture of light hydrocarbons with hydrogen sulfide and light mercaptans cooled to a temperature of from 15 to 20°C for condensation of hydrocarbons.

The drawing shows a diagram of the laboratory setup for determining the content of hydrogen sulfide and light mercaptans from gas condensate and oil.

Using the laboratory setup is exercised by the displacement of hydrogen sulfide and light mercaptans from gas condensate and oil air or inert gas through the hydrocarbon trap condensate in the absorbing solutions.

Installation for implementing the method includes a syringe for sampling 1, bottle 2 for ozonation gas condensate, air or inert gas, thermostat 3, in which p is derived temperature of 50-70°C, trap light hydrocarbons vapor 4, placed in a thermostat 5, flask with absorptive solutions 6 and 7, valve 8, the vacuum pump 9, which regulates the air supply.

The proposed method of determining the content of hydrogen sulfide and light mercaptans from gas condensate was tested in laboratory and field conditions on gas condensate Irgiz fields with different contents of hydrogen sulfide and light mercaptans.

Implementation of the method is demonstrated on the example of a specific implementation.

Example 1. For determining the content of hydrogen sulfide and light mercaptans used gas condensate Irgiz deposits with an estimated concentration of hydrogen sulfide 200-350 million-1(ppm), light mercaptans 12-40 million-1(ppm). The input sample is carried out by extrusion of gas condensate from the syringe 1 by weight of 2 g at the inlet of the flask 2, which is placed in a thermostat with 3 temperature 60°C, when the suction of the vacuum pump 9. To the flask 2 downstream trap 4, placed in a thermostat 5 at a temperature of 15°C for condensing light hydrocarbons flask with absorptive solutions 6 and 7, which are filled respectively by 10 cm35%-aqueous solution of sodium carbonate (hydrogen sulfide) and a 5%aqueous solution of sodium hydroxide (to absorb light mercaptans) and in counny pump 9 with regulating valve 8. The air purge is carried out for 2 min, after which quantitatively determine the content of hydrogen sulfide and light mercaptans method iodometric titration. The hydrogen sulfide content amounted to 188 million-1(ppm), and light mercaptans - 24.4 million-1(ppm).

Example 2. The study of gas condensate was carried out according to the scheme of the prototype. The hydrogen sulfide content amounted to 245 million-1(ppm), and light mercaptans - 32.8 million-1(ppm).

Table 1 shows the results of determining the content of hydrogen sulfide and light mercaptans from gas condensate on the proposed method and the prototype.

Table 1
no PPMass fraction of hydrogen sulfide million-1, (ppm)Mass fraction of light mercaptans, mn-1(ppm)
the proposed methodprototypethe proposed methodprototype
118824524,432,8
218 24722,931,0
318624822,531,5
433942624,335,2
535645724,438,2
6343441to 25.337,3

The value of the hydrogen sulfide content in the determination of the prototype is higher than the definition of the proposed method, on 20-24%, and light mercaptans - 25-36%due to the ingress of condensate of light hydrocarbons in the adsorption solution.

Example 3. Determination of the mass fraction of hydrogen sulfide and light mercaptans carried out according to the scheme given in example 1, but as gas Stripping used helium, nitrogen and associated gas not containing hydrogen sulfide.

Table 2 shows the results of determining the content of hydrogen sulfide and light mercaptans from gas condensate on offer with the person using different gases at the Stripping of the designated components.

Table 2
no PPName used gasMass fraction, m-1(ppm)
hydrogen sulfidelight mercaptans
1The air343to 25.3
2Helium34124,8
3Nitrogen34224,6
4Hydrocarbon gas, containing hydrogen sulfide34324,2

From the data presented in table 2, it follows that all of these gases can be used for Stripping in the determination of hydrogen sulfide and light mercaptans from gas condensate and crude oil.

Example 4. Determination of the mass fraction of hydrogen sulfide and light mercaptans in petroleum LTD TNS "Development" with the alleged content of hydrogen sulfide 300-600 million-1(ppm), and light mercaptans 2-10 million (ppm) was carried out according to the scheme given in example 1. Mass fraction of hydrogen sulfide and light mercaptans amounted to 517 and 5.3 million-1(PPT), respectively.

Example 5. Study of oil LTD TNS "Development" was carried out according to the scheme of the prototype. The hydrogen sulfide content amounted to 580 million-1(ppm), and light mercaptans - 6.1 million-1(ppm).

Table 3 presents the results of determining the content of hydrogen sulfide and light mercaptans in oil of the proposed method and the prototype.

td align="center"> 519
Table 3
no PPMass fraction of hydrogen sulfide, mn-1(ppm)Mass fraction of light mercaptans, mn-1(ppm)
the proposed methodprototypethe proposed methodprototype
15175805,36,1
2520581of 5.46,2
35785,36,0
43523975,15,9
53503904,85,6
6352390the 4.7of 5.4

Value content of hydrogen sulfide in oil when defining the prototype is higher than the definition of the proposed method, 10-13%, and light mercaptans - 13-17%due to the ingress of condensate of light hydrocarbons from oil absorbing solution.

The proposed solution can be used for analytical control of the content of hydrogen sulfide and light mercaptans from gas condensate and crude oil.

The advantage of this technical solution is the extension of functionality by increasing the accuracy of determining the content of hydrogen sulfide and light mercaptans from gas condensate and oil, with the possibility of use as gas Stripping inert to define the components of gases: helium, nitrogen uglevodorodnogo gas, does not contain hydrogen sulfide.

1. The method of determining the content of hydrogen sulfide and light mercaptans from gas condensate and oil, including the selection and preparation of samples with temperature control at temperatures of 50-70°C with simultaneous displacement of hydrogen sulfide and light mercaptans with an inert gas or air in consistently located absorbing solutions, and as an absorbing solution for hydrogen sulfide using a solution of carbonate of sodium, and as an absorbing solution for determining the light mercaptans use a solution of sodium hydroxide, quantitative determination of hydrogen sulfide and light mercaptans method iodometric titration, characterized in that prior to admission to consistently located absorbing solutions displaced from the sample air or inert gas mixture vapor light hydrocarbons with hydrogen sulfide and light mercaptans cooled to a temperature of from greater than 15 to 20°C.

2. The method of determining the content of hydrogen sulfide and light mercaptans from gas condensate and oil according to claim 1, characterized in that as the inert gas inert to hydrogen sulfide and light mercaptans gas, for example nitrogen, hydrocarbon gas, containing hydrogen sulfide and mercaptans.



 

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