SU1555593A1 - Method of charging vessels with gas mixture under pressure - Google Patents

Abstract

The invention relates to methods for producing gas mixtures of a given composition in cylinders under pressure and can be used in the gas, chemical, instrument-making and petrochemical industries for metrological and technical purposes. The purpose of the invention is to increase the stability of the composition of hydrogen sulfide gas mixtures - is achieved by initially filling the cylinder with hydrogen sulfide under an overpressure of 1 to 30 kgf / cm ² , being kept for 72 to 120 hours, after which the pressure is released to the partial pressure of hydrogen sulfide in the mixture and filled The balloon is the second component of the mixture until a high pressure is obtained. This contributes to the creation on the inner surface of the cylinders of a protective sulfide film, which prevents the mixture from contacting the metal with the wall. 1 tab.

Description

The invention relates to methods for producing gas mixtures of a given composition in cylinders under pressure and can be used in the gas, chemical, instrument-making, oil refining and petrochemical industries for metrological and technical purposes.

The aim of the invention is to increase the efficiency by increasing the stability of the composition of hydrogen sulfide-containing gas mixtures during storage.

The method is carried out as follows.

A pre-dried and ot-vacuumized stainless steel cylinder with a volume of l is filled with pure hydrogen sulfide under an overpressure of 1–30 kgf / cm3. The hydrogen sulfide cylinder is maintained for 72-120 hours, after which the hydrogen sulfide pressure in the balloon is reset to the partial pressure of hydrogen sulfide in the gas mixture with a given concentration of hydrogen sulfide and the balloon is filled with the second component of the binary gas mixture to obtain a high pressure. The resulting gas mixture with a given concentration of hydrogen sulfide is analyzed after filling the container after three days, month, two, four and six months after filling the container.

Example 1. Pre-dried and evacuated balloon

ate ate ate ate

50

OE

From stainless steel with a volume of 2 liters, they are filled with pure hydrogen sulfide at a typical pressure of 30 kgf / cm2. A cylinder of hydrogen sulfide is removed for 72 h, after which the pressure of hydrogen hydrogen in the cylinder drops to 25 kgf / cm2 and the cylinder is filled with nitrogen gas to a pressure of 80 kgf / cm2. The resulting gas mixture with a hydrogen concentration of about% is analyzed according to GOST after filling in three days, month, two, four, six months.

PRI mme R 2. A pre-dried and evacuated stainless steel cylinder with a volume of 40 liters is filled with pure hydrogen sulfide at a pressure of 10 kgf / cm2. The hydrogen sulfide cylinder is maintained for 96 hours, after which the hydrogen sulfide pressure in the balloon is dropped to 9.3 kgf / cm2 and the balloon is filled with air to a pressure of 79 kgf / cm2. The resulting gas mixture with a hydrogen sulfide concentration of 10.3 OBD is analyzed according to GOST after filling in three days, a month, two, four and six months.

Example The pre-dried and evacuated 8 l stainless steel cylinder is filled with pure hydrogen sulfide under an overpressure of 1 kgf / cm2. The hydrogen sulfide cylinder is maintained for 120 hours, after which the pressure in the balloon is dropped to 0.8 kgf / cm2 and the balloon is filled with helium to 60 kgf / cm2. The resulting gas mixture with a hydrogen sulfide concentration of 3.0 o6.% Is analyzed according to GOST after filling in i for three days, month, two, four and six months after filling the balloon.

An example. The pre-dried and evacuated 8 l stainless steel bottle is filled with pure hydrogen sulfide under an overpressure of 30 kgf / cm. The hydrogen sulfide cylinder is maintained for 60 hours, after which the pressure in the cylinder is dropped to 25 kgf / cm2 and the cylinder is filled with nitrogen to a pressure of 90 kgf / cm. The resulting gas mixture with a hydrogen sulfide concentration of 28.9 rD is analyzed according to GOST after filling in three days , month, two, four, six months.

five

0

five

0

five

0

five

0

five

PRI me R 5. A pre-dried and evacuated 10 l stainless steel cylinder is filled with pure hydrogen sulfide at a pressure of 1 kgf / cm2. The hydrogen sulfide cylinder is kept for hours, after which the pressure in the balloon is dropped to 0.5 kgf / cm2 and the cylinder is filled with nitrogen to a pressure of 70 kgf / cm. The resulting gas mixture with a concentration of hydrogen sulfide of 2.1 vol.% Is analyzed according to GOST after filling in three days, month, two, four and six months.

PRI me R 6. A pre-dried 10-vacuum stainless steel cylinder with a volume of 10 liters is filled with pure hydrogen sulfide at an excess pressure of 0.9 kgf / cm2. The hydrogen sulfide cylinder is kept for 72 hours, after which the pressure is dropped to 0.5 kgf / cm2 in the cylinder and the cylinder is filled with nitrogen to a pressure of 70 kgf / cm2.

The resulting gas mixture with a hydrogen sulfide concentration of 2.1 OBD is analyzed according to GOST after filling in three days, a month, two, four and six months.

PRI me R 7. A pre-dried and evacuated stainless steel cylinder with a volume of 10 liters is filled with pure hydrogen sulfide under an overpressure of 35 kgf / cm2, maintained for 72 hours, after which the pressure in the cylinder is dropped to 29 kgf / cm2 and filled The cylinder is filled with nitrogen up to a pressure of 90 kgf / cm2.

The resulting gas mixture with a hydrogen sulfide concentration of 33.3 OBD is analyzed according to GOST after filling in three days, a month, two, four and six months.

The table presents the results of the analysis of the hydrogen sulfide content in the gas mixture at different time intervals.

As can be seen from the table, hydrogen sulfide-containing gas mixtures have a stable composition during the initial filling of the balloon with hydrogen sulfide under a pressure of 1-30 kgf / cm2 and exposure of the balloon with hydrogen sulfide for 72-120 h (examples 1-3).

If the hydrogen sulphide is kept in a balloon of less than 70 hours or under a pressure of less than 1 kgf / cm2, the purpose of the invention is not achieved (examples k, 6), and

keeping more than 120 hours is not economically feasible (example 5), or under pressure

.30 kgf / cm2 is associated with the danger of this operation.

The initial filling of the balloon with hydrogen sulfide under a pressure of 1–30 kgf / cm2 was chosen to ensure that a protective film of the required thickness is created on its inner surface that prevents the metal of the balloon from the hydrogen sulfide from interacting with the stored mixture. Lower values of hydrogen sulfide pressure ensure the creation of a sulfide film for further storage of mixtures with a lower concentration of hydrogen sulfide, and greater pressure values for mixtures with large concentrations of hydrogen sulfide in the mixture.

The time interval for keeping the hydrogen sulfide cylinder from 72 to 120 hours was chosen in order to create a protective sulfide film of uniform structure and depends on the quality of the inner surface of the cylinder. A shorter holding time is used for cylinders with a better inner surface treatment, and a greater one for cylinders with a rougher surface. Besides,

The holding time of a hydrogen sulfide cylinder is inversely proportional to the pressure of hydrogen sulfide in the cylinder. 555593

ten

15

 ,

Claims (1)

Using the inventive method makes it possible to fill the stainless steel cylinder with hydrogen sulfide gas mixture under pressure and ensures the preservation of the stability of their composition during their subsequent long-term storage. The stability of the composition of hydrogen sulfide gas mixtures when stored in a cylinder under pressure allows them to be used for metrological calibration of gas analytical devices, which increases the accuracy and reliability of analytical work. Invention Formula The method of filling cylinders with a gas mixture under pressure, mainly hydrogen sulfide-containing, comprising feeding one of the components into the cylinders under its partial pressure and then filling the rest of the mixture components to obtain a high pressure, so as to increase the efficiency by increasing the stability of the composition of hydrogen sulfide-containing mixtures during storage, the cylinders 30 are filled with hydrogen sulfide under an overpressure of 1–30 kgf / cm2 and maintained for 72–120 h, after whereby the pressure is released to the partial pressure of the hydrogen sulfide in the mixture. 20 25