融点/滴点・軟化点のアプリケーション

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アプリケーション

融点とは
化合物の融点、物質の純度を評価する熱特性試験(沸点測定)

融点測定とは、定義された熱的特性による材料試験であり、品質検査や品質評価に一般的に採用されている試験方法です。

滴点測定とは
食用油脂やグリース類、石油化学製品の物性測定

軟化点・滴点測定の基本的な知識について解説します。 研究室での日常作業を改善する実践的なヒントをご紹介します。

融点とは

融点測定とは、定義された熱的特性による材料試験であり、品質検査や品質評価に一般的に採用されている試験方法です。

滴点測定とは

軟化点・滴点測定の基本的な知識について解説します。 研究室での日常作業を改善する実践的なヒントをご紹介します。

標準

国際標準と基準

MPとDPの標準ファインダー

AACC

StandardNo.YearTitleShort descriptionRemark
AACC58-53.012009Slip melting pointThe slip point (open tube melting point) is an index of temperature at which fat softens or becomes sufficiently fluid to slip or run.MP55/MP80

AOCS

StandardNo.YearTitleShort descriptionRemark
AOCSCc 3b-922009Slip melting point ISO Standard (see ISO 6321)The temperature at which a column of fat in an open capillary tube begins to rise under the conditions specified.MP55/MP80
AOCSCc 3-252009Slip melting point, AOCS Standard open tube melting pointThe temperature at which fat softens and becomes sufficiently fluid to slip in an open capillary tube.MP55/MP80
AOCSCc 1-252009Melting point capillary tube methodFats pass through a stage of gradual softening before they become totally liquid. The melting point then must be defined by the specific conditions of the method by which it is determined and, in this case, it is the temperature at which the test sample becomes completely clear and liquid.MP
AOCSCc 6-252009Cloud point test (on cooling)The cloud point is that temperature at which, under the conditions of this test, a cloud is induced in the test sample caused by the first stage of crystallization.Not available
AOCSCc 18-802009Dropping point of edible fats and oilThe dropping point of a fat or oil is the temperature at which the test sample will become fluid to flow under the conditions of the test.DP

JOCS

StandardNo.YearTitleShort descriptionRemark
JOCS2.2.4.22009Melting point (slipping point)Index of the temperature at which fat softens and becomes sufficiently fluid to slip in an open capillary tubeMP55/MP80

ASTM D

StandardNo.YearTitleShort descriptionRemark
ASTM D362014Softening point of bitumenThe softening point of bitumen in the range from 30 to 157°C (86 to 315°F) using the ring-and-ball apparatusAlternative for pure bitumen:
ASTM 3461 with DP
ASTM D872014Melting point of petroleum waxes (cooling curve)A plateau occurs with specimens containing appreciable amounts of hydrocarbons that crystallize at the same temperature, giving up heat of fusion, thus temporarily retarding the cooling rate.Not available
ASTM D972012Standard test method for pour point of petroleum products.Flow ability of the oil is tested when cooled down and crystallization starts, no stirring; instrument as used in ASTM D2500.Not available
ASTM D1272019Dropping point of petroleum waxes including petrolatumPre-melt sample, pour it into the sample cup, heating rate 2 K/min.
DP
ASTM D5662016Dropping point of lubricating greaseThermometer in sample cup.Automatic alternative:
ASTM D3954 with DP
 
ASTM D11772012Standard test method for Freezing point of Aqueous Engine Coolant.The freezing point of an engine coolant may be used to determine the approximate glycol content, provided the glycol type is known.Not available
ASTM D15192014Standard test method for Rubber chemicals-Melting RangeMelting range of commercial rubber processing chemicals either by use of capillary melting point tubes or by differential scanning calorimetry (DSC)MP
ASTM D21171988Melting point of semi-crystalline polymers by the hot stage microscopy method.
Note: discontinued without replacement.
Change of birefringence in polarized lightHot Stage
ASTM D22652015Dropping point  of lubricating grease over wide temperature rangeThis method uses mercury thermometerAutomatic alternative:
ASTM D3954 with DP
ASTM D23192014Softening point of pitchesCube in air methodNot available
ASTM D25002014Cloud point of petroleum oils

Visual observation

Not available
ASTM D31042014Softening point of pitches (Mettler softening point method)Pre-melt sample, pour it into the sample cup, heating rate 2 K/min.DP
ASTM D34612014Softening point of asphalt and pitch (Mettler cup and ball method)Pre-melt sample, pour it into the sample cup. Place lead ball of 3.2 ±0.1 g on the sample. Heating rate 2 K/min.DP
ASTM D39542010Dropping point of waxes
(The method duplicates D 566)
Start temperature 20 to 25°C below the expected dropping point, heating rate 2 K/min. Cup 2.8 mm hole.DP
ASTM D49502014Standard Classification and Specification for Automotive Service GreasesGreases CategoriesAutomatic alternative:
ASTM D3954 with DP
ASTM D57712015Standard Test Method for Cloud Point of Petroleum Products
(Optical Detection Stepped Cooling Method)
This test method covers the description of the determination of the cloud point of petroleum products and biodiesel fuels that are transparent in layers 40 mm in thickness, by an automatic instrument using an optical device.Not available
ASTM D57722015Standard Test Method for Cloud Point of Petroleum Products
(Linear Cooling Rate Method)
This test method covers the description of the determination of the cloud point of petroleum products and biodiesel fuels that are transparent in layers 40 mm in thickness by an automatic instrument using a linear cooling rate.Not available
ASTM D57732015Standard Test Method for Cloud Point of Petroleum Products (Constant Cooling Rate Method)This test method covers the determination of the cloud point of petroleum products and biodiesel fuels that are transparent in layers 40 mm in thickness by an automatic instrument using a constant cooling rate.Not available
ASTM D60382014Standard Test Method for Determining the Compatability of Resin/Solvent Mixtures by Precipitation TemperatureTesting the compatability of lithographic ink resins in high boiling ink solvents by precipitation temperature, manual and automatic mode.Not available (cooling)
ASTM D60902012Softening Point Resins
(Mettler Cup and Ball Method)
Sample cup with 6.35 mm aperture and steel ballDP

 

ASTM E

StandardNo.YearTitleShort descriptionRemark
ASTM E282014Standard Test Methods for Softening Point of Resins derived from pine chemicals and hydrocarbons by Ring-and-Ball Apparatus
Ring and ball apparatus, manual or automated
Not available
ASTM E3241999Relative initial and final melting points and the melting range of organic chemicals
Melting point capillary in a bath
Withdrawn in 2001,
Automatic alternative with MP

CEI/IEC

StandardNo.YearTitleShort descriptionRemark
CEI/IEC811-5-12006Common test methods for insulating and sheathing materials of electric cables. Part 5: methods specific to filling compounds
Section 1: Dropping point from nipple in glass tube and oil bath (Ubbelohde)Automatic alternative with DP

DIN EN

StandardNo.YearTitleShort descriptionRemark
DIN EN12382011Determination of the softening point of thermoplastic adhesives (ring and ball)Sample cup diameter (externally) 20.6 mm liquid bath  Not available
DIN EN18902006Surfactants - Determination of cloud point of non-ionic surface active agents obtained by condensation of ethylene oxideIn glass vial of 25 ml, with stirrerNot available
DIN EN230151994Petroleum products; determination of cloud pointReplaced DIN ISO 3015, visual observationNot available
DIN EN51801
Part 2
2005Determination of dropping point; Ubbelohde method for bitumenThermometer in sample. Sample cup aperture 3.0 mm.Withdrawn Automatic alternative ASTM D3104, D3461 with DP
DIN EN519202012Testing of carbonaceous material; determination of the Mettler softening point; binding and impregnating materialsSample cup with 6.35 mm aperture
DP
DIN EN520111986Testing of bitumen; determination of the softening pointRing and ballWithdrawn
Not available
DIN534081967Testing of plastics; determination of solubility temperature of PVC in plasticizersHeating rate 2°C/min, "clear point", microscope with magnification of 100Hot Stage

DIN ISO

StandardNo.YearTitleShort descriptionRemark
DIN ISO21761981Petroleum products; lubricating grease; determination of dropping pointThermometer in sample, sample cup aperture 2.8 mmAutomatic alternative: ASTM D3954 with DP
ISO30151992Petroleum oils determination of cloud pointThe method specified applies to petroleum products which are transparent in layers of 40 mm thickness and have a cloud point below 49 °C. The use of this standard may involve hazardous materials, operations and equipment.Not available
DIN ISO38411983Petroleum waxes, determination of melting point (cooling curve)Glass tube, thermometer in sampleNot available
ISO4625-22004Binders for paints and varnishes - Determination of softening point -Part 2: Cup and ball methodUses the softening cup (6.35 mm aperture) with steel ball of 8.7 mm and 2.77 gDP
DIN ISO222862018Determination of the dropping point of grease with an automatic apparatusThe initial temperature is set 20 °C above ambient. A heating rate of 10 °C/min is started until a temperature of 20 °C below the expected dropping point is reached. At this point, the heating rate is reduced to 1 °C/min until the dropping point is recorded.DP

IP

StandardNo.YearTitleShort descriptionRemark
IP552001Melting point of petroleum waxes (cooling curve)
see ASTM D87
Specifies a procedure for determination of the melting point of petroleum wax (cooling curve).
Not available
IP1322013Dropping point of lubricating grease
See ASTM D566
This test method covers the determination of the dropping point of lubricating grease. This test method is not recommended for use at bath temperatures above 288°C.
Automatic alternative:
ASTM D3954 with DP
IP3962002Determination of dropping point of lubricating grease - Automatic apparatus method
Specifies a method for determining the dropping point of lubricating grease by means of automatic dropping point apparatus.DP

ISO

StandardNo.YearTitleShort descriptionRemark
DIN ISO21761981Petroleum products; lubricating grease; etermination of dropping pointThermometer in sample, opening sample cup 2.8 mm.Automatic alternative:
ASTM D3954 with DP
DIN ISO38411983Petroleum waxes, determination of melting point (cooling curve)Glass tube, thermometer in sampleNot available
ISO9182011Determination of distillation characteristics
Volatile organic liquids for industrial use
Relates to liquids (excluding petroleum products) having a boiling point in the range 30 °C to 300 °C and are stable during distillation in atmospheric conditions.  Not available 
ISO10651991Non-ionic surface active agents obtained from ethylene oxide and mixed non-ionic surface active agents. Determination of cloud pointSample 15 ml, 14 mm diameter, visual observation
Specifies five methods of measurement. Methods A, B and C are applicable to agents derived by condensation with a lipophilic compound without oxypropylene groups. Methods D and E should be used only after agreement between the parties concerned.
Not available
Alternative
ASTM D2024
MP80
ISO30151992Petroleum oils determination of cloud pointThe method specified applies to petroleum products which are transparent in layers 40 mm in thickness and have a cloud point below 49 °C. The use of this standard may involve hazardous materials, operations and equipment.Not available
ISO31462002Plastics -- Determination of melting behavior (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methodsMethod A based on changes in shape of the polymer; can also be used for softening of non-crystalline polymers. Metal block furnace. Powder up to 100 μm.
Method B for hot stage, microscope magnification x50, powder or thin film
Hot Stage
MP
ISO4625-22004Binders for paints and varnishes - Determination of softening point -Part 2: Cup an ball methodUses the softening cup (6.35 mm) with steel ball 8.7 mm and 2.77 gDP
UNI EN ISO63212005Animal and vegetable fats and oils- Determination of melting point in open capillary tubes (slip point)Defines two methods for the determination of the melting point in open capillary tubes, commonly known as the slip point, of animal and vegetable fats and oils. - Method A is only applicable to animal and vegetable fats which are solid at ambient temperature and which do not exhibit pronounced polymorphism. - Method B is applicable to all animal and vegetable fats which are solid at ambient temperature, and is the method to be used for fats whose polymorphic behaviour is unknown.MP

OECD

StandardNo.YearTitleShort descriptionRemark
OECD1022011Melting point/melting rangeCapillary tube in a metal blockMP

JIS K

StandardNo.YearTitleShort descriptionRemark
JIS K00642011
Test method for melting point and melting range of chemical products
Transmitted light method
MP
JIS K41011993Testing methods for melting point of chemical products
Transmitted light methodMP

Ph.Eur.

StandardNo.YearTitleShort descriptionRemark
Ph.Eur.
2.2.142017Melting point – capillary method
Rate 1 K/min. Temperature at which the last particle passes into the liquidMP
Ph.Eur.2.2.152016Melting point – open capillary methodSlip point - rising melting pointMP55/MP80
Ph.Eur.
2.2.172016Drop PointThe drop point is the temperature at which the first drop of the melting substance to be examined falls from a cup under defined conditionsDP
Ph.Eur.2.2.182005Freezing pointThe freezing point is the maximum temperature occurring during the solidification of a supercooled liquid.Not available
Ph.Eur.2.2.602017Melting point – Instrumental methodEndpoint automaticMerged with Ph.Eur.2.2.14

ChP

StandardNo.YearTitleShort descriptionRemark
ChP06122016Determination of melting pointMetal block with capillaries (melting and slip melting point)MP

IPC

StandardNo.YearTitleShort descriptionRemark
IPC2.4.212014Melting range or temperatureMetal block with capillaries (melting and slip melting point)MP

FSSAI

StandardNo.YearTitleShort descriptionRemark
FSSAI8.02014Determination of melting point of fatOpen-tube capillary - slip methodMP55/MP80

JP

StandardNo.YearTitleShort descriptionRemark
JP2.602017Melting point determinationMetal block with capillaries (melting and slip melting point)MP

USP

StandardNo.YearTitleShort descriptionRemark
USP7412015Melting range or temperatureApparatus II: metal block with capillaries (melting and slip melting point)MP

WHO

StandardNo.YearTitleShort descriptionRemark
WHO1.2.12015Melting temperature and melting rangePulverizable substances and low melting solids (melting and slip melting point)MP

 

規制・規格団体:

ASTM: American society for testing and materials http://www.astm.org/
ISO: international standardization organization http://www.iso.ch
EN: CEN, European Committee for Standardization http://www.cenorm.be
Ph.Eur.: European Pharmacopoeia
DIN: Deutsches Institut für Normung http://www.din.de/
Standards: http://www2.beuth.de/
JIS: Japanese Industrial Standards http://www.jsa.or.jp/eng/index.htm
JP: Japanese Pharmacopoeia https://www.pmda.go.jp/english/rs-sb-std/standards-development/jp/0019.html
AACC: American Association for Clinical Chemistry: https://www.aacc.org/
JOCS: Japan Oil Chemists' Society http://www.jocs.jp/index-e.html
VDA: Verband der Automobilindustrie http://www.vda.de/
USP: United State Pharmacopoeia http://www.usp.org
ChP: Pharmacopoeia of the People's Republic of China http://wp.chp.org.cn/front/chpint/en/
IPC: Indian Pharmacopoeia Commission http://www.ipc.gov.in/
IP: Institute of petroleum http://www.petroleum.co.uk
NF: norme française http://www.afnor.fr
OECD: Organisation for Economic Co-operation and Development http://www.oecd.org/
UNI: Ente nazionale italiano di unificazione http://www.uni.com
AOCS: American Oil Chemists Society http://www.aocs.org//
CEI/IEC: The International Electrotechnical Commission http://www.iec.ch/
IPC: Institute for interconnecting and packaging electronic circuits http://www.ipc.org/
CEC: Co-ordinating European Council for the development of performance tests for transportation fuels, lubricants and other fluids.
WHO: World Health Organization http://www.who.int/en/