JP4801422B2 - 熱媒体油の定量方法及び管理方法 - Google Patents
熱媒体油の定量方法及び管理方法 Download PDFInfo
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- JP4801422B2 JP4801422B2 JP2005327246A JP2005327246A JP4801422B2 JP 4801422 B2 JP4801422 B2 JP 4801422B2 JP 2005327246 A JP2005327246 A JP 2005327246A JP 2005327246 A JP2005327246 A JP 2005327246A JP 4801422 B2 JP4801422 B2 JP 4801422B2
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- 238000007726 management method Methods 0.000 title claims description 4
- 238000012546 transfer Methods 0.000 title description 9
- 238000004445 quantitative analysis Methods 0.000 title description 4
- 239000003921 oil Substances 0.000 claims description 74
- 239000003925 fat Substances 0.000 claims description 39
- 238000000926 separation method Methods 0.000 claims description 24
- 239000012086 standard solution Substances 0.000 claims description 20
- 239000008157 edible vegetable oil Substances 0.000 claims description 18
- 238000004817 gas chromatography Methods 0.000 claims description 16
- 229940057995 liquid paraffin Drugs 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 238000012856 packing Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004927 clay Substances 0.000 claims description 6
- 239000003495 polar organic solvent Substances 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000004458 analytical method Methods 0.000 description 24
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 22
- 239000007789 gas Substances 0.000 description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 12
- 235000013305 food Nutrition 0.000 description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 235000014593 oils and fats Nutrition 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000004667 medium chain fatty acids Chemical class 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 238000012113 quantitative test Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 229910052604 silicate mineral Inorganic materials 0.000 description 2
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- IXWIAFSBWGYQOE-UHFFFAOYSA-M aluminum;magnesium;oxygen(2-);silicon(4+);hydroxide;tetrahydrate Chemical compound O.O.O.O.[OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] IXWIAFSBWGYQOE-UHFFFAOYSA-M 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
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- 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
- G01N33/02—Food
- G01N33/03—Edible oils or edible fats
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/12—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the preparation of the feed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/143—Preparation by elimination of some components selective absorption
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- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Immunology (AREA)
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- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Fats And Perfumes (AREA)
- Sampling And Sample Adjustment (AREA)
Description
現在、食用油脂製造工場や食品工場においては、熱媒体油の食用油脂中への混入量を100ppm未満とするような自主管理基準を設けて管理を行っていることがあるが、この管理基準値は、上記した従来の定量試験法の下限値に基づくものと考えられる。
上記充填カラムは適当な大きさに形成されるが、通常、ガラスカラムの内径を約20〜30mm程度、長さを約70〜130cm程度とするとよい。
こうした濃縮液は、定法によりガスクロマトグラフィーにかけて分析し、分析チャートから熱媒体油に基づく全ピーク面積値を求める。
分析例1の手順を以下に説明する。
(試料の調製)
熱媒体油としての流動パラフィンを、中鎖脂肪酸トリグリセライドの食用油脂1gの中に、33ppmの濃度に加えたものと、100ppmの濃度に加えたものと、熱媒体油を加えないもの(0ppm)の3種類の試料を用意した。この各試料1gのそれぞれに、ペンタンを加えて各々100mlになるように希釈した。
上記中鎖脂肪酸は、炭素数が6〜12の脂肪酸を主成分とするものである。
内径25mm、長さ100cmのフッ素樹脂製コック付きのガラス製カラムを用意し、このカラム中にアタプルガスクレー(アルミニウム・ケイ酸塩鉱物)を120g充填して分離カラムとした。
この分離カラムに、先ずジクロルメタン100mlを流し、次にペンタン150mlを流してカラムを洗浄し、カラムの上部にペンタンが僅かに残り、充填剤が空気に露出する前に上記コックを閉じ、流出液は廃棄した。
上記分離カラムの下に濃縮用試験管を置き、上記コックを開いて、上記した試料溶液を約5mlづつに分けて段階的に加えながら、ペンタン流出液を回収した。上記試料溶液100mlを全てカラムに流した後で、さらにペンタンを約5mlづつ加えて、ペンタン流出液を120ml回収した時点でコックを閉めて、分離操作を終了した。
上記分離操作によって回収したペンタン流出液を120mlの入った濃縮用試験管を30℃のウオーターバスに入れて、窒素ガスを緩やかに吹き付けてペンタンを蒸発除去して1mlまで濃縮した。
ガスクロ装置はヒューレットパッカード社製のHP6890、カラムはフロンティアラボ社製のUltra alloy-SIM(5m×0.53mm×0.1μl)、キャリアガスはヘリウム、圧力は1.3psi、注入法はスプリットレス、注入量は1μlであり、検出器はFIDを用いて、ガスクロ分析を行った。
ガスクロ分析の結果のチャートを図1に示す。
ガスクロ分析のチャート中、熱媒体油の流動パラフィンに基づくものが4min〜7minの間のピークによって示されている。
上記ガスクロ分析のチャートによって、流動パラフィンを33ppm含む標準液のピーク面積値、流動パラフィンを100ppm含む標準液のピーク面積値、流動パラフィンを加えない標準液(0ppm)のピーク面積値を求めた。
その結果は、下記表1に示すとおりである。
ガスクロ分析は3回行っており、図1に示すものは表1中の1回目の分析チャートである。また、3回行った平均値も併せて求め、表1中に記載した。
上記の分析結果を示す表1から判るように、熱媒体油の流動パラフィンの含有量が0ppm、33ppm、100ppmの面積値に明らかな差が見られる。
従って、上記した分析例に従って、熱媒体油の含有量が未知の食用油脂の分析を行い、全ピーク面積値を上記標準液のピーク面積値と比較することによって、食用油脂中の熱媒体油の含有量を測定することができることが判る。
(試料の調製)
熱媒体油としての流動パラフィンを、上記中鎖脂肪酸トリグリセライドの食用油脂1gの中に、0ppmの、10ppmの、20ppmの、33ppmの、100ppmの各濃度にした5種類の試料を用意し、その他は上記分析例1と同様にした。
上記分析例1と同じ内径25mm、長さ100cmのフッ素樹脂製コック付きのガラス製カラムを用意し、このカラム中にアルミナゲル10gを下に、アタプルガスクレー(アルミニウム・ケイ酸塩鉱物)100gを上に、二重に充填して分離カラムとした。
この分離カラムに、上記分析例1と同様に、先ずジクロルメタン100mlを流し、次にペンタン150mlを流してカラムを洗浄し、カラムの上部にペンタンが僅かに残り、充填剤が空気に露出する前に上記コックを閉じ、流出液は廃棄した。
ガスクロ分析の結果のチャートは、図2に示すとおりである。
上記図2に示すガスクロ分析のチャートによって、流動パラフィンを0ppm含む標準液、同10ppm含む標準液、同20ppm含む標準液、同33ppm含む標準液、同100ppm含む標準液の各ピーク面積値を求めた。
その結果は下記表2に示すとおりである。
上記した分析結果を示す図2及び表2から判るように、熱媒体油の流動パラフィンの含有量が、0ppm、10ppm、20ppm、33ppm、100ppmの各面積値に明らかな差が見られる。このように分離カラムにアタプルガスクレーとアルミナゲルとを組み合わせたものを使用することによって、更に熱媒体油の混入量が10ppm、20ppmの低含有量のものまで測定することが可能である。
Claims (3)
- 微量の熱媒体油である流動パラフィンを含有する極性を持った食用油脂を、炭素数5〜7の炭化水素の無極性の有機溶媒で希釈し、この希釈液を分離カラムに通して上記食用油脂をカラム充填媒体に吸着させ、上記熱媒体油を上記無極性の有機溶媒と共に分離カラムより流出させ、流出液を濃縮してガスクロマトグラフィーにかけ、流動パラフィンの標準液のガスクロマトグラフィー分析値と比較して定量する熱媒体油の定量方法。
- 上記分離カラムのカラム充填媒体がアタプルガスクレー、アルミナ、またはアタプルガスクレーとアルミナの多層充填のいずれかである請求項1に記載の熱媒体油の定量方法。
- 複数の含有量を有する熱媒体油である流動パラフィンを含有する極性を持った食用油脂の標準液を、炭素数5〜7の炭化水素の無極性の有機溶媒で希釈し、この希釈液を分離カラムに通して上記食用油脂をカラム充填媒体に吸着させ、上記流動パラフィンを上記無極性の有機溶媒と共に分離カラムより流出させ、流出液を濃縮してガスクロマトグラフィーにかけて各々の流動パラフィンのピーク面積を求めておき、未知の含有量の熱媒体油である流動パラフィンを有する食用油脂を上記標準液と同様に処理して得たガスクロマトグラフィーのピーク面積を、上記標準液のピーク面積と比較して上記熱媒体油の未知の含有量を求めて食用油脂の状態を管理する熱媒体油の管理方法。
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Application Number | Priority Date | Filing Date | Title |
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JP2005327246A JP4801422B2 (ja) | 2005-11-11 | 2005-11-11 | 熱媒体油の定量方法及び管理方法 |
PCT/EP2006/068312 WO2007054549A1 (en) | 2005-11-11 | 2006-11-09 | Quantitative test method for determining heat transfer oil in edible oil or fat |
US11/558,290 US20070128320A1 (en) | 2005-11-11 | 2006-11-09 | Quantitative test method for determining heat transfer oil in edible oil or fat |
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JP2005327246A JP4801422B2 (ja) | 2005-11-11 | 2005-11-11 | 熱媒体油の定量方法及び管理方法 |
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JP2007132839A JP2007132839A (ja) | 2007-05-31 |
JP4801422B2 true JP4801422B2 (ja) | 2011-10-26 |
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US (1) | US20070128320A1 (ja) |
JP (1) | JP4801422B2 (ja) |
WO (1) | WO2007054549A1 (ja) |
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CN104634894B (zh) * | 2015-01-30 | 2017-01-18 | 国网河南禹州市供电公司 | 一种变压器油气检测装置 |
CN105758969B (zh) * | 2016-05-05 | 2018-02-16 | 煤科集团沈阳研究院有限公司 | 一种矿井下用气相色谱仪及使用方法 |
CN109142655B (zh) * | 2018-08-24 | 2021-01-12 | 厦门光免生物技术有限公司 | 一种劣质食用油脂的鉴别方法 |
EP3894035A4 (en) * | 2018-10-23 | 2022-11-02 | George Stantchev | SEPARATION SYSTEM AND METHOD THEREOF |
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US6436713B1 (en) * | 1997-07-28 | 2002-08-20 | 3M Innovative Properties Company | Methods and devices for measuring total polar compounds in degrading oils |
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US6127185A (en) * | 1998-05-05 | 2000-10-03 | University Of Tennessee Research Corporation | Instrument and method for measurement of stability of oils |
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