ASTM E2412 2010 (1)

Prévia do material em texto

# 
ÍNTERNÃTfÕNAL 
Designation: E2412 - 1 0 
Standard Practice for 
Condition Monitoring of In-Service Lubricants by Trend 
Analysis Using Fourier Transform Infrared (FT-IR) 
Spectrometry^ 
This KtandaRl i.s ií,sLiod imdor the f ixai tlcsignaliiin B24I2; the number immcilialcly folluwiiiL' lhe designalion indiuules lhe year of 
Hrigina! adoption or, jii llie case of revíNÍon, the year of lasi revision, A number in prirenilieses inclicales ilie year of lasi reappTOval. A 
siípcrsenpl epsilon (e) indieali;s im eihloiial ehangy sinee lhe liisl rt'\'isii>a w rcappriwid. 
< 
ca 
O 
Q 
< 
CO 
X 
LU 
E 
X 
Ltl 
1. Scope 
1.1 This praclicc covcrs the use o í FTTR in nioniloriny 
additive depletion, eonlarninani buildup and base .stock degra­
dation in machincry lubricants. hydraulic Iluids and oíher fluids 
used in normal machinery opcration. Contaminants monitored 
inciude water. soot, ethyicnc glycol. fuels and incorrcct oil . 
Oxidation. nitration and sulfonation ot base stocks'are moni­
tored as evidence of degradation, Tiie objective of this moni­
toring activity is to diagnose the operational condition of the 
tnachiiie based on fault eoiiditions ubserved in the oil . Mea­
surement and data interpretation parameters ;iie presented to 
aliow operatons of diflerent PT-IR .speclroinelers to compare 
resulís by employing the same techniques, 
1.2 This practice is based on trcnding and distribution 
response analys.is from mid-infrarcd absorption measurements. 
While calibration to generate physieal concentraiion units may 
be possible, it is unnecessary or impractical in many cases, 
Warning or alarm limits (the point where maintenance action 
ou a machine being monitored is recommended t>r reqiiired) 
can be determined through statislical analysis. history i>f the 
same ()r similar equipmenl. round robin tesls or olhcr methods 
in ctjnjunetion with correlation to equipmenl performance. 
These warning or alarm limits can be a Hxed maxirnum or 
minimum value for comparison U) a single measurement ur can 
also be based on a rate of change of the response measureti 
( I T h i s practice describes distribations bui does nul preLhidt; 
using ratc-í)f-ehange warnings and alarms, 
NiiTi. 1—It i>; im ! lhe intent of t l iK prHClief Io ei^tíihlii^h or recumineni l 
iioimai, caulionary, warning or alert iimils ior any machinery. Such iimils 
shmilcl be estabiished in conjiinclidn wilh advicc and giiidancc f ru in lhe 
machinery nr;inuíaclurer íind maintenance group. 
' This pracliee is under the juriwUicliOn ol A.STM Commiltee D02 on Petroleum 
Products and l.ubricanis and is lhe direel rcftponsibilily wf Subcoiniiiiltcc Dli2.y6 on 
In-.Service Lubricant Tesling and Condition Monitoring Services, 
Currenl edilion approved May 1. 2010. Pubhshed Jane 2UHI. Origmaily 
approved ia 2004, Lusi previous edition approved in 20(14 as E2412-04. 
DOi:IO,l?2(>/F.24l2-ll). 
" The boldfaee numbcis in pureiitheses leter lo ihe li.st of lererenecs at lhe cnd i>f 
Ih IS standard. 
1.3 .Spectra and distribution proHles presented herein are for 
iliuslralive purposes only and are not to be conslrued as 
representing or establishing lubricant or machinery guidelines. 
1.4 This practice is designed as a fasl. simple speclroscopic 
check for condition monitoring of in-service lubricants and can 
bc uscd to assisi in lhe dclermination of general machincry 
healih through measurement of propcrties obscrvable in lhe 
mid-infrarcd spcctrum such as water, oil o.xidulion. and othcrs 
as noted in l . i . The infrared data gcncratcd by this practice is 
lypically usetl in cunjunclion wilh olher lesting methods. For 
example. infrared speclroscopy cannol determine wcar metal 
leveis or any olhcr lypc of elemeníul analysis, The practice as 
presented is nol inlended for lhe prediclion of lubricant 
physieal propcrties (for example, viscosily, total base nuinber. 
lota! acid number. ele.}. This practice is designed for monitor­
ing in-service lubricants and can aid in lhe dclermination of 
general machinery hcallh and is nol designed for the analysis of 
lubricanl composition, lubricant performance or adilitivc pack-
age fonnulations. 
\.5 The values stated in .SI units are lo be rcgarded as 
standard, No olher units of measurement are incitided in this 
standard. 
7///J- sUí/ii/i/n/ t/ae.i /nn piirpon la luk/res.s a// of rhe 
xofeiv C(y/tce//ii. (f (inv. tissocia/fí/ n-ií/i iis use. // is r/ie 
ivsjjonxihi/i/y of í/n- irsvr of fhis sMndíinf lo es/ah/ish appro-
primc Mi/eiv (imííieai/fi pnictices miJ íidcrmine ííie appiitri-
hi/ií\ rcí^iiíd/arv iim//(i!Í<>ns prii^r fc use. 
2. Rcfcrencod Documents 
2.1 AS/)í^ S/um/arc/s.-^ 
D445 Test Method for Kinemalic Viscosity of Transparent 
and Opaque Liquids (and Calculalion of Dynamic Viscos­
ity) 
D2896 Test Method for Base Number of Petroleum Products 
by Polenliomelric Perchioric Acid Titration 
' Fo r reíeieneed .^STM standards, visil ilie A.ST.VI wehsiíe. www.asim.org. or 
eoniati ASTM Cusioiner Servite al servieety'aMm.or^. Por Afinuaí Honk </fAS7'-M 
ShiiiiJiinh volume iniormation. rcfei to lhe .'ilaíidarU's Document .Summary page oji 
lhe ASTM websile. 
CopyngtilCíASTM Iriternallonal, 100 Barr Haibor Diiud. PO Box C700. Wu^i Gonsiiohotkyii. PA 19428-2959. UniieO States 
1 
A E2412 - 10 
03 
CL. 
E 
O 
o 
CM 
íD 
CN 
<jr> 
o o o 
CO 
CD 
CX> 
O 
D4057 Practice for Manual Sampliiig of Pclroleum and 
Petroleum Products 
! 8.T "lesl Mclliod for Ucierminalion of Additive lilcmcnis. 
Wear Metals, and Contaminants in Used Ijiliricating Oils 
and Deterniination of Selecíed HIements in Base Oils by 
Inductively Coupled Plasma Atomic Emission Spectrom-
etry (ICP-AES) 
D03()4Test Method for Determination of Water in Petro­
leum Products, Lubricating Oils. and Additives by Cou-
lometnc Karl Fischer Titration 
E I 3 i Terminology Relating to Molecular- Spectroscopy 
li!68 Practices for General Techniciues of Infrared Quantí-
tative Analysis 
E142I Practice for Describing and Measuring Performance 
of Fourier Transform Mid-lnfrared (FT-MIR) Spectrom-
eters: Levei Zero and Levei One Tests 
EI6.5,'í Practices for Infrared Multivariate Quantitativc 
Analysis 
2.2 /SO Síandanl^ 
KSO I??72 Condition monitoring and diagnostics of ma-
chines -- Vocabulury 
3. Terminuloyy 
3.1 DeJJnifionò—¥Qx dclinitions of tcrms relating lo infrared 
speclroscopy uscd in this practice. rcfcr lo Terminology Hl 31. 
3.2 Defi/iifhms: 
3,2.! Fourier íra/nform infrared (FTIR) .vpec/ra/nefrv, n—a 
form of infrared spectromelry in which an inlerferogram is 
oblained; Ihis inlerferogram is then subjecled to a Fourier 
transform to obiain an amplitude-wavenumber (or wavelength) 
speclrum. K131 
3.3 Defi/nfiofis o/Tertny òpecifw to Fhis Sra/idanJ: 
3.3.1 condition monitoring, n—ií ficld of technical activiíy 
in which scIccled physieal parameters associalcd with an 
operating machine are periodically or conlinuously senscd. 
measured and rccordcd for lhe Ínterim purpose of reducing. 
analyzing, comparing and displaying the data and iniormation 
so oblained and for the ultimatc purpose of using inicrim rcsuli 
lo support decisions relaled to the opcration and mainicnanee 
of the maehinc (ISO 13372), 
3.3.2 in-service oi/, n—ax appliedin t/ii.\-príiciice. a lubri­
cating oil thal is present in a machine which has been at 
ujjcij l i i ig icinpeiaiuie ioi ui leasi one hoiir. 
3.3.2.1 /Ji.ven.v.sion—Sainpling a in-servite oil alter al least 
one hour of opcration wil l alIow for the ineasurement of a base 
poinl for laler trend analysis. 
3.3.2.2 Di.vcui-.vion—'Any subsequeni addition of lubricant 
(for example, topping oif) may change the irending baseline. 
which may Icad lo erroneous conelusions, 
3.3.3 nuicfiinery /lealt/i, / / — - ; i qualilalive exprcssion of lhe 
operational status of a machine sub-componenl, componenl or 
enlirc machine, used to eommunicale mainlenance and opera-
' AvuilaWf from lnli;rnulional Organi/.aiion for SlundarOi/.ulioii (ISO). I, ch. de 
la Voic-Crcasi:, Case posiale.''6. C^H-lZI l , Ciciieva 21). Swii/.crlnnd, h i lp / / 
www,iso.or;!. 
tional rccommendalions or requiremenis in order to continue 
opcration. schedule maintenance t)r take immediale mainte­
nance action. 
3.3,4 /lewoi/. n—an oil laken from lhe original manulaciur-
cr's packaging. prior lo being added lo machinery. 
3-3..'i reference oi/. /;—see iieiv oi/. 
3.3.6 tremi unaiv.vii; n—m o/íf4ie(J in tiii.v practice. moni­
toring of lhe levei and rate of change over operating lime of 
measured parameters (1). 
4. Summary oí Practice 
4,1 Periodic samples are acquired from lhe engine or 
machine being monitored. An infrared absorbance spectnim of 
the sample is acquired. lypically covering the range of 4000 to 
.550 cm with sufíicient signal-lo-noise (.S/N) ratio to measure 
absorbance áreas of inierest. Exact data acquisiiion parameters 
wil l vary depending on instrumenl manufacturer but most 
sy^tems should be able lo colleet an absorbance speclrum 
adequate for most measurements in less than one minute. 
Fealures in the infiared speclrum indicative of the molecular 
levei components of interesi (1,7) (ihal is. water. fuel, 
antifreeze, additive. degradation, and st> forlh) are measured 
and reported. Condition aJerts anti alarms can then be triggered 
aect)rding to both lhe levei and the trends fiom lhe monitored 
system. 
5. Signilicance and Use 
5.1 Pcrtodic sampling and analysis of lubricants have long 
bccn uscd as a means to determine ovcrall machincry hcallh. 
Aiomie emission (AE) and atomic absorplion (AA) spcctro-
sct)py are oflcn employed for wcar meta! analysis (for 
example. Test Method D5185). A number of physieal property 
tests eomplemeni wear metal analysis and are used to provide 
iniormation on lubricant condition (for example. Test Melhods 
D445, 02896, and D6304). Molecular analysis of lubricants 
and hydraulic fluids by FT-IR spectroscopy produces direct 
information on inulccular species of interest. ineluding 
additives, fluid breakdown producls and e,\lernal contaminants. 
imd ihus complements wear metal and other analyses used in a 
condilion monitoring program (1,3-7), 
6. .Appuralus 
6. i NeifiiireJ Conifionents: 
6.1.1 /-'oiirier 7'nin.sforn! /n/noeJ Specínmieler //-'/'-/A'/— 
Instrumenl is ctinfigured wilh a source. beamspliller and 
detector lo adequalely cover the mid-infrarcd range of 4000 
em"' lo .550 cm"'. Most work has been done on systcms using 
a room tcmperalurc deulerated Iriglycine sulfate (DTGS) 
deleclor, air-cooled source and Gcrmanium coaling on Polas-
sium Bromidc (Ge/KBr) beamspliller. Alternate source. beam­
spliller and deleclor combinalions covering this range are 
eoinmercially available bui have nol been invesligaied for use 
in this practice. Olher detcctois may be suitable but should be 
used wilh caution. In particular, liquid nilrogen eooled Mer-
cury CadiTiium Telluride (MCT) deleetors are known to exhibil 
signiíicant nonlinearities. 
6.1.2 /nfrored /.iquici 7'rciii.\inis.vion .S'onip/i/ig Ce//— 
Sampling cells can be conslruclcd of /inc selenidc (/,nSe), 
2 
r 
ari' 
E2412 - 10 
o o 
CM 
tD 
CM 
in 
o 
"5 
T l 
01 
CL 
o o g 
CO 
CO 
o 
CO 
< 
q : 
O 
Q 
< 
CO 
X 
LU 
h-
barium fluoride (BaF>), potassiiim bromidc (KBr). or other 
suitable window material, with a pathlength of 0.1 mm (100 
pm), parallel (<0.5'' variance) cell spacer. Acceptable path­
length ranges are from O.OfíO to 0.120 min. Outside this range, 
poor sensitivity or data nonlinearity can occur. For the data 
provided in this document, lhe cells used were ZnSe. NaCl. or 
KBr as lhe measurements ranged from 4000 cm"' lo 700 cm"'. 
Some cell material information is iíiven belou. 
Malerial Comments 
ZnSe see 6 1 2.1 
KBr susceptible to water damage 
NaCI susceptible to water damage 
BaFg ammonium salts can damage 
CaFa ammonium salts can damage 
Ttansmission 
Range, cnr ' 
4000 - 550 
4000 - 400 
4000 - 650 
4000 - 850 
4000 - 1100 
Results should be corrected to O.iOO mm pathlength lo 
account for cell path variation and improve data comparison to 
olher instrumenls using this practice. 
6.1.2.Í Due lo the large refractive index change when lhe 
infnu^ed beam passes from air inlo lhe ZnSe windows. fringe 
reduclion is necessary lo provide consistem results, Fringe 
reduclion can be achieved clcclronically, oplically or mechani-
cally for ZnSe cells. For further expíanation. see Appendix X I . 
Care should be laken in selecling window materiais lo ensure 
that the desired parameters ean be measured wiihin the 
transmi.ssion region of thal material and compatíbilit\h the 
spccihc applicalion: for example. salt windows (KBr. NaCl. 
KCl) ean be uscd and may not rcquire fringe correclion but are 
susceptible to damage from waler contamination in lhe oil . 
Coaics and Sctli (3) have noted that oil nitration producls can 
reaci with salt windows. tlcpositing compounds ihai are ob-
served in iater samples. 
6.1.3 CeiíFius/iing/Cicíifiíng S<>(vc>!r~^\\^ ideal solvent lo 
llush lhe cell between samples Io minimi/.e carryover should 
have no signiíicant absorplion in lhe condition monitoring 
áreas of interest and should dry quickiy when air is pumped 
lhri)ugh the system. Typica! wash solvenís used for comnn)n 
pelri>leum and some synthctic lubricants are technical grade, 
lighi aliphalic hydroearbons such as hcplane or cyclohexane, 
Olhcr soívents may be required for more specialized synthetic 
lubricants. Health and safely issues on using, sloring. and 
disposing of lhese solvenís wil l nol be covered here. Local 
regulations and Material Safely Data Sheets (MSDS) should be 
f.onsiulted. 
6.2 OpTionai Components: 
6.2.1 Somple Pimipi/i},' Sysfenj—A pumping system eapable 
of transporling the sample to the trunsmission cell. emplying 
the cell and tlushing the cell between samples may bc uscd, 
Many commercial vendors offer various conhguralions of 
pump types. tubing and Iransmission cells for this lypc of 
application. l l should be noted thal non-homogeneily mlght 
occur if lhe oils are left slanding for too long. 
6.2.2 /v/V/'—The use of a parlieulaie hlter (for example. 
0.090 mm) to trap large parlieles is strongly recommended lo 
preveni cell clogging when a pumping system is used. If a 
parlieulaie hlter is not used, lhe cell should be back-llushed 
regularly to preveni clogging. 
6.2.3 SeaMSom/>le Con7fiar/ment—^\\& system conhgura-
tion should be consislent vvith preventing harmful. fiammable 
or explosive vapors from reaching the IR source, 
6.2.4 Hyi/rocar/Mm [.eal: Aíarni—When a sample pumping 
system is used, an independem tiammable vapor sensor and 
alarm system should be used to alert the operator when a leak 
occurs in lhe tubing, connectors or iransmission cell- This 
alarm sysiem is strongly recommended when a pumping 
system is used to pump samples and wash solvente inlo an 
enclosed area. 
6.2.5 C/ieck F/inW--A cheek fluid or qualily conlrol fluid 
can be analyzed as needed for individual laboratory qualily 
eontrol and procedure issues anti for comparison to olhcr 
laboralories. One IR manufacturer has used hcplane. A check 
sample should be a material that provides consislent results 
using the methods presented in lhe annexes to this practice. The 
purpose of this quality eontrol fluid is to verify propcr 
opcration o f the FT - IR spcctromcier/transmission cell 
combinalions, as well as any associalcd sample inlroduction 
and cleaning hardware. 
7. Sampling and Sample Handling 
7.1 Sample Ací/iiisttion—^\\^ objective of sampling is to 
obtain a test spccimen thal is representative oí lhe enlirc 
quanlity. Thus. laboratory samples should be laken in aecor-
dance with the instructions in Praclice D4057. 
7.2 Sanip/e Preparafio/i—No sample preparation is re­
quired. Laboratory samples should be shaken or agilated to 
ensure a representative sample is taken from lhe boitle. 
S. Instrumentation l*reparation 
8.1 Specinií Act/insiHon Fneon/e/e/w: 
8.1.1 Specínil He.\ol!i/iini K cm" or betier (lower numeric 
value). 
8.1.2Daío Poinl Spacing Pesolulion -A cm" or beller 
(lower numeric value), 
8.1.3 T)pica/Range-Aim lo 550 em ' (scc 6.1.2). 
8.1.4 SpeciraiAbsorbance as a function of wave­
number. 
8.1.5 Oíher Opfical, tiecíronic Filiering andInie/ferogrum 
CompuMiionol Paremiciers—^Thcsc parameters should be a,s 
recommended by lhe manufacturer or as determined necessary 
for adequate measuremcnl qualily. Individual parameters and 
setlins;s wil l vary depending on insiriunenr mani i factMrer hm 
mosi FT-IR spcclromcters should be able lo eollecl an adequate 
speclrum in Icss than t>ne minulc, 
N o i h 2---ldenliuMÍ scanning acLpiisilion painmelers sl imi ld be uscd Ibi ' 
ali ' iampics lo bf l i c n i i r J . 
8.2 PinkgroiifiJ Colleclioii: 
8.2.1 The single-beam background coMeclion lempty sys­
tem relerence seanned and stored on an FT-iR speclrometer) 
should be performed frequenily enough such that ambient 
chiinges in atmospheric water vapor leveis and other changing 
ambient eondilions do not signihcantly atlect the sample 
results (see Praclice FÍ421) . The trequency of background 
checks should be detei"mined by the individual laboratory 
eondilions and sampling technique; for example. al lhe 
complelion of each run when an autosampler is used. 
I 
4filí̂ E 2 4 1 2 - 1 0 
8.2.2 Note that changing water vapor leveis wi l l have the 
strongest effect, as water vapor is a strong infrared absorber, A 
water vapor cheek may be included in the software lo monitor 
lhe intensiiy of the water vapor in lhe single-beam background 
speetriun. For example. the waler vapor bands superimposed 
on the single-beam speclrum al 1540, 1559. and 1652 cm"' 
may be measured relative lo lhe average of baseline points at 
1609 to 1582 cm"'. Acceptable limits for opcration can be sei; 
for example, measiu'ed peaks diic to water vapor superimposed 
on the single-beam background should nol be more lhan 10 '--i: 
of the single-beanr inlcnsity. 
8,2..3 Most of lhe research and development work used in 
lhe development of this practice used a backgrt)und colleciion 
al least every 2 h. Individual parameters and settings will vary 
depending on instrumenl manufacturer but most FT-IR spec-
trometers should be able to colleet an adequate speclrum in less 
than one minute. 
B.3 CW/ Pafhlengíh Chi-ck—K cell pathlength ehcek is 
needed to verily lhe paihlenglh consisleney of lhe cell, ResuUs 
are refcrenced to 0.100 mm as menlioned in 0.1.2. This check 
is parlicularly imporlant for walcr-soluble salt cell windows 
(for example, KBr). For systems using a fixed llow cell, the 
check ean be performed at the same time as the background 
collection. DilTerent instrumenl manufacturers may use diíTer-
ent techniques for cell pathlength checks that may rcquire the 
use of a reference or calibration fltiid(s). A fringe-based method 
for determining cell pathlength is diseussed in lhe appendix. 
Manufacturers' inslructions and rccommendalions should bc 
considered. 
9. Proccdures, Cakulation, and Reportiiig 
9.1 Sample /inr(hiíicri(/r!—\e sample is intro-
duced inlo lhe infrared Iransmission cell. eilher manually or by 
an aulomalic pumping sysiem. Auiosamplers thal hold a 
variety of oil sample conlainer si/es are available from several 
manufacturers. 
9.2 Sainp/e hnegrity Check—^o ensure accurale and con-
sistenl results, the infrared speclrum of the sample should be 
checked lo verify lhal lhe cell is compictely fillcd and thal air 
bubbies passing through lhe cell during dala collection are nol 
alTecling lhe rcsulls. Mulliple, aulomalic, computcri/,ed inter­
pretation melhods exist for ihis procedure. A sample iniegrity 
cheek ba.scd on mcasuremenl of the absorbance inlcnsily over 
the wavenumber range from 3000 to 1090 cm"' is suitable for 
mulliple lubricant lypes. The exact absorbance inlcnsity wil l 
depcnd on the spectral rcsolution and the pathlength of lhe cell 
being uscil. The manufaeturcr's suggestions and rccommenda­
lions should be considered. 
9.2.1 Petroleum based lubricants have their maximum ab­
sorbance in the 3000 to 2800 cm' ' range (or transmittance 
value elose to O %T). 
9.2.2 Ester based lubricants have their maximum absor­
bance in the 1390 to lOyO cm ' range (or transmittance value 
dose lo 0%T) . 
9.3 Sample Sysiem Cleaning a/ul Checks—^>ò enstu-e lhe 
minimum amounl of sample cross-coniaminalion or sample 
carry-over. eilher a minimum volume of the nexl sample can be 
Hushed, or a volatile solvent can be flushed through lhe cell and 
the cell dried. I f the cell is dried, the amount of abst>rbance 
from eilher the previous sample or residual wash solvent in lhe 
sample cell can be checked. This check is performed by the 
same spectral analysis opcration as dcseribcd abovc. The 
maximum absorbance inlensily shotild be bclow a preset 
threshold in the monitoring region (that is, CH slrelch in 
petroleum based fluids), Ftir most petroleum and synthetic 
hibricanis and wash solvenís. this inlcnsity will be Icss lhan 0.2 
absorbance unils. The óptima! threshold will depend upon lhe 
speciíic system conligiiralion, in lhal some systems are de­
signed to "push-out" the residual o i l sample and wash solvent 
v«ith lhe nexl sample. The manufacturer's suggestions and 
reconmicndations shoakt be considered. 
9.4 Da/a Fn/cess/ng—AH spectra wi l ! bc proeessed in unils 
of absorbance as a function of wavenumber, Calculaied data 
must be corrected to lhe reference pathlength of 0.100 nmi 
prior to reporting lo accouni for cell pathlength variation thal 
wil l be seen in commerciaily available cells. Any olher spectral 
data Ireaimeni should occur prior to calculating results from the 
speclrum. 
9.4.1 Spectral dala processing results ean be irended di-
reclly from the in-service oil spectnim (direct trending). The 
only spectral data treatmenl is lhe correclion of Lhe speclrum or 
resulls lo the 0.100 mm reference pathlength and the applica­
tion of fringe reduclion algorithms to the speclrum, il required. 
9.4.2 Spectral dala processing results can also be obtained 
by spcclral subiraclion processing, which requires a reference 
spectruin (spectral subtraclion). Where spectral subtraction is 
used. processing o\s is done Irom lhe dilVerence spec­
lrum that is generateri by subtracting the app r t Jp r i a t e new oil 
reference spcctrum from lhe speclium o f lhe in-service oil 
sample. The in-serviee o i l speclrum and ncw oil reference 
spcctrum must both bc corrected to the reference pathlength of 
0.100 min prior lo subtraclion and a 1:1 subtraclion factor used. 
The subtraeted spectral results can be Irended over time and 
Ireated in a manner similar to those collected using lhe direel 
infrared Irending method. 
9,4.2,1 The most commonly used reference is a sample of 
new oil . If possible. the new oil should be from the same lol 
and drum as the in-serviee oil . An alternate approach thal mighl 
yield a more representative reference would be lo take a sample 
of oil one hour afler the oil has reached operating temperatures. 
9.4.3 Post-analysis data treatmenl can use siinple inultipli-
crs and olhcr scaling techniques: for example. "value x 100" at 
the requesl o f maintenance personnel for case in evalualion and 
preseniutitin (scc Annc\. 
9.5 Speciriíl Analysis af Sample Da/a—Seíecled spectral 
regions ct)ntaining iniormalitm rclcvani to condilion monitor­
ing are measured anti reported, The regions analy-:ed are 
specitic to diifcrent lubricating huid lypes, New oil sample 
parameters can be uscd as lhe point fonn which lo trend when 
milially iinplemcnting an analysis process for u lubricant lypc. 
Statislical analysis shown in lhe annexes also provides ex-
amples. Details of the spectral analysis process can be found in 
lhe annexes lo ihis Practice, 
Exemplar para uso exclusivo - T E X S A DO B R A S I L LTDA - 04.608.635/0001-27 (Pedido 526200 Impresso: 17/04/2015) 
r. "3 
5 ^ 
n "2. 
^ X . l i 3 
a a 
<t 3 K 
2. 
5r 3 c; 
era 
3 
£ 5 ^ 
. n -1 ? 
• c i S -
. . —, a 
I i: I 
33 
o 
a 3 - = 
?1 
O 
Op _ t : 
G EL -O 
_ „ _• et n 3 cr n 
C =r p p 
r. — 
0= ?í - = 
S (T £1' ~ 
a ^ — 
3 a> 
70 
r, ^ uu 
3- » ã. 
9: 
^ *^ ^ 
CD 
H l ^ 
a. ^ 
5 S ':ÍL o 
— ^ — - J f-; 
C ^ p C — 
(t 
. "3 
c ' 
i: í ' 
P c 
r, o 
3 5 
C 3 
„ 2 ^ 'T̂ ^ ^ 3 = 
n 3 ^ • 
i 
cr _. 
C _ 
— 2 <T 
=í 3 5 
ti- a- - n =• - F 
PI 5 
O 
3 
soueqjosqv 
f 
4 ^ E 2 4 1 2 - 1 0 
A N N E X E S 
(Mandatory Information) 
A l . MKASUREMENT OF MOITXTJLAR PARAMETERS I N VARIOUS SVSl E M S — D I R I C C f I ' R 1 ' : N I > I N G 
CL 
E 
o o 
fVJ 
U3 
CO 
< 
cu 
O 
Q 
< 
CO 
X 
LO 
TO 
CL 
E 
X 
LU 
A l . l This anncx does nol purpori lo discnss ali lubricanl 
types. Measurement parameters for pclroleum lubricants (for 
example, crankcase). extreme pressure petroleum lubricants 
and polyol esters are presented. As data becomes available, 
other lubricanl lypes can be added lo the annex, 
Noth. A l , l—I t is not llie iniunt of Ihis practice tu c t̂ablish or 
rCTOinmcnd noniial. caulionary. warning oi alcrl iimils lor any maciiinciy 
or fluids. Sueli iiinits siu)uk! bc ciiiablislicd in conjiinclion with advicc ami 
ciiidanct; IVoin llie i D a c i i i n c r y iiianidacliiicr and inainienance jruap 
A l . 2 P('fnjí(-iini /ji/'//cíi/ifx {7\/iitiil/v /Hexc/ Eiigiiir.s^— 
Monitoring of diesel crankcase oil is one of the most common 
applications of lubricant condition monitoring. Condilion 
monitoring in these systems is divided into contaminam 
monitoring (lypically waler, socit, fuel, glycol) and oil degra­
dation monitoring (lypically oxidation and nitration), Sulfation 
degradation producls may arise from lubricanl component 
breakdown but commonly arise from lhe by-producls of 
sulfur-conlaining diesel fuels. Measuring contamination from 
ga.soline is also possible but nol as widely applied, iis ctini-
panilively few gasoline engines are enrolled in condition 
monitoring programs. In addilion, monitoring of the /Jnc 
dialkyldithiophosphale (ZDDP) based antiwear component tif 
the additive package is also possible. The most common FT-IR 
condition monitoring parameters for crankcase engines are 
presented in Table A l . l . wilh some spectral mcasurcincnl 
examplcs presented as a guide in using band áreas. Throughout 
lhese examplcs, lhe use of integrated band area is preferred as 
noted in Practice EI6K bccause il has been "found lo be more 
accurale lhan pcak-hcighi inea»;m-cmcnis bccause one is. in 
effcct. averaging mullipoinl data." 
A 1,2.1 Wiikr: 
A 1.2.1.1 Water contamination is monitored in diese! crank­
case lubricants by measuring lhe hydrogen-bonded OH slrelch 
region given in Table A l . l . An example of varying leveis of 
water contamination is shown in Fig. A l . l . In the following 
examplcs (e.\cepl soot) lhe infrared speclrum is sliaded dovvn to 
the described baseline, giving a visual example of how lhe 
integrated absorbance area is measured. Measurement of lhese 
band áreas by eomputer assisted techniques is common in most 
infrared manufacturers" software packages. For the water 
measurement in crankcase oils, the area under the curve 
between 35U0 and 3150 cm"' is shaded. showing an example of 
lhe measurement described above. 
A 1.2.1.2 Water//iferferefice.s—High sool leveis (~ 10 9(- w/w 
solids) may interfere wilh water measurements in diesel 
engines. but interference has nol been seen until lhe sool limit 
has been exceedeil ithat is, > 3 tii 5'-í w7w solids). As a 
condititin limit (sool) has already triggered, action slioutd be 
taken irrespeclive of water. Exact quanlitalive measurement oi 
soot is difticull (lhal is. % w/w) due lo mulliple infrared 
contributing factors as well as the many diflerent soot mea­
surement methods available. 
A 1.2.2 Saul: 
At.2.2.1 Soot ioading is measured from lhe baseline ofiset 
al 2000 cm ' as described in Table A1 I . !-ic. :\ shows some 
examples of spectra showing low, intermediate, iiigh and very 
high sool Ioading leveis lincreasing leveis from I through 5). 
A 1.2.2.2 Sai'{ //ueifereine—High waler leveis have been 
t)bservcd to interfere with ihc measurement of soot in internai 
combuslion engine crankeascs. However, this interference does 
not become signiíicant until lhe waler levei is t>n lhe order of 
>5 (50 000 ppin). leveis which will immedialely eondemn 
the lubricanl and rcquire immediale maintenance action irre­
speclive of any olhcr indieators. 
A l .2.3 Oxh/afia/i. Nirranan a/id Sui/aíiaa: 
A 1,2.3.1 Uniike lhe previous examples. oxidation. nitration 
and sulfation breakdov\ products in crankcase oils cannol be 
easily quantilied by comparison to pure prepared standards. 
Here. there are a large number of dilferent oxidation and 
nitration compounds thal ean be produced and gradualiy buiid 
up in lhe oil . Fig. A 1.3 shows lhe measurement áreas for 
oxidation aud nitration pruduct buildup monitoring. with lhe 
sulfation rcgiíin highiiglilcd in Fir.. A l 4. 
A L 2.3.2 O \7i/í///('/i. Niiruliufi anJ Suiía/ion 
Jnterferences—As in the soot measurement. very high waler 
leveis can generate false positives for oxidaliiin and nitration. 
However. v\ater leveis of this magnitude wil l immedialely 
eondemn lhe lubricant. Very high l>5 %) glycol leveis m a 
crankcase oil may slarl inlerfering wilh sulfation measurement. 
bui again contaminam leveis of this magnitude would dictaie 
immediale maintenance action. Various additive packages, 
such as dctcrgcnts, dispersants, antioxidants, overbase 
additives. ele. may also generate signihcant absorbance in the 
condition monitoring regions of interest, lilends ol petroleum 
lubricants wilh signiíicant amounts of esler, whelher pari of the 
base-slock package or as an additive, wil l absorb strongly in 
lhe oxidation arca. These lubricants are not presented al this 
lime, 
A1.2.4 Fuei Conlainiíiafi<m: 
Ai.2.4.1 The pt)ssibility of fuel contamination may be 
indicated m diesel crankcase lubricants by measuring the peak 
at SIO c m ' . Spcclial characterislics of diesel (I ig'^. .-\l-,5 aiiJ 
-A 1 h) and other fuels noted in I able A l . l have been found to 
vary. Work is currently active on olher IR measurement áreas 
anti techniques, The measurement listed can bc uscd as a 
guideline but is not inlended to be lhe only infrared based fuel 
contamination measurement. An indcpendent lest. such as 
6 
E 2 4 1 2 - 1 0 
2 
Q. 
E 
o o 
CvJ 
CD 
CM 
o 
CO 
< 
cn 
O 
Q 
< 
CO 
X 
LO 
Q. 
E 
<D 
X 
UJ 
viscosity cliange. flash point. or gas chromatography can bc 
Lised to coníirm an indication ot" fuel presence in the bT-IR 
spectrum of the oil . 
A 1.2.5 Givcoi Afifi/reeze Cofiíami/iafian • 
Al.2.5.1 Glycol contamination is monitored in diesel crank­
case lubricants by measuring the carbon-oxygen strctch region 
as noted in fablc .'\. l . Spectral charactcristies oí" glycol 
contamination are shown in 1-ig. , ' \ l ,6. 
A 1-2.3.2 Ethylene glycol wi l l interfere with the abiliiy to 
accurately quantify water levei when present since it also 
contains hydroxyl groups. However. the converse is not true 
since glycol has other spectral fealures that are used for 
deteelion and quanlification. Therefore. when glycol is present. 
water can be dclceled bui nol reliably quuntified using FT-IR 
speclroscopy. This is not considered a problcm bccause of lhe 
grcaler signiíicance lhe presence of glycol has lo engine 
opcration. As wilh fuel. the presence of glycol can bc con-
finned by gas chroinatography or a colorimelric test, or more 
commonly, corroboraled using elemental analysis resulls for 
sodium and boron, 
A 1.3 Ex/n'fm' P/v.wmre (PP) P/iiiil\- iTv/>iraI/y Pcfralciuii 
Ceíir or HyelrtJií//r Fíiiiii.s-/. 
Al.3 .1 In addilion lo lhe above crankctise oil analysis. 
condilion monitoring of gear and hydraulic oil is also widely 
applied. In these systems, the mosl common parameters 
measured are water contamination and oxidalivc breakdown of 
lhe oil, which are presented in Tilile A 1,2, 
A 1.3.2 Wíifcr: 
A 1.3.2. í As water is the rntisieonnnon euiitaminajil in 
crankcase oils. it is also the most common contaminam in 
gcarboxes and hydraulic systems. In these systems. uniike the 
crankcase oils. however, interactions between water and the EP 
additives alter the infrared response, and thus water is mea­
sured ditTerently lhan in lhe crankcase lubricants. Fig. A 1,7 
demonstrales this differenl response of water. Water conlami-
nalion is manifesied as a geneial. horizontal baseline offset of 
lhe entire infrared speclrum. Here. the iniegraled area for lhe 
spectrum representing 3000 ppm (0.3'^í) waler is shaded. 
While this measurement becomes lhe principal waler measure­
ment in EP fluid systems. very high waler leveis (greater lhan 
2 %) wil l begin to show a similar hydrogen-bonded OH slrelch 
band as seen in the eiankcase oils. 
Al.3.2.2 Wtí/er//nerferences As the principal waler mea­
surement is based on the integrated absorbance with no local 
baseline correclion. soot. dirt and high conceniraiions of 
inlrared scatlering particulaies wil l generate higher lhan c\
pccted readings lor water. However. lypieal gearbo.Ncs and 
hydraulic systems wil l not coniain particulaie leveis high 
enough lo cause a signihcant baseline offset and tllt. Wcar 
metal analysis, parliclc counting or other applicablc tests 
should eondemn gear and hydraulic systems thal manifesl such 
extreme particulaie leveis. 
A 1.3.3 O.xiJulh/n: 
A 1.3.3.1 The oxidalive breakdown measurement shown in 
Fig. A 1.8 in pclroleum EP fluids is lhe same as in the 
petroleum-based crankcase fluids diseussed in .A 1,2.3.2, Note 
that while Fig. A 1.8 also shows an inciease in sulfation 
by-products. not ali F̂ P systems wil l show this effcct. 
A 1.4 Synthclic Polyoi Esrcr Li/brívants (Typiailly Aero-
Derivúíive Gos TiirhifiesK 
A 1.4-1 Condition monitoring of high-performance aircrafl 
turbine engines is widely applied in both the mililary and 
commercial avialion mainlenance industries. In addilion. many 
aero-derivaiive gas un'bines are u^ed in powcr generation. 
marine iransport and olher non-aeronautical applications. In 
these s>siems, lhe primarv lubricanl is a synthetic polyol esler 
and is available under a variety of diífereni mililary speciltea-
lions and commercial item descriptions and brand names. 
iLtble A l .3 lisls the condilion monitoring propcrties of interest 
nieasured by FT-IR along with lhe band measurement area and 
lhe baseline point(s). 
A 1.4.2 Waier: 
A 1.4.2.1 Just as lhe infrared measurement for water was 
adjusted lo accouni for the differenl interactions in the formu-
lalions in crankcase and EP oils, a differenl water measurement 
area is also required for the polyo! esters. Fig. A l .9 shows lhe 
area under the curve that is integrated for the determination of 
water contamination in these systems. wilh lhe measurement 
highlighted for a sample containing 1000 ppm of added water. 
Note that lhe water in these systems shows up as a broad band, 
similar lo whal is observed for w'aler in the crankcase oils. bui 
lhe -«trongest resptmse oceurs at higher frequencies than in the 
case of the crankcase nils (-3700 to 3600 cm ' for polyul cslcis 
versus 3500 to 3150 cm ' for crankcase oils} 
A 1.4-2,2 Wuwrlfi!í'r/crcníí'.\-''\\\'i mosl signiíicant interfei-
cnce found in lhe dclermination of water is interference fnnn 
lhe polyol esler lubricant breakdown I (see , \ l -4.3}. Under 
sevei"e eondilions ol' lubricanl degradation, this band will begin 
to overlap and contribute to the integrated water measurement 
area. As seen beiow in Fig. A 1.10 however, this elfect is only 
seen when lhe lubricant is already severely degraded, which 
dietatcs maintenance action from the degradation irrespeclive 
of the actual water levei. 
A1.4.3 Esrer Bose-.Sfock fíreakdown: 
A 1.4.3.1 As the polyol esters are a diflerent chemieal 
system than petroleum based lubricants. degradation of the 
polyol esler lubricant produces differenl breakdown products. 
Tlie m o s t e o i n i n o n d e g i i K l a t i t > n p ; i t h w ; i y ín é s t e r b u s e d lul^ii-
canls is lhe coiiversion of the éster inlo organic acids and 
alcoliols. 
.-M.4.3.2 E.sUT Ptrn-S/ock Pretikdonn /—The resulling 
polvol esler degradation products are lirst seen between 359.5 
and 3?()() em '. and lhe measurement is noted as esler base-
stock breakdov\ I in Table .A l 3 and highlighted in F Í L ' . A 1,10. 
As this area is closcly associalcd v^ith the waler measurement 
area, a locali/.ed. single-point baseline at 3595 cm"' provides a 
correclion for low leveis of water buildup (Fig, A1,10). 
Al.4.3.3 EsterBase-SíockBreakí/ownaddilion lo lhe 
breakdown area I , a second area associated with the Iraditional 
OH streteh (as measured for waler Ín crankcase oils) also 
incrcascs as lhe lubricanl breaks down. This esler basc-slock 
breakdown I I arca is also monitored as a measuremcnl of 
7 
E 2 4 1 2 - 10 
O 
CN 
^" 
O 
Ò 
O) 
Q. 
E 
degradation of the polyol éster kibrieants. The breakdown I I 
region is also highlighted in big. A L I O . 
A 1,4.3,4 £s/er Base-Slock Breakdown fníer/erences—fK^ 
noted above in A 1,4.2,2 where excessivo base-stock break­
down interferes with the water ineasurement. a similar elfect 
has also been noted with the lubricant breakdown measure­
ment. Excessive water leveis may cause the lubricant break­
down reading to be higher than the actual levei, Oncc again 
however. water leveis of this magnitude will eondemn tlie 
lubricant irrespeclive of the actual breakdown levei, 
A 1.4.4 Aníiwear C•jniponenf.s: 
Al.4.4.1 While lhe antiwear compounds used in crankcase 
oils and polyo! éster lubricants are lypically tliíTerenl species. 
the most ctimmon compounds used for both oiis have a 
phosphate funclional group. For this reason, lhe measuremcnl 
area developed for mt)nitoring leveis and trends of ZDDP has 
been foimd lo be equaily useful for monitoring iricresyl 
phosphate fTCP). Fig. A l . í l shows varying leveis of TCP 
blended into a polyol esler lubricanl. As previously noled, 
building calibration curves for measurement parameters (when 
pure or prepared standards are available) is possible. Ffowever, 
this is not necessary, as lubricant condition monitoring requires 
only rcliabie. repealuble measurements. Correlation of FT-IR 
measurements to physieal values is nol necessary. 
A 1.4..5 Fael Confiuninalion: 
A 1.4.5,1 Fuel contamination is monitored in polyol esler 
lubricants by measuring lhe peak at BIO cm"' as given in 
section A ! ,2,4. 
A 1,4.6 Olher FíidiJ Con/i!nn'Haíh>n: 
A 1.4.6.1 In adtlilion to fuel contamination. foreign oils and 
hvdraulic tluids may containinale lubricating oils (Ibr example. 
polyol éster coniaminated by a petroleum based lluid). In mosl 
case-̂ . identifying the presence of a foreign fluid is ali that is 
required to generate an appropriale mainlenance response. The 
wide viiriety ol polential etmlaminanls suggests an equaily 
wide variety of measurement methods may be desirablc, In 
addilion. mtilliple frequency dislributions may also be required 
and are nol given here. The measurement áreas given in Table 
A l 3 demonstrate the measurement used lo indicate the pres­
ence of petroleum oils. phosphate esler oils. or polyalphaoleíin 
(PAO)/diesler blend oils contaminating polyol esler oils. í ig . 
A 1 . 12 shows an example t)f polyol esler oil contaminated by a 
polyalphaolehn (PAO)/diester blend oil . 
TABLE A T I Petroleum Lubricant (for example, Crankcase) Condition Monitoring Parameters— -Direct Trending 
Component IVleasuroment Area, cnr ' Baseiine Point(s), cm' ' Reporting" 
Water 
Sool Loading 
Oxidation 
Nilralion 
Antiwear Componenis 
(Phosphate based, lypically ZDDP) 
Gasolmu 
Diesel (JP-5, JP-8)^ 
Suitale by-products 
Ethylene Glycol Cooiant 
Area 3500 to 3150 
Absorbance inlensity al ?000 
Area 1800 to 1670 
Area from 1550 tç 1600 
Area 1025 to 960 
Area 755 to 745 
Area 815 to 805 
Area 1180 lo 1120 
Area 1100 to 1030 
Mtnima 4000 lo 3680 and 2200 to 1900 
None 
Mínima 2200 to1900 and 650 lo 550 
Mínima 2200 to 1900 and 550 10 550 
Mínima 2200 to 1900 and 650 lo &50 
Mínima 780 lo 760 and 750 lo 730 
Minima 835 to 825 and 805 to 795 
Mmima 2200 to 1900 and 650 lo 550 
Mínima 1130 to 1100 and 1030 to 1010 
Report Vaiue as Measured 
Vaiuc X 100 
Report Vaiue as MuaEurtíd 
Repori Value as Measured 
Repor! Value as Measured 
Report Value as Measured 
(Value + 2) « 100 
Repori value as measured 
Report value as measured 
" Reporting values in absorbance/0,1 mm (see 6,1.2), 
^Spectral characterislics ot diese! and ottier noted fuels have been found lo vary. Work 
measurement listed can be used as a guideline bui is not intended Io be the onJy inlrared 
suggested lo vcrily presencu of indicator absorbance bands. 
IS cunently aclive on olfier IR measurement áreas and techniques. Ttic 
based fuei contamination measurement. Ci^ecking suspecl luel sources is 
CO 
< 
O 
< 
CO 
X 
UJ 
UJ 
Exemplar para uso exclusivo - TEXSA DO BRASIL LTDA - 04.608.635/0001-27 (Pedido 526200 Impresso: 17/04/2015) 
Exemplar para uso exclusivo - TEXSA DO BRASIL LTDA - 04.608.635/0001-27 {Pedido 526200 Impresso: 17/04/2015) 
E 2 4 1 2 - 1 0 
F u e l D i U i t i o n o f O i ! 
900 850 800 
Wavenumber (cm'^) 
750 
FIG. A l . 5 Fuel Measurement in Crankcase Oiis 
i- F u e l P e a k 
700 
o 
•g 
ij 
CD 
O. 
FIG. A1.6 Giycoi Contamination Measurement in Diesel Engine Oiis 
TABLE A1.2 Petroleum Based EP Fluid Condition IVIonitoring Parameters—Direct Trending 
Componenl Measurement Area, cm ' Basffliiie Point(s). cm"' Reporting'^ 
Watet 
Oxidation 
Area 3400 lo 3250 
Area 1800 to 1670 
No Baseiine 
Mínima 2200 to 1800 and 650 to 550 
Vaiue X 20 
Report Value as Measured 
" Reporting vaiues in absorbance/O.I mm (see 6.1.2). 
11 
Exemplar para uso exclusivo - TEXSA DO BRASIL LTDA - 04.608,635/0001-27 (Pedido 526200 Impresso: 17/04/2015) 
E 2 4 1 2 - 10 
TABLE A l .3 Polyol Ester Fluid Condition Monitoring Parameters—Direct Trending 
Componenl 
Measurement Ari;a. 
cm"' 
Baseline Poinl(s), cm ' Reporting'' 
Waliír Area 3 7 0 0 lo 3595 Minima 3 9 5 0 to 3770 Value X 1 0 
and 2 2 0 0 lo 1 9 0 0 
Esleí Base-Sloc)< Breakdown 1 Area 3 5 9 5 lo 3 5 0 0 Single poinl al 3 5 9 5 Value X 1 0 
Esler Base-Stock Breakdown í! Area 3 3 3 0 lo 3 1 5 0 Minima 3 9 5 0 lo 3 7 7 0 Value X 1 0 
and 2 2 0 0 lo 1 9 0 0 
AnlJwear Components (typJcally TCP) Area 1025 to 960 Minin"ia 2 2 0 0 lo 1900 Report vaiue as measured AnlJwear Components (typJcally TCP) 
and 650 lo 5 5 0 
Fuel (JP-4, JP-5, JP-S)*^ Area 8 1 5 to 8 0 5 Minima 635 to 625 (Value + 2 ) x 1 0 0 Fuel (JP-4, JP-5, JP-S)*^ 
and 8 0 5 to 795 
Other Coniaminants In Polyol Esler Synthetics Area 1 4 2 5 to 1 3 9 0 None Report value as measured 
(lor example. Petroleum Lubncants and Hydraulic Fluids) and 1 0 9 0 to 1 0 3 0 ^ 
" Reporting values in absorbance/0.1 mm (see 6.1 2). 
"Spectral ciiaracteristics of noted fuels have been found lo vary. Work is currently aclive on olher IR measurement áreas and techniques. The measurement listed can 
be used as a guideline bui is not intended to be the only infrared based fuel contamination measurement, Checking suspect luel sources is suggested to verify presence 
ot indicator absorbance bands. 
^Alternate multivariate techniques such as PCR, PLS and lactor analysis such as given sn Practice E1655 can also be used. 
E2412 - 10 
.35 -
.3 
o .25 
// a \c n .2 
jl ^^^^^\À^^ o 
(0 
Si 
< 
.15 
.1 
Breakdown i j /^^^'"í | \^ 
.05 ^ ^ ^ ^ ^ ^ ^ ^ ^ New Oil " - " ^ ^ ^ ^ ^ t s ^ ^ B ^ 
0 
3700 3600 3500 3400 3300 3200 3100 
Wavenumber (cm'^) 
FIG. Al.10 Ester Base-Stock Breakdown Measurements in Polyol Esler Lubricants 
0.5-1 , , , . , 
1000 980 960 940 920 900 
Wcwenumber (cm"̂ ) 
FIG. Al.11 Measurement of Antiwear (TCP) in Polyol Esler Lubricants 
14 
4§|!$' E2412 - 10 
Q-l ^ , , ^ 1 ^ 
1800 1600 1400 1200 1000 800 
Wavenumber (cm'^) 
FIG, Al.12 Polyol Ester Lubricant Contaminated witii PAO/Diester Oil 
A2. M E A S U R E M E N T O F M 0 1 . F : C U I . A R P A R A M E T E R S I N V A R I O U S S Y S T E M S — S P E C T R A L S U B T R A C I I O N 
A2.1 This iuiiiex does not purport to diseuss ali lubrieaní 
types. Measurement parameters for petroleum lubrieanis are 
presented. As data becomes available. olher lubricant types can 
be added to the annex. 
NOTE A2.I—It is not the intent of this praclice to eslahlish or 
recommend normal, cautionaiy. warning or aleil limits for any niítchincry 
or fluids. Such iimils should bc csiablishcd in conjunclion with advice and 
guidance from lhe machincry nianufaclurcr and maiiifenancc group. 
A 2 , l . l Searching a spectral library to find the best seleetion 
for reference subtraction sht)uld not be used, This approacli 
will generale inct>n"ect results. parlicularly for antilreeze. fuel 
and waler. l l is beiler lo make a choice of lubricant lypc and tisc 
it consislenlly if lhe oil type is nol known. It an appru|)rjate 
reference oil cannot be obtained, spectnil subtraction should 
not be performed. 
A2.2 Pcíroleiíin-fíased Crankaise ÍJihnca/i/s—-Ks stateti in 
Annc.\. condition monitoriuL: of crankcase oils is divided 
into contaminant monitoring and degradation monitoring. The 
analysis parameters for spectral subtraction are similar to those 
for the direct trending approach. Differeiít laboratories have 
developed slight variations on these analyses. These different 
approaches are equaily vaiid for trending but wil l produce 
results that ditter numerically. Consislent analyses should be 
applied for each application. Table A2.1 give examples of 
specihc analysis parameters u.sed to obtain data from difference 
spectra of in-serviee minus new oil. The information in the 
remainder of this section provides more detail about the 
individual parameters, The footnotes to Table A2,l should be 
reviewed carefully, 
A2.2.1 Waler Coniaminaih/n: 
A2.2.Í.I Water has two characteristic absorptions in the 
infrared (."5400 cm ' and 1640 cm"') which make detection 
possible at aroimd the O.O.̂ i to 0. l-wt*^/: levei. While this is nol 
as sensitive as soirie other techniques. it is at a levei where 
problems from the presence of water in lhe crankcase could 
begin. Water is detecied using a broad featiire, centered around 
3400 cm '. thal is caused by siretehing of the hydrogen-bonded 
hvdioxyl i -OHl yioiip. Wiitcr is mcíismcd ns depictcd in I ig. 
A2 I using a single-point baseline at 3700 cm ' and a peak 
height at 3428 cm '. Alternatively. lhe water maximum can be 
measured relative to a two-point baseline drawn from 3740 
em ' to 3120 ein The concentratioii values shown in the 
figure are for weight percent (wt'/í>) water, 
A2.2.I.2 Oi/ihraiion—Calibration is lypically done over the 
range froin O.O.*̂ to ^.5 wt'.í^, but may go as high as 1.0 wt*-f 
water. Beyond this point lhe behavior of water in petroleum 
lubricants becomes very nonlinear when measured in lubricat­
ing oil by an optical measurement technique such as infrared. 
Standards are prepared locally by adding water to dry oil, 
Water standards should be freshiy prepared and analyzed. 
15 
E2412 - 10 
Adequiite mixing is necessary tu ublain valid results. Mixing, 
sonicating or mechanical shaking for at least 15 minutes is 
considered adequate. Oo not use plastic containers. 
A2.2.I.3 I/iferfc/v/ices—^Ethylene glycol wil l interfere with 
the ability to accurately quantify waler levei when present 
since it atso contains hydroxyl groups. However, the converse 
is not true since glycol has other spectral feattires that are used 
for detection and quantihcation, Therefore, when glycol is 
present. water can be detected but not reliably quantitied using 
FT-IR. This is nol considered a problem bccause of the greater 
signíhcanee the presence ol" gl icol has Io engine operiitnm. 
A2.2.2 Sool Parlic/ex: 
A2.2-2,1 Suspended soot is lhe resull of lhe incomplele 
combustion of fuel. I l is usually only a consideration in diesel 
engines btit could be indicativeof carburetor or injeclor 
problems with other fuel systems. While soot has no specihc 
frequency of absorplion in the infrared spectrum, it causes a 
shift in the baseline of the spectmm due to absorption and 
scattering of light. Since there are no other spectral fealures in 
the region at 1950 em"', this area is used to assess the levei of 
soot in a sample as is shown in l 'ig, .\2,2, 
A2.2.2.2 In lhe case of soot, the baseline absorbance is 
measured prior to reference oil subtraction. Bccause lhe soot 
absorbance obtained is a measure of the amount of tilt in the 
spectra] baseline, a correction should be applied to the data ío 
account for the contribution of lhe iransmission cell lo llie 
baseline tilt i f the background is taken without the cell in the 
beam path. This value can be signihcant in the case of a ZnSe 
cell, on lhe order of 0.2 absorbance units with elean oil in the 
cell as ean be seen in the hgiu'e. The baseline shift caused by 
soot is attected by the amount o í soot present and the efíective 
particle size, The efíective particle sizc i-^ determined by lhe 
nalure of the combustion system and the dispersants in the oil . 
This fact makes it diflicull to directly assess or calibrate the 
quantily of sool. so factors thal relate the amounl of soot to the 
infrared absorbance value must be established with the engines 
aud lubricants of interest. 
A2,2.3 Oxidaiion (Caràonyi O.xidaíian Producls): 
A2.2.3.1 The broad featui"e centered al 1730 cm"' is due to 
the presence tif carbonyi-containing degradation products of 
oil . These have been identilied as lactones, esters, aldehydes, 
kelones, carboxylic acids, and carbtixylate salts. This feature is 
shown in Fig- A2,3. The baseline for carbonyi oxidation 
measurement, referred to as oxidation, is taken at 1950 cnT' 
and the maximum peak height between IKOO and 1650 cm"' is 
determined. Alternatively. some labs measure the absorbance 
of the peak closcst to 1709 cm"' relative to a single-point 
baseline at 1900 cm"'. 
A2.2,3.2 For esler based synthetic oiis: lhe measurement 
region can be shifted to ["ange from 17IOti] IbbOcm"' lo avoid 
the large carbonyi leature of the éster base oil . The broadness 
of lhe peak is a resull of lhe wide variety of materiais present. 
The point of maximum intensity wi l i vary as the oil and 
eondilions of its use are changed. The increase in peak height 
that occurs as the number of hours the oil has been run in the 
engine increascs has signiíicance in lhe measurement of 
degradation retated to TAN and viscosity. 
A2.2.4 Nilrogen Oxidalion Pniditcls: 
A2.2.4.1 The sharp feature at 1630 cm ' is Che resull of 
niírogen oxide ílxation into the oil as is shown in l i g , A2,3. 
The materiais leading to this feature are nitrate esters. The 
measurement of the nilrogen oxide feature is done by choosing 
the maximum peak intensity over the range of 1650 to 1610 
cm ' with a single-point baseline at 1950 cm"' or 1900 cm '. 
A2.2,4,2 Becatise of the interference lhal can be seen over 
the same region Irom metal soap products, some pet^ple prefer 
lo measiu"e lhe sharp feature as a shoulder on lhe broad 
underlying feature as a moie correcl measure of nitration. The^ 
formatíon of nilrogen lixalion pujducls is most signihcant in 
gasciline and natura! gas engines as well as some diesel systems 
that Use cxhatisl gas re-circulation, 
A2.2,5 SuIJnr (7xii/iiiion Prodticis: 
A2.2.5.I Anolhcr broad spectral leature. centered aiound 
1150 em"' as shown in I-ig, A2,3, is the resull of sulfate 
compounds as well as overlap wilh oxidalion products (car-
boxylate). A baseline poinl al 1950 cm"' is used. 
A2.2.5,2 Sulfate material rcsuits from the introduction of 
sulfur from the combustion of diesel fuels or from the 
oxidation of sulfur from lhe base oil and additives in gasoline 
or natural gas engines, This band is a fairly specihc measure of 
over basing additive consumption and directly relutes ii) the 
TBN assay for engine oils. 
A2.2.6 P/ios/dicire Anriwear Addiíive Dei>ieiion: 
A2-2.6.1 Monitoring the tlisappearance of phosphate anti­
wear additive (typicídiy zinc dialkyldithiophosphale) can indi-
cate unusual wear or severe operating eondilions, The deple­
tion of these additives will occur prior to the poinl where the 
oxidatuin of the lubricant begins to acceleraie. making its 
trending a useful indicator of the lubricanl's remaining useful 
life Ihis compt^nent is monitoreil as a negative peak in the 
dillbrcncc spcctrum since the new oil wil l coniain a greater 
concenlration of lhe additive than the in-service oil. In this case 
the maxirnum negative peak in lhe range from 1020 to 930 
cm' ' with baseline points over the same range is used as shown 
in Fig. A2.3. 
A2,2.7 Fuel Residiie: 
A2.2.7,l As menlioned previously, the measurement of luel 
residues or raw fuel is very difllcult by any method. The main 
difference between lhe fuel and base oil is Ín molecular weight 
or boiling range and the relative pcrecnlage of aromatic 
materiais. Fuel has a lower boiling range and a higher 
pcrecnlage of aromatic material, Conventional methods such as 
gas chromatography or ílash poinl make use of the lower 
boiling range, while the infrared approach examines the 
aromatic content lo indicatc if fuel is present. 
A2,2.7,2 The spectral fetiture causeti by aromatic bands 
over lhe range from 817 lo 804 cm"' is used lor ihis purpose. 
A peak area over this range is used as is depicled in Fig. .••\2,4. 
The íigurc shows lhe peak area increase as lhe wt^f tif 
weathcred diesel fuel increascs. In some cases, notably winler 
diesel fuel, the peak used for fuel rcsidtic is broader than that 
shown in Fig. A2.4. A wider range for lhe baseline points can 
be used to achieve better sensitivity, allhough this caused a 
reduclion Ín lhe selectivily. 
J6 
E 2 4 1 2 - 1 0 
CO 
< 
cn 
O 
Q 
< 
CO 
X 
LU 
A2,2.7.3 The Liccuracy of meiísurement is strongl\d 
by the standard material used to calibrate the instrumcnt and 
the levei ío which the fuel is evaporaíed within the engine 
crankcase- This is why weuthered fuel should bc used to 
calibrate the system and calibration of fuel should be done 
based on fuels obtained regionally. In addition, there is a 
criticai need to match the new-oil reference properiy, as 
diseussed earlier. It is the change in base oil aromatic content 
that is the major factor leading to errors from reference 
mis match. 
A2.2.7.4 Calibration for diesel fuel is lypically done over a 
range from 2 lo 10 weight percent and gasoline from I to 10 
weight percent, Weathered fuel is used as the standard material, 
Procedures for preparing representative weathered fuei may 
vary. but lhe following should serve as a guideline: Diesel fuel 
is brought lo approximateiy 107 dcgrecs Centigrade then held 
at ihis tcmpcralure lor 30 minutes, This represents a loss oí 
around 5 % of die original volume. Gasoline is hcated at low 
lemperalure until around 40 7r of the original volume is 
evaporaíed. Note: Greal caro should be laken when preparing 
these materiais to avoid íire ha/ard or exposure to the vapors, 
A2,2.7.5 Gast)line contamination tlctectiun is less problciri-
atic than detection of diesel fuel contamination bccause of the 
higher relative aromatic content of gasoline. Quanlification o! 
gasoline is calibrated using a peak area over lhe range of 734 
to 721 em"'. 
A2.2.7.6 An independem test, such as viscosity change. 
flash point. or gas chromatography, can be used to coníirm an 
indication of fuel presence in the FT-IR spectrum of the oil, 
A 2.2.8 O/) í 'ol Cantaniinii/iun: 
A2.2.8.I This contaminant has characteristic absoi'ptions in 
the infrared that make its detection possible at aroimii lhe 0.1 % 
levei. While this is not as sensitive as scime other techniques, it 
is at a levei where problems froiri lhe presence of íhese 
contaminants in the crankcase could begin, Glycol has the 
same broad hydroxyl (-OH) group feature, centered on 3400 
cm"', as seen for waler.However. glycol has other character­
istic peaks thal dilferentiate il from walci' around S80, 1040. 
and 1080 cm"' us can bc seen in f ig .-\2..'̂ . 
A2.2,8.2 The peak height at 883 cm"' with a single-point 
baseline at 917 cm"' is used to quantify glycol since it is nol 
subject to inlerferences to the same extenl as the bands at 1040 
and 1080 cm"'. This efltct can be seen by looking at Mg. t\15. 
which shows a large sulfate band with glyeol peaks on the righi 
shoulder. Even fhough the peaks at 1040 and 1080 cm"' are 
larger than the one at 880 cm' ' , it i,s very diííicult lo accuralely 
measure them in the presence of other oil breakdown producí. 
Instead the peaks aí 1040 and 1080 cm ' are used to conhrm the 
presence of glycol. 
A2-2.8.3 In praclice, a 2nd derivative spectrum can be used 
to Hnd lhe eorrect peak location for these peaks and absorbance 
intensity limits can be used to trigger whelher glycol appears to 
be present, l-ig. A2,5 shows the intensity increase in the glycol 
bands at lhe C()ncentration increascs over the range Irom 0,0? 
lo 0.8 wt%. 
A2.2.8.4 /nre/ff/Y'/!ct'.v—Glycol wil l interfere wilh lhe quan-
tilation of water levei when present. but lhe converse is not 
true. Therefore. when glycol is present. water canntn be 
reliably quaniihed using the FT-IR measurement, This is not 
considered a pix)blem bccause of lhe greater signiíicance the 
presence of glycol has lo cngiiic operaiion. As wilh fuel. the 
presence oí glycol can be confirmetl by gas chromatography or 
a colorimelric test, or more commonly, corroboraled using 
elemental analysis results for sodium and boron. 
A2.2.8.5 Glycol standards ciui be prepared t)ver a range 
from 0.1 to 0.5 weight percent glycol using a 50:50 mixture of 
glycol-based antifreeze and water. Calculations should be 
made based on lhe actual amounl of glycol-based antilree/e 
added. not on the amounl of lhe 50:50 mixlurc. Glycol 
standards should be freshiy prepared and analyzed. Adequate 
mixing is necessary to obtain valid results. Mixing. sonicating 
or mechanical shaking for al least 15 ininules is considered 
adequate. Do nol use plastic containers. 
A2.2.9 Reponing ofD(i!(i—^The values determined Irom lhe 
infrared spectnim for lhe components diseussed in the preced-
ing sections on speclral subtraction are reported in different 
v> ays because ol lhe nalure of lhe materiais present. Certain of 
the components are not calibrated. ineluding o.KÍdalion. 
nitration. sulialion, soot. anil phosphate antiwear additive. 
Olheis are calibrated. ineluding diesel fuel. gasoline. water, 
and glycol, Recommendalions for calibration prcicedures were 
included in previous sections of Anne\. 
A2.2.y. i Oxidation, nitration and sulfation components are 
not reported as eoncentraiion values, because there are many 
dilTcreni Chemical ctimpounds formed thal contribute to the 
measured absorption. Since no singic product Is formed. 
standard materiais are not available lo generate the calibration 
curves needed to relate absi>rbance to eoncentraiion. Abscir-
bance values related to the thickness of sample exposed to light 
are reported. The units usetl for reporting are absorbance per 
0.1 milliineter Íabs/O.l mm), which relates directly to the peak 
intcnsities observed in the dilfcrencc spcctrum of the in-service 
oil. The information for these components is most useful in 
trend analysis. 
A2.2,9.2 The carbori particles that iorm scxit do not cause 
locali/ed absorption. Instead, an offset of the spectral baseline 
due to light scatlering and absorption is observed. The magni­
tude of this otlsci is deiermined by tlie particle si/.e ol lhe soot 
as ucl l as its concenlralitm, 'fhe particle si/e observed is 
aflectcd by the engine type anti lubricant, .A.bsorbance per 0.1 
mm (abs/0.1 mm) value.s are reported, 
A2,2.9.3 Phosphate antiwear additive. lypically various 
fonns of zinc dialkyldithiophosphate in crankcase oils. is 
reported in absorbance per 0.1 millimeter (abs/0.1 mm) the 
same as the above oxidation components. However, lhe anti­
wear addiíive is reported as a negalive value since in the 
in-scrvicc used oil diíTcrcncc spcctrum the peak is negative due 
to lhe depletit)n of the additive compared to lhe original 
reference oil . 
A2.2.9,4 Fuel. water, glycol and gasoline are reported in 
weight percent values from calibralions with siandards. "fhe 
calibrations prepared for diese! fuel and gasoline may not 
accurately rellecl the fuels in use in particular regions of lhe 
worid. Because of this. these components should be calibrated 
wilh locally geiíerated weathered fuel standards, Water and 
!7 
4% E 2 4 1 2 - 1 0 
glycu! shuiikl not be routinely calibrated locally because otthe 
ditticuity ín making and analy/.ing standai"ds. 
A2,2.9.5 In practice. tlie approacii íaken ti) make uso oí the 
absorbance values tor the non-calibr;ited components is to note 
their increase over time within an engine, From a p!ot or table 
of the change in absorbance with time. judgments about when 
to change lhe lubricant can bc madc. 
TABLE A2.1 Petroleum Crankcase Lubricant Condition Monitoring Parameters—Spectral Subtraction 
Componení Measurement (cm'') Baseline (cm"'] Reporting LJnits Footnoies 
Water - A Heighl at 3428 1 point at 3700 wt% [calibrated method) 9 
Water - B Maximum near 3400 2 point: 3120, 3740 A/cm or wt%, vol% calibrated method 1, 2. 3, 9 
Soot - A Heighl at 1950 No baseiine Abs/0.1 mm 4 
Soot - B Absorbance at 2000, 1950 or 1900 No baseiine A/cm or wt% (calibrated method) 5, 9 
Oxidalion - A Max, Height 1800 to 1660 1 point: 1950 Abs/0,1 mm 6 
Oxidalion - B Pealí Closet lo 1709 in range of 1695-1725 1 point: 1900 Aí'cm 
Nitration Max. Height 1650 to 1610 1 point at 1950 Abs/0,1 mm 7 
Phosphate Antiwear Mm. Heighi 1020 lo 930 2 point 1020 and 930 Abs/0.1 mm 8 
(Negaiiue peak height) 
Gasoline Area 734 to 721 2 point 734 and 721 wi% (calibrated method) 9. 10 
Diesel Area 817 lo 804 2 point 617 and 804 wt% (calibrated method) 9,10 
Verificatlon peak: Veritjcalion peak; 
Area 883 to 854 883 to 854 
Sulfation Height at 1150 1 poinl at 1950 Abs/0,1 mm 
Ethylene Glycol Heighl at 883 1 poinl at 901 wl% (calibrated method) 1, 9, 11, 12 
Verifioation peaks: Verificalion peaks: 
May hl 1098 to 1069 Min 1110 Io 1098 
Max ht 1050 to 1030 Min 1063 to 1051 
Min 1029 lo 1023 
As noted in 9.4.2, tor ali components excepi soot, spectial subtraclion is done lollowed by till correction over lhe range Irom 4UU0 to 650 cm-1 For'sool',' íollów ilié 
specillc recommendalions In Table A2.1, After soot calcuiation. subtraction is done and a spoclrai tilt correclion is applied Irom 4000 to GbO. 
Noi"i-; 1—Calibrated methods lor waler and ethylene g lyco l are developed usui^ sliindard preparalions u t waler or cihyleiíe g lycol in appropriale 
uscd o i l mali iees. 
NoTii 2—Peak máxima may bc easily idcn i i t icd usirig second t lenval ivc ".peeira. 
Nor i í Waler measurements can be ai i jusled lor glyeol conicn i . 
NoTK 4—Soot calculatod f rom i insi iblractod síunple speclrum, 
N o i h 5—Soot oaloulated f rom siibCracled spectrucn, bcforc t i l l eoi rect ion. 
NoTf-. 6—Oxidat ion region Ibr lubr icant bicnds w i l h dicslcrs ba^c o i l can be adjuslcd Lo 1710 lo 1660, 
NoTt 7—Ai lc rna lc lUL-lhod for n i l ra l ion has been suggcsicíi lo el iminaie metal soap conl r ib i i l íon using peak al 1630 v«'iih baselinL' m in ima in rãnsí-
1655 10 1640 and 1620 to 1595. 
N c n : 8—Phoipha lc ant iwear i.s a ricjzalivc peak l ie ig l i l since it rcpresenls addi l ivo deplet ion eoinpiired to lhe new o i l . 
NoiH 'J—Calibrated meti iods are based on standard l inear regp^essíoii j i iodeis. 
NoTC 10—Fuel calibration.'^ are basod on wcalbered fuel and need lo bc adjuMcd lor locai variat ion in luels, 
NoTH I I — E t h y l e n e g lyco! calibralion.s ba.scii on 50:51) g l yeo lwa te r mix lurcs. 
N u i h 12—Glycol vcr i l i ca l ion peak local ions can bcsl be dcr ived I rom lhe '.ecoiid dcr iva i lvc speclrum. 
E 
18•|5I|^ E 2 4 1 2 - 1 0 
FIG. A2.1 Water Analysis Region for Petroleum Crankcase Lubricants 
Peak H e i g h t 
@ 1 9 5 0 c m - i 
(No baseline) 
FIG. A2.2 Soot Analysis Region Tor Petroleum Crankcase Lubricants 
19 
E 2 4 1 2 - 1 0 
0} 
CL 
E 
o 
o 
CN 
CO 
CM 
in 
o -o 
XD 
d) 
CN 
O 
O 
O 
íS 
CO 
cõ o 
CD 
•<* 
O 
< 
Q 
< 
ca 
O 
Q 
< 
to 
X 
LU 
1.0 
0.9 
0.8 
0.7 
0.6 
Oxidation: 
Max. Height 
1800-1660 cm-' 
Nitration: 
Max. Height 
1650-1610 cm-i 
Sulfation: phosphate 
Peak Height 
@1150cnr i^^^_ Height 
' '1020-930 cm-i 
Baseline 
1020-930 cm-i 
2000 1900 1800 1700 1600 1500 1400 1300 1200 1100 1000 900 
Wavenumbers (cm') 
FIG. A2.3 Oxidation, Nitration, Sulfation, and Phosphate Antiwear Additive Analysis Regions 
0.036 
0.032 
0.028 
0.024 
0.020 
0.016 
0.008 
0.004 
0-000 
P e a k A r e a 
8 1 7 - 8 0 4 c m - i 
(Baseline points the same) 
870 860 860 840 030 B20 
Wavenumbers fcm') 
810 800 790 780 
FIG. A2.4 Diesel Fuel Analysis Regions lor Petroleum Crankcase Lubricants 
TO 
O . 
E 
0) 
X 
LJJ 
20 
E2412 - 10 
QJ 
O. 
E 
o 
o 
FIG. A2.5 Glycol Analysis Regions for Petroleum Crankcase Lubricants 
A3. DISTRIBUTION PROFILES AND STATISTICAL ANALYSIS 
CO 
< 
O 
Q 
< 
CO 
X 
UJ 
Q. 
E 
X 
LU 
A3, l Stntistica) analysis of histuric datu from a sufru-icntly 
large population of machincry can bc uscd to explore possible 
relationships between condition monitoring test data and ma­
chinery failuro modes- Such statislical analyses are a tooí used 
in establishing alarm limits for condition monitoring tests, A 
thorougli diseussion of distribution prolite analysis and alarm 
limit determination is beyond the scope of this practice. This 
annex merciy provides a summ;iry of distribution profile 
analysis for the interested uscr. Mure deliiiJcd descriptions can 
be found in Ref (1). 
A3.2 /-yegutyicy Disf/ihiiiion Phts—Hi.sfograms-
A3,2.l Distribution pk)ts are a eoinmon toul u,sed in lhe 
statislical analysis ol' condilion monitoring dala. The abscissa 
oi" the plot is the test data result. and the ordinale is the 
frequency at which a specitic resull occurs in lhe lest popula­
tion. Fig. A3.I shows an example distribution plot. In this 
exainple. the dala is from a population of 1910 diesel engine 
oils. The abscissa represents the integrated nitration result, A 
vertical bar is used lo represem the number of oils for which 
lhe test resull falis between lhe two abscissa vaiues. For 
example. lhe tallesl bar indicates thal approximateiy 410 
nitration values were between 7 and 8 A/cm. 
A3,2.2 To develop reliable alarm Iimils from statislical 
analysis t)f condition monitoring lesi data, the dala must be 
appri>ximalely nonnally distribuied. The histogram should 
have roughly a bell-shaped appearance and be free of niulli-
modal fealures, The histogram in f i g . ,A."í.l shows an appruxi-
mate in)rmal distribution. 
A3.2.3 When the Ff-IR resulls are limited lu non-ncgativc 
values. and lhe median of the distribution is close to zeio. the 
disiiibution will not appear normal (see for example f"ig. A3.2). 
While a inean and standard dcvialion can slill be calculaied, lhe 
iiser should verify thai alarm limits based on these statistics are 
descriplive of the actual distribution. For exainple, only about 
5 of lhe values shnuld fali above lhe mean plus iwo standard 
deviations. 
A3.2,4 Multimodal dislribulions (Fig, A3.3) and broad. ílal 
dislributions {Fig. A3.4) should not be ulilized for statislical 
analysis, Both examples are indicative of multipie sources of 
lhe same data. low ralio of normal dala to failure dala or poor 
measurement precision, 
A3.? Samp/ing Consideranony. 
A3.3.1 The data used in the statislical analysis should 
inciude a history of ali machines of a like type for al icast one 
overhaul peritid, The population should inciude a minimum of 
several hundred resulls t\ir meaningful statislical tmalysis 11 
the population of machines is very large. less than one overhaul 
perioíl may be siifticient. 
A3,3.2 Uniess analysis demonstrates olherwise. segregate 
and separalely analyze resuils írtmi dilferenl machine types and 
for machines using dilferenl t>il Ibrmulalions. Even machines 
wilh diflerent sump sizes or dilferenl melallurgies should 
inilially be anaU/.ed separalely, If the inilial analyses yield 
similar limits for ali lest parameters, it iriay be appropriale lo 
pool results. 
21 
E 2 4 1 2 - 1 0 
A3.3.3 RanUuin selectiun of samples does not neeessarily 
provide for normally distributed results. Sequential samples 
over the course of the overhaul period are more likeiy to yield 
normally distributed results. 
A3.3.4 The p()pulalion analyzed niusi inciude exainples of 
ali oil-related failure modes, at typical failure rates, I f too many 
examples of failures are included, the distribution may be 
broad and calculaied limits inay be too high. Alternatively. i f 
failure modes are underrepresented, the distribution may be 
narrow. and the calculaied limits may be too low. 
A3.4 Te/ihilive Ahir/n Liinif Ca/cii/ario/is-—The specilic cal­
culations and Iimils used in a condition-monitoring prt)2ram 
are established wilh advice and guidance from the machinery 
manufacturer and mainlenance group. The íollov\ing are pro­
vided only as an exainple. 
A3.4.! The user must hrst esiablish calegories l\)r test leveis 
and alarms. 'lypically a warning or alert levei wil l bc used as 
an early indication of a polential problem. and an alarm levei 
wil l be used as an indication t)f lhe need for immediale 
correelive ttction. More leveis inay be used. but at the expense 
of increased complcxiiy. 
A3.4,2 PIol the oil test resull dala on histograms, marking 
data that corresponds to oil-related failures. Verify that the 
frequency distribution is approxiinalely normally distributed. 
A3.4.3 Calculate tentative limits based on lhe average and 
standard devialion of the oil test results. 
A3.4.3.I Calculate a tentative alert (warning) limit as the 
average plus two standard deviations. This assumes a tesi resull 
for which the value incrcascs wilh lime. For results where the 
value decreases vvith time, the Iimils would be the average 
minus lhe corresponding number of standard deviations. 
A3.4,3.2 Calculate a tentative alarm limit as the average 
piíis f o L i r slantlard deviations. 
Nitration Distribution 
N -r. 1910 
- 1501 
IUILII r^lilralion Valui: {Acm '} 
Tliesç ref.ulis are calculated as orca tmder the curvo. 
FIG. A3.1 Distribution of Nitration Measurements from -1900 Diesel Engine Oils 
22 
Exemplar para uso exclusivo - TEXSA DO BRASIL LTDA - 04,608.635/0001-27 (Pedido 526200 Impresso: 17/04/2015) 
C =3-
^ ^ TL. Ç 
S 3 ^ G 
ri — 
E . c 
cr 5 
d 
í o. 3- ^ ^ 
3 ^ -3 £í 
^ o —. 1/; 
=- 3^ ^ 5 
_ fC -1 — • 
5 CL 
^ H Sr =̂ 
C " ET 
=/ C í í" 
í 3 ? 
P « 
H á 
'J: ~-
^ C 
cr 5-
•a E : -• r. o 
r i !^ r-, 
" C 
c X 
o — 
5̂ i 
o 3-
5 2 
c 
o 
í 3 
cl ^ 
3 f; 
3 _ 3 
— O C 3 3rí 
=̂ =• r, 3-
3 5 -
d — 
3 
_ 
(T 
^ . 3 
'T' n r. 
13 ^ . 
3 c; 
d « 3 
-1 '•/c 3 . 
C- 5. = ^ • o i . F, 
—̂ 3 
™ o — 3 — 
p 3 
3 
c —• 
c 
t j —- _ 
„ 3 C5 ^ 
3 < FL S" 
< 'ro ^- c ^ 
? 3-cjc 3 a 
3-
c H 
c 
c c 
c 
3: 5 0 3 - = . -
3" c r ::r 3 ^ O 31 w 
1^ rr- G ÇP 
0 0 3 3' 1-
3 n l 17/ 
ã 3" n' 
ri 
O" 
£J 
3 
C 
í 5 
r. 
li 
n 
0 "3 r— 
CC CL 
3, 
li 
3 3 a 
r ; d 3 r. 
3 
c 
< = r 3 
P . 
r, ,—̂ ti) 
3' f/a B" •~< 
ô a 
r. 3 
c • — o 
2 ~̂ ir: fí 
5: o 
rc — 
d 
"2, : Í £L 
3 . — 
^ — 3̂ 3- » TI; 
o 'Til 
13 ^ 
n — ^ — 
— .-' Ti c 3 
'—' 
r/o 
0 3_ 
— 
3 
C-
A 3 
<~J\ 
0 
3 
5 3 
= 3 
3 
O" d 
o ^ 3 
'— SO 
a 
3 •6 
D. 
0 3r 
0 
E: 
rc 3-
•jf. 0 
3-
•jf. 0 
O-
era 
3" 
•^ 
CI­ 3 0 
í C c; 3- :3 3 2 d " 5- = 
1 í r. 
r: 3- n. 
r. 
r, 
rJ <• 
i/: —. 
7= 
C ? z 5 7= 
C 
=r 
•9 3-
r. 
f í 3' 
3 < Õ r . 
-4.. 
O ' 3" 
3 C 11; 
ri ''3 
Q. 
n. ;— 3 
—' ' Í : 
r. 
c 
rr 3 0 
X 
2 
z 
Q 
- j 
Tl 
H 
Z 
z 
z 
-n 
?= 5i> 
C C -™^ 
c 
5 
> 2 
~ i 
c/í 
Z 
(/) 
í* 
O 
r 
> 
o I—I 
X 
CL 
X 
UJ 
A E 2 4 1 2 - 1 0 
R E F F R E I N C E S 
l í l Touis. 1,. A. , aíii l Turns. A . M . Miniiinen OilAmiívsis: Meilukís. 
Aimniíirioiiií: fícne/iis, 3rd cd i l iun , S T L E , ZDUS, 
12) Mi is lcr . D., "ConJ i l i nu M i m i i o i i n c ;irnl Di; i ! ini islÍLs uf M;n l i incs A n 
niTierging Tni i is t l isc ip l ine Mi iv int^ TOWLIIIIS Sli i iKlardi/aiJcn,'* Coihíi-
liíiii MiwiiiH-iiig'94. Jwies. M , . ed.. Piíu-i idg f Pru^s, 1994, pp. .í-17. 
(3) Coaltís, .[.. Hnd Sc l l i . L.. " I n l i a i p d Sprchuscopy a Tool Ibr 
M o n i l o n n g Oi l Uegradal ion," Ax/itxrs of Liiljncimí Oxidíifiaii, ASTM 
S/miul Ih/miairPiib/íraiiri/i 9/ò. A .STM, 1986. pp. 57-78. 
(4j Garry. M . , " A p p l i e d Interpretai ion o f K f - I R O i l Analysis Resulls; lor 
Impr t iv ing Predicl ive Maintenance Programs," Froceeding.\ lhe 
1992 Joiíil Oil Aiiíih >/.! Pn/i^ruiii /iiu-niuihuMl (.'iiiii/iiidii Mi/iiiit/riiií; 
Owfcn-m-c. J C A P - T S C . 1992. pp. 233-2.'^4. 
1.̂ 1 Powel l . J,. and C'oinpton, U., ' "A i i lomalcd FTIK SpcflroiTn;i!y lor 
M o n i l u r i n g H y d r o c a r b u n - I í a s e d Eng ine O i N . " Liibrictiiiíin 
l-fmm-i-rm^. 49.' M. i iv l i 199. \. 2.TV2.Í9, 
i(>i lo i íTi . : \ . . and Poviel l , J., "Molee i í la r Analysis o l ' L i i i i r icai i ls by F I - I R 
Speclromeu-y, ' P/RM 7h/iiMh^v. lO, 4, Augusl 1997, pp. ."iS-M. 
i7) Laicas, M , , and Anderson. D.. "Labo ra lo i y I K o d Oi l Analys is 
Me lhods . " CaC/S/lJi J'rilio/a5>v Daia Haitdhaok. ed.. K. Booser. 
C R C Press. 1997 
ASTM International takes no pasition respectlng the validity ol any palent rights asserted in connection wilh any item menlioned 
in this standard. Users ot /'us standard are expressly advised that dclermination o! the validity ol any such palent nghis. and the nsk 
of iniringement ol such righis. are entirely their awn responsibility. 
This standard is subject to revision al any time by the responsible technical committee arid musi Se reviewed every tive years and 
Unol revised. either reapprovetí or withdrawn. Your comments are invited either tor revision al this standard or lor addilional standan^s 
and should be addressed to ASTI\â International Headquarters. Your comments will receive carelul consideration at a meeting of the 
responsible technical committee. which you may altend. II you leei that your comments have nol received a tair hearing yau should 
make your views known to the ASTM Committee on Standards, at the address shown below. 
01 
Q. 
CO 
< 
ca 
O 
Q 
< 
X 
UJ 
This standard IS copyrighted by ASTM International. 100 Ban Harbor Drive. PO Box C700. WesI Conshohocken. PA 19428-2959. 
United Stales. Individual reprints (single or multipie copies) ot this standard may be oblained by contaciing ASTM at ttie above 
address or at 610-332-9585 (phone). 610-832-9555 (lax). or service@astm.org (e-inail): or through the ASTM website 
(www.astm.org) Permission righis to photocopy lhe standard may also be secured Irom the ASTM website iwww.astm.org/ 
COPYRIGHT/) 
25