CS258160B1 - Method of monoethylene glycol identification and semiquantitative determination in engine oil - Google Patents
Method of monoethylene glycol identification and semiquantitative determination in engine oil Download PDFInfo
- Publication number
- CS258160B1 CS258160B1 CS863660A CS366086A CS258160B1 CS 258160 B1 CS258160 B1 CS 258160B1 CS 863660 A CS863660 A CS 863660A CS 366086 A CS366086 A CS 366086A CS 258160 B1 CS258160 B1 CS 258160B1
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- CS
- Czechoslovakia
- Prior art keywords
- monoethylene glycol
- mixture
- ethanol
- benzene
- engine oil
- Prior art date
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000010705 motor oil Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 239000012086 standard solution Substances 0.000 claims abstract description 9
- 239000002594 sorbent Substances 0.000 claims abstract description 8
- 239000003921 oil Substances 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 4
- -1 N, N-dimethylamino Chemical group 0.000 claims abstract description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 15
- 238000004809 thin layer chromatography Methods 0.000 claims description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims 3
- 239000002826 coolant Substances 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000000265 homogenisation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012206 semi-quantitative assay Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Řešení oe týká zjištování kvality motorového oleje u spalovacích motorů, znečištěného chladicí kapalinou, tvořenou monoetylenglykolem. Vzorek oleje se po homogenizaci smísí s etanolem a ke směsi se přidá činidlo. Tato směs se nanese na destičku s tenkou vrstvou sorbentu a vedle standardní roztok. Ten je tvořen monoetylenglykolem, rozpuštěným v etanolu za přítomnosti činidla. Destička se podrobí působení mobilní fáze a po časovém úseku se provede porovnání skvrn u směsi a standardního roztoku. Jako činidlo se používá p-/N,N-dimetylamino/benzen-p'-azobenzoylchlorid.The solution is to determine quality engine oil for internal combustion engines contaminated with coolant formed monoethylene glycol. Oil sample with mixed with ethanol after homogenization an agent is added to the mixture. This mixture is applied to a thin layer plate sorbent and in addition to the standard solution. It consists of monoethylene glycol dissolved in ethanol in the presence of reagent. The plate is treated with a mobile phase and after a period of time, a comparison is made spots in the mixture and standard solution. The reagent used is p- (N, N-dimethylamino) benzene-p'-azobenzoyl chloride.
Description
Vynález se týká způsobu identifikace a semikvantitativního stanovení monoetylenglykolu v motorovém oleji metodou tenkovrstvé chromatografie.The invention relates to a method for the identification and semi-quantitative determination of monoethylene glycol in engine oil by thin-layer chromatography.
Podstatou složkou chladicí kapaliny, používané ve spalovacích motorech, je monoetylenglykol. Při průniku chladicí kapaliny do motorového oleje dochází jednak k nežádoucím reakcím s aditivy, jednak může dojít ke kondenzačním reakcím, jejichž produkty mohou zapříčinit tak zvané zalepení motoru. Je proto žádoucí sledovat přítomnost monoetylenglykolu v motorových olejích. Je známo používat bud postup azeotropní destilace s následnou oxidací kyselinou dusičnou nebo postup infračervené spektrometrie. Tyto postupy jsou časově náročné a nákladné vzhledem k přístrojové technice a v žádném případě je nelze využít v provozních podmínkách mimo speciální laboratoř.The essential component of the coolant used in internal combustion engines is monoethylene glycol. When the coolant enters the engine oil, unwanted reactions with additives occur and, on the other hand, condensation reactions can occur, the products of which can cause so-called engine sticking. It is therefore desirable to monitor the presence of monoethylene glycol in engine oils. It is known to use either azeotropic distillation followed by oxidation with nitric acid or infrared spectrometry. These procedures are time-consuming and costly in terms of instrumentation and in no way can they be used in operating conditions outside a special laboratory.
Dále je z USA spisu č. 3 635 677 známo zjištování glykolu v oleji tim způsobem, že vzorek oleje je třepán s vodným roztokem oxidačního činidla, načež se vodná fáze nechá působit na sorbent s naneseným činidlem reagujícím barevně na aldehydy. Podle NSR spisu č. 2 261 200 se zjištuje obsah alkoholu v palivu. V trubici je na nosiči silikagelu nebo laumině nanesen 8-hydroxychinolinester kyseliny o-vanadičité a po průtoku daného množství vzorku je délka barevné zóny úměrná obsahu alkoholu.Further, it is known from U.S. Pat. No. 3,635,677 to detect glycol in oil by shaking the oil sample with an aqueous solution of an oxidizing agent, and then allowing the aqueous phase to act on the sorbent with a color-reactive aldehyde reagent. According to German Pat. No. 2,261,200, the alcohol content of the fuel is determined. O-vanadic acid 8-hydroxyquinolinester is deposited in a tube on a silica gel support or laumina, and the color zone length is proportional to the alcohol content after a given amount of sample has flowed.
♦♦
Tyto způsoby jsou rovněž náročné na přístrojovou techniku.These methods are also labor-intensive.
Uvedené nedostatky odstraňuje způsob identifikace a semikvantitativního stanovení monoetylenglykolu v motorovém oleji metodou tenkovrstvé chromatografie podle vynálezu.These drawbacks are overcome by the method of identification and semi-quantitative determination of monoethylene glycol in engine oil by the thin-layer chromatography method of the invention.
Jeho podstata spočívá v tom, že se vzorek oleje zhomogenizuje a smísí s etanolem a protřepe, načež se k etanolové vrstvě přidá činidlo, tvořené p-/N,N-dimetylamino/benzen-p'-azobenzoylchloridem, rozpuštěným v benzenu, poté se tato směs nanese na destičku s tenkou vrstvou sorbentu a vedle standardní roztok, tvořený monoetylenglykolem, rozpuštěným v etanolu a smíchaným s činidlem v benzenu. Poté se destička s tenkou vrstvou sorbentu podrobí působení mobilní fáze tvořené směsí hexan-etylacetát v poměru 3:2, a po časovém úseku se provede porovnání skvrn u směsi a standardního roztoku.It consists in homogenizing the oil sample and mixing it with ethanol and shaking, followed by the addition of a reagent consisting of p- / N, N-dimethylamino / benzene-p'-azobenzoyl chloride dissolved in benzene, to the ethanol layer. apply the mixture to a thin sorbent plate and next to a standard solution consisting of monoethylene glycol dissolved in ethanol and mixed with the reagent in benzene. Thereafter, the thin-bed plate of the sorbent is treated with a 3: 2 hexane-ethyl acetate mixture, and after a period of time, the stains of the mixture and the standard solution are compared.
Základní výhoda způsobu podle vynálezu spočívá v tom, že umožňuje jednoduše identifikovat monoetylenglykol v motorovém oleji v provozních podmínkách bez nároků na složitou přístrojovou techniku. Dále je možno semikvantitativně zjištovat množství monoetylenglykolu v motorovém oleji. Mez detekce činí 0,1 % hmot. glykolu.The main advantage of the process according to the invention is that it makes it possible to easily identify monoethylene glycol in engine oil under operating conditions without the need for complex instrumentation. Furthermore, the amount of monoethylene glycol in the engine oil can be determined semi-quantitatively. The limit of detection is 0.1% by weight. glycol.
Způsob je dále blíže popsán na konkrétním příkladu provedení.The method is described in more detail below on a specific embodiment.
PříkladExample
Vzorek oleje byl zhomogenizován a bylo odebráno 5 ml do širší zkumavky. Poté se přidalo 2,5 ml etanolu, směs se důkladně protřepala a nechala ustát. Poté se 0,5 ml etanolové vrstvy odebralo do menší zkumavky a přidalo 0,5 ml činidla, tvořeného 0,1 g p-/N,N-dimetylamino/benzen -p'-azobenzoylchloridu, rozpuštěného v 50 ml benzenu. Tato směs se opět promíchala. Pak se 5/ul této směsi naneslo na start destičky s tenkou vrstvou sorbentu. Vedle pak byl nanesen standardní roztok monoetylenglykolu, tvořený smícháním 0,5 ml x % rotokumonoetylenglykolu v etanolu s 0,5 ml shora uvedeného činidla. Takto upravená destička s tenkou vrstvou sorbentu se vložila do kádinky s mobilní fází tak, aby mobilní fáze dosahovala asi 0,5 cm pod start. Kádinka byla zakryta hodinovým sklíčkem. Pak bylo vyvíjeno tak dlouho, až mobilní fáze dosáhla vzdálenosti 10 cm za startem. Pokud byl ve zkoušeném vzorku motorového oleje monoetylen glykol, objevila se skvrna ve stejné vzdálenosti od startu jako nejbližší skvrna od startu u standardního roztoku.The oil sample was homogenized and 5 ml was collected into a wider tube. Then 2.5 ml of ethanol was added, the mixture was shaken vigorously and allowed to stand. Then, 0.5 ml of the ethanol layer was collected into a smaller tube and 0.5 ml of a reagent consisting of 0.1 g of p- / N, N-dimethylamino / benzene-p'-azobenzoyl chloride dissolved in 50 ml of benzene was added. This mixture was mixed again. Then, 5 µl of this mixture was applied to the start of a thin sorbent plate. Next, a standard solution of monoethylene glycol, consisting of mixing 0.5 ml x% rotocumonoethylene glycol in ethanol with 0.5 ml of the above reagent, was applied. The thin sorbent plate thus treated was placed in a beaker with a mobile phase such that the mobile phase reached about 0.5 cm below the start. The beaker was covered with a watch glass. It was then developed until the mobile phase reached a distance of 10 cm behind the launch. If there was monoethylene glycol in the engine oil sample to be tested, the spot appeared at the same distance from the start as the closest spot from the start of the standard solution.
Celková doba pro jedno samostatné stanovení činila přibližně 30 minut. Při semikvantitativ ním stanovení je nutné nanášet na destičku s tenkou vrstvou sorbentu přesný objem zkoušeného vzorku motorového oleje a zároveň nanášet standardní roztoky s odstupňovaným množstvím monoetylenglykolu.The total time for one separate assay was approximately 30 minutes. For a semi-quantitative assay, it is necessary to apply an accurate volume of the engine oil sample to the plate with a thin sorbent layer and at the same time to apply standard solutions with graduated amounts of monoethylene glycol.
Protože se vzorek vytřepává do polovičního množství etanolu, je nutné výsledek dělit dvěma.Since the sample is shaken to half the amount of ethanol, the result should be divided by two.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS863660A CS258160B1 (en) | 1986-05-20 | 1986-05-20 | Method of monoethylene glycol identification and semiquantitative determination in engine oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS863660A CS258160B1 (en) | 1986-05-20 | 1986-05-20 | Method of monoethylene glycol identification and semiquantitative determination in engine oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS366086A1 CS366086A1 (en) | 1987-05-14 |
| CS258160B1 true CS258160B1 (en) | 1988-07-15 |
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ID=5377290
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS863660A CS258160B1 (en) | 1986-05-20 | 1986-05-20 | Method of monoethylene glycol identification and semiquantitative determination in engine oil |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS258160B1 (en) |
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1986
- 1986-05-20 CS CS863660A patent/CS258160B1/en unknown
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| Publication number | Publication date |
|---|---|
| CS366086A1 (en) | 1987-05-14 |
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