US4288402A
Expired / Lapsed
US
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Acid field test kit for refrigeration oils containing a leak detector
Assignee: Hoechst Celanese Chemical Co
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Filing: 1979-04-25
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Granted: 1981-09-08
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Expires: 1999-04-25
Abstract
Abstract A field test kit which uses a single vial is useful in testing acidity in refrigeration oils contaminated with a colored leak detector. This vial contains a pre-measured indicator solution and has sufficient additional volume that the test oil can be added directly to the indicator solution and accurately measured within the vial. After shaking, the mixture quickly separates into two phases. The color of the bottom phase indicates whether or not the acidity of the refrigeration oil exceeds 0.05 acid number.
Inventors
- 👤 Leonard C. Ellis
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 09:59
CPC Classifications
G; G01; G01N; G01N33/00; G01N33/26; G01N33/28; G01N33/2835; G01N33/2876
Claims Analysis
Total Claims: 31
Claim 1
Independent Claim
279 words
An acid field test kit for determining the acidity of oil samples, said test kit being of the two-phase type and operable within a single vial which has a selected internal volume, and said test kit being used: for measuring a sample of a refrigeration oil containing a highly colored leak detector; for carrying out a test procedure on said sample by fast phase separation into a solvent top layer and a highly ionic aqueous bottom layer; and for obtaining reliable test results as to acidity of said oil; and said test kit comprising: A. at least one said vial having a means for indicating said selected internal volume; B. a water-immiscible solvent, which is disposed within said vial; and C. an indicator stock solution which is disposed within said vial, comprising: (1) 20-28% by weight of a lower alcohol, (2) 56-79% by weight of water, (3) 6-12% by weight of a water-soluble inorganic salt, (4) 0.2-0.3% by weight of a concentrated aqueous solution of a selected indicator having an unmistakable first color at a selected baseline pH which is at about the alkaline limit of the pH range for said indicator, (5) sufficient alkaline hydroxide solution to create said baseline pH, and (6) an amount of alkaline hydroxide solution which permits an unmistakable selected second color to appear within said aqueous bottom layer only when the acid number of said oil sample exceeds about 0.05 by limiting the change in pH from said baseline pH to a selected acidic pH at about the acid limit of said pH range after said oil sample has been mixed within said vial with said water-immiscible solvent and said indicator stock solution.
Claim 2
Dependent Claim
279 words
An acid field test kit for determining the acidity of oil samples, said test kit being of the two-phase type and operable within a single vial which has a selected internal volume, and said test kit being used: for measuring a sample of a refrigeration oil containing a highly colored leak detector; for carrying out a test procedure on said sample by fast phase separation into a solvent top layer and a highly ionic aqueous bottom layer; and for obtaining reliable test results as to acidity of said oil; and said test kit comprising: A. at least one said vial having a means for indicating said selected internal volume; B. a water-immiscible solvent, which is disposed within said vial; and C. an indicator stock solution which is disposed within said vial, comprising: (1) 20-28% by weight of a lower alcohol, (2) 56-79% by weight of water, (3) 6-12% by weight of a water-soluble inorganic salt, (4) 0.2-0.3% by weight of a concentrated aqueous solution of a selected indicator having an unmistakable first color at a selected baseline pH which is at about the alkaline limit of the pH range for said indicator, (5) sufficient alkaline hydroxide solution to create said baseline pH, and (6) an amount of alkaline hydroxide solution which permits an unmistakable selected second color to appear within said aqueous bottom layer only when the acid number of said oil sample exceeds about 0.05 by limiting the change in pH from said baseline pH to a selected acidic pH at about the acid limit of said pH range after said oil sample has been mixed within said vial with said water-immiscible solvent and said indicator stock solution.
Claim 3
Dependent Claim
14 words
The acid field test kit of claim 1, wherein said indicator is phenol red.
Claim 4
Dependent Claim
42 words
The acid field test kit of claim 1, wherein said indicator stock solution occupies 51.4% of said selected internal volume, said indicator is thymol blue, and the weight ratio of said oil sample to one milliequivalent of said alkaline hydroxide is 1122.
Claim 5
Dependent Claim
18 words
The acid field test kit of claim 3, wherein said selected internal volume is about two fluid ounces.
Claim 6
Dependent Claim
25 words
The acid field test kit of claim 3, wherein the ratio in milliliters of said water to one milliequivalent of said alkaline hydroxide is 1400-1950.
Claim 7
Dependent Claim
17 words
The acid field test kit of claim 5, wherein said water to alkali hydroxide ratio is 1690.
Claim 8
Dependent Claim
26 words
The acid field test kit of claim 3, wherein said alkaline hydroxide is selected from the group consisting of potassium hydroxide, sodium hydroxide, and lithium hydroxide.
Claim 9
Dependent Claim
15 words
The acid field test kit of claim 7 which comprises 0.775 mg. of potassium hydroxide.
Claim 10
Dependent Claim
29 words
The acid field test kit of claim 3, wherein said water-soluble inorganic salt is selected from the group consisting of sodium chloride, calcium chloride, magnesium chloride, and sodium bromide.
Claim 11
Dependent Claim
35 words
The acid field test kit of claim 9, wherein said water-soluble inorganic salt is sodium chloride and the weight ratio in grams of said sodium chloride to one milliequivalent of said alkaline hydroxide is 135-275.
Claim 12
Dependent Claim
20 words
The acid field test kit of claim 10, wherein said weight ratio of sodium chloride to alkaline hydroxide is 201.
Claim 13
Dependent Claim
25 words
The acid field test kit of claim 11, wherein the ratio in milliliters of said alcohol to one milliequivalent of said alkaline hydroxide is 600-900.
Claim 14
Dependent Claim
17 words
The acid field test kit of claim 12, wherein said alcohol to alkaline hydroxide ratio is 751.
Claim 15
Dependent Claim
20 words
The acid field test kit of claim 3, wherein said water-immiscible solvent occupies exactly 22.7% of said selected internal volume.
Claim 16
Dependent Claim
30 words
The acid field test kit of claim 14, wherein said water-immiscible solvent principally comprises cyclic carbon compounds having no carboxyl groups, alcohol groups, or ether linkages in the side chains.
Claim 17
Dependent Claim
28 words
The acid field test kit of claim 15, wherein said cyclic compounds are selected from the group consisting of benzene, toluene, the xylenes, mesitylene, isopropyl benzene, and cyclohexane.
Claim 18
Dependent Claim
14 words
The acid field test kit of claim 16, wherein said cyclic compound is cyclohexane.
Claim 19
Dependent Claim
45 words
The acid field test kit of claim 17, wherein said indicator stock solution comprises, on a weight basis: 23.86% of isopropanol as said lower alcohol, 67.78% of water, 8.08% of sodium chloride as said water-soluble inorganic salt, and 0.26% of said concentrated aqueous indicator solution.
Claim 20
Dependent Claim
22 words
The acid field test kit of claim 18, wherein said concentrated aqueous indicator solution contains 1.0% by weight of thymol blue indicator.
Claim 21
Dependent Claim
18 words
The acid field test kit of claim 19, wherein the contents of said vial are protected with nitrogen.
Claim 22
Dependent Claim
77 words
The acid field test kit of claim 19, wherein, after filling said vial with said sample of a refrigeration oil so that said selected internal volume is fully utilized and shaking, a two-phase mixture is obtained in which said bottom layer is blue when said refrigeration oil has an acid number of 0.02, green when said refrigeration oil has an acid number of 0.04, and distinctly yellow when said refrigeration oil has an acid number of 0.06.
Claim 23
Dependent Claim
267 words
The process of assembling an acid field test kit for determining acidity of refrigeration oil samples, comprising: A. dissolving a pH indicator, having a pH range of about 8-10, in distilled water to form a concentrated aqueous indicator solution; B. preparing an indicator stock solution under an inert gas atmosphere by the following steps: (1) preparing an indicator mixture by mixing 20-28% by weight of a lower alcohol, 56-79% by weight of distilled water, 6-12% by weight of a water-soluble inorganic salt, and 0.2-0.3% by weight of said concentrated aqueous indicator solution; (2) using a pH meter, adjusting the pH of said indicator mixture to 9.5 by adding 1.0 N alkaline hydroxide solution to said indicator mixture to form an adjusted mixture; (3) adding to said adjusted mixture, to form said indicator stock solution, exactly the amount of additional alkaline hydroxide solution that the weight ratio of oil to be tested to one milliequivalent of said additional alkaline hydroxide is 1122; and C. preparing a plurality of test kit vials, each vial having a mark thereon to indicate a selected internal volume, by the following steps while protecting the contents thereof with an inert gas: (1) adding to said each vial a quantity of a water-immiscible solvent equalling 22.7 percent of said selected internal volume, and (2) adding to said each vial a quantity of said indicator stock solution equalling 51.4 percent of said selected internal volume, said oil to be tested in each said test kit vial being obtained from said refrigeration oil samples and being added within said selected internal volume up to said mark.
Claim 24
Dependent Claim
267 words
The process of assembling an acid field test kit for determining acidity of refrigeration oil samples, comprising: A. dissolving a pH indicator, having a pH range of about 8-10, in distilled water to form a concentrated aqueous indicator solution; B. preparing an indicator stock solution under an inert gas atmosphere by the following steps: (1) preparing an indicator mixture by mixing 20-28% by weight of a lower alcohol, 56-79% by weight of distilled water, 6-12% by weight of a water-soluble inorganic salt, and 0.2-0.3% by weight of said concentrated aqueous indicator solution; (2) using a pH meter, adjusting the pH of said indicator mixture to 9.5 by adding 1.0 N alkaline hydroxide solution to said indicator mixture to form an adjusted mixture; (3) adding to said adjusted mixture, to form said indicator stock solution, exactly the amount of additional alkaline hydroxide solution that the weight ratio of oil to be tested to one milliequivalent of said additional alkaline hydroxide is 1122; and C. preparing a plurality of test kit vials, each vial having a mark thereon to indicate a selected internal volume, by the following steps while protecting the contents thereof with an inert gas: (1) adding to said each vial a quantity of a water-immiscible solvent equalling 22.7 percent of said selected internal volume, and (2) adding to said each vial a quantity of said indicator stock solution equalling 51.4 percent of said selected internal volume, said oil to be tested in each said test kit vial being obtained from said refrigeration oil samples and being added within said selected internal volume up to said mark.
Claim 25
Dependent Claim
12 words
The process of claim 22, wherein said alkaline hydroxide is potassium hydroxide.
Claim 26
Dependent Claim
22 words
The process of claim 22, wherein said concentrated aqueous indicator solution contains 1.0% by weight of thymol blue as said pH indicator.
Claim 27
Dependent Claim
21 words
The process of claim 24, wherein 0.26% by weight of said thymol blue solution is added for preparing said indicator mixture.
Claim 28
Dependent Claim
11 words
The process of claim 22, wherein said lower alcohol is isopropanol.
Claim 29
Dependent Claim
17 words
The process of claim 26, wherein said isopropanol is 23.86% by weight of said indicator stock solution.
Claim 30
Dependent Claim
13 words
The process of claim 22, wherein said soluble inorganic salt is sodium chloride.
Claim 31
Dependent Claim
18 words
The process of claim 28, wherein said sodium chloride is 8.08% by weight of said indicator stock solution.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-09-07 | 1985-03-09 | 1985-09-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-09-07 | 1989-03-09 | 1989-09-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-09-07 | 1993-03-09 | 1993-09-08 | $7700.00 | Window Closed / Lapsed |