40 CFR 60.648 - Optional procedure for measuring hydrogen sulfide in acid gas

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§ 60.648 Optional procedure for measuring hydrogen sulfide in acid gas—Tutwiler Procedure. 1

Footnote(s):
1 Gas Engineers Handbook, Fuel Gas Engineering Practices, The Industrial Press, 93 Worth Street, New York, NY, 1966, First Edition, Second Printing, page 6/25 (Docket A-80-20-A, Entry II-I-67).

(a) When an instantaneous sample is desired and H2S concentration is ten grains per 1000 cubic foot or more, a 100 ml Tutwiler burette is used. For concentrations less than ten grains, a 500 ml Tutwiler burette and more dilute solutions are used. In principle, this method consists of titrating hydrogen sulfide in a gas sample directly with a standard solution of iodine.
(b) Apparatus. (See Figure 1.) A 100 or 500 ml capacity Tutwiler burette, with two-way glass stopcock at bottom and three-way stopcock at top which connect either with inlet tubulature or glass-stoppered cylinder, 10 ml capacity, graduated in 0.1 ml subdivision; rubber tubing connecting burette with leveling bottle.
(c) Reagents.
(1) Iodine stock solution, 0.1N. Weight 12.7 g iodine, and 20 to 25 g cp potassium iodide for each liter of solution. Dissolve KI in as little water as necessary; dissolve iodine in concentrated KI solution, make up to proper volume, and store in glass-stoppered brown glass bottle.
(2) Standard iodine solution, 1 ml=0.001771 g I. Transfer 33.7 ml of above 0.1N stock solution into a 250 ml volumetric flask; add water to mark and mix well. Then, for 100 ml sample of gas, 1 ml of standard iodine solution is equivalent to 100 grains H2S per cubic feet of gas.
(3) Starch solution. Rub into a thin paste about one teaspoonful of wheat starch with a little water; pour into about a pint of boiling water; stir; let cool and decant off clear solution. Make fresh solution every few days.
(d) Procedure. Fill leveling bulb with starch solution. Raise (L), open cock (G), open (F) to (A), and close (F) when solutions starts to run out of gas inlet. Close (G). Purge gas sampling line and connect with (A). Lower (L) and open (F) and (G). When liquid level is several ml past the 100 ml mark, close (G) and (F), and disconnect sampling tube. Open (G) and bring starch solution to 100 ml mark by raising (L); then close (G). Open (F) momentarily, to bring gas in burette to atmospheric pressure, and close (F). Open (G), bring liquid level down to 10 ml mark by lowering (L). Close (G), clamp rubber tubing near (E) and disconnect it from burette. Rinse graduated cylinder with a standard iodine solution (0.00171 g I per ml); fill cylinder and record reading. Introduce successive small amounts of iodine thru (F); shake well after each addition; continue until a faint permanent blue color is obtained. Record reading; subtract from previous reading, and call difference D.
(e) With every fresh stock of starch solution perform a blank test as follows: introduce fresh starch solution into burette up to 100 ml mark. Close (F) and (G). Lower (L) and open (G). When liquid level reaches the 10 ml mark, close (G). With air in burette, titrate as during a test and up to same end point. Call ml of iodine used C. Then,
Grains H2S per 100 cubic foot of gas=100 (D—C)
(f) Greater sensitivity can be attained if a 500 ml capacity Tutwiler burette is used with a more dilute (0.001N) iodine solution. Concentrations less than 1.0 grains per 100 cubic foot can be determined in this way. Usually, the starch-iodine end point is much less distinct, and a blank determination of end point, with H2S-free gas or air, is required.
Figure 1. Tutwiler burette (lettered items mentioned in text)

Title 40 published on 2013-07-01

The following are only the Rules published in the Federal Register after the published date of Title 40.

For a complete list of all Rules, Proposed Rules, and Notices view the Rulemaking tab.

  • 2014-05-16; vol. 79 # 95 - Friday, May 16, 2014
    1. 79 FR 28439 - Quality Assurance Requirements for Continuous Opacity Monitoring Systems at Stationary Sources
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      ENVIRONMENTAL PROTECTION AGENCY
      Final rule.
      This final rule is effective on November 12, 2014.
      40 CFR Part 60

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U.S. Code: Title 42 - THE PUBLIC HEALTH AND WELFARE

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Title 40 published on 2013-07-01

The following are ALL rules, proposed rules, and notices (chronologically) published in the Federal Register relating to 40 CFR 60 after this date.

  • 2014-07-17; vol. 79 # 137 - Thursday, July 17, 2014
    1. 79 FR 41752 - Oil and Natural Gas Sector: Reconsideration of Additional Provisions of New Source Performance Standards
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      Proposed rule; Notice of Public Hearing.
      Comments. Comments must be received on or before August 18, 2014, unless a public hearing is requested by July 22, 2014. If a hearing is requested on this proposed rule, written comments must be received by September 2, 2014. Public Hearing. If anyone contacts the EPA requesting a public hearing by July 22, 2014 we will hold a public hearing on August 1, 2014. If a public hearing is requested by July 22, 2014, it will be held on August 1, 2014 at the EPA's Research Triangle Park Campus, 109 T.W. Alexander Drive, Research Triangle Park, NC 27711. The hearing will convene at 10:00 a.m. (Eastern Standard Time) and end at 5:00 p.m. (Eastern Standard Time). A lunch break will be held from 12:00 p.m. (Eastern Standard Time) until 1:00 p.m. (Eastern Standard Time). Please contact Virginia Hunt at (919) 541-0832, or at hunt.virginia@epa.gov to request a hearing, to determine if a hearing will be held and to register to speak at the hearing, if one is held. If a hearing is requested, the last day to pre-register in advance to speak at the hearing will be July 30, 2014. Additionally, requests to speak will be taken the day of the hearing at the hearing registration desk, although preferences on speaking times may not be able to be fulfilled. If you require the service of a translator or special accommodations such as audio description, please let us know at the time of registration. If no one contacts the EPA requesting a public hearing to be held concerning this proposed rule by July 22, 2014, a public hearing will not take place. If a hearing is held, it will provide interested parties the opportunity to present data, views or arguments concerning the proposed action. The EPA will make every effort to accommodate all speakers who arrive and register. Because these hearings are being held at U.S. government facilities, individuals planning to attend the hearing should be prepared to show valid picture identification (e.g., driver's license or government-issued ID) to the security staff in order to gain access to the meeting room. Please note that the REAL ID Act, passed by Congress in 2005, established new requirements for entering federal facilities. These requirements will take effect July 21, 2014. If your driver's license is issued by Alaska, American Samoa, Arizona, Kentucky, Louisiana, Maine, Massachusetts, Minnesota, Montana, New York, Oklahoma or Washington State, you must present an additional form of identification to enter the federal buildings where the public hearings will be held. Acceptable alternative forms of identification include: Federal employee badges, passports, enhanced driver's licenses and military identification cards. In addition, you will need to obtain a property pass for any personal belongings you bring with you. Upon leaving the building, you will be required to return this property pass to the security desk. No large signs will be allowed in the building, cameras may only be used outside of the building and demonstrations will not be allowed on federal property for security reasons. The EPA may ask clarifying questions during the oral presentations, but will not respond to the presentations at that time. Written statements and supporting information submitted during the comment period will be considered with the same weight as oral comments and supporting information presented at the public hearing. If a hearing is held on August 1, 2014, written comments on the proposed rule must be postmarked by September 2, 2014. Commenters should notify Ms. Hunt if they will need specific equipment, or if there are other special needs related to providing comments at the hearing. The EPA will provide equipment for commenters to show overhead slides or make computerized slide presentations if we receive special requests in advance. Oral testimony will be limited to 5 minutes for each commenter. Verbatim transcripts of the hearings and written statements will be included in the docket for the rulemaking. The EPA will make every effort to follow the schedule as closely as possible on the day of the hearing; however, please plan for the hearing to run either ahead of schedule or behind schedule. Information regarding the hearing (including information as to whether or not one will be held) will be available at: http://www.epa.gov/airquality/oilandgas/actions.html. Again, all requests for a public hearing to be held must be received by July 22, 2014.
      40 CFR Part 60