RECOMMENDED METHODS OF ANALYSIS AND SAMPLING CODEX STAN .

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RECOMMENDED METHODS OF ANALYSIS AND SAMPLINGCODEX STAN 234-1999PART IMETHODS OF ANALYSIS AND SAMPLING BY ALPHABETICAL ORDER OFCOMMODITY CATEGORIES AND NAMES1

Table of ContentsCereals, Pulses and Legumes and Derived ProductsCocoa Products and ChocolateFats and Oils and Related ProductsFish and Fishery ProductsFoods for Special Dietary UsesFruit JuicesMilk and Milk ProductsNatural Mineral WatersProcessed Fruits and VegetablesProcessed Meat and Poultry Products and Soups and BrothsQuick Frozen Fruits and VegetablesSugars and HoneyMiscellaneous Products2

Commodity StandardProvisionMethodPrincipleTypeCereals, Pulses and Legumes and Derived ProductsCertain pulsesMoistureISO 665:1977 (confirmed 1995)GravimetryIDegermed maize (corn) meal andmaize (corn) gritsAshAOAC 923.03ISO 2171:1993ICC Method No 104/1 (1990)GravimetryIDegermed maize (corn) meal andmaize (corn) gritsFat, crudeAOAC 945.38F; 920.39CGravimetry (ether extraction)IDegermed maize (corn) meal andmaize (corn) gritsMoistureISO 712:1998ICC Method No 110/1 (1986)GravimetryIDegermed maize (corn) meal andmaize (corn) gritsParticle size (granularity)AOAC 965.22SievingIDegermed maize (corn) meal andmaize (corn) gritsProteinICC Method No 105/1 (1986)Titrimetry, Kjeldahl digestionIDurum wheat semolina and durumwheat flourAsh (semolina)AOAC 923.03ISO 2171:1993GravimetryIDurum wheat semolina and durumwheat flourMoistureISO 712:1998ICC Method 110/1 (1986)GravimetryIDurum wheat semolina and durumwheat flourProtein (N x 5.7)ICC Method No 105/1Titrimetry, Kjeldahl digestionIDurum wheat semolina and durumwheat flourSamplingDescribed in the Standard (According toCodex Sampling Instructions)--Maize (corn)Aflatoxins, totalAOAC 979.18Holaday-Velasco mini columnIIMaize (corn)MoistureISO 6540:1980 (confirmed 1994)GravimetryIPeanuts (raw)Aflatoxins, totalAOAC 991.31Immunoaffinity column (Aflatest)IIPeanuts (raw)Aflatoxins, totalAOAC 993.17Thin layer chromatographyIII3

Commodity StandardProvisionMethodPrinciplePeanuts (intended for furtherprocessing)Aflatoxins, totalAOAC 975.36Romer minicolmnIIIPeanuts (intended for furtherprocessing)Aflatoxins, totalAOAC 979.18Holaday-Velasco minicolumnIIIPearl millet flourAshAOAC 923.03GravimetryPearl millet flourColourModern Cereal Chemistry, 6th Ed., D.W.Kent-Jones and A.J. Amos (Ed.), pp. 605612, Food Trade Press Ltd, London, 1969.Colorimetry using specific colourgraderPearl millet flourFat, crudeAOAC 945.38F; 920.39CGravimetry (ether extraction)IPearl millet flourFibre, crudeISO 5498:1981 (B.5 Separation)GravimetryIPearl millet flourMoistureISO 712:1998ICC Method No 110/1 (1986)GravimetryIPearl millet flourProteinAOAC 920.87Titrimetry, Kjeldahl digestionISorghum flourAshAOAC 923.03ISO 2171:1993ICC Method No 104/1 (1990)GravimetryISorghum flourColourModern Cereal Chemistry, 6th Ed., D.W.Kent-Jones and A.J. Amos (Ed.), pp. 605612, Food Trade Press Ltd, London, 1969.Colorimetry using specific colourgraderSorghum flourFat, crudeAOAC 945.38F; 920.39CGravimetry (ether extraction)ISorghum flourFibre, crudeICC Method No 113 (1972)ISO 6541:1981 (confirmed 1996)GravimetryISorghum flourMoistureISO 712:1998ICC Method No 110/1 (1986)GravimetryISorghum flourParticle size (granularity)AOAC 965.22SievingISorghum flourProteinICC Method No 105/1 (1986)Titrimetry, Kjeldahl digestionISorghum flourTanninsISO 9648:1988 (confirmed 1994)SpectrophotometryI4TypeIIVIV

Commodity StandardProvisionMethodPrincipleSorghum grainsAshAOAC 923.03ISO 2171:1993ICC Method No 104/1 (1990)GravimetryISorghum grainsFat, crudeAOAC 945.38F, 920.39CGravimetry (ether extraction)ISorghum grainsMoistureISO 6540:1980 (confirmed 1994)GravimetryISorghum grainsProteinICC Method No 105/1 (1986)Titrimetry, Kjeldahl digestionISorghum grainsTanninsISO 9648:1988 (confirmed 1994)SpectrophotometryISoy protein productsAshAOAC 923.03ISO 2171:1993 (Method B)GravimetryISoy protein productsFatCAC/RM 55-1976 - Method 1Gravimetry (extraction)ISoy protein productsFibre, crudeISO 5498:1981GravimetryISoy protein productsMoistureAOAC 925.09Gravimetry (vacuum oven)ISoy protein productsProteinAOAC 955.04D (using factor 6.25)Titrimetry , Kjeldahl digestionIIVegetable protein productsAshAOAC 923.03ISO 2171:1993 (Method B)Gravimetry, DirectIVegetable protein productsFatCAC/RM 55-1976 - Method 1Gravimetry (extraction)IVegetable protein productsFibre, crudeAACC (1982) 32-17Ceramic fiber filterationIVegetable protein productsMoistureAOAC 925.09Gravimetry (vacuum oven)IVegetable protein productsProteinAOAC 955.04D (using factor 6.25)Titrimetry, Kjeldahl digestionIIWheat flourAshAOAC 923.03ISO 2171:1993ICC Method No 104/1 (1990)GravimetryIWheat flourFat acidityAOAC 939.05TitrimetryIWheat flourMoistureISO 712:1998ICC Method No 110/1 (1986)GravimetryIWheat flourParticle size (granularity)AOAC 965.22SievingI5Type

Commodity StandardProvisionMethodPrincipleTypeWheat flourProteinICC Method No 105/1 (1986)Titrimetry, Kjeldahl digestionIWheat glutenDenaturation of glutenAACC Method 38-20PharinographyIWheat glutenFibre, crudeAOAC 962.09Ceramic fiber filterationIWheat glutenProteinAOAC 976.05 (using factor 6.25)Titrimetry, Kjeldahl digestionIIWheat glutenSamplingISO 2170:1980--Whole and decorticated pearl milletgrainsAshAOAC 923.03GravimetryIWhole and decorticated pearl milletgrainsFat, crudeAOAC 945.38F; 920.39CGravimetry (ether extraction)IWhole and decorticated pearl milletgrainsFibre, crudeISO 5498:1981 (B.5 Separation)GravimetryIWhole and decorticated pearl milletgrainsMoistureISO 712:1998ICC Method No 110/1 (1986)GravimetryIWhole and decorticated pearl milletgrainsProteinAOAC 920.87Titrimetry, Kjeldahl digestionIWhole maize (corn) mealAshAOAC 923.03ISO 2171:1993ICC Method No 104/1 (1990)GravimetryIWhole maize (corn) mealFat, crudeAOAC 945.38F; 920.39CGravimetry (ether extraction)IWhole maize (corn) mealMoistureISO 712:1998ICC Method No 110/1 (1986)GravimetryIWhole maize (corn) mealParticle size (granularity)AOAC 965.22SievingIWhole maize (corn) mealProteinICC Method No 105/1 (1986)Titrimetry, Kjeldahl digestionICocoa products and chocolateArsenicAOAC 952.13 (Codex general method)Colorimetry (diethyldithiocarbamate)IIChocolateAsh, totalAOAC 972.15Gravimetry (at 600 C)ICocoa Products and Chocolate6

Commodity StandardProvisionMethodPrincipleChocolateCocoa butter, percentage ofAOAC 963.15IOCCC 14-1972(Gravimetry (Soxhlet extraction)IChocolateCocoa solids, fat-freeAOAC 931.05Oven evaporation and factorIChocolateCopperAOAC 960.40 (Codex general method)Colorimetry (diethyldithiocarbamate)IIChocolateFat, totalAOAC 963.15Gravimetry (Soxhlet extraction)IChocolateLeadAOAC 986.15 (Codex general method)Anodic stripping voltammetryIIChocolateMoisture / Loss on dryingAOAC 931.04IOCCC 1-1952GravimetryICocoa (cacao) nib, cocoa (cacao)mass, cocoa press cake and cocoa dust(cocoa fines), for use in themanufacturing of cocoa and chocolateproductsAsh insoluble in HClAOAC 972.15Gravimetry (at 600 C)ICocoa (cacao) nib, cocoa (cacao)mass, cocoa press cake and cocoa dust(cocoa fines), for use in themanufacturing of cocoa and chocolateproductsAsh, totalAOAC 972.15Gravimetry (at 600 C)ICocoa (cacao) nib, cocoa (cacao)mass, cocoa press cake and cocoa dust(cocoa fines), for use in themanufacturing of cocoa and chocolateproductsCocoa shellAOAC 968.10 and 970.23Spiral vessel count, Stone cell countICocoa (cacao) nib, cocoa (cacao)mass, cocoa press cake and cocoa dust(cocoa fines), for use in themanufacturing of cocoa and chocolateproductsCopperAOAC 971.20 (Codex general method)Atomic absorption spectrophotometryII7Type

Commodity StandardProvisionMethodPrincipleCocoa (cacao) nib, cocoa (cacao)mass, cocoa press cake and cocoa dust(cocoa fines), for use in themanufacturing of cocoa and chocolateproductsLeadAOAC 972.25 (Codex general method)Atomic absorption spectrophotometryIICocoa butter confectioneryAsh, totalAOAC 972.15Gravimetry (at 600 C)ICocoa butter confectioneryCocoa butterAOAC 963.15IOCCC 14-1972Gravimetry (Knorr tube extraction,Soxhlet extraction)ICocoa butter confectioneryCopperAOAC 971.20 (Codex general method)Atomic absorption spectrophotometryIICocoa butter confectioneryLeadAOAC 972.25 (Codex general method)Atomic absorption spectrophotometryIICocoa butter confectioneryMilk proteinIOCCC 17-1973AOAC 939.02Titrimetry, Kjeldahl digestion; afterextraction of milk proteinsIICocoa butter confectioneryMilkfatIOCCC 5-1960AOAC 945.34; 925.41B; 920.80Titrimetry/DistillationICocoa butter confectioneryMoistureIOCCC 26-1988AOAC 977.10Karl FischerIICocoa butter confectionerySugarsAOAC 980.13Liquid chromatographyIICocoa buttersCopperAOAC 990.05ISO 8294:1994IUPAC 2.631(Codex general method)Atomic absorption spectrophotometry(direct graphite furnace)IICocoa buttersCopperAOAC 960.40 (Codex general method)Colorimetry (diethyldithiocarbamate)IIICocoa buttersFatty acids, freeIUPAC 2.201TitrimetryIICocoa buttersIodine valueIUPAC 2.205TitrimetryICocoa buttersIronAOAC 990.05ISO 8294:1994IUPAC 2.631(Codex general method)Atomic absorption spectrophotometry(direct graphite furnace)II8Type

Commodity StandardProvisionMethodPrincipleCocoa buttersIronBS 684 Section 2.17:1976ColorimetryIIICocoa buttersLeadAOAC 934.07Colorimetry (dithizone)IICocoa buttersLeadIUPAC Method (Pure and Appl. Chem. 63)Atomic absorptionSpectrophotometry, graphite furnaceIIICocoa buttersMelting behaviour (i) Slippoint (ii) Clear melting pointIOCCC 4-1961Melting point measurementICocoa buttersRefractive indexIUPAC 2.102RefractometryIICocoa buttersSaponification valueIUPAC 2.202TitrimetryIICocoa buttersUnsaponifiable matterIUPAC 2.401GravimetryICocoa powders (cocoa) and dry cocoa- Ash, total (in cocoa mass andsugar mixturescocoa press cake)AOAC 972.15Gravimetry (at 600 C)ICocoa powders (cocoa) and dry cocoa- Cocoa buttersugar mixturesIOCCC 14-1972 and 18-1973Through total fat and total sterolcontent by GLCICocoa powders (cocoa) and dry cocoa- Coppersugar mixturesAOAC 960.40 (Codex general method)Colorimetry (diethyldithiocarbamate)IICocoa powders (cocoa) and dry cocoa- Leadsugar mixturesAOAC 986.15 (Codex general method)Anodic stripping voltammetryIICocoa powders (cocoa) and dry cocoa- Leadsugar mixturesAOAC 934.07Colorimetry (dithizone)IIICocoa powders (cocoa) and dry cocoa- Moisture / Loss on dryingsugar mixturesAOAC 931.04IOCCC 1-1952GravimetryICocoa powders (cocoa) and dry cocoa- Sugarssugar mixturesAOAC 980.13Liquid chromatographyIIComposite and filled chocolateCentre in composite and filledchocolateMethod described in ALINORM 83/23, p.27GravimetryIIIComposite and filled chocolateCoating in composite andfilled chocolateMethod described in ALINORM 83/23, p.27GravimetryIII9Type

Commodity StandardProvisionMethodPrincipleTypeFats and oilsAcidityIUPAC 2.201ISO 660:1996TitrimetryIFats and oilsArsenicAOAC 952.13 (Codex general method)IUPAC 3.136Colorimetry (diethyldithiocarbamate)IIFats and oilsArsenicAOAC 942.17 (Codex general method)Colorimetry (molybdenum blue)IIIFats and oilsArsenicAOAC 985.16 (Codex general method)Atomic absorption spectrophotometryIIIFats and oilsAOCS Cb 2-40Baudouin test (modifiedVillavecchia or sesameseed oiltest)Colour reactionIFats and oilsCarotenoids, totalBS 684 Section 2.20SpectrophotometryIIFats and oilsCopperAOAC 990.05ISO 8294:1994IUPAC 2.631(Codex general method)Atomic absorptionSpectrophotometry (direct graphitefurnace)IIFats and oilsCrismer valueAOCS Cb 4-35TurbidityIFats and oilsFatty acid compositionIUPAC 2.301 2.302 2.304ISO 5509:1978 5508:1990Gas chromatography of methyl estersIIFats and oilsHalphen testAOCS Cb 1-25ColorimetryIFats and oilsInsoluble impuritiesIUPAC 2.604ISO 663:1992GravimetryIFats and oilsIronAOAC 990.05ISO 8294:1994IUPAC 2.631(Codex general method)Atomic absorption spectrophotometry(direct graphite furnace)IIFats and Oils and Related Products10

Commodity StandardProvisionMethodPrincipleFats and oilsLeadAOAC 994.02IUPAC 2.623ISO 12193:1994(Codex general method)Atomic absorption spectrophotometry(direct graphite furnace)IIFats and oilsMatter volatile at 105 CIUPAC 2.601ISO 662:1996Gravimetry (open-drying)IFats and oilsPeroxide valueIUPAC 2.501 (as amended)AOCS Cd 8b-90Titrimetry using iso-octaneIFats and oilsRefractive indexIUPAC 2.102ISO 6320:1995RefractometryIIFats and oilsReichert & Polenske valuesIUPAC 2.204TitrimetryIFats and oilsRelative densityIUPAC 2.101PycnometryIIFats and oilsSaponification valueIUPAC 2.202ISO 3657:1988 (confirmed 1992)TitrimetryIFats and oilsSlip pointISO 6321:1991Open ended capillary tubeIFats and oilsSoap contentBS 684 Section 2.5GravimetryIFats and oilsSterol compositionISO 6799:1991IUPAC 2.403Gas chromatographyIIFats and oilsTitreIUPAC 2.121ISO 935:1988ThermometryIFats and oilsTocopherol compositionIUPAC 2.432HPLCIIFats and oilsUnsaponifiable matterIUPAC 2.401 (part 1-5)ISO 3596-1:1996Titrimetry after extraction withdiethyl etherIMargarineFatIUPAC 2.801GravimetryIMargarineMilkfatCAC/RM 15-1969TitrimetryIMargarineSodium chlorideAOAC 971.27 (Codex general method)PotentiometryIIMargarineVitamin AAOAC 960.45SpectrophotometryII11Type

Commodity in DAOAC 936.14BioassayIIMargarineVitamin EIUPAC 2.411TLC followed by spectrophotometryor GLCIIMargarineWaterCAC/RM 17-1969GravimetryIMinarineFatIUPAC 2.801GravimetryIMinarineMilkfatCAC/RM 15-1969TitrimetryIMinarineSodium chlorideAOAC 971.27 (Codex general method)PotentiometryIIMinarineVitamin AAOAC 960.45SpectrophotometryIIMinarineVitamin DAOAC 936.14BioassayIIMinarineVitamin EIUPAC 2.411TLC followed by spectrophotometryor GLCIIMinarineWaterCAC/RM 17-1969GravimetryIOlive oilSesameseed oil testAOCS Cb 2-40ColorimetryIPalm oilDensity, apparentISO 6993:1995 with the appropriateconversion factorPycnometryIPalm oilSlip pointAOCS 3-25 (1992)Open ended capillary tube (for 60 C)IFish and fishery productsMercuryAOAC 977.15Flameless atomic absorptionspectrophotometryFish and fishery products: Frozen fishand fishery productsThawing and cookingproceduresDescribed in the StandardsThawing and heatingICanned crab meatDrained weightDescribed in the StandardWeighingICanned crab meatNet weightDescribed in the StandardWeighingICanned finfish (mackerel and jackmackerel)Net weightDescribed in the StandardWeighingIFish and Fishery Products12III

Commodity StandardProvisionMethodPrincipleCanned salmonDefectivesDescribed in the StandardClassificationICanned salmonNet weightDescribed in the StandardWeighingICanned sardines and sardine-typeproductsNet weightDescribed in the StandardWeighingICanned shrimps or prawnsDrained weightDescribed in the StandardDrainingICanned shrimps or prawnsNet weightDescribed in the StandardWeighingICanned shrimps or prawnsSize, determination ofDescribed in the StandardNumber per 100 gICanned tuna and bonitoNet weightDescribed in the StandardWeighingIQuick frozen blocks of fish fillet,minced fish flesh and mixtures offillets and minced fish fleshNet content of frozon fishblocks covered by glazeDescribed in the StandardGravimetryIQuick frozen blocks of fish fillet,minced fish flesh and mixtures offillets and minced fish fleshParasitesDescribed in the StandardVisual examinationIQuick frozen blocks of fish fillet,minced fish flesh and mixtures offillets and minced fish fleshProportion of fish fillet andminced fishAOAC 988.09Physical separationIQuick frozen blocks of fish fillet,minced fish flesh and mixtures offillets and minced fish fleshSodium chlorideAOAC 971.21 (Codex general method)PotentiometryIIQuick frozen fish filletsNet weight of productscovered by glazeDescribed in the StandardWater spraying and sievingIHistamineQuick frozen fish sticks (fish fingers)and fish portions - Breaded or in batterAOAC 977.13FluorimetryIIQuick frozen fish sticks (fish fingers)Net weightand fish portions - Breaded or in batterDescribed in the StandardWeighingIQuick frozen fish sticks (fish fingers)Proportion of fish fillet andand fish portions - Breaded or in batter minced fishAOAC 988.09GravimetryI13Type

Commodity StandardProvisionMethodPrincipleTypeQuick frozen fish sticks (fish fingers)Proportion of fish fillet andand fish portions - Breaded or in batter minced fish (for certain fishspecies with soft flesh, such ashakes from the SouthernHemisphere)Described in the StandardGravimetryIVSodium chlorideQuick frozen fish sticks (fish fingers)and fish portions - Breaded or in batterAOAC 971.27 (Codex general method)PotentiometryIIIFoods for Special Dietary UsesSpecial foodsAshAOAC 942.05GravimetrySpecial foodsCalciumAOAC 984.27ICP emission spectrometryIIISpecial foodsCalories by calculationMethod described in CAC/VOL IX-Ed.1,Part IIICalculation methodIIISpecial foodsCarbohydratesMethod described in CAC/VOL IX-Ed.1,Part IIICalculationIIISpecial foodsChlorideAOAC 971.27 (Codex general method)PotentiometryIISpecial foodsDietary fibre, totalAOAC 985.29Gravimetry (enzymatic digestion)ISpecial foodsFatCAC/RM 55-1976Gravimetry (extraction)ISpecial foodsFat in foods not containingstarch, meat or vegetableproductsCAC/RM 1-1973, B-2GravimetryISpecial foodsFill of containersCAC/RM 46-1972WeighingISpecial foodsFolic acidAOAC 944.12MicrobioassayIISpecial foodsLinoleate (in the form ofglycerides)AOAC 922.06; 969.33; 963.22Acid hydrolysis, preparation ofmethyl esters and gaschromatographyIISpecial foodsLinoleate (in the form ofglycerides)AOAC 922.06; 979.19Acid hydrolysis andspectrophotometryIII14

Commodity StandardProvisionMethodPrincipleSpecial foodsLoss on dryingAOAC 934.01AOAC 925.23GravimetryISpecial foodsLoss on drying (milk based)AOAC 925.23IDF Standard 21B:1987ISO 6731:1989GravimetryISpecial foodsNicotinamide for foods notbased on milkAOAC 961.14ColorimetryIISpecial foodsNicotinamide for milk-basedfoodsAOAC 944.13MicrobioassayIISpecial foodsPantothenic acid/enrichedfoodsAOAC 945.74MicrobioassayIISpecial foodsPantothenic acid/non-enrichedfoodsThe Analyst 89 (1964):1, 3-6, ibid. 232US Dept Agr., Agr. Handbook 97 (1965)MicrobioassayIVSpecial foodsPhosphorousAOAC 986.24Colorimetry (molybdovanadate)IISpecial foodsProtein efficiency ratio (PER)AOAC 960.48Rat bioassayISpecial foodsProtein, crudeMethod described in CAC/VOL IX-Ed. 1,Part IIITitrimetry, Kjeldahl digestionISpecial foodsRiboflavinAOAC 970.65FluorometryIISpecial foodsSodium and potassiumISO 8070:1987 (confirmed 1992)IDF Standard 119A:1987Flame emission spectrophotometryIISpecial foodsSodium and potassiumAOAC 984.27ICP emission spectrometryIIISpecial foodsThiamineAOAC 942.23FluorometryIISpecial foodsVitamin AAOAC 974.29ColorimetryIVSpecial foodsAOAC 941.15Vitamin A in foods in whichcarotenes have been added as asource of vitamin ASpectrophotometryIIISpecial foodsVitamin B12MicrobioassayIIAOAC 952.2015Type

Commodity StandardProvisionMethodPrincipleTypeSpecial foodsVitamin B6AOAC 961.15MicrobioassayIISpecial foodsVitamin CAOAC 967.22MicrofluorometryIISpecial foodsVitamin CAOAC 967.21Colorimetry (dichloroindophenol)IIISpecial foodsVitamin DAOAC 936.14Rat bioassayIVSpecial foodsVitamin D (D3, milk basedinfant formula)AOAC 992.26Liquid chromatographyIISpecial foodsVitamin EAOAC 971.30ColorimetryIVSpecial foodsVitamin E (milk based infantformula)AOAC 992.03Liquid chromatographyIIFoods with low-sodium content(including salt substitutes)IodineAOAC 925.56TitrimetryIIFoods with low-sodium content(including salt substitutes)Silica (colloidal, calciumsilicate)AOAC 950.85NGravimetryIVInfant formula and follow-up formulaDietary fibre, totalAOAC 991.43Gravimetry (enzymatic digestion)IInfant formula and follow-up formulaIodine (milk based formula)AOAC 992.24Ion-selective potentiometryIIInfant formula and follow-up formulaPantothenic acidAOAC 992.07MicrobioassayIIInfant formula and follow-up formulaPantothenic acidThe Analyst 89 (1964)(1) 3-6, 232US Dept Agr., Agr. Handbook 97 (1965)MicrobioassayIVInfant formula and follow-up formulaVitamin AAOAC 974.29ColorimetryIVInfant formula and follow-up formulaVitamin A (retinol isomers)AOAC 992.04Liquid chromatographyIIInfant formula and follow-up formulaVitamin A (retinol)AOAC 992.06Liquid chromatographyIIInfant

Soy protein products Moisture AOAC 925.09 Gravimetry (vacuum oven) I Soy protein products Protein AOAC 955.04D (using factor 6.25) Titrimetry , Kjeldahl digestion II Vegetable protein products Ash AOAC 923.03 ISO 2171:1993 (Method B) Gravimetry, Direct I Vegetable protein products Fat CAC/RM 55-1976 - Method 1 Gravimetry (extraction) I

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