MIL-G-53006 7June1982 MILITARYSPECIFICATION GASCHOL ...everyspec.com/MIL-SPECS/MIL-SPECS-MIL-G/download.php?spec=MIL-G-5300… · MIL-G-53006 7June1982 MILITARYSPECIFICATION...

MIL-G-530067 June1982

MILITARYSPECIFICATION

GASCHOL,AUTOMOTIW,LEADEDOR UNLEADED

Thisspecificationis approvedof the”Department

1. SCOPE.

of Defense.for by allDepartmentsand/@encies

1.2 Classification

leadedl.i Scope. Thisspecificationcoverscommercial or unleaded. foruse in automotive,spark-ignitionenginesunderallclimaticconditionswithintheContinentalUnitedStates(includingAlaskaandHawaii),(see6.1).

1.2.1 Grades. TheleadedandunleadedGasoholsfollows.major differencesamongthesegrades

Gasohol

shallbe of.threegradesasarein theantiknockindex

levels.

Grade ASTMantiknockindex

LimitedRegularPremium

1.2.2 Classes.Ea&miscibili~ses, asconditions(see3.6and

SeetableIVSeetableIVSeetableIV

gradeis dividedintofivevolatilityandwaterfollows,to provideforlocalandseasonalclimatictablesI, 11,IVand V):

I

‘Beneficialcorrwnents(recommendations,additions,deletions)and,

anypert~nentdatawhichmaybe of usein ’improvi~thikdocumentshouldbe addressedto: USArmyMobilityEquipmentResearch:’ad’DevelopWntCorrnnand,ATTN: DRDK-DS,FortBelvoir,VA 22M”0by’usingttiesel’%ddressedStandardizationDocunentImprovementProposal(DDForm1426)appearingattheed of thisdocumenterbyIletter. ., 8 [

Downloaded from http://www.everyspec.com

MIL-G-53CI06

Classlatility WaterMiscibility Conditionof use: ambienttemperature

A 1 .VeryI-btB 2 Hotc 3 WarmD 4 MildE 5 Cold

%0/

2. APPLICAEi_EDOCUMENTS

2.1 Governmentdocuments.

2.1.1 Specificationsandstandards.Unlessotherwises~ecified(see6.2),thefollowingspecificationsandstandardsof theissuelistedin thatissue’of

1

theDepartmentof DefenseIndexof SpecificationsandStandards(~DISS)specifiedin thesolicitation,formspecifiedherein.

SPECIFICATION

FEDERAL

vv-G-16m

STANDARDS

FEDERAL

FED-STD-791

a partof thisspecificationto theextent

- Gasoline,Automotive,Leadedor Unleaded.

‘4

-Lubricants,LiquidFuelsandRelatedProducts;Methodsof Testing.

MILITARY

I’4IL-STD-105

MIL-STD-25Q

SamplingProceduresandTablesInspectionby Attributes.

for

Packaging,Packing,andMarkingof PetroleumandRelatedProducts.

(Copiesof militaryspecificationsandstandardsrequiredby manufacturersinconnectionwith~ecificacquisitionfunctionsshouldbe obtainedfromtheprocuringactivityorasdi;ectedbythecontractingofficer.)

2.1.2 OtherGovernmentdocuments,drawings,andpublications.TheotherGovernmentdocuments,drawint$;andpublicationsforma partofspecificationto theextentspecifiedherein.

followingthis

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“W

iJ

M“IL-G-53Q06

U.S.ENVIRONMENTALPROTECTIONAGENCYPUBLICATION

EPAMSAPCAdvisoryCircularA/CNo. 26-B.

(EPApublicationsmaybe obtainedfromtheU.S.EnvironmentalProtectionAgency,401M Street,SW,Washington,DC 204@.)

CODEOF FEDERALREGULATIONS

27CFR 211-

27CFR 212-

49CFR 171-to 179

Bureauof Alcohol,Tobacco,andFirearmsR&gulationsRelatingto theDistributionand Useof DenaturedAlcoholandRum.Bureauof Alcohol,Tobacco,andFirearmsRegulationsRelatingto FormulasforDenaturedAlcoholandRum.Departmentof TransportationHa.zardousMaterialsRegulations.

(TheCodeof FederalRegulationsis availablefromtheSuperintendentofDocuments,US GovernmentPrintingOffice,Washington,DC 20402. OrdersforabovepublicationsshouldcitetheapplicableCFRpartnumber.)

2.2 Otherpublications.Thefollowingdocumentsforma partof thisspecificationto theextentspecifiedherein, Theissueof thedocumentswhichareindicatedas DoDadoptedshallbe the issuelistedin thecurrentDoDISSandthesupplementthereto,if applicable.

AkERICANSOCIETYFORTESTINGANDMATERIALS(ASTM)STANDARDS

D86- Distillationof PetroleumProducts.D 130- Detectionof CopperCorrosionfromPetroleumProductsby the Copper

StripTarnishTest.D 270- SamplingPetroleumand PetroleumProducts.D 323- VaporPressureof PetroleumProducts(ReidMethod).D 381- ExistentGumin Fuelsby JetEvaporation.D 525- OxidationStabilityof Gasoline(InductionPeriodMethod).D 1266-D 1613-D 1744-D 22~6-D 2533-D 2547-D 2551-D 2599-D 2622-“D2699-D 2700-D 2885-D 3116-D 3229-D 3231-D 3237-

Sulfurin PetroleumProductsand LiquifiedPetroleumGases.Acidityin VolatileSolventsandChemicalIntermediates.Waterin LiquidPetroleumProductsby KarlFisherReagent.ParticulateContaminatein AviationTurbineFuels,Appendix2.Vapor-LiquidRatioof Gasoline.Leadin Gasoline,VolumetricChromateMethod.VaporPressureof PetroleumProducts(MicroMethod),Leadin Gasolineby X-RaySpectrometry.SulfurF~yX-Ray$pectrometry.Knocl$Characteristicsof MotorFuelsby theResearchMethod.Knock,Qh@racteristicsof MotorFuelsby theMotorMethod.Reseax@ andMo$orMethodOctaneRatingsUsingOn-lineAnalyzers.TraceAmountsof Leadin Gasoline.LowLevelsof Leadin Gasolineby X-RaySpectrometry.Phosphorusin Gasoline.Leadin Gasolineby AtomicAbsorptionSpectrometry.

3


MIL-G-53006

D 3242- TotalAcidityin AviationTurbineFuels.E 203- TestforWaterUsingKarlFischerReagent.

Thetestmethodslistedaboveareincludedin Part23,24,25,29,or 47 of the WAnnualBookofASTM Standards.Themethodscanalsorepurchasedseparately.

(@plicationforcopiesshouldbe addressedto theAmericanSocietyforTestingandMaterials,1916RaceStreet,Philadel~ia,PA 19103.)

(Industryassociationspecificationsandstandardsaregenerallyavailableforreferencefromlibraries.TheyarealsodistributedamongtechnicalgroupsandusingFederalagencies.)

2.3 Orderof precedence.In theeventof a conflictbetweenthetextof thisspecificationandthereferencescitedherein,thetext-ofthisspecification“shalltakeprecedence.

3. REQUIREMENTS

3.1 Materials.TheGasoholshallbe composedof 90 percentvolumegasolineand 10 percentvolumeethylalcohol.A toleranceof 1 percentis established.

3.2 Legalrequirement.Gasoholfurnishedunderthisspecificationmustmeetallapplicablelegalrequirementsin accordancewiththeCodeof FederalRegulations.

3.3 Gasoline.Thegasolinesshallbe volatilehydrocarbonfuelsconformingto VV4-1690. Theymustcontainno oxygenizedblendingcomponents(alcoholsorethers)otherthanminoramountsusedas anti-icingadditives.“ ‘4;

3.4 Ethylalcohol.Theethylalcoholshallhavea minimumpurityof 98.5percentby volumeandshallbe completelydenatured.Thetotalvolumeofdenaturant,whichis approvedforfuelalcohol,maybe includedin thevolumeofethy-1alcoholprovidedit doesnotexceedthe5 percentvolumespecified.Theethylalcoholto be usedshallbe derivedfromrenewablesourcesandshallexcludealcoholmadefrompetroleum,naturalgas,andcoal.

3.5 Additives.TheunleadedGasoholmaycontainantioxidant,metaldeactivators,corrosioninhibitors,dyesandnomosphoruscontaining‘depositmodifiers.TheleadedGasoholmaycontainantioxidant,metaldeactivators,corrosion-inhibitors,leadantiknockcompounds,phosphoruscontainingdepositmodifiersanddyes.

3.5.1 Antiknockcompounds.The.leadantiknockcompoundpresentin thefinishedleadedGasoholshallnotexceedthelimitsspecifiedin tableIII. Theantiknockcompoundsor mixturesshallcontainappropriatequantitiesofscavengercompoundsas requiredin blendingautomotivegasolines.

3.5.2 Otheradditives.Additivesotherthanthosespecifiedabove,suchasdetergents,dispersants,emulsifiers,solventoils,etc.,willbe permittedin

4


MIL-G-53006

procurementof Gasoholprovidedpriorexaminationshaveverifiedtheabsenceoftheirpotentialdeleteriouseffects.Permissionfortheirusemustbe obtained

fromtheUS ArmyMobilityEquipmentResearchandDevelopmentCommand,ATTN:DRDK-GL,FortBelVOir~vA 220a0 Thisrequestshallbe accompaniedbyareportshowingthechemicalpropertiesof theadditive,laborato~yengineperformancetest-sandcontrolledfleettestsusingfuelscontainingthemaximumrecommendedconcentrationof theadditive.Suchadditivesmustbe compatible

withanyof thematerialsincludedin thisspecificationandmustnotappreciablyaffectthe specifiedchemicalor physicalproperties.

3.6 Physicalandchemicalrequirements.Thephysicalandchemicalrequirementsof Gasoholshallbe as specifiedm tables1, II,III,andIV. ‘

T9BLE1. Volatilityclasses.

characteristic

distillationl~oevapt,‘C max

50% evap.,‘C min

50%evap.,‘C max

9wo evap.,OC max

Endpoint,‘C max~/

Reidvapor_~ressure(RVP’kPamax~i

Temperature,‘CVapor/Liquid(v/L)ratio=

lassA

(70)

(77)

121

190

225

(62)

(60)

RecIirement4/ 1ClassC lassD ClassE

,I

ClassB

(65)

(77)

118

190

225

(69)

(56)I

(60)

(77)

116

185

225

(79)

(51)

:55)

:77)

113

U35

225

(93)

(47)

(50)

(77)

110

185

225

(103)

(41)

~/ Valuesgivenpertainto productat pointof acceptance.Limitingvaluesshownin parenthesisareapplicableonly-tothebasegasoline,VV-G-1690.

2/ Endpointincludesadditiveresidueif present.~/ Reidvaporpressurevaluesaregivenforeachclassbut theyarenot

limiting.Thelimitingcriteriaforcontrollingoverallhotfuelhandling(vaporlock,etc.)is thetemperatureat whichtheV/L = 20.

4/ At 763mm. Hg.pressure(101.3kPa).

5

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MIL-G-53006

TABLE11. Watermiscibility’

Characteristic

Watertolerance;Phaseseparationafteradditionof 0.1%volwatershallnotoccurat a temperature(°C)greaterthan,

RequirementClass1 Class2 Class3 - Class4 Class5

5 0 -lo -25 _@..

T/!BLEIII. Chemicalrequirements.

●

Property

Unwashedgum,mg/100ml

Existentgum,”m@100ml,max

Sulfur,% wt,max

unleadedleaded

Particulates~

Water,ppm

Corrosivenessto copper

Leadcontent,g/1 (g/gal

unleaded

500

max

c, max

Oxidationstability,minutes,min

Ethylalcoholz/% Vol

Water,% wt,max

Organicacidity(FreeKCWg (wt%),max

acidas Acetic),mg of

Value

Report

5

00

1015

Report

Report

1A

0.013(0.05201.1(4.2)

240

10 (@%)

1.25

0.070 0.0076

6v

.


‘L’

MIL-G-5~06

TABLE111. Chemicalrequirements.(Continued)

F

Denaturant:% vol,maxType

ltheralcohols,% vol,max

3therimpurities,max

‘hosphorus,g/1 (g/gal)~max

unleaded

Value

5Report

1.0

Trace

.

0.0013(0.005)

1/ Run accordingtoASTM D 2276,Appendix2, exceptuse0.45micronmembrane

filter.2/ Theintentionaladditionofleadcompoundsis notpermitted.~/ Ethylalcoholmusthavea minimumpurityof98.5%. Requirements—

shownapplyonlyto ethylalcohol.

TABLEIV. Antiknockqualityrequirements!-./.

lasoholGrade:;tateGroup .

LIMITED#1#2#3#4#5#6

REGULlM3#1itz#3#4#5#6

PREMIUM#1#2

GRADE:

GRADE:

GR.ADE:

AntiknockIndexg/(R+M)/2Minimurn

Leadedm

unleaded~

86.3 84.385.5 83.584.8 82.884.0 82.082.5 “ 80.5

‘ 8988.587.587.587.086.0

9392.5

87.0?/86.385.584.884.082.5

90.089.5

‘u . 7


MIL-G-53006

TABLEIV. AntiknockqualityrequirementsL/, (Continued)

IAntiknockIndex~/

GasoholGrade: (R+M)/2StateGroup Minimum

PREMIUMGRADE: (Continued) Leaded Unleaded#1 87,0 “ 85.0#3 91.5 88.5#4 . 91.5 88.5#5 91.0 88.0#6 ~ 90.0 87.0

~/ Seefigurel.2/ Averageof theResearchOctaneNumberandtheMotorOctaneNumber.~/ MinimumMotorOctaneNumbermustbe 82. 0

3.7 Volatility.Thevolatilityclassesof Gasoholas definedin tableIshallbe suppliedaccordingto therequirementsof tableV. Whenalternateclassesarepermitted,thecontractormayprovideeitherclass. Adjustmentsinaltitudeandclimaticconditionshavebeenconsideredin preparingthisdistributionscheduleto minimizeoperationalproblemsarisingfromhot fuelhandlingandcoldstartirg.Thelimitingguidetemperatures,maximumninetiethpercentile,utilizedfordeterminingthevolatilityclassdistributionareshownbelow:

Class Dailyhi@ temperature .

A Greaterthan43°C (109°F)B Lessthan43°C (109°F)c Lessthan36°C (95°F)D Lessthan29°C (84°F)E Lessthan21°C (70°F)

3.8 Watermiscibility,Thewatermiscibilityclassesof Gasoholas definedin table11 shallbe suppliedaccordingto therequirementsof.tableVI. Thelimitingguidetemperatures,minimumtenthpercentileswhichhavebeenroundedfor.theareasandperiodstabulatedexceptforclassestablishthewatermiscibilityclassesshownbelow:

1, havebeenusedto

Class

12345

NiMlv LowTem~erature

Greaterthan5° C (41°F)Greaterthan0°C (32°F)Greaterthan-lOOC (14°F)Greaterthan-25°C (-13°F)Greaterthan-40°C (-40°F)

8 ‘d


MIL-G-53006

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‘?J2F-%a-$

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MIL-G-53006

3.9 Workmanship.TheGasoholshallbe visuallyfreefromundissolvedwater,sediment,andsuspendedmatterandshallbe clearandbricJtat theambienttemperatureor 21°C whicheveris higher.

3.10 Overseasprocurement.Unlessotherwisespecifiedin thecontractorpurchaseorder(see6.2),Gasoholprocuredoverseasshallconformto therequirementsof thisspecificationat thetimeof delivery.

10 ●

I


L #

MIL-G-!53006

TN3LEV. [email protected]/.

State

AlabamaAlaskaArizonaArkansasCalifornia:Z/NorthCoastSouthCoastSoutheastInterior

ColoradoConnecticutDelawareDist.of ColumbiaFloridaGeorgiaHawaiiIdahoIllinois:N 40°Lat.S 40° La.t

IndiahaIowaKansasKentuckyLouisianaMaineMarylandMassachusettsMichiganMinnesotaMississippiMissouriMontanaNebraskaNevada:Ns

New

NewF/ewNs

New

38°Lat.38°Lat.HampshireJerseyMexico:34°Lat.34° Lat.York

NorthNorthChio

CarolinaDakota.

Jan

DEDE/D

E/DDDE/DEEEEDDcE

EEEEEEDEEEEEDEEE

EDEE

E/DDEE/DEE

Feb

DED/CD

DDD/CDE/I)EEEDDcE/D

EEEEE/I)E/DDEEEEEDE/DEE

E/l)D/CEE

DD/CEDEE

FE

D/CEC/BD/C

DDCADD/CE/DE/DE/DD/CD/CcD

E/DE/DEMIE/OD/CDD/CE/DE/I)E/DE/DE/DD/CDE/Dm

DC/BE/l)E/G

I

D/c

C/BE/DDEmE/D

Apr

cEBc

D/CD/CBD/CcDDDcccD/C

DD/CDD/CcD/CcDDDDDcD/CD/CD/C

D/CBDD

‘cmBDD/CDD

F@-

CE/DB/Ac

cC/BB/AC/BCAD/CD/CD/CcccC/B

D/CcD/CccmccD/CD/CD/CD/CD/CcccmC/B

cmWAD/CD/C

B/AB/AD/CcD/CD/C

11

Jun

cEA)dcm

cmBABBccccccB

cccC/BBccccccccC/BBB

BAcc

AAccCA3c

Tii

C/BDAB

BBABB/AccccC/BcB

cC/BcB/CBccmcccccC/ElBBB

BAcc

AAcC/BBc

Au~

BDAB

BBABA/BccccBcB

cB/CccBcBcccccBBBB

BAcc

A/BAcBBc

Sept

B/CD/EAB/C

BBABBC/DcccB/CcB

ccccBcB/CC/DcC/DcmcB/CB/CB/cB

BAcmC/D

BA/BCA)B/CB/Cc

Ott

cEA/Bcm

B/CB/CA/BB/CB/CDcmC/DcccB/C

CA)C/DCA)C/DB/CC/DcDcmDDC/DcC/DcmB/C

B/CA/BDD

0/CB/CDC/DCA)c/o

Nov

:/DrLB/CD

cm:/DB/CC/DcmD/ED/ED/ECA)C/DcC/D

D/EDD/ED/EcmD/EcmD/ED/ED/ED/ED/ECA)DD/EC/D

CA)B/CD/ED

cmC/D13/EDD/EWE

E-

3~:/03/E

)/E2C/DD/ED/EEEEDDcD/E

ED/EEED/EEDEEEEEDD/EED/E

D/EC/DEE

DDED/EEE


. .

MIL-G-53006

TABLEV. Geographicalandseasonaldistributionof volatilityclasses~/.

(

‘State

OklahomaOregon:E 122°long.w 1220 long.

PennsylvaniaRhodeIslandSouthCarolinaSouthDakotaTennesseeTexas:E ~9° long.W 99° long.

JtahYermontiirginiaWashington:E 122°long.w 122° long.

lestVirginia~isconsin~yoming ..

m

E/D

EEEEDEE/D

DDEEE

EEE

-FEE

D

E/l)E/DEEDED

DD/CE/I)EEM)

EEEEEJ

-m

D/C

Df)EA)E/DDE/DD

D/CC/BDE/DD

Em ;E/D~En :VD:A)

*

c

DDDD0/CD/CD/C

cB)/c))/c

1)1)I/c

T@

C/B

D/CD/CD/CD/CcC/Bc

BB/AC/ElD/Cc

D/CD/CD/CD/Ccm

-3iE

B

cmccccBc

CAABcc

cmcccBI-J

-m

B

BccccmBCA

BAB/Acc

Bmu-iuT

;

~

B

BcccBBB

BAAA3cc

B’cC(c

B B/C

B/C CA)c C/Dcm DC/D “ DB/C CA)B B/CB/C CA)

B B/CA/B B/CB w cC/D Dc CA)

B/C cmc C/D.c cmc C/D

IIBB B/C

m

C/D

DD/ED/ED/EDC/DD

cmC/DC/DD/ED/E

D/ED/ED/EYE2AI

~/ Wheretwoclassesaregiven(i.e.,A/B,C/b,etc.),thisremesentsatransitionalmonthin thatbothclassesare-permitted. ‘

~\ Detailsof statedivisionbycountyas indicated:

California,NorthCoast-

California,Interior .

California,SouthCoast-

California,Southeast -

%----

D/E

D/EEEEDD/ED/E

DDD/EEE

EEEED/E

w’

Alameda,Contra~sta, DelPbrte,Humboldt,Lake,Marin,Mendocino,Monterey,Napa?SanBeni~o,SanFrancisco,SanMateo,SantaClara,SantaCruz,Solano,Sonoma,Trinity. “Alpine,Amador,Butte,Calaveras,Colusa,ElDorado,Fresno,Glenn,Kern(exceptthatportionlyingeastof theLosArigelesCountyAqueduct),Kings,Lassen,Madera,Mariposa,Merced,Modoc,NevadajPlacer,Plumas,Sacramento,SanJoaquin,Shasta,Sierra,Siskiyou,Stanislaus,Sutter,Tehama,Tulare,Tuolumne,Yolo,YubaLosAngeles(exceptthatportionnorthof theSanGabrielMountainrangeandeastof theLosAngelesCountyAqueduct),Orange,SanDiego,SanLuisObispo,SantaBarbara,VenturaImperial,Inyo,Kern(thatportionlyirigeastoftheLosl@gelesCounty~ueduct),LosAngeles(thatportionnorthof theSanGabrielMountainrangeandeastof theLosAngelesCountyAqueduct),Mono,Riverside,SanBernardino

12.

.,I

‘w’

,.,,.i

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MIL-G-53006

$4u+

TABLEVI. GeoaraDhicalandseasonaldistributionof classesforwatermiscibility.

StateAlabamaAlaskaArizonaN. of34° LatitudeS. of 34° Latitude

RrkansasCalifornia~/NorthCoastSouthcoastInterior

DloradoE. of105° Lo~.W. of 105°Long.

Connecticutlelawarelist,of Columbia‘loridaN. of29° LatitudeS. of 29° Latitude

~eorgiaiawaii[dahoIllinois[ndianaIowa(ansas -(entucky.ouisianadai.nelaryland~assachusettsdichigandinnesotaMississippiiissouri!ontanaJebraskaJevadaN. of38° LatitudeS. of 38° Latutude

JewHampshire@w JerseyJewMexicoN. of34° LatitudeS. of 34° Latitude

EiT5

433

323

54433

32314444433444453454

4344

43

Feb35

433

223

44433

213144444334344534“44

4344

43

ET5

322

223

44323

21314444432433442344

4233

32

lipF23

211

112

33212

112“13333321322331233

3132

21

May12

111

111

22111

11112222211211.221122

2121

11

F12

111

111

11111

11111111111111111111

1111

11

mr1

111

111

11111

11111111111111111111

1111

11

Aug11

11“1

111

11111

11111111111111111111

1111

11

.

Sept12

211

111

22111

11112112211211121122

2121

22

J..

~

Ott23

311

i-12

33222

11213223311322232233

3132

33

Nov-34

422

223

44333

213143343223333433.44

4233

43

ET4

433

323

44433

32314444433434453444

4343

43


MIL-G-53C)06

TABLEVI. Geographicalandseasonaldistributionof classesforwatermiscibility.

StateNewYorkNorthCarolinaNorthDakotaOhioOklahomaOregonE, of122° Long.W. of 122°Long.

PennsylvaniaN. of41° Long.

S. of 41°Long.RhodeIslandSouthCarolinaSouthDakotaTennessee“TexasN. of 31°LatitudeS. of 31°Latitude

UtahVermontVirginiaWashingtonE. oflzz” Low.W. of 122°Long.

WestVirginiaflisconsinWyoming

1/ California.Nort- ,

mT3544

34

444353

43443

34454

Feb43543

34

4’4434.3

32443

33444

Coast-

California,SouthCoast-

.California,Interior

lvhT43433

33

433343

32343

33344

@F-32322

22

322232

212

r

32

22233

May21211

11

2’-1

i121

11121

11122

ntra

~n11111

11

111111

11111

11111

m

1111

11

111111

11111

11111

ml ‘Aug1“ ‘1

1111

11

111111

1.1111

11111

I, DelNor

Sept21.121

12

111121

11221

12222

mT2232

“23

222232

21332

23333

e,Hum~

Nov33343

34

333243

32333

33344

,m

Ez-3453

34

444343

33443

34444

Marin,Mendocino,Monterey,Napa~SanBenitojSanFrancisco,SanMateo,SantaClara,SantaCruz,Solano,Sonoma,Trinity.Orange,SanDiego,SanLuisObispo,SantaBarbara,Ventura,LosAngeles(exceptthatportionnorthoftheSan’Gabriel-Mountainrangeandeastof theLosAngelesLassen,Amador,Fresno,eastofMadera,

CountyAqueduct).Modoc,Plumas,Sierra,Siskiyou,Alpine,Butte,Calaveras,Colusa,El Dorado,Glenn,Kern(exceptthatportionlyingtheLosAngelesCountyAqueduct),Ki~s,Mariposa,Merced,Placer,Sacramento,San

‘u’

Joaquin,Shasta,Stanislaus,Wtter, Tehama,Tulare,Tuolumne,Yolo,Yuba,Nevada,Imperial,Riverside,SanBernardino,LosAngeles(thatportionnorthof theSanGarbrielMountainrangeandeastof theLosAngelesCountyPqueduct),Mono,Inyo,Kern(thatportionlyi~east of theLosAngelesCountyAqueduct).

14 ‘w’


MIL-G-53006

4. QUALITYASSLHWCEPROVISIONS

.

w

.

4.1 Responsibilityforinspection.Unlessotherwisespecifiedin thecontractor purchaseorder,thecontractoris responsiblefortheperformanceofall inspectionrequirementsas specifiedherein. Exceptas otherwisespecifiedin thecontractor order,the contractormayusehisownor anyotherfacilitiesuitablefortheperformanceof inspectionrequirementsspecifiedherein.

4.2 Lot.,

4.2.1“Bulklot. An indefinitequantityofa homogeneousblendof Gasoholofonegradeandoneclass,offeredforacceptancein a single,isolatedcontaineror manufacturedin a singleplantrun (notexceeding24 hours),throughthesameprocessingequipment,withno changein the ingredientmaterials.

4.2.2 packagedlot..An indefinitenumberof 55-gallondrumsor otherunitcontainersof identicalsizeandtype,offeredforacceptanceandfilledwithahomogeneousblendof Gasoholof onegradeandoneclass,froma single,isolatecontainer;or filledwitha homogeneousblendof Gasoholof one gradeandoneclass,manufacturedin a singleplantrun (notexceeding24 hours),throughthesameprocessingequipment,withno changein theingredientmaterials.

4.3 Sampling.

4.3.1 Samplinqfortheinspectionof filledcontainers.Takea randomsampleof filledcontainersfromeachlotin accordancewithMIL-STD-105,at inspectiolevelII and acceptablequalitylevel(AQL)= for2.5 percentdefective.

4.3.2 Samplingfortests. Takesamplesfortestin accordancewithASTMD270.

4.4 Inspection.Performinspectionin accordancewithmethod9@l ofFED-STD-791.

4.4.1 Examinationof filledcontainers.Examinesamplestakenin accordancewith4.3.1forcompliancewithMIL-STD-290withregardto fill,closure,sealing,leakage,packaging,packing,andmarkingrequirements.Rejectany

containerhavingoneor moredefectsor undertherequiredfill. Rejectthelotrepresentedby a samplei’fthenumberof defectiveor underfilledcontainersexceedstheacceptancenumberfortheappropriatesamplingplanof MIL-STD-105

4.5 Classificationof tests. Alltestsarequalityconformancetests,

4.6 Testmethods. Performstestsin accordancewithtableVII.

15


—

MIL-G-53006

TABLEVII, Testmethods.

Test

EthylalcoholcontentOtheralcoholor ethersDistillationExistentgutiunwashedgumSulfurPhosphorus_eadcontent

danganesecontentz/corrosiveness)xidationstability#ater%rticulatecontamination(neckcharacteristics,researchoctanemethod(neckcharacteristics,motoroctanemethod(neckcharacteristics,researchandmotoroctanemethodsusingon-lineanalyzers

iatertolerance

NeutralizationNumber,Aciditydetectionof MethylAlcoholiapor-liquidratio(V/L)?eidvaporpressures

.

1/—

2/

3/

4/

y

g

7/

b

t

ASTMMethodNo.

SeeAppendix,TestMethod1SeeAppendix,TestMethod5D 86D 381D 12660rD 2622L/D 3231D 2547,D 2599,D 3116,D 3237?/ orD 3229

D 130D 525D 17440rE 203&D 2276D 2699D 2700

.0 2885SeeAppendix,TestMethods2and42D 1613or D 3242SeeAppendix,TestMethod3D 25339D3230r D 2551LJ

-,

ASTMD 2622,Sulfurin PetroleumProducts(x-rayspectrogra~icmethod)maybe usedas an alternativemethodfordeterminingsulfurcontent,ASTMD 3237,Leadin Gasolineby atomicabsorptionspectrometryisdesignatedas therefereemethod,othermethodsmay be usedas alternates.D 3237is themethodtheEnvironmentalProtectionAgency(EPA)hasdesignatedforunleadedgasolines.Manganesewillbe determinedby themethodgivenin theEPA MSAPCAdvisoryCircularA/CNo,26-B,p 4 or otherequivalentmethods,ASTMD1744is to be usedin thedeterminationof waterin theGasohol,ASTME203is to be usedin thedeterminationof waterin theethanol.Eithermethodmaybe usedforthedeterminationof watertolerance;howeverin theeventof a discrepancy,TestMethod4 willbe usedas therefereemethod.ASTMD2533mustremodifiedto usemercuryin thelevelingbulbin placeofglycerin.ASTMD 2551,VaporPressuresof PetroleumProducts(Micromethod)maybe usedaG an alternativemethodfordeterminingvaporpressure.ASTMD323mustbemodifiedas describedin theASTMInformationDocumenton Gasoholin the1981ASTMStandardPartNo.23.

16


MIL-G-53C)06

5. PACKAGING

5.1 Containersandmarking.Unlessotherwisespecifiedin thecontract(see6.2),containersandmarkingshallbe in accordancewithMIL-STD-290,

6, NOTES

6.1 Intendeduse. Gasoholfurnishedunderthisspecificationis intendedforimmediateusein allspark-ignitioninternal-combustionenginesandallotherequipmentdesignedto operateon gasoline.Gasohol,aswell as gasolinesprocuredunderVV-G-1960,is not intendedforstaticstorageenvironments.Itshouldnotbe storedformorethan60 dayswithoutreplenishmentbecauseofpossibleauto-oxidationandwaterabsorptionwhichcanresultin deteriorationof theoverallqualityof gasohol.

Baseduponrecentlycompletedresearchinvestigations,satisfactoryutilizationof gasoholwilloccurif the followingconditionsandreservationsareadheredto:

a.

b,

c.

d.

601,11971(or

Gasoholshouldneverbe introducedintoanyaboveor undergroundtankagewherewaterbottomsor sumpsareknownto exist. Thisaccumulatedwaterwillcauseextractionof ethylalcoholandaresultantlossin product.Wheregasoholhasbeeninadvertentlycontaminatedwithwateranda twophasemixtureexists,separationof waterwithuseof standardmilitarydesignedfilter-separators(asis normallydonewithgasolineturbinefuel,etc.)is notrecommended.Specificinstructionscanbe providedfromtheUS ArmyMobilityEquipmentResearchandDevelopmentCommand,ATTN: DRDNE-GL,FortBelvoir,VA 22060.Wherewatercontaminationin gasoholis suspect,microbiologicalorganismsmayproliferatein thoseareaswhererelativelymildorwarmambienttemperatureexist. To controlthisgrowthofmicrGorganisms,theadditionof an approvedbiocideadditivemayberequired.Specificinstructionrelativeto thebiocideadditioncanbe providedfromtheabovementionedaddress[see6.1(b)1.“Gasoholis notrecommendedforusedin thosemultifiredengines(LD/LDT/LDS-495seriesandLDS-427)currentlypoweringthe2-1/2-tonand5-tonmilitarytruckfleet. Theadditionof ethylalcoholtogasolineproducesan unusuallylowcetanenumberwhicheffectsstartabilityandcreatesabnormalcombustionproblems,

Limited-gradeGasohol.Limited-gradeGasoholis intendedforusein~ater)commercialandadministrativevehiclesequippedwiththelower

compressionratiospark-ignitionenginesdesignedto operateon a reducedantiknockqualityproduct.Thisgrademaybe usedin manyearliermodelvehiclesequippedwithlowercompressionenginesdescribedaboveor whichhavebeenmodifiedto accomodatethisgrade(seel.2.1).

6.1.2 Regular-gradeGasohol.Regular-gradeGasoholis intendedforuseinspark-ignitionenginesdesignedto operatewitha productof thisantiknock

.17


— —

MIL-G-53006

qualityor,whenso requiredby equipmentmanufacturer’srecommendations(see1.2.1)0 Thisgrademaybe requiredin 1971or latermodelvehiclesthathaveantiknockrequirementswhichexceedthoseof limitedgrade.

6.1.3 Premium-gradeGasohol.PremiuwgradeGasoholis intendedforuseinspark-ignitionenginesdesignedto operatewitha productof thisantiknockqualityor whenso requiredby equipmentmanufacturer’srecommendations(see1.2.1). Thisgrademaybe requiredin 1971or latermodelvehiclesthathaveantiknockrequirementswhichexceedthoseof limitedgrade.

6.2 Orderingdata. Purchasersshouldselectthe preferredoptionspermittedhereinand includethe followinginformationin procurementdocuments:

(a) Title,number,anddateof thisspecification,(b) Gradeandclassesof Gasoholrequired(seel.2and3.6).(c) @antityof Gasoholrequired.Theunitof purchaseis oneUS gallon

(3.7851iters)at60°F (15.6°C).(d) Typeandsizeof containersrequired(see5.1).(e) Markingrequired(see5.1). ,(f) ~rity of ethylalcoholanddenaturantused,

6.3applyurider

Definitions.Thedesignations‘ftimited,’t“Regular)llandlfPremium’lgradesto gasolinesfurnishedunderVV-G-1690in additionto theGasoholgradesthisspecification.

6.3.1 Leadantiknock.UnleadedGasoholis definedas Gasoholto whichtheadditionof leadantiknockis notpermitted-.LeadantiknockpresentshallnotexceedthatamountwhichresultsfromcontaminationwhengoodrefineryanddistributionpracticesarefollowedandshaU notexceed0.013g/1(O.05g/gal). Additionally,thephosphoruscontentof unleadedGasoholshallnotexceed0.0013g/1 (0.005g/gal).

Custodians: Preparingactivity:Army- ME Army- NENavy- YDAirForce- 68 Project9130-0105

Reviewactivities:Army- MDNavy- SAY.SH,MCDLA- PS

‘J

Useractivity:Army- AT

.,. “

18 u’


MIL-G-53Q06

APPENDIX

GASOHOL,AUTOMOTIVE,LEADEDOR UNLEADED

10* SCOPE

10.1 Scope. Thetestmethodscontainedwithinthisappendixareto determine”theamountof denaturedalcohol(ethanol)in Gasohol(TestMethod1),watertoleranceof Gasohol(TestMethods2 and4),detectionof methylalcoholinGasohol(TestMethod3) anddete~ini~ oxygenatesin @sohol (TestMethod5)”Thisappendixis a mandatorypartof thespecification.Theinformationcontainedhereinis forcompliance.

20,

20.1

APPLICA3LED~UWNTS

AbfiRICANSOCIETYFORTESTINGAND M4TERIALS

‘w’

ASTMD2500- CloudPointof PetroleumOils

(Applicationforcopiesshouldbe addressedto theAmericanSocietyforTestingandMaterials,1916RaceStreet,Philadel~ia,PA 19103.)

19


.

MIL-G-53006

APPENDIX

TESTMETHOD1

TESTMETHODFORDETERMININGTHEAMOUNTOFDENATUREDETHyLAL~HOL (ETHANOL)INGASCHOL

w

1. SC@E

1.1 Thismethodis fordeterminingtheamountofdenatureo’ethanolinGasohol,Thismethodis intendedto providea simpleandreliablemeansfordeterminationof theethylalcoholcontentof Gasohol,Quantitativetechniquesemployinggas liquidchromatographyandinfraredspectroscopybeingdevelopedwhitiwillbe availableshortly,

2. SUMMARYOF METHOD

arecurrently

2.1 A sampleof Gasoholis shakenat roomtemperaturewithethyleneglyco},Thechangein volumeof theethyleneglycollayeris relatedto theamountofdenaturedethanolin thesampleof Gasohol,

30 APPARATUS

3.1 Graduatedglassmixingcylinder,glass-stoppe~ed,100-mlwithl-mlgraduations,Thismustbe capableof acceptinga totalvolumeof in exeessof110ml withthestopperin place.

3.2 Pipet,volumetric,10 ml,type1,classB.

3.3 Pipetfilleror bulb,Koroseal,30 ml,

40 REAGENTS

4.1 Ethyleneglycol,reagentgradewith0.02g/1000ml methylvioletdyeadded(methyleneblueor otherwatersolubledyesmayalsobe used).

4.2 Acetone,commercialgrade.

5. PREPARATIONOF APPARATUS

5.1 Cleanthegraduatedcylinderthorouc$lybeforecarryingoutthistestasfollows.

5.1.1 Removetracesof fuelandethyleneglycolfromthegraduatedcylinderandstopperby flushingtwicewithacetoneanddraindry.

5,1.2 Rinsetwicewithsampleof Gasoholto be testedanddrain.

5,2 Cleanpipetby fillingtwicewithacetone,drain,andairdry,usingthebulb,

20


MIL-G-53006

APPENDIX

6. FFWEDURE

6.1 Measure1~ ml of Gasoholsampleto be testedintothegraduatedmixingcylinderat roomtemperatureto thenearest0.2ml andstopperthecylinder.

6.2 Removestopperandpipet10 ml of ethyleneglycolintothecylinderanastopperthecylinder.(Caution:.Drawethyleneglycolintothepipetusingthepi.petfilleror Korosealbulb. Do notsuckwithmouth(see9.2).

6.3 Invertthecylinderholdingthestopperwitha fingerandshakethecylinderbackand forthfor15 seconosusingabout10-inchstrokesfora totalof 25 backand forthstrokes,

6.4 Immediatelyplacethecylinderon a vibratiowfreesurface,andallowthecontentsto settleundisturbedfor5 minutes. >

6.5 Recordthevolumeof theethyleneglyco~alcohollayerin thebottomofthecylinderto the nearest0.2ml,

7. CALCULATION

7.1 Calculatethevolumepercentageof denaturedethanolusinga previouslypreparedcalibrationcurve,developedusingappropriatemixtures(i.e.,5, 8,10,12,15 and20 percent)of thespecifieddenaturedalcoholandblendedintothebasegasoline.

8. PRECISION

8.1 Repeatability- Duplicateresultsby thesameoperatorforGasoholcontaining10percentdenaturedethanolshouldbe consideredsuspectif theydifferby morethanl.Oml.

9. PRECAUTIONARYSTATEfVENTS

9.1 Gasohol- Volatileandextremelyflammable.Harmfulor.fatalifswallowed.Keepawayfromheat,sparks,or openflame. Keepcontainerclosed.Useonlyin wellventilatedarea. Avoidprolongedorrepeatedbreathingofvaporor contactwithskinor eyes.“ ‘Ifswallowed,do notinducevomitirg.Calla physicianimmediately.

9.2 Ethyleneglycol- Harmfulorfatalif swallowed.If swallowed,inducevomitingimmediately.ull a physicianimmediately.Washthoroughlyafterhandling.

9.3 Acetone- Extremelyflammable.awayfromheat,sparks,or openflame.adequateventilation.Avoidprolongedcontactwitheyesandskin.

Maycauseeyeandskinirritation.KeepKeepcontainerclosed. Usewithor repeatedbreathingof vapors.Avoid

21


1.

1.1

2.

2.1

MIL-G-5~06

APPENDIX

TESTMETHOD2

TESTltTHODFORDETERMININGTHEWATERTOLERANCEOF GASOHOL

SCOPE

Thismethodis usedto

SUMMARYOF METHID

Specificamountshazeappears,thewater

3.

3.1

3.2

3.3

4.

4.1

5.

5.1

5.2

measurethe

of wateraretoleranceof

watertoleranceof Gasohol.

Graduatedglassmixingcylinder,

addedto measuredvolumesof Gasohol.Ifthe Gasoholis unacceptable.

glassstoppered,100ml.

Micropipette,50 u1.

Micropipettetips,5-~0 u1,

REAGENTS “

Distilledwater

f%OCEDURE

Testis tobe conductedatroomtemperature(approximately70°F).

Rinsethe 100-mlmixingcylinderandstopper-withGasoholto be testedanddrain.

5.3 Fillthecylinderwith100ml of Gasoholsample.

5.4 Addwaterusingthe50-u1micropipetteanddisposabletipas follows:

Water MinimumAmbient Waterto addrolerance Temp.,‘F,where to theGasoho.ClassA/ Gasoholwillbe used sample,U1

1 41 1502 32 2003 14 2504 -13 3005 -40 35Q

#

a

~/ Seegeogra~icalapplicationtableVI.

22

.


MIL-G-53D~6

U5.5

6.

6.1

7.

7.1

7.2

Stopperthemixingcylinder

PRECAUTIONARYSTATEMENTS

Seeparagraph9.1 from“

REIWRT

est

APPENDIX

and shakesamplevigorouslyforoneminute.

ethod1.

If hazepersistsafterone-minuteshake,report:FAIL.

If no hazeappearsafterone+ninuteshake,report:PASS.

Lf’

23


1. SCOPE

1.1 Thisin Gasohol.

MIL-G-53006

APPENDIX

TESTtvETHOD3

FIELDTESTMETHODFOR THEDETECTIONOF tvETHYLALCOHOLAS AN ADULTERANTIN GASCHOL

methodcoversthedetectionof 1 percentor moreof mekhylalcohol

2. SM44RY 0FMETH3D

2.1 Thetestwasd&elopedto detectabout!1 percent(ormore)of methylalcoholin Gasohol.Thesensitivityof theprocedurecanbe increased,butconditionswereestablishedto preventa“falseconclusionbaseduponthepresenceof onlya smallamountof methylalcohol.A faintcoloris a negativetest. Undertheconditions,no testwasobserveo’forgasolineor Gasoholpreparedfromethanol.A strongpositivetestis obtainedif theGasoholcontains1 percentmethanol.Thetemperatureof lU1°C is recommendedas watercanbe boiledwithimmersionheatersoperatingoff an automobile battery(cigarettelic$terattachment)forfielduse. Theadditionof thesolidreagentsis notcriticalin amount. If a smallexcessof chromotropicacidispresent(asa precipitate)it doesno harm. Thetestformethanoliswellestablishedin theliteratureandhasbeenadoptedforthedetectionof methylalcoholin Gasohol.

3.

3.1

3,2

3.3

3.4

3.5

3.6

3.7

3.8

3.9

4.

4.1

APPARATUS

Flask,Erlenmeyer,glassstoppered,2~-ml withgraduations.

Bottles,reagent,narrowmouth,250-mlwithstoppers,3 each.

Cylinder,graduated,capacity100-ml,

Cylinder,graduated,capaci.ty 10+1.

Balance,fourbeam,Cen&O-GramOhaus.

Plastictransferpipets,capacity5-ml,length5-3/4-inch.

Testtube,OD 16-mm,length150+m.

Beaker,250+1 capacity.

Heater,capableof

REAGENTS

Phosphoricacid,5concentrated(87percent)

boilingwater.

percentsolution,preparedbydiluting6-mlofphosphoricacidto 100+1 withwater.

24 ‘u”


MIL-G-53006

APPENDIX

4.2 Potassiumpermanganatesolution,5 percentpreparedby adding5 g ofpotassiumpermanganateto 95 ml water.

4.3 Solidsodiumbisulfite(~ HS~) .

4.4 Sulfuricacid,72 percentsolution,preparedby adding150ml ofconcentratedsulfuricacid(98perceot)to 100ml of

4.5 Chromotropicacid(1,8- dihydroxynapthalene

5. PR02EDURE

water(see6.2).

- 3,6- disulfonicacid).

5.1 To 100ml of Gasoholadd50 ml of waterintoglassstopperedshakeandallowto settle.

5.2 Usinga medicinedropperor transferpipet,takea sampleoflayerandtransfer3 dropsto testtube. Do notusemouthpipeting

5,3 Add1-2dropsof the phosphoric acid solution and 1-2drops

Erlenmeyer,

thebottomtechniques.

of thepotassiumpermanganatesolutionto thetesttube. Shakefor1/2minute.

5.4 Add a small amountof sodiumbisulfite(approximately100mg),shakeandif the solutionis notdecolonized,addan additionalamountof sodiumbisulfite.If a brownprecipitateforms,addan additionaldropof thephosphoricacidsolutionto clearthesolution.

5.5 Add4 ml of thesulfuricacidsolutionanda smallamountof solidchromotropicacid(about50 mg).

5.6 Placethetesttubeintoa1000C) for1 minute. An intense,

6. PRECAUTIONARYSTATEMENTS

beakerof boilingwater(era waterbathblueto purplecoloris a positivetest.

at

6.1 The reaqents used in this test method may cause eye and skin irritation,burns,andmay-beharmfulor fatalif swallowed.Keepreagentcontainersclosed. Useonlyin wellventilatedareas. Avoidprolongedor repeatedbreathingof vaporandcontactwithskinor eyes.

6.2 Sulfuricacid- usegreatcautionin mixingwithevolutionthatcausesexplosivespatterimj.Alwaysaddthereverse.

waterdueto heattheacidto water,never

6.3 SeeTestMethodl,9.1.

25


.—

MIL-G-53006

APPENDIX

TESTl’ETHOD4

TESTMETHODFORDETERMININGTHEWATERTOLERAKEOF GASC1-10L,REFEREEMETH3D

1. SCWE “

1.1 Thismethodcoversthe abilityforGasoho\percentvolumewaterwithoutexhibitinganyphaseto specifiedtemperatures.

to tolerateadditionsofO.10separationafterbeingexposed

2* SUMMARYOF METHOD

2.1 AfteradditionofO.10 percentvolwatertoa 100ml Gasoholsample,thesolutionis cooledat a specifiedratedownto thetemperaturerequired.Theprescribedcoolingrateusedis identicalto thatspecifiedunderD 2~0,StandardTestMethodforCloudPointof PetroleumFuels. l’hetemperatureatwhicha “cloudlayerll,approximately1 to 1.5mm irrthickness,formsat thebottomof thetestjaris interpretedas the ~~watertoleranceor separation~oint~’. The minimum temperature specifiedis baseduponthewatermiscibilityclassificationof the Gasoholsanples;i.e.,class1 designedforhotenvironments.hasto meeta minimumtemperatureof 5° C (41°F) whereasclass5(desig~~dforcoldenvironments)mustmeeta minimumtemperatureof -40°C (-40°F).

3. APPARATUS

3.1 Testbottle,clearglass,cylindricalform,flatbottom,118to120 mlcapacity, 150mm in heightand 35 mm in diameter.Testbottlemustbeableto fitintoreceptacldja&etof coolingbathapparatususedto determineCloudPoint,D 2500. Testbottlesimilarto theonesidentifiedin chemicalcataloguesas OilDeterminationBottleor OilSampleBottle.

3.2 Thermometers,havingtherangesshownu~derparagraph4.2ofD 2500.

3.3 Cork,to fitthetestjar,boredcentrallyto takethetestthermometer.

3.4 Coolingbathapparatus,of thetypesspecifiedunderparagraph4.4throu@ 4.7 fordeterminingCloudPoint,D 25D0.

.3.5 Syringe,tuberculin,l.Oml capacity.

3.6 Graduatedglasscylinder,glass-stoppered,100+1, withl-mlgraduations.

4. REAGENT5

4.1 Water,distilled.

5. PROCEDURE

4’

26


MIL-G-53006

APPENDIX

5.1 Usingthesyringe,add0.10ml distilledwaterto the1OO-M1graduateocylinder.Transfer99.9ml of Gasoholto thegraduatedcylinderso thatthetotalvolumeis 100.Oml. Replacewithglassstopperandshakethorouc$ly.

5.2 TransfertheGasoholsolutionto the 125-mltallformsamplebottle.

5.3 Closethetestbottletic$tlyby corkcarryingthetestthermometer(usea thermometerappropriateto thetemperaturerequired).Adjustthepositionofthecorkandthethermometerso thatthecorkfitsti@tlyj thethermometerandthebottlearecoaxial,andthermometerbulbis locatedmidwayin theGasoholmixture.

5.4 Followingthesamec~olingrateas prescribedunderparagra~s5.5through5.7of D 2500fordeterminingCloudPointwiththeexceptionthateachtesttemperaturereadingshouldbe a multipleof 5° C (18°F),bringthetemperaturedownto thatspecified.

5.5 At thetesttemperature,removethetestbottlefromthecoolingjacketquickly,inspectfortheappearanceand‘he “clOudlayer”‘omationat ‘hebottomof thebottle.

5.6 If theinspectionrevealsa distinct“cloudlayer”of approximately1 to1.5mm in thickness,raisethetemperature1° C. If thecloudlayerdisappears

the sampleis acceptable.If thecloudlayerpersists!thesamPleis not .acceptable. .

6. PRECAUTION~YSTATEMENTS

6.1 Seeparagraph9.1fromTestMethod1.

7. REPORT

7.1 Reportthetesttemperaturerecordedin5.6 as the “watertolerancepoint”. ~is reportedtemperaturemustbe no greaterthanthatspecifiedforthewatermiscibilityclasstobe consideredacceptable.

27


.

MIL-G-53006

APPENDIX

TESTFIZTHOD5

TESTlETHODFORDETERMINE-OXYGENATESIN GASOHOLBY GASCEROM4TOGRAPHY

1. Scope

1.1 This method is fordeterminingtheamountof methanol,ethanol,isopropylalcohol,tert-butylalcohol,andtert-butyletherin hydrocarbonmixtures.

2, SUVIMARY0FMETH3D

2.1 A tw~columnchromatogra~icsystemconnectedto a thermalconductivitydetectoris used. A reproduciblevolumeof sampleis injectedintothecolumncontaininga polarliquidphasey Theli~t hydrocarbonsthrou@methylcyclopentaneareventedto theatmosphereas theyelute. Thecolumnisbackflushedimmediatelyaftertheelutionof methylcyclopentane,andthecomponentsremainingin thecolumnaredirectedintothesecondcolumncontainingan activesolid. In thiscolumn,theoxygenateselutebeforetheremaininghydrocarbons.Immediatelyaftertheoxgenatesof interesthaveeluted,the flowthrou@ theactivesolidcolumnis reversedto backflushtheremaininghydrocarbonsfromthecolumn. ~antitativeresultsareobtainedfrommeasuredareasof therecordedoxygenatepeaksby utilizingfactorsobtainedfromtheanalysesof blendsof knownoxygenatecontent.

3. APPARATUS

3.1 Gaschromatogra@- A gaschromatogra~equippedwitha dualthermalconductivitydetectorwithprovisionforinstallinga valvein thecolumnovenor otherheatedzone. Provisionmustalsobe made,eitherwithinthechromatographyor externally,to operatethesecondcolumnat a highertemperaturethanthefirstcolumnandthevalve.“

3.2 Valve- Eightportrotaryor equivalent.

3.3 Integrator- Electronicintegrationisrecommended.

3.4 Recorder- A l-mVrecorderwitha l-ret.fullscaleresponse.Ifelectronic”integrationis notused,a minimumchartwidthof2~ mm andaminimumchartspeedof l-cm/minuteis required.

3.5 Columnl - A stainlesssteelcolumn2.4+ long,3.5-mmID (3/16”00)packedwith80-100meshChromosorbP coatedto a 25 wt-percentlevelwithtetracyanoethylatedpentaerythritol(TCEPE).

w

‘d’

3.6 Column2- A stainlesssteelcolumn4.6-mlong,3.5-m ID (3/16”00)packedwith80-100meshPorapakP. “

●

28

,- .


MIL-G-53006

APPENDIX

4. REAGENTSANDMATERIALS

4.1 Carriergas- Chromatogra@icgradehelium (hydrogen shouldbe triedbeforethemethodis finalized).

4.2 Purecompoundsforcalibration- shallincludemethanol,isopropylalcohol,tert-butylalcohol,methyltert-butylether,methylcyclopentaneandtoluene.Thepurityof allthereagentspercentor greater.

ethanol,

shall be 99

5. PREPARATIONOF APFRARATUS

5.1 Installthevalveand thecolumnsas shownin figure1.

5.2 Column2 is placedin a separateheatedzone. Anynecessaryconnectinglinesshouldbe of minimumdiameterandlengthandshouldbeheaded.

5.3 Therestrictorshown is optional and is used to reduce baselinedisruption when the position of the valve is changed. It consists ofa shortlength of 0.25-mm ID stainless steel capillary tubing and approximates therestriction of column 2.

5.4 Establish the instrument parameters shown in table 1,

TABLEI. Operatingconditions.

Carriergas helium

Carriergas flowrate 60 ni_/minute

Detectortype thermalconductivity

Detectortemperature 200 c

Injectionporttemperature 170 c

Column1 temperature 115C isothermal

Valvetemperature 115c

Column2 temperature’ 170C isothermal,

Samplesiz& ‘ ~ 2.5U1 (reproducible)I

29.


MIL-G-53006Al?PEZtDIx

RESTRICTOf

ITeor *-.

L COL*I

FLOW CONTROLLER #,‘[I

.

INJECT POSITION

\ \K

1

INJECTION PORT

FLOW CONTROLLER*2

‘1W!*

t.

1INJECTION PORT

FLOW CONTROLLER h M FLOW CONTROLLER #2

ANALYZE POSITION

‘d

●

FIGURE L Eight poft valve

IX-40551m


MIL-G-53006

APPENDIX

?

6. CALIBRATION

6.1 Prepare,by precisewei~ing,a calibrationblendof oxvaenatesin -tolueneat levelsapproximatingthosein thesamplesto be ana~~zed.Thisblendshouldalsocontain10 percent methylcyclopentane.Usirtgdensities,convertthecalculatedweight-percentto liquidvolume-percent.

6.2 Chromatogra@thisblendwiththevalvein theinjectpositionwiththedetectoron polarity 11611. Determinethetimein secondsat whichmethylcyclopentanehascompletelyeluted. CallthistimeT1.

6.3 Chromatographytheblendwiththedetectoron polarity“A”. At timeT1switchthevalveto theanalyseposition.Whenthelastoxygenatehaseluted,switchthevalveto theinjectposition.Call this timefigure2.

finterestT2. See

6.3.1 Referringto figure2, acetoneelutesat theisopropylalcoholsite,n-propylalcoholelutesbetweentert-butyl alcohol and methyl tert-butyl ether.Sec-butylalcoholandn-butylalcoholeluteseparatelyaftermethyltert-butylether,buthydrocarbonsbeginto elute in this region andmay preventquantitation.

6.4 Measuretheareasof theoxygenates.Calculatetheresponsefactor “(volume-percentper unitof area)foreachof thelsecomponentsfromthefollowing formula:

F=L7i

Where:

A=

F=

L=

peakareaof the component

response factorof thecomponent

concentrationof thecomponent,liquidvolume-percent

6.5 Calculatetheresponsefactorto at leastthreesignificantfigures.

6.6 Theblendpreparedin6.1 abovecontainsveryvolatilecomponentsandmaynotbe stableforan extehdedperiod. Becauseof this,an alternativecalibrationproceduremay be used.

6.6.1 Prepare and analyze the blend as described inresponsefactors(F)to determinethe responseof eachtert-butylalcoholas follows:

6.1to6.5. Usetheoxygenaterelativeto

FR .Jc T

31

.


.

MIL-G-53006APPENDIX

y--t-- ”p---l. -~---l--–”I

II I

1 I‘--~--+---T---~ ---&--”Ii, II I

IL

------ i_.-.-~---~-----}---I

~’11’

:11

t---~-–;---*–--:–--\––-

! i 1’!’+---I f+ +~--- ‘-- ---f--- ‘--

Ii---j--- L---L--L--} ---II ! I \.1[

I+1

I~--–: ----- ‘-- -------1 I I ~ IIIt

1 I--- +--–~-–-F”–T——F”I I 1’ ! I

Il’+ +4+—— —— —— —— -— +--I I 1I I I 1

~~==’%=

.

.

.

.

.

1

-- -y+–-~--:-

1 I i 1I

--~---r--~-1 I I-J J---+~11I II.

M!

-- ++.-+

1~~-t 1 :“------- ---Ill

--- -4----+---~-I\l{-t

I--- ---~---r

{

‘?

_;

iiI

ill--- f--:---;-

)I

--+--{—-y-

1,1.

e

-- t+-- ---I

v I+ - -- ---i--–~--+--—— -

FIGURE 2. Oxygenate spectrograph


MIL-G-53006

APPENDIX

Where:

F = responsefactorforan oxygenatec

R = relativeresponseof thatcomDonent

Tc=relativeresponseof tert-butylalcohol

6.6.2 Preparea blend(Blend2) containingtert-butylalcohol in toluene asdescribedin 6.1. Usethisblendas thedailycalibrationblend,determini~responsefactorsfortheotheroxygenatesas follows:

F =FRd tc

Where:

F = dailyresponsefactorforeachoxygenated

F= responsefactorfortert-butylalcoholfromBlend 2,t calculated as describedin 6.4

R = relativeresponseof theindividualoxygenate,previouslyc determinedin 6.6,1

6.6.3 Redetermine relativeresponsefactorsmonthlyor afteranyapparatuschangeby preparinga newblendas describedin 6.1

7. Procedure

7.1 Chromatogra@thesamplesusingthete~niquedescribedfortheblendin6.3. llhevolumeof sampleinjectedmustbe exactlythesameas thevolumeofblendinjected.

7.2 Measuretheareasof theoxygenates.Unitesmustbe consistentwith6.4above.

8. CALCULATION

8.1 Calculatetheliquidvolunwpercent(LV-percent) of each exygenatepresentin thesampleusingthe followingequation:

Co~onent$LV-Percent - FC

Where:

c = peak area for that component

F = response factor, previously defined (Fd if the alternativecalibration is used)

●

33


8.2basis

9.

9.1

MIL-G-53006

APPENDIX

Reporttheconcentrationof theindividualoxygenateson an absoluteto the nearest0.1percent.

PRECAUTIONS

Thisequipment.appropriatelimitations

standard may involve theuseof hazardous materials,operationsandIt is theresponsibilityof whoeverusedthisstandardto establishsafety practices and to determinetheapplicablitityof regulatoryprior-touse. ..

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