JPS5862559A - Simple measurement of total base in internal-combustion engine lubricant - Google Patents
Simple measurement of total base in internal-combustion engine lubricantInfo
- Publication number
- JPS5862559A JPS5862559A JP16232681A JP16232681A JPS5862559A JP S5862559 A JPS5862559 A JP S5862559A JP 16232681 A JP16232681 A JP 16232681A JP 16232681 A JP16232681 A JP 16232681A JP S5862559 A JPS5862559 A JP S5862559A
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- indicator
- total base
- base number
- liquid
- 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
- 238000002485 combustion reaction Methods 0.000 title claims description 20
- 238000005259 measurement Methods 0.000 title description 5
- 239000010705 motor oil Substances 0.000 title 1
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 239000010687 lubricating oil Substances 0.000 claims description 23
- 230000003472 neutralizing effect Effects 0.000 claims description 19
- 238000006386 neutralization reaction Methods 0.000 claims description 14
- 125000004432 carbon atom Chemical group C* 0.000 claims description 11
- 125000001931 aliphatic group Chemical group 0.000 claims description 8
- 238000002845 discoloration Methods 0.000 claims description 5
- 239000002736 nonionic surfactant Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 abstract description 7
- 239000007793 ph indicator Substances 0.000 abstract description 2
- 239000000314 lubricant Substances 0.000 abstract 2
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 abstract 1
- 229940005991 chloric acid Drugs 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 8
- 239000003921 oil Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000006866 deterioration Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- -1 sorbitan fatty acid Chemical class 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- PRZSXZWFJHEZBJ-UHFFFAOYSA-N thymol blue Chemical compound C1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=CC(O)=C(C(C)C)C=2)C)=C1C PRZSXZWFJHEZBJ-UHFFFAOYSA-N 0.000 description 3
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 229920001214 Polysorbate 60 Polymers 0.000 description 2
- 239000004147 Sorbitan trioleate Substances 0.000 description 2
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000013040 bath agent Substances 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 235000019252 potassium sulphite Nutrition 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- 235000019337 sorbitan trioleate Nutrition 0.000 description 2
- 229960000391 sorbitan trioleate Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- JCZPMGDSEAFWDY-SQOUGZDYSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanamide Chemical compound NC(=O)[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO JCZPMGDSEAFWDY-SQOUGZDYSA-N 0.000 description 1
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920001213 Polysorbate 20 Polymers 0.000 description 1
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 description 1
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- IJCWFDPJFXGQBN-RYNSOKOISA-N [(2R)-2-[(2R,3R,4S)-4-hydroxy-3-octadecanoyloxyoxolan-2-yl]-2-octadecanoyloxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCCCCCCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCCCCCCCCCCCC IJCWFDPJFXGQBN-RYNSOKOISA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010710 diesel engine oil Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L magnesium sulphate Substances [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 235000011071 sorbitan monopalmitate Nutrition 0.000 description 1
- 239000001570 sorbitan monopalmitate Substances 0.000 description 1
- 229940031953 sorbitan monopalmitate Drugs 0.000 description 1
- 239000001587 sorbitan monostearate Substances 0.000 description 1
- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 0.000 description 1
- 239000001589 sorbitan tristearate Substances 0.000 description 1
- 235000011078 sorbitan tristearate Nutrition 0.000 description 1
- 229960004129 sorbitan tristearate Drugs 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000010913 used oil Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000008096 xylene Substances 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
本発明は内燃威関潤滑油、特に舶用内燃機関用潤滑油の
全塩基価を簡易、迅速に測定するノJ法に関するもので
ある。
内燃機関用潤滑油は使用時間と共に燃料中Vこ存在する
硫黄分の燃焼生成物および空気中の窒素酸化物が燃焼室
より混入して強酸を生ずるためにtす]Iiさノし、生
成した強酸はピストンリング、/リンダーライナーおよ
び軸受等を摩耗損傷せしめる原因となる1゜
’1.!+に、セミディーゼル機関を含む舶用ディーゼ
ル1筬関の軸受の損傷は、−塵発生するとたとえそJt
が軽度であっても確実に進行し、最後には暖間を停止し
なくてはならない状態にまで進行(7、延いでは海上事
故につながり、jpに経済的損失にととまらず人命事故
にもつながる問題に発展するり能性がある。
一般に内燃機関用潤滑油中には、これら」二連の問題を
回避するために生成する酸を中和する塩基性物質が含ま
れており、したがってこの塩基性物質の量つまり全塩基
価が内燃機関用潤滑油の劣化程度を判定する重要な指標
の一つとなる。
通常、内燃機関用潤滑油の全塩基価を測定する方法とし
て、日本工業規格の石油製品中和価試験方法の全塩基価
及び強塩基側試験方法(、Tl5K2501、5 、2
)の中の塩酸法(J工S K2SO3、5。
2.2)や過塩素酸法(J工S K2SO3,5,2,
3)などの電位差滴定法が用いられている。しかしこれ
らの方法はかなりの熟練度を必要とするため誰にでも簡
単に測定できるものではなく、また複雑な測定機器を必
要とし、特に後者の方法では有害ガスを発生する過塩素
酸を使用人るため、現場で測定することは困難であり、
従来、使用油をそれぞれの試験室に持ち帰り、上記方法
に準拠してその全塩基価を測定してきた。
L7かしながら、4″11滑油使用者にとっては現在使
用している油の劣化状態をjE’、 (i+7−に知る
ことが心安であり、したがって日常のff7j滑油管理
に適月1でき、4″lj滑油の使用現場で誰もが簡単に
行うことができる潤滑油の正確な全塩基価の測定方法の
開発が望−ま7t1ていた。このことは特に長ル1間に
わたって陸地との接触を持゛たない船舶の内燃機関用潤
滑油を管理していくうえでは切火な問題であった。11
11−米、この目的のために開発さ第1たI′I^if
?油の劣化状態を判定する簡易な試験方法としては特公
昭133−.1249号、特公昭3[1−2096号お
よび特公昭31i −5+)4141号などに聞手され
ているスポットテストが翔られている3、シかしながら
これらの方法し1あるもの(・1実施不能であり、ある
ものはスポットの色別がイ・明確で、またスポットのに
じみが出るなどの実+11−にの欠陥があった。また特
公昭5[1−:36193号にはチューブテストによる
測定方法が開示さiしているが、上記方法も含めて、こ
れらの方法はいずれも潤滑油の劣化程度を指示薬の呈色
により判断するため全塩基価の正確な値をもとめること
にできず、しかも測定結果にかなりの個人差が出るもの
であった。さらに特公昭49−18837号ではスポッ
トテストでのスポットの発色同心円の幅により潤滑油の
塩基価をもとめる方法が開示されているが、塩基価をも
とめるのに約刃分という長い時間を要し、しかも依然と
して全塩基価を幅としてしか把握できず、正確な値をも
とめることはできなかった。しかもここにあげた方法は
いずれもJISK2501.5.2.2の塩酸法に規定
する全塩基価に対応するものであり、J工5K2501
.5.2.3の過塩素酸法に規定する全塩基価に対応す
るものではなかった。
そこで本発明者らは上記の問題点を解決するために研究
を重ねた結果、本発明を完成するにいたった。
本発明はJ工5K2501 、5.2.3に規定する′
Ii1.位差滴定法(過塩素酸法)に相当する全塩基価
を、分析時に場所をとらず、現場で短時間にかつ171
)単に測定する方法を提供することを目的とする。
すなわち、本発明は内燃機関用潤滑油試料、し1〕M削
および[n)指示薬液を試験管に採取し、さらに+++
g中和液を加えてスポットテストにより中和点を’Fi
l断し、その中和点に達する1でに要したLIIIJ中
和液の液量より試料の塩基価をもとめる方法において、
〔1〕溶剤、[1)]指示薬液および(III)中和t
1kがそれぞれ
11〕溶 剤:(1)炭素数6〜8の芳香族炭化水素(
2)炭素数5以下の脂肪jM 1価アルコール←←張、
および
(3)水
+−++ j 指示薬液: (1) h記溶剤、(2)
水中でのpH変色域が1.0〜:3.OであるpH4W
示薬(叫〜2.0 +−(1: +1i’、係、および
(3)非イオン界面活性剤1〜1()東+、i。
条
[111J中和液:(I)塩酸、および(2)炭素数5
以下の脂肪族111Iliアルコール
なる組成を有することを特徴とする内燃機関用1174
滑油の全塩基価簡易測定方法を提供するものである。
以下、本発明による内燃機関用潤滑油の全塩基価簡易測
定方法についてより具体的に説明する。
本発明でいう[1)溶剤は測定試料である内燃機関用潤
滑油もしくはその潤滑油中のスラッジを溶解もしくは分
散により希釈して測定操作を容易にするとともに、滴定
液との接触効率を高め、潤滑油中の塩基成分と塩酸溶液
との中和反応を円滑に行わせるだめのものであり、これ
は(1)炭素数6〜8の芳香族炭化水素、(2)炭素数
5以下の脂肪族アルコールおよび(3)水よりなる混合
溶剤である。
(1)の炭素数6〜8の芳香族炭化水素としては、例エ
バベンゼン、トルエン、キシレン、エチルベンゼンおよ
びそれらの混合物などがあげられるが、特にトルエンが
好ましい。また(2)の炭素数5以下の脂肪族1価アル
コールとしては例えばメチルア、x :+ −7t、、
エチャア、、ヨーヤ、。−17”0/ぐノー21、イン
プロパツール、n−ブタノール、インブタノール、n−
アミルアルコール、インアミルアルコールおよびそれら
の混合物などがあげられるが、特にイソゾロ・ぐノール
が好ましい。
(1)、(2)および(3)の混合割合は任意であるが
、(1)=20〜80容量部、(2):Δ)〜80容敏
容量よび(3) :0.]〜5.0容量部よりなる混合
溶剤であることが好まThe present invention relates to a method for simply and quickly measuring the total base number of lubricating oils for internal combustion engines, particularly lubricating oils for marine internal combustion engines. As lubricating oil for internal combustion engines is used over time, combustion products containing sulfur present in the fuel and nitrogen oxides in the air enter the combustion chamber and form strong acids. Strong acids can cause wear and damage to piston rings, cylinder liners, bearings, etc. ! In addition, damage to the bearings of marine diesel engines, including semi-diesel engines, can occur even if dust is generated.
Even if the damage is mild, it will surely progress, and eventually it will progress to a state where warming has to be stopped. In general, lubricating oils for internal combustion engines contain basic substances that neutralize the acids produced to avoid these two problems. The amount of basic substances, or the total base number, is one of the important indicators for determining the degree of deterioration of lubricating oil for internal combustion engines.The Japanese Industrial Standards are usually used to measure the total base number of lubricating oil for internal combustion engines. Total base number and strong base side test method of petroleum product neutralization number test method (Tl5K2501, 5, 2
) in the hydrochloric acid method (J Engineering S K2SO3, 5. 2.2) and perchloric acid method (J Engineering S K2SO3, 5, 2,
Potentiometric titration methods such as 3) are used. However, these methods require considerable skill and cannot be easily measured by anyone, and they also require complicated measuring equipment, and the latter method in particular does not require workers to use perchloric acid, which generates harmful gases. It is difficult to measure on-site due to
Conventionally, oils used have been taken back to their respective testing laboratories and their total base number has been measured in accordance with the above method. However, for users of 4"11 lubricating oil, it is reassuring to know the deterioration state of the oil they are currently using, and therefore it is important to know the deterioration state of the oil they are currently using, and therefore, it is convenient for daily ff7j lubricating oil management. It was desired to develop a method for accurately measuring the total base number of lubricating oil that could be easily carried out by anyone at the site where 4" lj lubricating oil is used. This was a serious problem in managing lubricating oil for ships' internal combustion engines, which do not have contact with ships.11
11 - America, the first I'I^if developed for this purpose
? A simple test method for determining the state of oil deterioration is described in Japanese Patent Publication No. 133-. 1249, Special Publication No. 3 [1-2096 and Special Publication No. 31i-5+) No. 4141, etc.3, but there are some of these methods (・1 In some cases, the color separation of the spots was clear, and in some cases, there were actual defects such as blurring of the spots.In addition, the tube test was not carried out in Tokuko Sho 5 [1-: 36193]. However, all of these methods, including the above method, cannot determine the exact value of the total base number because the degree of deterioration of the lubricating oil is determined by the coloration of the indicator. Moreover, there were considerable individual differences in the measurement results.Furthermore, Japanese Patent Publication No. 18837/1983 discloses a method for determining the base number of a lubricating oil based on the width of the coloring concentric circles of a spot in a spot test. However, it took a long time, about a knife's length, to determine the base number, and the total base number could still only be understood as a range, making it impossible to determine an accurate value.Furthermore, none of the methods listed here It corresponds to the total base number specified in the hydrochloric acid method of JISK2501.5.2.2, and is JISK2501.5K2501.
.. It did not correspond to the total base number specified in the perchloric acid method in 5.2.3. Therefore, the present inventors conducted repeated research to solve the above problems, and as a result, completed the present invention. The present invention is defined in J Engineering 5K2501, 5.2.3'
Ii1. The total base number, which is equivalent to the potentiometric titration method (perchloric acid method), can be determined in a short time on-site without taking up much space during analysis.
) is simply intended to provide a way to measure. That is, the present invention collects a lubricating oil sample for an internal combustion engine, 1) M cutting and [n) indicator liquid in a test tube, and further +++
g Add neutralizing solution and check the neutralization point by spot test.
In the method of determining the base number of the sample from the amount of LIIIJ neutralizing solution required in step 1 to reach the neutralization point,
[1] Solvent, [1)] Indicator solution and (III) Neutralization
1k is 11 respectively] Solvent: (1) Aromatic hydrocarbon having 6 to 8 carbon atoms (
2) Fat with carbon number of 5 or less jM monohydric alcohol ←← Zhang,
and (3) water +-++ j indicator liquid: (1) h solvent, (2)
pH discoloration range in water is 1.0 to 3. pH4W which is O
Indicator (scream ~ 2.0 + - (1: +1i', and (3) Nonionic surfactant 1-1 () East +, i. Article [111J Neutralizing solution: (I) Hydrochloric acid, and (2) Number of carbons: 5
1174 for internal combustion engines characterized by having the following aliphatic 111Ili alcohol composition:
This provides a simple method for measuring the total base number of lubricating oil. Hereinafter, the method for simply measuring the total base number of lubricating oil for internal combustion engines according to the present invention will be explained in more detail. In the present invention, [1] the solvent dilutes the lubricating oil for internal combustion engines, which is the measurement sample, or the sludge in the lubricating oil by dissolving or dispersing it to facilitate the measurement operation, and also increases the contact efficiency with the titrant liquid. This is to facilitate the neutralization reaction between the base component in the lubricating oil and the hydrochloric acid solution, and it is composed of (1) aromatic hydrocarbons having 6 to 8 carbon atoms, and (2) fats having 5 or less carbon atoms. It is a mixed solvent consisting of a group alcohol and (3) water. Examples of the aromatic hydrocarbon having 6 to 8 carbon atoms (1) include evabenzene, toluene, xylene, ethylbenzene, and mixtures thereof, with toluene being particularly preferred. In addition, examples of the aliphatic monohydric alcohol having 5 or less carbon atoms in (2) include methyla, x: + -7t,
Echaa,, yoya. -17”0/Guno 21, Improper Tool, n-butanol, imbutanol, n-
Examples include amyl alcohol, in-amyl alcohol, and mixtures thereof, with isozolo-gnol being particularly preferred. The mixing ratio of (1), (2) and (3) is arbitrary, but (1) = 20 to 80 parts by volume, (2): Δ) to 80 parts by volume, and (3): 0. ] ~5.0 parts by volume of mixed solvent is preferred.
【7く、さらには(1)=40〜
6o容量部、(2) : 40−口答1□i部および(
3) : 0.3〜1.0容量部よりなる混合浴剤であ
ることがより好ましい。
また本発明でいう〔]〕指示薬液とは(1)上記浴剤、
(2)水中テノpH変色域が1.0〜3.0であるpH
指示薬0.1〜3.0車量チ、好1しくは1.0〜2.
0車量チおよび(3)非イオン界面活性剤1〜10東に
%、好ましくは13〜6重量%からなる混合溶液である
3、この(2)のpH変色域が1.0〜3.0であるp
H指示薬としては例えハメタニルエロー、チモールブル
ーおよヒトロベオリンOOなどがあげられるが、特にチ
モールブルーが好ましい。、また(3)の非イオン界面
活性剤と、″
してはエチレンオキサイド系、ジェタノールアミン系、
ソルビトール系、グルコシド、グルコンアミド系、グリ
セリン、グリシドール系その他の非イオン界面活性剤が
使用できるが、特にソルビタン脂肪酸部分エステル、ポ
リオキシエチレンソルビタン脂肪酸部分エステルエーテ
ル、例えばンルビタンモノラウレート、ソルビタンモノ
パルミテート、ソルビタンモノステアレート、ソルビタ
ンモノオレエート、ソルビタントリステアレート、ソル
ビタントリオレエート、ポリオキシエチレンソルビタン
モノラウレート、ポリオキシエチレンソルビタンモノ/
eルミテート、ホリオキシエチレンフルビタンモノステ
アレート為るいはトリステアレート、ポリオキシエチレ
ンソルビタンモノオレエートあるいはトリオレエートな
どが好ましい。
本発明においては上記〔l)溶剤と[0)指示薬液を内
燃機関用潤滑油試料に対して別々に加えてもよく、また
場合によってはあらかじめ両者を混合して保存しておき
、混合溶液の形で加えてもいっこうにさしつかえない。
さらに本発明でいう[111)中和液とは(1)塩酸お
よび(2)炭素数5以下の脂肪族1価アルコールからな
る塩酸溶液である。この(1)で使用する塩酸の濃度は
任意であるが、JISK8180に規定する含量が35
、(1〜37.0%の塩酸を使用することが好ましい1
゜(2)の炭素数5以下の脂肪族1価アルコールとして
はi1■記〔l)溶剤の説明において列挙したアルコー
ルが使用でき、また〔1〕溶剤の成分として使用するア
ルコールと同じでも異なっていてもよいが、同一である
ことが好ましい。そしてこの両者を混合した〔IN〕の
中和液の塩酸濃度も任意であるが、]14’l ’7に
の尚滑油の全塩基価の測定では0.10−0.15 m
定であることが好ましい。
次に本発明の方法にしたがって内燃機関用潤滑?li’
lの全塩基価を測定する方法を述べる。。
試峡管に一定駄好ましくは1rnlの試料を採取し、こ
れに一定敏好ましくは2 meの〔l〕浴剤と−’tt
+i女f−:E L <は0.5 meのCID指示
薬液を加え試験・θを倣しく振る。次にこれに〔■〕中
和液をA−’tpk加えて檄しく振盪した後、この混合
液を1滴スポット紙上に滴下して一定時間経過後スポッ
トのリングの色を見る。この色が塩基性色である時は、
さらに[+11.)中和液を加えて激しく振盪してスポ
ットテストを行い、同様の操作をスポットのリングの色
が中和色になるまで繰り返す。この際にあらかじめスポ
ットテストの結果が塩基性色、中和色、酸性色であるス
ポット紙を用意しておき、それを色の対照として用いれ
ば中和点の判断が容易である。
そして中和点に達するまでに要した[i[l)中和液の
液量より、計算もしくはあらかじめ作成しておいた対応
グラフを用いてJ工5K2501.5.2.3の規定に
相当する全塩基価を容易にもとめることができる。
なお、本発明の方法では、スポットテスト後にクリヤー
ラッカーをスポット紙に吹きつけることにより、スポッ
トテストの結果を変色なしに長期にわたって保存できる
という利点もある。
実施例
溶剤、指示薬液および中和液としてそれぞれ以下の組成
のものを使用した。
ml剤:)ルエン(資)容量部、イソプロ/IPノール
49.5容量部および水0.5容量部からなる混合溶剤
指示薬液:チモールブルー0.59およびソルビタンモ
ノラウレート2.0 ?を上記混合溶剤40 mlに溶
解させた溶液
中和液=35%塩酸18−とインゾロノeノール2tと
の混合溶液(規定度: 0.1030 )この溶剤、指
示薬液および中和液を用いて各種の舶用ディーゼルエン
ジン油試料についてその全塩基価を測定した。
−まず1〇−容量の試験管に試料1 meを採り、溶剤
4 nleと指示薬液0.5−を加えて加〜加抄間試験
管を激しく振った31次に中和液0.5mlを加えて試
験管を13分間激しく振盪した後、この液を1滴スデッ
ト紙上に滴下して3分間放置した。、3分後にスポット
紙上のスポットに中和色、すなわち薄桃色のリングが出
るかどうか観察し、この色が塩基性色、すなわち黄色の
ときはさらに中和液U、5 mJを加え振盪してスポラ
1トチストを行い、スポットのリングの色が中和色にな
るまでこの操作を繰り返した。
この中和点の判断は、あらかじめ用意した塩基性色、中
和色、酸性色を示しているスポットテスト結果と対照し
て行った。
こうして中和点に達するまでに加えた中和液の量と、J
IS K 2501 、5 、2’、 3に規定する計
算式を準用した次式により試料の全塩基価を9出した、
。
Br=x X O,1030X 56.1ここにBr:
全塩基価(qKOH/f/)X :中和点までに要しl
L中和液のfli:(4ne)0.1030 :使用し
た中和液の規定度本実施例の結果をJIS K 250
1.5.2.3に規定した方法により測定した全塩基価
と対比して次灸に示した。。
この実施例かられかるように、本発明の方法は、1.!
lLめで簡単かつ短時間に、しかも熟紳を“皮せずに内
1.<11i関川潤滑油の全塩基価を測定することがで
きるものであり、さらにその結果はJ、rSK25(+
1 。
5.2.3に規定する方法による1ゝ塩基洒と非常によ
く一致しており、使用油の性状チェック作業における省
力化、合理化の推進に大いに役立つものである。
特許出願人 日本石油株式会社
一丁 続ン會暑11t−=Lj
(U+ムin審査官 殿)昭和56
嘔f 特 il 願 第162326号;3.補11
をする者
氏名(名称>(444)11本イ]油株式会ン14、代
理人
(1所 東京都港1ス南青山−]l1IWt1号6、
補11の対象
明細書中「特−請求の範l」
1発明の詳細な説明Iの欄
7、補任の内容
(1)明りl書第1頁第4行目から同第2負第51j目
までの「特許請求のIf!IFIをJを別紙のとおりに
訂正する。
(2)明細書第6頁第13行目[0,1〜2.OJをr
O,1〜3.03 トKT’iEする。
(3)明細書第7頁第11行目「脂肪族」を「脂肪族−
価jと訂正する。
(4)明細書第12頁第10行目[4−1と1をr4
all、 J トUiEtル。
1゛2、特許請求の範囲
内燃機15El川釣消油試料、(1)溶剤おまぴ(U)
指承ik油を試験管に採取し、さら【こ[11)中和液
を加えてスポットテストにJ、り中和白を判断し、中和
点に達するまでに要した(III)中和液の液間より試
料の勉)、(価をもとめるyi法においで、II)溶剤
、(IT)指示#5液、l; 、1.σ(Ill)中和
液がそれぞれ〔1〕溶剤:(1)炭素数6へ・801”
、ft&炭化水系
(2)炭素数5以]・の脂肪族11111アル]−ル
(:う)水
(II ) JHHI3’lk :
(1)ト記溶剤
(2)水中での1】11変色域が1.0〜3.0である
P H指示薬
0.1〜3.0Φ品%、おJ、び
(:3)非イAンW面粘竹剤1・〜
10φ品%
(1)中和液:(1)塩酸、および
(2)炭素数5以下の脂肪族1
価アルコール
なる組成を有することを特徴とする内燃機関用潤滑油の
全塩基価簡易測定方法。[7, and even (1) = 40~
6o capacity part, (2): 40-Oral answer 1□i part and (
3): A mixed bath agent containing 0.3 to 1.0 parts by volume is more preferable. In the present invention, the indicator liquid refers to (1) the bath agent mentioned above;
(2) pH at which the pH color change range in water is 1.0 to 3.0
The indicator has a volume of 0.1 to 3.0, preferably 1.0 to 2.
(3) A mixed solution consisting of 1% to 10%, preferably 13% to 6% by weight of a nonionic surfactant, and (2) has a pH discoloration range of 1.0 to 3. p which is 0
Examples of the H indicator include hametanil yellow, thymol blue, and hytroveolin OO, with thymol blue being particularly preferred. , and the nonionic surfactant (3) is ethylene oxide type, jetanolamine type,
Sorbitol, glucoside, gluconamide, glycerin, glycidol and other nonionic surfactants can be used, in particular sorbitan fatty acid partial esters, polyoxyethylene sorbitan fatty acid partial ester ethers, such as nrubitan monolaurate, sorbitan monopalmi tate, sorbitan monostearate, sorbitan monooleate, sorbitan tristearate, sorbitan trioleate, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan mono/
Preferable examples include e-lumitate, polyoxyethylene fulvitan monostearate or tristearate, and polyoxyethylene sorbitan monooleate or trioleate. In the present invention, the above [l) solvent and [0] indicator liquid may be added separately to the lubricating oil sample for internal combustion engines, or in some cases, both may be mixed and stored in advance to form a mixed solution. Even if it is added in form, it is no problem at all. Furthermore, the [111) neutralizing solution in the present invention is a hydrochloric acid solution consisting of (1) hydrochloric acid and (2) an aliphatic monohydric alcohol having 5 or less carbon atoms. The concentration of hydrochloric acid used in this (1) is arbitrary, but the content specified in JISK8180 is 35
, (preferably using 1 to 37.0% hydrochloric acid 1
As the aliphatic monohydric alcohol having 5 or less carbon atoms in (2), the alcohols listed in the description of i1 ■ [l) solvent can be used, and the alcohols listed in [1] may be the same or different from the alcohol used as a component of the solvent. However, it is preferable that they be the same. The concentration of hydrochloric acid in the neutralized solution [IN] obtained by mixing both of them is also arbitrary, but in the measurement of the total base number of the lubricating oil in ]14'l'7, it was 0.10-0.15 m
Preferably, it is constant. Then lubrication for internal combustion engines according to the method of the invention? li'
A method for measuring the total base number of 1 will be described. . Collect a sample, preferably 1 rnl, into a test tube, and add a certain amount, preferably 2 me [l] of bath salt and -'tt.
+i Female f-: For E L <, add 0.5 me CID indicator solution and shake test θ in the same manner. Next, [■] Neutralizing solution A-'tpk is added to this and shaken gently. One drop of this mixed solution is dropped onto the spot paper and the color of the spot ring is observed after a certain period of time has elapsed. When this color is a basic color,
Furthermore [+11. ) Perform a spot test by adding neutralizing solution and shaking vigorously, and repeat the same operation until the color of the spot ring becomes the neutralized color. At this time, the neutralization point can be easily determined by preparing in advance spot paper whose spot test results are basic color, neutral color, and acid color, and using it as a color contrast. Then, from the amount of neutralizing solution [i[l] required to reach the neutralization point, the amount corresponding to the provisions of J Engineering 5K2501.5.2.3 can be calculated using a corresponding graph prepared in advance or calculated in advance. The total base number can be easily determined. The method of the present invention also has the advantage that by spraying a clear lacquer onto the spot paper after the spot test, the spot test results can be stored for a long period of time without discoloration. Example The following compositions were used as the solvent, indicator liquid, and neutralizing liquid, respectively. ml agent:) Mixed solvent indicator solution consisting of 1 part by volume of luene, 49.5 parts by volume of isopro/IPnol and 0.5 part by volume of water: Thymol blue 0.59 and sorbitan monolaurate 2.0? was dissolved in 40 ml of the above mixed solvent. Neutralized solution = mixed solution of 35% hydrochloric acid 18- and insolonol 2t (normality: 0.1030) Using this solvent, indicator solution and neutralizing solution, various The total base number of marine diesel engine oil samples was measured. - First, take sample 1me in a 10-capacity test tube, add 4 ml of solvent and 0.5 ml of indicator solution, and shake the test tube vigorously between addition and addition.Next, add 0.5 ml of neutralizing solution. In addition, the test tube was shaken vigorously for 13 minutes, and then one drop of this solution was placed on Sudet paper and left for 3 minutes. After 3 minutes, observe whether a neutralized color, that is, a pale pink ring appears on the spot on the spot paper, and if this color is a basic color, that is, yellow, add 5 mJ of neutralizing solution U and shake. Spora 1 spot was applied, and this operation was repeated until the color of the ring of the spot became a neutralized color. The neutralization point was determined by comparing with spot test results prepared in advance showing basic color, neutralized color, and acidic color. In this way, the amount of neutralizing solution added until reaching the neutralization point and J
The total base number of the sample was determined to be 9 using the following formula, which was applied mutatis mutandis to the calculation formula specified in IS K 2501, 5, 2', and 3.
. Br=x X O, 1030X 56.1 Br here:
Total base number (qKOH/f/)X: l required to reach neutralization point
fli of L neutralizing solution: (4ne) 0.1030: Normality of neutralizing solution used The results of this example are JIS K 250
The results are shown in the following table in comparison with the total base number measured by the method specified in 1.5.2.3. . As can be seen from this example, the method of the present invention includes: 1. !
It is possible to easily and quickly measure the total base number of 1.
1. The results are in very good agreement with the 1゜ base concentration obtained by the method specified in 5.2.3, and are of great help in promoting labor-saving and rationalization in the work of checking the properties of used oil. Patent Applicant Nippon Oil Co., Ltd. 11t-=Lj (U + Muin Examiner) 1982
Special Application No. 162326; 3. Supplement 11
Name of the person (Name > (444) 11 A) Oil Co., Ltd. 14, Agent (1 location, Minami Aoyama, Minami-Aoyama, Minato 1, Tokyo) 11 IWt No. 6,
Supplement 11 "Claims I" in the subject specification 1 Column 7 of Detailed Description of the Invention I, supplementary content (1) Explanation 1, page 1, line 4 to 2nd negative line 51j ``If!IFI of the patent claim is corrected as shown in the attached sheet. (2) Page 6, line 13 of the specification [0, 1 to 2.
O, 1-3.03 ToKT'iE. (3) On page 7, line 11 of the specification, “aliphatic” is replaced with “aliphatic-”
Correct it to value j. (4) Page 12, line 10 of the specification [4-1 and 1 are r4
all, J to UiEt le. 1.2. Claims Internal combustion engine 15El river fishing oil sample, (1) Solvent oil sample (U)
Collect the sampled ik oil in a test tube, add neutralizing liquid and conduct a spot test to determine whether it is neutralized or not, and determine the amount of neutralization required to reach the neutralization point (III) (In the yi method for determining the value of the sample from the liquid interval), (II) Solvent, (IT) Instruction #5 liquid, l; , 1. σ(Ill) Neutralizing liquid is [1] Solvent: (1) Carbon number is 6 and 801"
, ft & hydrocarbon system (2) carbon number of 5 or more] - aliphatic 11111 al]-l (:U) water (II) JHHI3'lk: (1) solvent (2) 1]11 discoloration area in water PH indicator with 1.0 to 3.0 0.1 to 3.0 Φ product%, OJ, bi (:3) non-I A W-face sticky bamboo agent 1 to 10 Φ product% (1) A simple method for measuring the total base number of a lubricating oil for an internal combustion engine, characterized in that it has a composition of: (1) hydrochloric acid, and (2) an aliphatic monohydric alcohol having 5 or less carbon atoms.
Claims (1)
液を試験管に採取し、さらに〔題〕中和液を加えてスポ
ットテストにより中和点を判−■し、中和点に達するま
でに袂した〔■〕中和液の液1.;:より試料の塩基価
をもとめる方法において、シl」溶剤、〔n〕指示薬液
およびCu1l))中和液がそれぞれ(1)溶剤;(1
)炭素数6〜8の芳香族炭化水素(2)炭素数5以下の
脂肪族1価アルコール (3)水 [1)指示薬液: (1)上記溶剤 (2)水中でのpH変色域が1.0〜3.0であるpH
指示薬0.1〜2.0■量チ、および (3)非イオン界面活性剤1〜1()重!什チ[110
中和液;(1)塩酸、および (2)炭素数5以下の脂肪族+ 1dtiアルコール なる組成を有することを特徴とする内燃機関用側、・け
油の全塩基価簡易測定方法。[Claims] Samples of lubricating oil for internal combustion engines, [1] solvent, and (1) indicator liquid are collected in test tubes, and [subject] neutralizing liquid is added to determine the neutralization point by a spot test. Then, add the neutralizing solution [■] until it reaches the neutralization point 1. ;: In the method of determining the base number of a sample from (1) solvent; (1) solvent;
) Aromatic hydrocarbon having 6 to 8 carbon atoms (2) Aliphatic monohydric alcohol having 5 or less carbon atoms (3) Water [1) Indicator liquid: (1) The above solvent (2) pH discoloration range in water is 1 pH between .0 and 3.0
Indicator: 0.1 to 2.0 mass, and (3) nonionic surfactant: 1 to 1 () mass! Tithe [110
A simple method for measuring the total base number of a neutralizing liquid for internal combustion engines, characterized by having a composition of (1) hydrochloric acid, and (2) aliphatic + 1 dti alcohol having 5 or less carbon atoms.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP16232681A JPS5862559A (en) | 1981-10-12 | 1981-10-12 | Simple measurement of total base in internal-combustion engine lubricant |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP16232681A JPS5862559A (en) | 1981-10-12 | 1981-10-12 | Simple measurement of total base in internal-combustion engine lubricant |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS5862559A true JPS5862559A (en) | 1983-04-14 |
JPH0131587B2 JPH0131587B2 (en) | 1989-06-27 |
Family
ID=15752404
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP16232681A Granted JPS5862559A (en) | 1981-10-12 | 1981-10-12 | Simple measurement of total base in internal-combustion engine lubricant |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5862559A (en) |
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US9829476B2 (en) | 2012-03-19 | 2017-11-28 | Yanmar | Measurement method and device, for determining degree of engine oil dilution by FAME |
US11081701B2 (en) | 2017-01-06 | 2021-08-03 | Waseda University | Secondary battery |
Families Citing this family (1)
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CN108226450A (en) * | 2017-12-29 | 2018-06-29 | 沪东重机有限公司 | Marine diesel lubricating oil detection method |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5576950A (en) * | 1978-11-17 | 1980-06-10 | Kyodo Sekiyu Kk | Agent for total basicity simplified measurement of lubricating oil |
-
1981
- 1981-10-12 JP JP16232681A patent/JPS5862559A/en active Granted
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5576950A (en) * | 1978-11-17 | 1980-06-10 | Kyodo Sekiyu Kk | Agent for total basicity simplified measurement of lubricating oil |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1239281A3 (en) * | 2001-03-09 | 2003-08-13 | Schmack Biogas GmbH | Rapid test for detecting acidic or alkaline components in oils |
US9829476B2 (en) | 2012-03-19 | 2017-11-28 | Yanmar | Measurement method and device, for determining degree of engine oil dilution by FAME |
US9778242B2 (en) | 2013-08-30 | 2017-10-03 | Illinois Tool Works Inc. | Metal working fluid composition and method of detecting fluid deterioration |
US11081701B2 (en) | 2017-01-06 | 2021-08-03 | Waseda University | Secondary battery |
Also Published As
Publication number | Publication date |
---|---|
JPH0131587B2 (en) | 1989-06-27 |
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