Kit and method for testing liquids for hydrogen sulfide content

• US 4,174,202 A
• Filed: 11/28/1977
• Issued: 11/13/1979
• Est. Priority Date: 11/28/1977
• Status: Expired due to Term

• Current Assignee: Dowell Schlumberger Incorporated (Schlumberger NV)
• Original Assignee: The Dow Chemical Company (Dow, Inc.)
• Inventors: Simpson, Benny E.
• Primary Examiner(s): Scovronek, Joseph
• Assistant Examiner(s): Turk, Arnold
• Application Number:
  US05/855,540
• Time in Patent Office: 715 Days
• Field of Search: 23/230 R, 23/253 TP, 23/254 R, 23/232 R, 23/253 R, 23/259
• US Class Current: 436/121
• CPC Class Codes: G01N 31/02 using precipitation measuring deposition or liberation of materials from an electrolyte G01N27/42
• CPC Class Codes: G01N 31/224 for investigating presence of dangerous gases
• CPC Class Codes: Y10T 436/184 Only hydrogen sulfide

Abstract

A method for quickly determining whether or not the H₂ S concentration in fluids exceeds a preselected level, such as that set by government standards for oil field fluids, comprises: (1) admixing a preselected quantity of a liquid to be tested with a quantity of metal ion (such as Cd⁺⁺) capable of reacting with sulfide ion to form a precipitate, the quantity of metal ion being equal to that required to precipitate a preselected amount of sulfide ion; (2) purging any residual H₂ S from the liquid (such as by generating CO₂ in situ); (3) contacting a reagent colorimetrically and selectively responsive to the presence of H₂ S (such as lead acetate) with gas purged from the liquid; and (4) observing the color of colorimetrically responsive reagent.

A kit convenient for use in carrying out the method in the field comprises: a capped bottle containing a premeasured quantity of a reagent reactable with hydrogen sulfide to form a precipitate; a second cap for the bottle, the second cap having mounted on at least a portion of its inner face a water-absorbent paper or fabric which serves as the substrate for the colorimetrically responsive reagent; an effervescent alkali metal bicarbonate tablet which is chargeable to the bottle; a second bottle containing the colorimetrically reactive reagent, said reagent bottle being normally closed, and means for transferring a portion of the colorimetrically responsive reagent to the water-absorbent substrate on the second cap.

Claims

1. A method for qualitatively determining whether or not a liquid contains hydrogen sulfide in a concentration in excess of a preselected concentration, which comprises, in sequence:

(a) admixing a preselected quantity of the liquid to be tested with a quantity of a metal cation capable of reacting with sulfide ion to form a precipitate, which quantity of cation is stoichiometrically sufficient to react with the hydrogen sulfide which would be present in said preselected quantity of liquid if said hydrogen sulfide were initially present at said preselected concentration;

(b) purging the liquid with an inert gas to remove unreacted hydrogen sulfide from the liquid;

(c) contacting a reagent colorimetrically and selectively responsive to the presence of hydrogen sulfide with the gas purged from the liquid;

(d) observing the color of the colorimetrically responsive agent, a color change in response to hydrogen sulfide being indicative that the liquid tested contained hydrogen sulfide at a concentration in excess of said preselected concentration.

2. The method of claim 1 wherein said purging step includes generating said inert gas in situ.

3. The method of claim 1 wherein said colorimetrically responsive reagent is supported on a water-absorbent substrate.

4. The method of claim 1 wherein the colorimetric reagent contains Pb.sup.(II), Cu.sup.(II) or Hg.sup.(II).

5. The method of claim 4 wherein the colorimetric reagent is an aqueous solution of lead acetate.

6. The method of claim 1 wherein said inert gas is carbon dioxide.

7. The method of claim 6 wherein said carbon dioxide is generated in situ.

8. The method of claim 7 wherein said carbon dioxide is generated in situ by reacting at least one alkali metal bicarbonate with water in the reaction medium.

9. The method of claim 1 wherein the precipitate-forming cation is Cd.sup.(II), Zn.sup.(II), Cu.sup.(II), Fe.sup.(II), Hg.sup.(II), Ni.sup.(II), Pb.sup.(II), or Sn.sup.(II).

10. The method of claim 9 wherein the precipitate-forming cation is Cd.sup.(II).

11. The method of claim 10 wherein the Cd.sup.(II) is present as cadmium sulfate in an aqueous solution of sulfuric acid having a pH between about 3 and 7.

12. The method of claim 10 wherein the colorimetric reagent is lead acetate.

13. The method of claim 12 wherein the Cd.sup.(II) is present as cadmium sulfate in an aqueous solution of sulfuric acid having a pH between about 3 and 7, and wherein the inert gas is generated in situ by adding at least one alkali metal bicarbonate to the reaction medium.

14. The method of claim 13 which comprises:

(a) adding the preselected volume of said liquid to be tested to a reaction vial having an opening adapted to be sealably closed by a lid and containing the cadmium sulfate solution;

(b) closing the reaction vial and agitating its contents for a period of time sufficient to permit said cadmium to react with hydrogen sulfide which may be contained in said liquid;

(c) in rapid succession, opening the vial, adding an alkali metal bicarbonate effervescent tablet to the vial, and reclosing the vial with a lid having mounted on its inner face, an absorbent paper or fabric moistened with an aqueous solution of lead acetate so that gas evolved from said liquid may contact said lead acetate treated paper;

(d) upon cessation of effervescence, observing said paper for the appearance or absence of a dark brown or black color.

15. A test kit for qualitatively analyzing a sample of liquid to determine whether said liquid contains hydrogen sulfide in excess of a preselected concentration, which comprises:

(a) at least one reaction vial having an opening sealably closeable by a lid means and containing means for removing a quantity of hydrogen sulfide from a sample of liquid, said removal means comprising a preselected stoichiometric quantity of reagent in aqueous solution said reagent being reactable with said preselected concentration of hydrogen sulfide to form a precipitate;

(b) at least one first lid means sealably but removably closing said vial opening;

(c) at least one second lid means adaptable for sealably but removably closing said vial opening upon removal of said first lid means, said second lid having an inner face in fluid communication with the interior of said vial when said lid sealably closes the vial, and, mounted on at least a portion of said inner face, a water-absorbent paper or fabric adapted to support an indicating means;

(d) at least one means for generating an inert gas, comprising an effervescent alkali metal bicarbonate tablet chargeable to said reaction vial via said opening upon removal of said first lid means;

(e) a reservoir vial having an opening and containing means for indicating the presence of hydrogen sulfide, said indicating means comprising an aqueous solution of a reagent colorimetrically and selectively reactive with hydrogen sulfide, said opening being normally closed by means for closing said opening; and

(f) means for transferring a portion of said indicating means from said reservoir vial to said water-absorbent paper or fabric.

16. The kit of claim 15 wherein the reaction vial has at least one calibration to indicate a preselected volume within said vial.

17. The kit of claim 16 wherein said means for removing is an aqueous solution of cadmium sulfate having a pH between pH 3 and 7, said indicating means is an aqueous solution of lead acetate, and said means for closing and transferring is an eyedropper adapted to sealably close said reservoir vial.