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 [
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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$;andpublicationsforma partofspecificationto theextentspecifiedherein.
followingthis
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U.S.ENVIRONMENTALPROTECTIONAGENCYPUBLICATION
EPAMSAPCAdvisoryCircularA/CNo. 26-B.
(EPApublicationsmaybe obtainedfromtheU.S.EnvironmentalProtectionAgency,401M Street,SW,Washington,DC 204@.)
CODEOF FEDERALREGULATIONS
27CFR 211-
27CFR 212-
49CFR 171-to 179
Bureauof Alcohol,Tobacco,andFirearmsR&gulationsRelatingto theDistributionand Useof DenaturedAlcoholandRum.Bureauof Alcohol,Tobacco,andFirearmsRegulationsRelatingto FormulasforDenaturedAlcoholandRum.Departmentof TransportationHa.zardousMaterialsRegulations.
(TheCodeof FederalRegulationsis availablefromtheSuperintendentofDocuments,US GovernmentPrintingOffice,Washington,DC 20402. OrdersforabovepublicationsshouldcitetheapplicableCFRpartnumber.)
2.2 Otherpublications.Thefollowingdocumentsforma partof thisspecificationto theextentspecifiedherein, Theissueof thedocumentswhichareindicatedas DoDadoptedshallbe the issuelistedin thecurrentDoDISSandthesupplementthereto,if applicable.
AkERICANSOCIETYFORTESTINGANDMATERIALS(ASTM)STANDARDS
D86- Distillationof PetroleumProducts.D 130- Detectionof CopperCorrosionfromPetroleumProductsby the Copper
StripTarnishTest.D 270- SamplingPetroleumand PetroleumProducts.D 323- VaporPressureof PetroleumProducts(ReidMethod).D 381- ExistentGumin Fuelsby JetEvaporation.D 525- OxidationStabilityof Gasoline(InductionPeriodMethod).D 1266-D 1613-D 1744-D 22~6-D 2533-D 2547-D 2551-D 2599-D 2622-“D2699-D 2700-D 2885-D 3116-D 3229-D 3231-D 3237-
Sulfurin PetroleumProductsand LiquifiedPetroleumGases.Acidityin VolatileSolventsandChemicalIntermediates.Waterin LiquidPetroleumProductsby KarlFisherReagent.ParticulateContaminatein AviationTurbineFuels,Appendix2.Vapor-LiquidRatioof Gasoline.Leadin Gasoline,VolumetricChromateMethod.VaporPressureof PetroleumProducts(MicroMethod),Leadin Gasolineby X-RaySpectrometry.SulfurF~yX-Ray$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.
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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
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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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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
.
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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
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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
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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 ●
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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
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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.
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1.
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$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
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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’
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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.
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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.
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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
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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’
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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
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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
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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
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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
.
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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
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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”
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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
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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
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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
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.
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
,- .
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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.
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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
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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
.
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.
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
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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
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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. ..
.
“%+34
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