JP2007315988A - 潤滑剤中のサリチレートの分析方法 - Google Patents
潤滑剤中のサリチレートの分析方法 Download PDFInfo
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Abstract
【解決手段】 潤滑剤に三フッ化ホウ素を溶解したメタノールまたはジアゾメタンを加え、サリチレートのカルボキシル基をメチルエステル化するか、または、ピリジン及び無水酢酸を加え、サリチレートの水酸基をアセチル化する。メチルエステル化またはアセチル化されたサリチレートを、ガスクロマトグラフィーによって直接分析する。
【選択図】 図1
Description
サリチレートが含まれている潤滑油Aの10mg(0.01g)に、メタノールで7%に希釈した三フッ化ホウ素溶液を0.1g添加し、80℃に加熱して1時間反応させた。放冷後、ヘキサンを0.15g及び10重量%食塩水を0.5g添加し、ヘキサンで溶媒抽出した。
上記実施例1と同じサリチレートが含まれている潤滑油Aの5mg(0.005g)に、ピリジンを0.03g及び無水酢酸を0.03g添加し、80℃に加熱して1時間反応させた。放冷後、アセトンを0.1g添加して希釈し、これを試料2として1μl採取し、MSを備えたガスクロマトグラフ(ガスクロマトグラフ質量分析計:GCMS)に供した。尚、ガスクロマトグラフ装置と分離カラムは、上記実施例1と同じものを用いた。
サリチレートが含まれている潤滑油B(新油)と、同じ潤滑油Bで使用時間の異なる使用中の潤滑油B−1(使用期間60日)及びB−2(使用期間120日)の各1mg(0.001g)に、それぞれメタノールで7%に希釈した三フッ化ホウ素溶液を0.1g添加し、80℃に加熱して1時間反応させた。放冷後、ヘキサンを0.15g及び10重量%の食塩水を0.5g添加し、ヘキサンで溶媒抽出した。
Claims (3)
- サリチレートを含有する潤滑剤に、三フッ化ホウ素を溶解したメタノールまたはジアゾメタンを加え、サリチレートのカルボキシル基をメチルエステル化した後、得られた反応物をガスクロマトグラフィーに供することを特徴とする潤滑剤中のサリチレートの分析方法。
- サリチレートを含有する潤滑剤にピリジン及び無水酢酸を加え、サリチレートの水酸基をアセチル化した後、得られた反応物をガスクロマトグラフィーに供することを特徴とする潤滑剤中のサリチレートの分析方法。
- 上記請求項1または2のサリチレートの分析方法により得られたクロマトグラムから、劣化後のメチルエステル化またはアセチル化されたサリチレートのピーク面積を劣化前のピーク面積と比較することにより、サリチレートの劣化の程度を評価することを特徴とする潤滑剤の劣化判定方法。
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JP2006147637A JP4738253B2 (ja) | 2006-05-29 | 2006-05-29 | 潤滑剤中のサリチレートの分析方法 |
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JP2007315988A true JP2007315988A (ja) | 2007-12-06 |
JP4738253B2 JP4738253B2 (ja) | 2011-08-03 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010044400A1 (ja) | 2008-10-14 | 2010-04-22 | 旭化成株式会社 | 熱反応型レジスト材料、それを用いた熱リソグラフィ用積層体及びそれらを用いたモールドの製造方法 |
WO2013111812A1 (ja) | 2012-01-27 | 2013-08-01 | 旭化成株式会社 | 微細凹凸構造体、ドライエッチング用熱反応型レジスト材料、モールドの製造方法及びモールド |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56155849A (en) * | 1980-05-07 | 1981-12-02 | Mitsui Petrochem Ind Ltd | Method for analyzing aromatic carboxylic acid |
JPH09184832A (ja) * | 1995-12-29 | 1997-07-15 | Cosmo Sogo Kenkyusho:Kk | 潤滑油組成物の分析方法 |
JPH09235579A (ja) * | 1996-02-29 | 1997-09-09 | Tonen Corp | 潤滑油組成物 |
JPH1151918A (ja) * | 1997-08-01 | 1999-02-26 | Nippon Oil Co Ltd | 油性物質中のサリシレートの分析方法 |
-
2006
- 2006-05-29 JP JP2006147637A patent/JP4738253B2/ja not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56155849A (en) * | 1980-05-07 | 1981-12-02 | Mitsui Petrochem Ind Ltd | Method for analyzing aromatic carboxylic acid |
JPH09184832A (ja) * | 1995-12-29 | 1997-07-15 | Cosmo Sogo Kenkyusho:Kk | 潤滑油組成物の分析方法 |
JPH09235579A (ja) * | 1996-02-29 | 1997-09-09 | Tonen Corp | 潤滑油組成物 |
JPH1151918A (ja) * | 1997-08-01 | 1999-02-26 | Nippon Oil Co Ltd | 油性物質中のサリシレートの分析方法 |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010044400A1 (ja) | 2008-10-14 | 2010-04-22 | 旭化成株式会社 | 熱反応型レジスト材料、それを用いた熱リソグラフィ用積層体及びそれらを用いたモールドの製造方法 |
US9257142B2 (en) | 2008-10-14 | 2016-02-09 | Asahi Kasei E-Materials Corporation | Heat-reactive resist material, layered product for thermal lithography using the material, and method of manufacturing a mold using the material and layered product |
WO2013111812A1 (ja) | 2012-01-27 | 2013-08-01 | 旭化成株式会社 | 微細凹凸構造体、ドライエッチング用熱反応型レジスト材料、モールドの製造方法及びモールド |
US9597822B2 (en) | 2012-01-27 | 2017-03-21 | Asaki Kasei E-Material Corporation | Fine concavo-convex structure product, heat-reactive resist material for dry etching, mold manufacturing method and mold |
US9623590B2 (en) | 2012-01-27 | 2017-04-18 | Asahi Kasei E-Materials Corporation | Fine concavo-convex structure product, heat-reactive resist material for dry etching, mold manufacturing method and mold |
US9701044B2 (en) | 2012-01-27 | 2017-07-11 | Asahi Kasei Kabushiki Kaisha | Fine concavo-convex structure product, heat-reactive resist material for dry etching, mold manufacturing method and mold |
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