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(12) United States Patent (10) Patent No.: US 6,358,747 B1 Condit Et Al

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(12) United States Patent (10) Patent No.: US 6,358,747 B1 Condit Et Al USOO6358747B1 (12) United States Patent (10) Patent No.: US 6,358,747 B1 Condit et al. (45) Date of Patent: Mar. 19, 2002 (54) METHOD AND APPARATUS FOR D. S. Gaibakyan etal, J. Anal. Chem. 1970, 25, 2056–2059.* QUANTIFYING MOLYBDATE IN BRINES A. M. Kiememeljet al, Anal. Chem. 1976, 48,575-578.* (75) Inventors: David A. Condit, Avon; Mark R. H. Llambias et al, Chem. Abstr. 1978, 88, abstract 53021f.* Jaworowski, Glastonbury; Xia Tang, West Hartford, all of CT (US) Lis et al., Journal of Alloys and Compounds 303-304, 132-136, 2000.* (73) ASSignee: sayier Corporation, Farmington, CT Water Analysis Handbood, HACH Company, Loveland, Colorado, “Molybdenum, Molybdate', pp. 636. (*) Notice: Subject to any disclaimer, the term of this patent is extended or adjusted under 35 * cited by examiner U.S.C. 154(b) by 0 days. (21) Appl. No.: 09/324,376 Primary Examiner Arlen Soderquist y - - - 9 (22) Filed: Jun. 2, 1999 (57) ABSTRACT (51) Int. Cl. ................................................ G01N 33/20 Amethod and apparatus are provided for quantifying molyb (52) U.S. Cl. ............................. 436/83; 422/61; 436/73; date corrosion inhibitor concentrations in lithium halide 436/166 brines of absorption refrigeration Systems. This permits (58) Field of Search ............................ 436/73, 83, 166; monitoring and control of the inhibitor level. A reagent is 422/61 chosen for reacting with the molybdate in the brine to provide a readily identifiable characteristic color, the inten (56) References Cited sity of which is a function and measure of the molybdate U.S. PATENT DOCUMENTS concentration. The reagent is an acidified reducing agent a which reacts to provide a significant characteristic color 5,106,581. A 4/1992 Jaunakais et al. ............, 422/56 capable of optical detection without interference. In a 5,547,600 A : 8/1996 Downey ...................... 252/68 lithium bromide brine, the molybdate concentration is con E. A : B.E. SE et al... "... veniently identified by reaction with stannous chloride SnCl in hydrochloric acid Hel (aq). The resulting color corre FOREIGN PATENT DOCUMENTS sponds to a wavelength of about 550-560 nm (pink), and the JP 8-105.835 * 4/1996 intensity is a function of molybdate concentration. Portable measuring equipment, Such as a hand held OTHER PUBLICATIONS Spectrophotometer, or colorimeter, provide a convenient N. Gandolfo GazZ. Chim. Ital. 1945, 75, 62–70.* means for making on-site measurements. I. Barshad Anal. Chem. 1949, 21, 1148–1150.* T. D. Rees et al, Talanta 1968, 15, 1312-1314.* 5 Claims, 3 Drawing Sheets 0.6 O. 4 - o: O 50 150 2OO 2MoC4 CONCENTRATION (PPM) U.S. Patent Mar. 19, 2002 Sheet 1 of 3 US 6,358,747 B1 S s a-N voo 3 3 ONW8OSSW S U.S. Patent Mar. 19, 2002 Sheet 3 of 3 US 6,358,747 B1 / US 6,358,747 B1 1 2 METHOD AND APPARATUS FOR Carrier Corporation, which patent is incorporated herein by QUANTIFYING MOLYBDATE IN reference. Moreover, this improved System of corrosion ABSORPTION REFRGERATION SYSTEM inhibitors is employed in the WB-1 inhibited Li Brabsorp BRINES tion chillers manufactured and Sold by Carrier Corporation. The aforementioned WB-1 inhibited Li Br absorption TECHNICAL FIELD chiller of the Carrier Corporation uses an aqueous Solution This invention relates generally to absorption refrigera of water and a lithium halide, specifically lithium bromide tion Systems. More particularly, the invention relates to (Li Br), as the working fluid (sometimes termed “brine”), and diagnostics for absorption refrigeration Systems. More par employ a further solution of lithium molybdate (LiMoO), ticularly Still, the invention relates to a method and apparatus lithium borate and lithium silicate as the corrosion inhibitor. for performing diagnostics on a corrosion inhibitor present Although the lithium borate and lithium silicate inhibitors in absorption refrigeration Systems. remain in Solution in the aqueous working fluid in adequate quantities throughout the life of the fluid System, the same BACKGROUND may not be so with respect to the molybdate inhibitor. The There are a number of different pairs of refrigerants and 15 lithium molybdate is only sparingly soluble in the LiBr absorbents that are used in absorption refrigeration Systems. brine, and must be maintained in the 100-200 ppm range to One Such pair is water and a halogen Salt of lithium, Such as assure the desired action as a corrosion inhibitor. However, lithium bromide, lithium chloride or lithium iodide mixed to during Start-up and/or during other times of StreSS on the form a concentrated aqueous Solution of the lithium salt. refrigeration System, the molybdate inhibitor may become Another Such pair is water and ammonia. sufficiently depleted as to take it below the preferred con Iron and iron alloys like Steel and copper and copper centration range and thus expose the System to corrosion alloys are typical construction materials used in absorption problems. refrigeration Systems. Corrosion of these materials can cause To minimize the risk of corrosion problems which may difficulties. Not only is metal loss of concern but also the 25 result from an insufficient concentration of the molybdate oxidation of ferrous metal can be accompanied by evolution inhibitor, it has been the practice to obtain Samples of the of gaseous hydrogen. If not purged, the hydrogen can LiBr brine in the field at the site of the absorption refrig interfere with the proper operation of the System. Corrosion eration System and to then Send them to another location for is of particular concern in Systems that use halogen Salts of analysis. That analysis is typically performed by a non lithium. And regardless of the refrigerant/absorbent pair portable, relatively expensive technique and equipment, used in a particular System, metal corrosion rates increase as Such as inductively coupled plasma-atomic emission Spec System temperatures increase. troscopy (ICP-AES). This process occasions undesirable delays (measured in days) and Significant monetary costs. It is well known in the prior art that the addition of a salt Although various types of on-site analyzers and analysis of chromium, Such as lithium chromate, to the refrigerant/ techniques have been employed for monitoring the level of absorbent Solution in an absorption refrigeration System, is 35 chromate inhibitor concentrations, including color compara effective in reducing metallic corrosion. The presence of the tors and spectrometers, those techniques as they presently chromate compound promotes the formation of a protective exist are not Suitable for determining molybdate concentra layer of iron and chromium oxides on the Surfaces of the tions. Similarly, existing analytical processes for determin system that are in contact with the absorbent. With a ing concentrations of molybdate in refrigeration Systems are decrease in iron oxidation, there is also a corresponding 40 decrease in the production of noncondensible hydrogen. operative if the working fluid is water, but not if it contains There is Some concern, however, about the health risks that a lithium halide brine, Such as lithium bromide. chromium presents. At least one government authority, the Accordingly, there is a need for determining molybdate U.S. Environmental Protection Agency, has identified chro inhibitor concentrations in lithium halide brines using a mium as a carcinogen, and has prohibited the presence of 45 method and/or apparatus which facilitates on-site analysis. chromium compounds in Systems that are open to the The method and apparatus for making Such on-site analysis atmosphere. Absorption refrigeration Systems are, of course, should be relatively portable and economical, and provide closed Systems, but a certain amount of working fluid from rapid and accurate determination of molybdate inhibitor the System can become exposed to the atmosphere through concentration. the taking of Samples, the manufacturing process and Spills 50 during handling and filling. And, at the end of the Service life SUMMARY OF THE INVENTION of a System, the System charge will necessarily require The present invention provides a method and apparatus disposal of the working fluid, including the chromium for making a rapid and accurate analysis of the concentration compounds that it contains. of molybdate inhibitor in a lithium halide brine at the site of To address the foregoing concern, there has recently been 55 a refrigeration System containing the brine. The analysis developed a chromium-free aqueous Solution, typically of a may be performed using relatively Standard, portable equip halogen Salt of lithium, for use as a working fluid in an ment in a non-complex manner. absorption refrigeration System. In addition, the Solution According to the invention, there is provided a method also contains a compound containing a molybdate, a com and apparatus for quantitatively analyzing molybdate inhibi pound containing a borate and perhaps also, a compound 60 tor in a lithium halide brine, including lithium bromide containing a Silicate. The added constituents act as effective and/or lithium chloride, typically at the Site of a refrigeration corrosion inhibitors, with the inhibiting performance of the System containing the brine. The System compriseS reagent fluids being Superior to lithium chromate inhibitors. This means and a means for determining molybdate concentra improved system of corrosion inhibitors is described in tion based on color analysis. The reagent means is mixed greater detail in U.S. Pat. No. 5,547,660 for Absorption 65
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