WO2000019194A1 - Field test apparatus and method for analysis of coolants and heat-exchange fluids - Google Patents
Field test apparatus and method for analysis of coolants and heat-exchange fluids Download PDFInfo
- Publication number
- WO2000019194A1 WO2000019194A1 PCT/IB1999/001577 IB9901577W WO0019194A1 WO 2000019194 A1 WO2000019194 A1 WO 2000019194A1 IB 9901577 W IB9901577 W IB 9901577W WO 0019194 A1 WO0019194 A1 WO 0019194A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sample
- acidic reagent
- amount
- titration vessel
- coolant
- Prior art date
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/11—Automated chemical analysis
- Y10T436/115831—Condition or time responsive
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/11—Automated chemical analysis
- Y10T436/115831—Condition or time responsive
- Y10T436/116664—Condition or time responsive with automated titrator
Definitions
- This invention relates to a method and apparatus for testing the quality of engine coolants and heat-exchange fluids containing long life organic corrosion inhibitors, comprising alkali metal, ammonium or amine salts of carboxylic acids.
- coolants are usually referred to as Organic Acid Technology (OAT) coolants or heat-exchange fluids.
- OAT Organic Acid Technology
- this invention relates to an easy, straightforward field test, requiring a minimum of operator interaction, optionally determining, separately or combined in one test sequence, values for carboxylate inhibitor content, contamination level, pH and frost protection of the tested coolant or heat-exchange fluid.
- OAT corrosion inhibitor packages in aqueous and glycol concentrates are used in automotive, heavy duty, marine and industrial applications.
- OAT inhibitors are also used in secondary cooling systems and in a variety of industrial heat exchange fluids.
- the use of monocarboxylic or dicarboxylic acids, or the salts of such acids, as corrosion inhibitors in antifreeze/coolant and heat-exchange fluid compositions is disclosed for instance in EP-A-0 479 470, -0 564 721 and -0 573 287.
- compositions may also contain a variety of additives for special purposes, such as hydrocarbyl triazoles for corrosion protection of copper and copper alloys (EP-A-0 564 721) .
- additives for special purposes, such as hydrocarbyl triazoles for corrosion protection of copper and copper alloys (EP-A-0 564 721) .
- organic acids were neutralized with alkali metal hydroxides (preferably NaOH or KOH) to obtain the inhibitor salts used in the new organic formulations, see for example US-A-4 647 392; US-A-4 851 145; US-A-4 759 864 etc. It was soon realized that an acid titration of an OAT solution could provide information on the total carboxylic acid inhibitor content.
- US-A- 5 366 651 shows in Figure 1 some titration curves for combinations of carboxylate inhibitors with an organic pH buffer such as imidazole.
- the end user In order to evaluate the OAT coolant quality in the field, the end user needs to be able to check the amount of contamination with other coolants, as well as carboxylate inhibitor content.
- the pH of the used coolant provides information on further suitability for use. pH values that are too high or too low may be detrimental to some engine- or heat -exchange system materials. Finally, if applicable, a check on the freezing point will provide information on frost protection.
- a test method for determining the content of carboxylic acid- based corrosion inhibitors in a coolant or heat exchange fluid which comprises:
- a method wherein the content of contaminant in the sample is determined from the amount of acidic reagent required to reach the first equilibrium point.
- a method wherein the amount of freezing point depressant in the sample is determined from the refractive index of the sample.
- a method wherein the pH is determined by means of a calibrated electrode in the titration vessel.
- a method wherein at least one quantity selected from the observed values of pH, the amount of carboxylic acid corrosion inhibitor, the amount of contaminant, the refractive index, and the freezing point of the sample is displayed visually.
- an apparatus for conducting a test method as described above which comprises a titration vessel, first and second reservoirs for acidic reagent and waste neutralizing agents respectively, a first pump means for transferring acidic reagent from the first reservoir to the titration vessel and a second pump means for transferring waste neutralizing agent to the titration vessel from the second reservoir, stirring means for stirring samples in the titration vessel, a pH electrode in the titration vessel, display means for displaying information determined by tests conducted in the apparatus, and electronic control means for controlling said apparatus.
- the present invention is directed towards a field- or laboratory test technique to determine the quality of antifreeze/coolant or aqueous heat-transfer fluids.
- An apparatus and method are described by means of which it is possible to measure the content of carboxylate corrosion inhibitors in OAT coolants or heat exchange fluids, such as Havoline Extended Life Coolant (XLC) , or heat exchange fluids containing Havoline Extended Life Corrosion Inhibitor (XLI) or mixtures thereof.
- the method is used to also measure the contamination level in XLC contaminated by traditional borate or phosphate containing coolant or with the more recently introduced hybrid OAT- traditional coolants such as Havoline Antifreeze Coolant (AFC) .
- AFC Havoline Antifreeze Coolant
- the measurement of contamination level, carboxylate corrosion inhibitor content is combined with a measurement of the pH of the test solution.
- the measurements of contamination level, total carboxylate inhibitor content and pH are combined with a refractometric determination of the freezing point of the test solution.
- Figure 1 is a graphical plot showing the effect of the metered addition of acid upon the pH of aqueous solutions of certain commercial OAT coolants.
- Figure 2 is a graphical plot showing the effect of the metered addition of acid upon the pH of aqueous solutions of mixtures of OAT coolant with a commercial coolant .
- Figure 3 is a graphical plot showing the effect of the metered addition of acid to aqueous solutions of borax and silicate inhibitors.
- Figure 4 is a graphical plot of carboxylic acid content and equilibrium points for a carboxylic based coolant.
- Figure 5 shows a graph of the refractive index of systems containing different percentages of onoethylene glycol .
- Figure 6 is a schematic view of one embodiment of apparatus according to the invention.
- Figure 7 is a view of one embodiment of the apparatus according to the invention.
- the corrosion inhibitors used in engine coolants are inorganic and/or organic compositions which can be considered as chemical bases.
- a coolant has a pH of approximately 6.5-9.5 in order to ensure adequate protection of the metals used in engines and cooling and heat-exchange systems.
- an analytical technique such as an acid-base titration with hydrogen chloride can be used for the determination of the inhibitor concentrations .
- Figure 1 shows the difference between the acid-base titration of a hybrid coolant containing borate, silicate and benzoate and carboxylate based inhibitors. These are Havoline Antifreeze Coolant (hereinafter indicated by the abbreviation AFC) and a fully carboxylate based technology Havoline Extended Life Coolant (hereinafter indicated by the abbreviation XLC) .
- Figure 1 shows the effect upon pH of the addition of 2N hydrochloric acid to eight samples showing various amounts of AFC and XLC in deionized water (DIW) .
- DIW deionized water
- the titration curves are numbered 1 to 8. The curves show respectively 10%, 20%, 30% and 50% AFC in DIW and respectively 10%, 20%, 30% and 50% XLC in DIW.
- Figure 2 shows the effect upon pH of metered addition of 2N hydrochloric acid to different mixtures of AFC and XLC.
- Curves 1 to 7 show respectively 5%, 10%, 15%, 20%, 30%, 40% and 50% of AFC in XLC: curve 8 shows pure AFC.
- Figure 3 shows the effect upon pH of metered addition of 2N hydrochloric acid for solutions of borax and silicate. The influence on the positioning of the first equilibrium point is clearly shown. This makes it possible to evaluate unequivocally the amount of traditional inhibitors in a titrated coolant sample, and consequently the amount of contamination .
- Figure 4 shows the correlation between the carboxylic acid contents and the measured acid volumes added between the first and second equilibrium points. It will be seen that the data points representing VI - V2 for the four percentage concentrations lie in a straight line.
- Figure 6 shows one possible preferred embodiment (in schematic fashion) of an apparatus according to the invention for measuring the contamination levels in OAT, the total carboxylate content, and optionally, the coolant pH and extent of frost protection.
- FIG. 7 shows an overview from above and one side of an apparatus according to the present invention.
- the apparatus comprises a titration vessel (1) , a metering burette (not shown) for transferring a metered sample of coolant to the titration vessel, a pH electrode (9) , a first reservoir (2) for acid reagent and a second reservoir (3) for a neutralizing agent, for neutralizing titrated samples after testing.
- a first metering pump (4) is provided for transferring metered additions of reagent acid from the first reservoir (2) to the titration vessel (1) , by way of tubes (6, 6a) .
- a second metering pump (5) is provided for transferring neutralizing agent from the second reservoir (3) to the titration vessel (1) by way of tubes (7, 7a) , after the pH and any other measurements have been carried out.
- Means such as a magnetic stirrer (8) are provided in order to obtain good mixing of the test solution. If desired, another mixing device can be employed instead of the magnetic stirrer.
- a pH electrode (9) and optionally a refractometric probe (14) are provided for determining the pH and refractive index of the contents of the titration vessel (1) , They are connected to a control unit (11) containing electronics including a start button (12) , an analog signal treatment device (13) , an analog to digital converter, and a microcontroller with program software to treat the signals from the pH electrode, to and from the metering pumps, and to an alphanumerical display (10) to show the results and test comments.
- the electronics also contain means for signal treatment to and from the refractometric probe, and software for signal processing of pH reading and determination of the freezing point based on a refractometric measurement, indicating the content of freezing point depressant.
- the display (10) can provide customised messages according to the results of the test.
- Means are also provided in terms of software and standard solutions to calibrate the pH measurement and optionally the measurement of refractive index. Titration procedure
- a fixed volume for example 25 ml of coolant, is taken out of an engine, radiator or expansion vessel of the cooling or heat-exchange system with a fixed metering pipette, and transferred to the titration vessel (1), e.g. with a syringe .
- the calibrated pH-electrode (9) is brought into the titration vessel and acid reagent is pumped into the vessel through polytetrafluoroethylene (PTFE) tubes (6, 6a) connected to the first reservoir (2) containing hydrogen chloride solution at a fixed concentration (for example 2N HC1) .
- PTFE polytetrafluoroethylene
- the start button (12) is activated to begin the measuring process.
- the liquid is stirred for instance by a magnetic stirrer (8) .
- a wait cycle starts for stabilizing purposes.
- the pH of the test solution is recorded in the memory of the controller. If the initial pH is below a limited value acceptable for the coolant, the process stops and a warning message is displayed on the LCD. Optionally, the initial pH is shown on the LCD screen. 5. If the pH is above this limit, the microcontroller generates a pulsed signal to the first metering pump (4) and acidic reagent is dosed at an exact rate into the titration vessel (1) .
- a typical addition rate is lcm 3 /min.
- the microcontroller keeps track of the measured pH and the dosed amount of reagent. If the pH reaches the first equilibrium point, corresponding to a pH of 7.0, the quantity of reagent acid that has been added is stored and used to calculate the "Contamination level". This contamination level is displayed on the LCD screen. If this level exceeds a limit value which is unacceptable for further use of the coolant (contamination limit) , the process is stopped and a warning message is displayed.
- the system continues and starts counting the amount of acid reagent dosed, in a second memory. The process continues until the pH reaches the second equilibrium point at pH 3. At this point the microcontroller stops the activating pulse signal to the metering pump (4) . The recorded quantity of reagent dosed between the contamination point and the inhibitor level point is used to calculate the actual carboxylate corrosion inhibitor content. This value (in % reading) is displayed on the LCD screen.
- the microcontroller then starts the generation of an activating pulse signal to the second metering pump (5) , and a controlled amount of caustic waste treatment fluid is pumped from the second reservoir (3) through tubes (7,7a), which may also be formed from PTFE, into the titration vessel (1) . This continues until the solution reaches a fixed pH value. The test fluid can then be removed and disposed of, together with normal coolant waste.
- the microcontroller can, for example, be a BS2-IC model made by Parallax, Inc.
- the pumps can, for example, be MLP-200 and/or MLP-50 models made by Tagasago Electric, Inc..
- the content of freezing point depressant is measured at step 4.
- This can be done by means of a refractometer probe (14) .
- Means are provided to reduce the influence of incident radiation (e.g. a near infrared transmitting filter on the detection side) .
- a pulse technique is used to reduce aging of emitters and detectors.
- the apparatus can be easily modified to calculate and display the contamination levels and carboxylate contents for other coolants then XLC and AFC. Since this measurement is virtually independent of the base fluid, it can be used in aqueous glycol-free solutions or in mixtures of water and glycol and/or other freezing point depressants.
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU56440/99A AU763860B2 (en) | 1998-09-28 | 1999-09-23 | Field test apparatus and method for analysis of coolants and heat-exchange fluids |
JP2000572649A JP2002525628A (en) | 1998-09-28 | 1999-09-23 | Field test apparatus and analysis method for coolant and heat exchange fluid |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP98307868A EP0989402A1 (en) | 1998-09-28 | 1998-09-28 | Field test apparatus and method for analysis of coolants and heat-exchange fluids |
EP98307868.4 | 1998-09-28 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2000019194A1 true WO2000019194A1 (en) | 2000-04-06 |
Family
ID=8235081
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/IB1999/001577 WO2000019194A1 (en) | 1998-09-28 | 1999-09-23 | Field test apparatus and method for analysis of coolants and heat-exchange fluids |
Country Status (5)
Country | Link |
---|---|
US (2) | US6495372B1 (en) |
EP (1) | EP0989402A1 (en) |
JP (1) | JP2002525628A (en) |
AU (1) | AU763860B2 (en) |
WO (1) | WO2000019194A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005505908A (en) * | 2001-10-17 | 2005-02-24 | テキサコ ディベラップメント コーポレイション | Corrosion protection compositions and methods for fuel cell coolant systems |
WO2010085750A3 (en) * | 2009-01-26 | 2010-11-04 | M-I L.L.C. | Cation exchange capacity titration unit |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB0218693D0 (en) * | 2002-08-10 | 2002-09-18 | Hajatdoost Sohail | Quick titration device |
US20070041871A1 (en) * | 2005-08-16 | 2007-02-22 | Frank Lecrone | Gravimetric field titration kit and method of using thereof |
US20080019873A1 (en) * | 2006-07-17 | 2008-01-24 | Shah Vatsal M | System, apparatus and method for evaluating the constituents of a heat exchange fluid having corrosion inhibitors therein |
WO2010075025A2 (en) * | 2008-12-16 | 2010-07-01 | Shell Oil Company | Device for evaluating a heat exchange fluid |
JP2010164465A (en) * | 2009-01-16 | 2010-07-29 | Dkk Toa Corp | Automatic titrator |
US8815605B2 (en) | 2011-04-19 | 2014-08-26 | Dexsil Corporation | Methods and kits for quantitative determination of total organic acid content in a coolant |
US20170370017A1 (en) * | 2016-06-27 | 2017-12-28 | Tel Nexx, Inc. | Wet processing system and method of operating |
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US4227976A (en) * | 1979-03-30 | 1980-10-14 | The United States Of America As Represented By The Secretary Of The Army | Magnesium anodize bath control |
US5366651A (en) * | 1992-04-06 | 1994-11-22 | Texaco Services (Europe) Ltd. | Corrosion-inhibited antifreeze formulations having monocarboxylic, triazole, and imidazole compounds |
FR2748112A1 (en) * | 1996-04-30 | 1997-10-31 | Tlti Toute La Telephonie Ind | Automatic method for determining the acidity level in food or non- food oils |
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US4209416A (en) * | 1979-01-02 | 1980-06-24 | Basf Wyandotte Corporation | Antifreeze containing amino silanes, amino siloxanes and a hydroxybenzoic acid |
DE2905287A1 (en) * | 1979-02-12 | 1980-08-21 | Siemens Ag | METHOD FOR THE AUTOMATIC ELECTROCHEMICAL FINAL POINT DETERMINATION OF A TITRATION |
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CH666554A5 (en) * | 1985-01-18 | 1988-07-29 | Mettler Instrumente Ag | METHOD AND DEVICE FOR TITRIMETRIC SALARY DETERMINATIONS IN CHEMICAL REACTION SYSTEMS. |
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US4920056A (en) * | 1988-02-19 | 1990-04-24 | The Dow Chemical Company | Apparatus and method for automated microbatch reaction |
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US5242621A (en) | 1992-06-03 | 1993-09-07 | Texaco Chemical Co. | Combinations of alkanoic hydrocarbyl dicarboxylic and carbocyclic alkanoic acids or salts useful as heat transfer fluid corrosion inhibitors |
-
1998
- 1998-09-28 EP EP98307868A patent/EP0989402A1/en not_active Ceased
-
1999
- 1999-09-23 AU AU56440/99A patent/AU763860B2/en not_active Ceased
- 1999-09-23 WO PCT/IB1999/001577 patent/WO2000019194A1/en active IP Right Grant
- 1999-09-23 JP JP2000572649A patent/JP2002525628A/en active Pending
- 1999-09-27 US US09/406,057 patent/US6495372B1/en not_active Expired - Fee Related
-
2001
- 2001-03-30 US US09/821,050 patent/US6475438B2/en not_active Expired - Fee Related
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DE715397C (en) * | 1940-09-22 | 1941-12-20 | Vaw Ver Aluminium Werke Ag | Device for automatic electrometric titration |
US4227976A (en) * | 1979-03-30 | 1980-10-14 | The United States Of America As Represented By The Secretary Of The Army | Magnesium anodize bath control |
US5366651A (en) * | 1992-04-06 | 1994-11-22 | Texaco Services (Europe) Ltd. | Corrosion-inhibited antifreeze formulations having monocarboxylic, triazole, and imidazole compounds |
FR2748112A1 (en) * | 1996-04-30 | 1997-10-31 | Tlti Toute La Telephonie Ind | Automatic method for determining the acidity level in food or non- food oils |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005505908A (en) * | 2001-10-17 | 2005-02-24 | テキサコ ディベラップメント コーポレイション | Corrosion protection compositions and methods for fuel cell coolant systems |
WO2010085750A3 (en) * | 2009-01-26 | 2010-11-04 | M-I L.L.C. | Cation exchange capacity titration unit |
EA019684B1 (en) * | 2009-01-26 | 2014-05-30 | Эм-Ай Эл.Эл.Си. | Cation exchange capacity titration unit |
US9011775B2 (en) | 2009-01-26 | 2015-04-21 | M-I L.L.C. | Cation exchange capacity titration unit |
Also Published As
Publication number | Publication date |
---|---|
AU5644099A (en) | 2000-04-17 |
AU763860B2 (en) | 2003-07-31 |
JP2002525628A (en) | 2002-08-13 |
EP0989402A1 (en) | 2000-03-29 |
US20020000535A1 (en) | 2002-01-03 |
US6495372B1 (en) | 2002-12-17 |
US6475438B2 (en) | 2002-11-05 |
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