JPS5954964A - Composition of handily measuring total base value in lubricating oil - Google Patents
Composition of handily measuring total base value in lubricating oilInfo
- Publication number
- JPS5954964A JPS5954964A JP16498582A JP16498582A JPS5954964A JP S5954964 A JPS5954964 A JP S5954964A JP 16498582 A JP16498582 A JP 16498582A JP 16498582 A JP16498582 A JP 16498582A JP S5954964 A JPS5954964 A JP S5954964A
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- acid
- total base
- sample
- composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 14
- 239000000203 mixture Substances 0.000 title claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 56
- 238000000605 extraction Methods 0.000 claims abstract description 23
- 238000010790 dilution Methods 0.000 claims abstract description 11
- 239000012895 dilution Substances 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 239000012445 acidic reagent Substances 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 3
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract 2
- 230000005484 gravity Effects 0.000 claims abstract 2
- 229910052760 oxygen Inorganic materials 0.000 claims abstract 2
- 239000001301 oxygen Substances 0.000 claims abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- -1 polyoxyethylene Polymers 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 4
- SQCZQTSHSZLZIQ-UHFFFAOYSA-N 1-chloropentane Chemical compound CCCCCCl SQCZQTSHSZLZIQ-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002845 discoloration Methods 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims 2
- 150000002367 halogens Chemical class 0.000 claims 2
- 125000000217 alkyl group Chemical group 0.000 claims 1
- IODDQGMEFSNLGV-UHFFFAOYSA-N butane;hydrochloride Chemical group Cl.CCCC IODDQGMEFSNLGV-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 20
- 238000012360 testing method Methods 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000007796 conventional method Methods 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 2
- 239000007793 ph indicator Substances 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 239000002585 base Substances 0.000 description 29
- 238000000034 method Methods 0.000 description 21
- 239000002270 dispersing agent Substances 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000010710 diesel engine oil Substances 0.000 description 4
- 239000010705 motor oil Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- ZPLCXHWYPWVJDL-UHFFFAOYSA-N 4-[(4-hydroxyphenyl)methyl]-1,3-oxazolidin-2-one Chemical compound C1=CC(O)=CC=C1CC1NC(=O)OC1 ZPLCXHWYPWVJDL-UHFFFAOYSA-N 0.000 description 1
- 206010008631 Cholera Diseases 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- BELBBZDIHDAJOR-UHFFFAOYSA-N Phenolsulfonephthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2S(=O)(=O)O1 BELBBZDIHDAJOR-UHFFFAOYSA-N 0.000 description 1
- 241000269821 Scombridae Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 235000020640 mackerel Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229960003531 phenolsulfonphthalein Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000010729 system oil Substances 0.000 description 1
- 239000010913 used oil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2835—Specific substances contained in the oils or fuels
- G01N33/2876—Total acid number
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Food Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
□ 本発明は内燃″機関用潤滑油の全塩基価簡易測定用
組成物に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a composition for simple measurement of total base number of lubricating oil for internal combustion engines.
□内燃機関用潤滑油子なわちガソリンエンジン
□□ 油、′Ｉｎ’ｈディーゼ′）レニンジン油並び１
に船舶用：□ディー論ルエンジン油；こは各−の添加剤
が配合さ□れている示特に重要な添加剤の一つとして清
浄分散剤があげられる。とれはエンジン□での燃焼によ
らて星成される種々の物質がピストンあ周面やクランク
ケース内などに層積□するめを防ぎ、油中に分散包含さ
せエンジン各部を清浄に保つ目的で配合される。同時に
燃料中のいおうの燃焼による硫酸や潤階油自 ：′身の
酸化による酸憔！質を中和する塩基性成 。□Lubricating oil for internal combustion engines, i.e. gasoline engines
□□ Oil, 'In'h Diesel') Renginsin oil line 1
For marine use: □ diesel engine oil; this shows that various additives are blended □ One of the particularly important additives is detergent and dispersant. This is a compound that prevents the various substances formed by combustion in the engine from forming a layer on the piston circumferential surface and inside the crankcase, and disperses them into the oil to keep each part of the engine clean. be done. At the same time, the combustion of sulfur in the fuel produces sulfuric acid and oil: acidity due to oxidation! A basic compound that neutralizes the quality.
分としての働きを示す。It shows the function as a minute.
その塩基性成分の指標として全塩基価（単位ｍ ｇＫ
ＯＩ−Ｉ ／ ｇ ）があり、それが清浄分散剤の濃度
を示すとも言える。The total base number (unit: m gK) is used as an indicator of its basic component.
OI-I/g), which can also be said to indicate the concentration of the detergent-dispersant.
清浄分散剤はエンジン油の使用に伴なって熱、水分、酸
性物質、摩耗による金属粉などの影響を受け、徐々にあ
るいは急激に劣化、消耗する。As engine oil is used, the detergent/dispersant is affected by heat, moisture, acidic substances, metal powder due to wear, etc., and gradually or rapidly deteriorates and wears out.
その劣化、消耗の程度を常に把握することがエンジンの
正常な運転を保持するのに重要であり、全塩基価を測定
することが有効な手段となる。特にいおうを多量に営む
燃料を使用する船舶用エンジンにおいては一層重要であ
る。It is important to constantly understand the degree of deterioration and wear to maintain normal engine operation, and measuring the total base number is an effective means. This is particularly important in marine engines that use fuel containing a large amount of sulfur.
全塩基価を測定する方法としてはＪ Ｉ Ｓ Ｋ ２５
０１ ［石油製品中和価試験方法］がある。JIS K 25 is a method for measuring total base number.
01 [Petroleum product neutralization value testing method].
しかしながらこの方法は十分に整備された測定機器と熟
練した試験員を要するため潤滑油□の使用場所で誰でも
手軽にできるとい・うもの、ではない。とりわけ船舶に
おいては長期にわ１ ′ ・
たって海上を航海する事から、潤滑油に対す→諭確な判
定をその場で行なう方法が必要とされる。However, this method requires well-equipped measuring equipment and experienced testers, so it is not something that anyone can easily perform at a location where lubricating oil □ is used. In particular, since ships travel on the sea for long periods of time, a method is needed to make accurate judgments about lubricating oil on the spot.
それに対し簡易的；こ全塩基価を測定する方法が幾つか
提案されているが、定量性の高いものとして０１〜Ｃ３
アルコール水溶液に無機中性塩、混合指示薬を加えた溶
液に一等量の試料潤滑油を加えて、溶液中にアルカリ性
成分を抽出さぜ、その呈□色で全塩基価を判定する方法
（特公昭４５′−２０２３６′）があった。この方法は
それまでの例えば特公昭３６−５６９９ ＋と開示され
ているスポットテストよる定性的方法と比べると定量性
を持たぜた点ですぐれた方法といえるが、試料油の量が
多いためしばしば溶液と試料油とが分離しにくいという
欠点が見られた。On the other hand, several methods have been proposed for measuring the total base number, but 01 to C3 are highly quantitative.
A method of adding an equivalent amount of sample lubricating oil to an aqueous alcohol solution, adding an inorganic neutral salt, and a mixed indicator, extracting the alkaline components from the solution, and determining the total base number based on its color (special method). Kosho 45'-20236'). This method can be said to be superior in that it has quantitative properties compared to the previous qualitative method using a spot test disclosed in Japanese Patent Publication No. 36-5699 +, but because of the large amount of sample oil, it is often A drawback was found that it was difficult to separate the solution and sample oil.
そこで本発明者等は鋭意検討の結果特定の希釈溶剤と抽
出溶剤を組合せさらに特定の解丸化剤を特定割合加える
事で希釈溶剤と抽出溶剤の分離性が非常に改善されるこ
とを晶し本発明に至ったものである。As a result of intensive studies, the present inventors have found that by combining a specific diluent and extraction solvent and adding a specific de-balling agent in a specific proportion, the separability of the dilution solvent and extraction solvent can be greatly improved. This led to the present invention.
類似のものとして特公昭５ ０ − ３ ６ １ ９
３が提案されているが、これに開示されてい．る方法で
は陸上ディーゼルエンジン油あるいは最近の舶用トラン
クピストンエンジン油のように、塩基性清浄分散剤の他
に、無灰系分散剤を含んでいる潤滑油使用油、あるいは
長期間使用して劣化が激しい使用油に適用した場合、下
層の抽出層と上層の希釈層の分離が困難になることが見
い出された。また混合指示薬を溶解するものとしてアル
コールが用いられているが、指示薬の一部には溶解性の
低いものがあり、低温で保存するとその一部が析出する
という欠点も見られた。As a similar example, the Special Public Interest Publications 50-3619
3 has been proposed, but it is not disclosed in this. In this method, lubricating oils that contain ashless dispersants in addition to basic detergent dispersants, such as land diesel engine oil or recent marine trunk piston engine oils, or lubricating oils that deteriorate after long-term use are used. It has been found that when applied to heavily used oils, it becomes difficult to separate the lower extraction layer and the upper dilution layer. Alcohol is also used to dissolve mixed indicators, but some indicators have low solubility, and some of them precipitate when stored at low temperatures.
本発明はこれらの欠点を克服し、これまでの方法では分
離困難であった試料の場合でもすみやかに分離判定でき
る簡易全塩基価測定用試薬及び溶剤を提供するものであ
る。The present invention overcomes these drawbacks and provides a simple reagent and solvent for measuring total base number that can be used to quickly separate and determine even samples that are difficult to separate using conventional methods.
本発明はへの抽出溶剤．と希釈溶剤とより構成される。The present invention is an extraction solvent. and a diluting solvent.
抽出溶剤
（１）溶媒
ジメチルスルフオギソドの２０〜８０容量チ水溶液
（２）指示薬
水溶液中のＰ Ｒ変色域がＰ Ｉ−Ｉ ：３〜１１まで
、のもので、これらを１種あるいは２種以上混合して任
意のＰ 、、、］−Ｉで変色できるよ・う調製したもの
であり、例えば、フェノール１／ツド、クレゾールレツ
．ド、ブロムフェノールブルーなどがあげられる。添加
量は抽出溶剤中に０００１〜０．１重量係である。Extraction solvent (1) A 20 to 80 volume aqueous solution of dimethyl sulfogisodine (2) An aqueous indicator solution with a PR discoloration range of P I-I: 3 to 11, and one or two of these It is prepared so that it can change color with any P,...]-I by mixing more than one species, for example, phenol 1/T, cresol. and bromophenol blue. The amount added is 0.0001 to 0.1% by weight in the extraction solvent.
（３）無機中性塩
抽出溶剤と希釈溶剤の分離を良好なものとするために中
性の無機塩を１〜２０重量係好ましくは１〜１０重量％
加える。無機中性塩の例としては塩化カリウム、塩化す
１・リウムがあげられる。 □・： ・（４）酸
試薬
潤滑油中の全塩基価は舶用エンジン油に限ってもシステ
ム油の全塩基価１ｍ□ｇ’ Ｋ ＯＩ−Ｉ／ｇからトラ
ンクビス１〜ン機関用泊め４０ｍ １１ Ｋ、 ０１−
Ｉ ／ ｇまで幅があり、一方、□試薬の変色するＰＩ
３は一定であるため抽出溶剤中のＰ Ｉ−Ｉを調整し、
広範囲の全塩基価を測定できるように酸試薬を必要に応
じて加える。酸としては、塩酸、硫酸、過塩素酸などを
用いる事ができる。(3) Inorganic neutral salt In order to achieve good separation between the extraction solvent and the diluting solvent, 1 to 20% by weight, preferably 1 to 10% by weight, of a neutral inorganic salt is added.
Add. Examples of inorganic neutral salts include potassium chloride and monolithium chloride. □・: ・(4) Acid reagent The total base number in lubricating oil is limited to marine engine oil, but the total base number of system oil is 1 m□g' KOI-I/g to trunk screw 1 to 40 m for trunk engine. 11K, 01-
There is a range of up to I/g, while □ reagent color change PI
Since 3 is constant, adjust P I-I in the extraction solvent,
Acid reagents are added as needed to allow measurement of a wide range of total base numbers. As the acid, hydrochloric acid, sulfuric acid, perchloric acid, etc. can be used.
希釈溶剤 ：
（１）溶媒
抽出溶剤より庇重が′軽く、潤滑油試料を容易に溶解で
きる有機□炭化水素溶剤、含塩素系溶剤及び含酸素系溶
剤の中から選ばれた１種または２種以上□を混合して用
いる。例としては、ｎニヘキサン、１−塩化ブタン塩化
アミルなどがあげられる。Diluent solvent: (1) One or two types selected from organic hydrocarbon solvents, chlorinated solvents, and oxygenated solvents that have a lighter weight than solvent extraction solvents and can easily dissolve lubricating oil samples. A mixture of the above □ is used. Examples include n-nihexane, 1-butane chloride, amyl chloride, and the like.
（２）Ｍ乳化剤
アルキルフェノールにポリオキシエチレンを６〜□１３
１毛ル丁好ｔしくは１ｏ〜「２モル刊加ぎせた非イオン
界面活性剤を抽出浴□剤と希釈溶□剤□とめ解乳化済１
ｊとして使用する使用量は′希釈溶剤中１・とｏ、１〜
巨重量係、□好ましぐは２〜５重量ヴである。(2) Add polyoxyethylene to M emulsifier alkylphenol from 6 to □13
Preferably 1 to 2 moles of nonionic surfactant are added to the extraction bath □ agent and diluted with □ agent □ and demulsified.
The amount used as j is '1 and o in diluting solvent, 1~
Huge weight, preferably 2 to 5 weight.
全塩基価判定方法
以上□の抽出溶剤と希釈溶剤とをそれぞれ等量ずつ栓付
試験管に採取する。次に測定すべき試料油を小さなガラ
ス棒などで、−滴ずつ滴下する。試験管をよく振とうし
、静の、試料油の滴下数から全塩基価を判定する。Method for Determining Total Base Number Collect equal amounts of each of the extraction solvent and dilution solvent in the above □ into test tubes with stoppers. Next, drop the sample oil to be measured drop by drop using a small glass rod or the like. Shake the test tube well and determine the total base number from the number of drops of sample oil.
この方法で判定される全塩基価：ま全て、Ｉ■５Ｋ２５
ｏ１の過塩素酸法の値との相関を有するが、塩酸法との
相関について表示することも不可能ではない。Total base number determined by this method: All, I■5K25
There is a correlation with the perchloric acid method value of o1, but it is not impossible to display the correlation with the hydrochloric acid method.
”−１−
また試料−滴の量を多くすれば概略の値が得られ、少な
くすればより詳細な値が得られる。なお得られる全塩基
価の値はその範囲として示される。すなわち試：料油の
全塩基価が２０ ｍ ｇ Ｉ＜ ＯＨ”／ ｊｌのと□
き、１滴加える事で抽出層が呈悪変化する□ように溶剤
を調製した時、未知の試料を分：、析して１滴で色が変
化したとすすると、その：試料油の全塩基価は２０．
ｍ 、ｙＫｌ、’、ＯＩ−Ｔ ／ ９以上である。"-1- Also, if you increase the amount of sample droplets, you can get a rough value, and if you decrease it, you can get more detailed values. The total base number value obtained is shown as a range. That is, sample: If the total base number of the feedstock oil is 20 mg I< OH”/jl□
When a solvent is prepared in such a way that the addition of one drop causes a change in the extraction layer, if an unknown sample is analyzed and the color changes with just one drop, then all of the sample oil Base number is 20.
m, yKl,′, OI-T/9 or higher.
従って２滴で色が変トれば１’Ｏ〜２０ｍ、！ｉｔＫ
ＯＴ（／ 、９ 、３滴で些、が変化すれば１．６．７
〜１０ｍｇＫＯＨ／、ｌ！と判定できる。Therefore, if the color changes with 2 drops, it will be 1'O ~ 20m! itK
If OT(/, 9, trivial, changes with 3 drops, 1.6.7
~10mgKOH/, l! It can be determined that
ここで試料油−滴の量をもつと小さくすれば、さらにそ
の範囲を狭める事ができ、より正確な値が得ら□れる。If the amount of sample oil droplets is reduced, the range can be further narrowed and a more accurate value can be obtained.
この方法の抽出溶剤中に使用したジメチルスルフオキシ
ドは、、・溶□解性のよい無害の溶媒として知られてお
り、アルコニル系溶媒には溶けにくい指示薬（例えばメ
チルレッド）も容易にしかも安定に溶解させ置市が ８
−
できる。The dimethyl sulfoxide used in the extraction solvent for this method is known as a harmless solvent with good solubility, and it can easily and stably handle indicators that are difficult to dissolve in alconyl solvents (e.g. methyl red). It was dissolved in 8
− I can.
従来の抽出溶剤と希釈溶剤だけでは分離が困難で全塩基
□価の判定に時間がかかったが、分離を□良くする手段
として解乳化剤を検討し、非イオン系界面活性剤が有□
効である事を見い出した。非イオン系界面活性剤の中で
もアルキルフェノールボリオギソエチレン付加物が最も
有効であり、例えば、ノニルフェノールポリオキシエチ
ｌ／ン伺加物、オクヂルフエノ・−ルポリオキツエヂレ
ン付加物があげられ、オキンエチレン付力１モル数は６
〜１；３モ□ル、□好ましくは１０〜１２モルの物□が
最□適である。Separation was difficult with conventional extraction solvents and dilution solvents, and it took time to determine the total base value, but we considered demulsifiers as a means to improve separation, and found that nonionic surfactants were effective.
I found that it was effective. Among nonionic surfactants, alkylphenol polyoxyethylene adducts are the most effective, such as nonylphenol polyoxyethyl l/ene adducts, oxalphenol polyoxyethylene adducts, and oxyethylene adducts. 1 mole is 6
~1;3 mol □, □preferably 10 to 12 mol □ is most suitable.
こレラ□の化合物はアルキルフェノールにポリオキシエ
チレンを、アルカリ性触媒を用いて縮合させて製造し、
最終工程でこのアルカリを中和するために酸を用いてい
る。The compound of Cholera□ is produced by condensing alkylphenol with polyoxyethylene using an alkaline catalyst.
An acid is used in the final step to neutralize this alkali.
この酸は炭酸などの弱酸を用いるより、塩酸などの強酸
を用いる方が解乳化剤として優れた効果を発揮するもの
が得られ本用途に有効である事も同時に見い出した。It has also been found that using a strong acid such as hydrochloric acid is more effective as a demulsifier than using a weak acid such as carbonic acid, and is therefore more effective for this purpose.
以上の様に調製した簡易測定用組成物を用いる事により
、潤滑油の使用現場で、迅速にしかも簡単に全塩基価（
Ｊ Ｉ ５Ｉ（２５０１過塩素酸法）を測定する事が可
能となり、使用油の劣化状況を適確に判断できる。By using the composition for simple measurement prepared as described above, it is possible to quickly and easily measure the total base number (
It becomes possible to measure J I 5I (2501 perchloric acid method), and the deterioration status of the oil used can be accurately determined.
従って本方法は潤滑油の管理上非常に有用な方法を提供
するものである。Therefore, this method provides a very useful method for lubricant management.
以下に実施例をあげて具体的に説明するが、本発明の実
施態様はこれらの実施例に限定されるものではない。Examples will be specifically described below, but the embodiments of the present invention are not limited to these examples.
実施例１゜ 試薬の調製 抽出溶剤と希釈溶剤を下記のように調製する。Example 1゜ Preparation of reagents The extraction solvent and dilution solvent are prepared as follows.
（１）抽出溶剤
フェノールレッド４ｍｇ、ブロムチモールブルー２ｍｇ
をジメチルスルフオキシド４０ ｍＡに溶解させ、そこ
に蒸留水５５ｍＡに塩化カリウム５ｇを溶解させた水溶
液を攪拌しながら加え１．最後に１／１、ＯＮ塩酸を加
え、Ｐ Ｉ（、３，４に調製する□ この時必要な１／
］ （Ｉｌｌ Ｎ塩酸は理論的には］、、 ５２ ｍ、
Ｌである。(1) Extraction solvent phenol red 4mg, bromothymol blue 2mg
was dissolved in 40 mA of dimethyl sulfoxide, and an aqueous solution of 5 g of potassium chloride dissolved in 55 mA of distilled water was added thereto with stirring.1. Finally, add 1/1 ON hydrochloric acid and prepare to PI (, 3, 4) □ At this time, 1/1
] (Ill N hydrochloric acid is theoretically],, 52 m,
It is L.
（２）希釈溶剤
１−塩化ブクン］、ＯＯｍｔと、ノニルフ１／−ルホＩ
Ｊ ７１−キンエチレン１０モル°伺加物５ｇを常温に
て攪拌、混合する。(2) Diluent solvent 1-Bukun chloride], OOmt, and Nonilph 1/-Rufo I
J 71-10 moles of ethylene and 5 g of additives were stirred and mixed at room temperature.
実施例２゜
測定方法
１０ｍＡの目盛付試験管に抽出溶剤３ｍｔをとり、次に
希釈溶剤３ｍｌをとる。試料。Example 2 Measurement method 3 mt of extraction solvent is placed in a 10 mA graduated test tube, and then 3 ml of dilution solvent is placed. sample.
油の全塩基価の大まかな値が知りたい時は、先端に直径
４ｍｍの球をもったガラス棒で試料油−滴を加え、栓・
をして試験管をよく振り、静置後、分離した下層の抽出
溶剤の色を観察する。変色していないときはこの操作を
続け、抽出溶剤の色が、黄色から黄橙色に変った時点で
の、試料油の滴下数から全塩基価を巾として読みとる。If you want to know the approximate value of the total base number of an oil, add a drop of sample oil with a glass rod with a 4 mm diameter ball at the tip, and use a stopper.
Shake the test tube well, let it stand, and then observe the color of the extracted solvent in the separated lower layer. If the color does not change, continue this operation, and when the color of the extraction solvent changes from yellow to yellow-orange, read the total base number as a range from the number of drops of sample oil.
滴下数と全塩基価の関係を第１表に示す。゛
さらに詳細な値を知りたい時は、内径０．６５ ｍ、ｍ
の針をつけた注射器で同様に滴下してゆきその滴下数か
ら全塩基価を求める事ができる。なおガラス棒−滴は平
均０．０３５ｇで内径Ｑ、 ５５ ｍｍの注射針をつけ
た注射器−滴の３倍の量である。Table 1 shows the relationship between the number of drops and the total base number.゛If you want to know more detailed values, please refer to the inner diameter of 0.65 m, m
The total base number can be calculated from the number of drops by using a syringe fitted with a needle. The glass rod drop weighs 0.035 g on average, which is three times the amount of the drop from a syringe equipped with a 55 mm inner diameter Q needle.
また、抽出溶剤を２ｍＡｚ希釈溶剤を３ｍｔとると、希
釈溶剤中の酸の量が減少するので判定される全塩基価の
値の巾も異なってくる。第２表に抽出溶剤を２ｍｔ採取
した場合の滴下数と全塩基価の関係を示すが、第１表と
併用する事により全塩基価の値をより狭い範囲で知る事
ができる。Furthermore, when the extraction solvent is 2 mAz and the dilution solvent is 3 mt, the amount of acid in the dilution solvent decreases, so the range of the determined total base number value also changes. Table 2 shows the relationship between the number of drops and the total base number when 2 mt of extraction solvent is collected, but by using it in conjunction with Table 1, the value of the total base number can be determined in a narrower range.
−１５−
測定結果、・・、、・ 、 、 ・ 、 ・
・上記実施例１．で調製した測定、用組成物を用いて・
、、実１施例２４．の測定方法に、従って実際にエンジ
ンで使用されたエンジン油の全塩基価の測定結果をＪＩ
ＳＫ２５０１過塩□素酸法の□値と比″ｉし□て第３表
云び第４表に示す霞、１
。-15- Measurement results...
・Above Example 1. For measurement, using the composition prepared in
,,Example 1 Example 24. According to the measurement method of JI, the total base number measurement result of the engine oil actually used in the engine is
SK2501 persalt □ Hydrogen acid method □ value and ratio "i" □ The haze shown in Table 3 and Table 4, 1
.
１
第３表は鯖用ディーゼルエンジン油使用油の結果であり
、第４表は陸用ディーゼルエンジン油使用油の結果を示
したものであるなお、全塩基価の判定は、抽出溶剤：３
ｍＡによる結果と、２ｍｔによる結果とから、より狭い
範囲の全塩基価を推定している。1 Table 3 shows the results for the diesel engine oil used for mackerel, and Table 4 shows the results for the land diesel engine oil used.The total base number is determined based on the extraction solvent: 3
The total base number is estimated in a narrower range from the mA results and the 2mt results.
１７−
−１６−
１８−
第３表、第４表の結果を見るに本発明による測定結果は
ＪＩＳＫ２５０１過塩素酸法による測定結果といずれも
よい一致を示しており、本発明の方法が優れた簡易分析
法である事を示している。17- -16- 18- Looking at the results in Tables 3 and 4, the measurement results according to the present invention are in good agreement with the measurement results according to the JIS K2501 perchloric acid method, indicating that the method of the present invention is superior. This shows that it is a simple analysis method.
特許出願人 三菱石油株式会社
（他１名）
１０−
手続補正書（方式）
％式％
１、事件の表示
昭和５７年特許願第１．６４．９ ’８５号２ 発明の
名称 ：
潤滑油の全塩基価簡易測定用組成物
３、補正をする者
事件との関係 特許出願人
東京都港区虎ノ門−丁目２番４号
（５９９）三菱石油株式会社
４、代理人
〒２１０ 神奈川県川崎市川崎区扇町４−１三菱石油株
式会社研究所管理部内
（電話 ０４４−：う４４−１．１．４１ ）７、補正
の内容
第１表ないし第４表の枠線がボールモノ書きであるもの
を墨書きに補正（内容に変更なし）。Patent applicant: Mitsubishi Oil Corporation (1 other person) 10- Procedural amendment (method) % formula % 1. Indication of case 1985 Patent Application No. 1.64.9 '85 2 Title of invention: Lubricating oil Composition for Simple Measurement of Total Base Number 3, Relationship with the Amendment Case Patent applicant: 2-4 Toranomon-chome, Minato-ku, Tokyo (599) Mitsubishi Oil Corporation 4, Agent: Kawasaki, Kawasaki City, Kanagawa Prefecture 210 Mitsubishi Oil Corporation Research Institute Management Department, 4-1 Ogimachi, Ward (Tel: 044-: U44-1.1.41) 7. Contents of the amendments The frame lines in Tables 1 to 4 are written in ball letters. Corrected to black writing (no change in content).
８、添付書類の目録 訂正済の第１表ないし第６表。8. List of attached documents Revised Tables 1 to 6.
以上 １−that's all 1-
Claims (1)
液に変色域Ｐ Ｉ−Ｉ ３〜１１のＰ Ｉ−１指示薬１
種・または２種以上をｏ、ｏ、ｏｉ〜０．１重量′チと
無機中性塩１〜２０重量係、さらに酸試薬を加えた抽出
溶剤（Ａ）と、この溶剤（Ａ）より低比重であって試料
潤滑油を溶解’Ｌ； ’ｌ’る有機炭化水素溶剤、含ハ
ロゲン系溶剤及び含酸素系溶剤の内から選ばれた１種ま
た□は２′種以上の混合物に、アルキルフェノ−□ル□
・ポリオキシエチレン付加物を０．１〜１０重□量チ加
え光希□釈溶剤（ＩＢ）とからなる潤滑油の全塩基価簡
易測定用組成物。 ′ □ （２）希釈溶剤（Ｂ）中のアルキルフェア ’＝ルポ□
リオキシエチレン付加物のオギソ°工升しソが６〜１３
モル付加してける事を特徴とする特許請求の囲（１）項
記載のｍｌ成物。 −（３）アルキルフェノールポリオ
キソエチレン□付加゛ 物は製造の際、最終工程の中和
□反応で使用ず−る□酸妄強酸□とする事を特徴とする
特許請求範□ 囲（１）項記載の組成物。 （４）含ハロゲン系溶剤が、塩化ブタン、塩化アミ□
ルである事を特徴とする特許請求範囲（３）項記載め植
成物。′ （５）酸試薬が塩酸、硫酸、過塩素酸などの強酸である
□事を特徴とする特許請求範囲（１）項記載の□ 組成
′：物。[Scope of Claims] (1) P I-1 indicator 1 in the discoloration range P I-I 3 to 11 in a 20 to 80 volume f% aqueous solution of dimethyl sulfoxide
An extraction solvent (A) containing a species or two or more species, o, o, oi to 0.1% by weight, an inorganic neutral salt 1 to 20% by weight, and an acid reagent, and an extraction solvent (A) containing an acid reagent. One type or a mixture of two or more types selected from organic hydrocarbon solvents, halogen-containing solvents, and oxygen-containing solvents that have specific gravity and dissolve the sample lubricating oil, Phenol□Ru□
- A composition for simple measurement of the total base number of lubricating oil, which comprises 0.1 to 10 weight squares of a polyoxyethylene adduct and a light dilution solvent (IB). ' □ (2) Alkyl faire in diluent solvent (B) ' = report □
The size of the lyoxyethylene adduct is 6 to 13.
ml composition according to claim (1), characterized in that molar addition is possible. - (3) Claims □ Item (1) characterized in that the alkylphenol polyoxoethylene □ adduct is □ acid depleted strong acid □ used in the final step neutralization □ reaction during production. Compositions as described. (4) The halogen-containing solvent is butane chloride, amyl chloride□
A plant according to claim (3), characterized in that the plant is (5) □ Composition': Product according to claim (1), characterized in that the acid reagent is a strong acid such as hydrochloric acid, sulfuric acid, or perchloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16498582A JPS5954964A (en) | 1982-09-24 | 1982-09-24 | Composition of handily measuring total base value in lubricating oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16498582A JPS5954964A (en) | 1982-09-24 | 1982-09-24 | Composition of handily measuring total base value in lubricating oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5954964A true JPS5954964A (en) | 1984-03-29 |
| JPH0373817B2 JPH0373817B2 (en) | 1991-11-25 |
Family
ID=15803638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16498582A Granted JPS5954964A (en) | 1982-09-24 | 1982-09-24 | Composition of handily measuring total base value in lubricating oil |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5954964A (en) |
-
1982
- 1982-09-24 JP JP16498582A patent/JPS5954964A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0373817B2 (en) | 1991-11-25 |
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