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United States Patent [19] [11] Patent Number: 5,683,914 Miller Et A]

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United States Patent [19] [11] Patent Number: 5,683,914 Miller Et A] US0056839 14A United States Patent [19] [11] Patent Number: 5,683,914 Miller et a]. [45] Date of Patent: Nov. 4, 1997 [54] METHOD FOR CHLORIDE ION REMOVAL 5,439,593 8/1995 Pn'ce ..................................... .. 210/660 PRIOR TO CHEMICAL OXYGEN DEMAND ANALYSIS FOREIGN PATENT DOCUMENTS 45320 2/1982 [75] Inventors: Donald G. Miller. Slater; Scott V. 3529670 211987 Brayton. Ames. both of Iowa 4125627 2/1993 54-31792. 3/1979 [73] Assignee: Hach Company. Ames, Iowa 55-2959 1! 1980 58-161895 9/1983 58-205899 1 l/l 983 [21] Appl. No.: 533,251 59-179187 10/1984 [221 Filed: Sep. 25, 1995 60-18098 10/1985 60-219598 l 1/1985 Japan . [5 1] Int. Cl.° ............................. .. GtIlN 1/00; G01N 1/28; GOIN 1134 UI'HER PUBLICATIONS [52] US. Cl. ........................ .. 436/175; 210/266; 210/282; F.P. Treadwell ct al. ed. “Analy?cal Chemistry” 1930, John 422/79; 436/62; 436/145; 436/146; 436/166; Wiley & Sons. Inc.: New York. pp. 222-227. 433/177; 433/183 W. Rigby J. Chem. Soc. 1950. 1907-1913. [53] Field of Search ...................... .. 422/101, 79; 436/62. V.S. Rogov et al. Razved. Okhr: Neda 1984, 58-59. 436/145, 146, 166, 175, 177, 178. 183; M. Namiki et a1. Fresenius J. Anal. Chem. 1992, 344. 210/266, 282, 283 265-268. Begemann et al., “Bi4O-,. Das Erste De?nierte Biniire Bis [56] References Cited mnt(IlI,V)-OXID", Jul. 1989. pp. 123-127. U.S. PATENT DOCUMENTS M.H. Ford-Smith et :11, Kinetics of Oxidation-Reduction Reactions Between Elements of Groups V and VII. Part I. 956,332 4/1910 Fuller 210/474 Bismuth(v) with Halide Ions and Other Reductants. 1973, 3,337,451 8/1967 Calmon ...... .. 210/683 pp. 461-464, J.C.S. Dalton. 3,346,617 10/1967 Hiroki et a1. 260/4653 Habib Firouzabadi et :11, Zinc Bismuthate Zn(BiO3)2. I. A 3,387,038 6/1968 Koch . .. 260/604 3,608,736 9/1971 Wong 210/477 Useful oxidizing Agent for the E?icient Oxidation of 3,763,879 10/1973 Jaworek 210/266 X Organic Compounds, Apr, 1992, pp. 1131-1134. The 3,787,334 1/1974 Yamada . .. 252/468 Chemical Society of Japan. 4,131526 12/1978 Moeglich .. 204/149 Membrane Filuation—Chromat0graphy Catalog, Amicon, 4,234,317 11/1980 Lucas et al 4221101 X Inc., Publication No. 387, 1995 Amicon. Inc. 4,241,216 12/1980 Bergman et a] 560/99 V. S. Rogov et a1. Chem. Abstr. 1984, 100. 167338m. 4,447,405 5/1984 Ahn et a1 423/88 4,485,015 11/1984 Smith ...... .. 210/455 Primary Examiner—Arlen Soderquist 4,787,971 11/1988 Donald 42%101 X Attorney Agent, or Firm-Zarlcy, McKee. Thomte, 4,832,842 5/1989 Limb .. 210/249 Voorhees. & Sease 4,859,336 8/1989 Savas et a]. .. 210/416.1 4,956,298 9/1990 Diekmann . 4221101 X [57] ABSTRACT 5,055,409 1011991 Astr?m .. 436/52 5,076,922 12/1991 Deane ...... .. 2101282 A method of pretreating aqueous chemical oxygen demand 5,104.529 4/1992 Becker .. 210/195.1 (COD) samples to remove the risk of potential chloride ion 5,167,819 12/1992 Iana et a1 .... .. 2101474 interference. The method comprises acidifying an aqueous 5,186,830 2/1993 Rait 210/232 COD test sample, and thereafter passing the acidi?ed sample 5,219,529 6/1993 Ngo et al 422/102 5,264,184 11/1993 Aysta et a1 . 422/101 through a source of pentavalent bismuth (Bi5+) such as 5,304,305 4/1994 Lehrer ............. .. 210/346 sodium bismuthate. 5,368,729 11/1994 Ste?zovich et al 210/266 5,411,661 5/1995 Heiligman ............................. .. 210/264 12 Claims, 1 Drawing Sheet 5,683,914 1 2 METHOD FOR CHLORIDE ION REMOVAL the dichromate which will give false high COD readings. PRIOR TO CHEMICAL OXYGEN DEMAND The end products of organic oxidations are carbon dioxide ANALYSIS and water. After the oxidation step is completed, the amount of dichromate consumed is determined either titrimetrically or FIELD OF THE INVENTION colorimetrically. Either the amount of dichromate reduced The ?eld of the present invention relates to tests for (Chromium III) or the amount of unreacted dichromate determination of Chemical Oxygen Demand (COD) in aque (Chromium VI) remaining can be measured. If the latter ous samples. More particularly, it relates to a method of method and colorimetry are chosen, the analyst must know removal of chloride ion from COD test samples, so that the the precise amount of dichromate added and be able to set chloride ion does not cause an erroneous high sample the instrument wavelength very accurately, since readings reading. are routinely taken on the “shoulder” of the Chromium VI absorbance peak. Wavelength settings must be reproduced BACKGROUND OF THE INVENTION precisely in order to avoid errors when using a previously IS generated calibration curve. Oxygen demand is an important parameter for determin Dichromate was ?rst used in the COD test over 50 years ing the effect of organic pollutants on receiving water. As ago. Before that time, potassium permanganate was the microorganisms in the environment consume these oxidant of choice. Analysts have tried many other reagents, matm'ials, oxygen is depleted from the water. This can have such as potassium persulfate, cerium sulfate, potassium an adverse e?’ect on ?sh and plant life. iodate and oxygen itself. Generally these other oxidants There are three main methods of measuring oxygen have not been satisfactory. demands: directly, by biochemical oxygen demand (BOD) A prior case of this same inventor, U.S. Ser. No. 08/475. and/or chemical oxygen demand (COD), and indirectly by 187, ?led Jun. 7, 1995, now U.S. Pat. No. 5,556,787, and total organic carbon (TOC) procedures. BOD, because it entitled “Manganese 111 Method For Chemical Oxygen uses microorganisms for oxidation, gives the closest picture 25 Demand Analysis”, relates to a new COD test that eliminates of the biological processes occun'ing in a stream. However, the use of dichromate in sulfuric acid and replaces it with results are not available for five days, and the BOD test is another COD test reagent containing Mn+3 ions and of inadequate as an indicator of organic pollution when used improved performance. The subject matter of that applica with industrial waste water containing toxic materials which tion is incorporated herein by reference. poison the microorganisms and render them unable to oxi 30 As mentioned previously, the current state of the art dize wastes. involves the addition of mercuric compounds added to Unlike BOD. the two other methods do not use biological reduce interference from the oxidation of chloride ions by processes, and are therefore faster and not affected by toxic the dichromate. The addition of mercuric salts, while satis materials. A strong oxidizing agent or combustion technique factory to eliminate interference from chloride ion in aque is used under controlled conditions in the TOC method to 35 ous COD samples, is itself unsatisfactory because mercury measure the total amount of organic material in a sample. is a pollutant and known toxicant. which makes it undesir The results obtained may not be as accurate as the results able for use in COD analysis. Mercury has its own polluting reached through the COD or BOD method in predicting and environmental risks. There is, therefore, a present and environmental oxygen demand because oxygen demands continuing need for the development of a means of remov may di?’er between compounds with the same number of ing potentially interfering chloride ions from aqueous COD organic carbons in their structures. The difference in oxygen samples which avoids use of mercury salts, and which does demand between two compounds containing the same not in any way interfere with the accuracy of the COD amount of organic carbon can be seen in the following analytical procedure. This invention has as its primary equations showing the oxidation of oxalic acid and ethanol: objective the ful?llment of this need. 45 An additional objective is to provide a carnidge device which can be provided in a kit for chemical COD analysis that can be conveniently used by operators to conduct a pretreatment chloride removal step prior to analysis of an Each molecule of ethanol uses up six times as much aqueous COD sample. oxygen as an equivalent amount of oxalic acid, and thus The method and means of accomplishing each of the would have a much greater elfect on the dissolved oxygen above objectives will become apparent from the detailed present in a receiving water. Estimating environmental oxy description of the invention which follows. gen demand (as with BOD and COD) requires complete oxidation of carbon and hydrogen present in the organic BRIEF DESCRIPTION OF THE DRAWINGS matter. Thus, while TOC is a more direct expression of total 55 FIG. 1 is a perspective and exploded view of the cartridge organic content than BOD or COD, it does not provide the of the present invention with the inner and outer sections same kind of information. An empirical relationship can aligned for mating relationship. exist between TOC, BOD and COD, but the speci?c rela FIG. 2 shows the inner and outer sections in mating tionship must be established for a speci?c set of sample relationship. conditions. FIG. 3 shows in cross section a complete cartridge unit Currently, the COD test has a fairly speci?c and universal inserted in a test tube. meaning: the oxygen equivalent of the amount of organic FIG. 4 shows a bottom view of the inner cartridge.
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