# US 10,119,948 B2 · Sulfur solubility in gas measurement system

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- Number: US 10,119,948 B2
- Document ID: US10119948B2
- Status: Granted
- Kind: B2
- Application number: 14/989,660
- Filed: 2016-01-06
- Published: 2017-07-06
- Granted: 2018-11-06
- Earliest claimed: 2016-01-06
- Assignees: Saudi Arabian Oil Company
- Applicants: Saudi Arabian Oil Company
- Inventors: Abdelmounam Sherik; Abderrazak Traidia; AbdulJalil Rasheed; Arnold Lewis
- Web page: https://patentgrep.com/patent/US10119948B2

## CPC

- G01N 33/0036: {specially adapted to detect a particular component (physical analysis of gaseous biological material G01N33/497)}
- C10L 3/103: {Sulfur containing contaminants}
- G01G 19/00: Weighing apparatus or methods adapted for special purposes not provided for in the preceding groups {(electric measuring arrangements involving comparison with a reference value G01R17/00)}
- G01N 33/225: {Gaseous fuels, e.g. natural gas}
- G01N 25/14: by using distillation, extraction, sublimation, condensation, freezing, or crystallisation (G01N25/02 takes precedence)
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- C10L: FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
- G01G: WEIGHING (sorting by weighing B07C5/16)

## Abstract

This present disclosure is directed to a method and apparatus for collecting small amounts, sub mg levels, of elemental sulfur (or other trace elements such as mercury) deposited from the ppm levels of elemental sulfur (or other trace elements such as mercury) contained in gases found in typical oil production environments or gas streams with anticipated sulfur deposition problems, as well as in industries other than oil and gas. An analytical chemistry technique for determining the amount of sulfur collected is used and from this result, the solubility of sulfur in a gas at a fixed temperature, pressure and gas composition can be calculated.

## Claims

### Claim 1

A method for measuring the sulfur solubility of a test gas at a test temperature and test pressure in a laboratory apparatus, comprising:
saturating the test gas with water;
flowing the test gas into a first conduit, wherein the first conduit is packed with elemental sulfur, and is maintained at least at a first temperature that is sufficient to result in the uptake of elemental sulfur by the test gas in excess of the natural equilibrium solubility level of elemental sulfur in the test gas at the test temperature;
introducing the test gas containing elemental sulfur into a second conduit, the second conduit being in fluid communication with the first conduit and maintained at least at a second temperature sufficient to lower the temperature of the test gas to a temperature that is equal to the test temperature, whereby the amount of elemental sulfur in the test gas is reduced to its natural equilibrium solubility level in the test gas at the test temperature;
flowing the test gas into a third conduit that is in fluid communication with the second conduit, wherein at least a portion of the third conduit is maintained at a third temperature sufficient to result in deposition of the elemental sulfur from the test gas into a portion of the third conduit; and
calculating the sulfur solubility of the test gas based on the amount of elemental sulfur deposited in the third conduit.

### Claim 2 (depends on 1)

The method of claim 1, wherein the test gas comprises CH4.

### Claim 3 (depends on 2)

The method of claim 2, wherein the test gas further comprises CO2 and H2S.

### Claim 4 (depends on 1)

The method of claim 1, wherein the step of calculating the sulfur solubility comprises:
weighing the sulfur deposited in the third conduit for a select run time; and
measuring the volume of the test gas that passes through the third conduit during the select run time.

### Claim 5 (depends on 1)

The method of claim 1, wherein the third conduit comprises a U-shaped tube.

### Claim 6 (depends on 1)

The method of claim 1, wherein the first temperature is a maximum of 95° C.

### Claim 7 (depends on 1)

The method of claim 1, wherein the test temperature is 10-15° C. lower than the first temperature.

### Claim 8 (depends on 1)

The method of claim 1, wherein the third temperature is 0° C.

### Claim 9 (depends on 1)

The method of claim 1, wherein the laboratory apparatus is free of direct contact with gas-handling equipment that contains the test gas.

### Claim 10

A system for measuring the sulfur solubility of a test gas at a test temperature, comprising:
a source of the test gas;
a first station in fluid communication with the source of test gas, the first station comprising a first conduit packed with elemental sulfur, wherein the first conduit is maintained at conditions sufficient to result in the uptake of elemental sulfur by the test gas as the test gas flows through the first conduit, the uptake of elemental sulfur being in excess of the natural equilibrium solubility level of the elemental sulfur in the test gas at the test temperature;
a second station comprising a second conduit in fluid communication with the first conduit, wherein the second conduit is maintained at conditions sufficient to lower the temperature of the test gas to the test temperature, whereby the amount of elemental sulfur in the test gas is reduced to its natural equilibrium solubility level in the test gas at the test temperature; and
a third station comprising a third conduit in fluid communication with the second conduit, wherein the third conduit is maintained at conditions that cause deposition of the elemental sulfur from the test gas, the third conduit being configured such that the deposited elemental sulfur can be collected and weighed to calculate the sulfur solubility of the test gas based on a measured flow rate of the test gas through the system; and
a fourth conduit in fluid communication with the source of test gas and upstream of the first conduit, wherein the conditions of the fourth conduit are sufficient to saturate the test gas with water as the test gas flows through the fourth conduit prior to entering the first station.

### Claim 11 (depends on 10)

The system of claim 10, wherein the system is a continuous flow loop system.

### Claim 12 (depends on 10)

The system of claim 10, wherein the first station includes a first medium for elevating a temperature of the test gas flowing through the first conduit; the second station includes a second medium for decreasing the temperature of the test gas to the test temperature and the third station includes a third medium for quenching the sulfur-saturated test gas by decreasing the temperature thereof.

### Claim 13 (depends on 12)

The system of claim 12, wherein the first, second, and third mediums comprise water contained within respective first, second and third baths, the first, second and third conduits being surrounded by the first, second and third mediums, respectively.

### Claim 14 (depends on 10)

The system of claim 10, wherein the fourth conduit is located within the second station.

### Claim 15 (depends on 10)

The system of claim 10, wherein the first conduit comprises a plurality of first tubes arranged in series and contained within a first medium that is heated to elevate the temperature of the test gas.

### Claim 16 (depends on 15)

The system of claim 15, wherein the plurality of first tubes are configured in a serpentine arrangement.

### Claim 17 (depends on 10)

The system of claim 10, wherein the second conduit comprises a plurality of second tubes arranged in series and contained within a second medium that is cooled to decrease the temperature of the test gas to the test temperature.

### Claim 18 (depends on 17)

The system of claim 17, wherein the plurality of second tubes are configured in a serpentine arrangement.

### Claim 19 (depends on 10)

The system of claim 10, wherein the third conduit comprises an inflow section for maintaining the test gas at the test temperature, a trap section for collecting the deposited sulfur, and an outflow section downstream of the trap section for carrying the test gas from the third station, wherein the inflow section and the outflow section are elevated above the trap section.

### Claim 20 (depends on 19)

The system of claim 19, wherein the trap section comprises a U-shaped tube.

### Claim 21 (depends on 10)

The system of claim 10, further including a flow meter for calculating a flow rate of the test gas through the system, thereby allowing a total volume of test gas to be calculated for a given experimental run.

### Claim 22 (depends on 10)

The system of claim 10, further including a pressure regulator for maintaining a pressure of the test gas within a prescribed range as the test gas flows through each of the first, second and third stations.

### Claim 23 (depends on 10)

The system of claim 10, further including a temperature controller for monitoring the temperature of the test gas and adjusting the temperature of the test gas.

### Claim 24 (depends on 10)

The system of claim 10, wherein the source of test gas comprises a tank of sour gas collected from a gas field of interest.
