PAPER from 10th International Colloquium Fuels Conventional and Future Energy for automobiles 

January 20‐22 2015 Technische Akademie Esslingen in Stuttgart/Ostfildern. 

 

 

 

 

 

 

 

 

 

 

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InjectoDeposi Jim Barker Innospec Ltd Jacqueline RInnospec Ltd Abstract Early studieswere limited majority of thdecompositiocontrolled bydiesel fuel syarchitecture afuel, coupledfuels such asits different sin deposit forsystem. Furthin nature wheto be not onlybut also, in th(IDID), layerdeposits haveespecially ondeposits are msevere issuesemissions, ansystems are ninjection gasDCAs have talso new gencombat theseand range of effectivenesstreating these Introduction The worldwicontinues withe United Stregulations inproposed or clocomotive trinjector manuand temperatmanufacturer

or and Fits

d, Ellesmere P

Reid d, Ellesmere P

s of deposits into injector no

hese deposits on during the y deposit contrystems with hiand the severe

d with the intros Ultra Low Susolubilising carmation at varher, historical ereas the latesy complex inohe case of intered in nature. e been found tn the fuel filtermanifested in s with drivabilnd engine failunow also beinoline systemstheir place in cneration DCAse deposits. Thif deposits founs of some of the deposits.

n

ide legislative th for exampltates, China Vn India. Therecoming into eransport. Theufacturers goitures to attain rs have had to

Fuel Sys

Port, UK

Port, UK

n injectors andozzle orifice dwere the resucombustion prol additives (igh pressure ce conditions itoduction of hiulphur Diesel apacity, has serious points innozzle depos

st deposits havorganic and orernal diesel injIt is also the cthroughout thrs. The resultsfield problem

lity, fuel consuure. Problemsg observed wi

s. Although cocombating deps that have beis paper discu

nd, their originhe new DCA c

drive to redue Tier 3 being

V in China ande are also regueffect regardine result of thising to ever-higthese targets

o re-engineer t

stem

d fuel systemseposits. The

ult of fuel process and we(DCA). Modecommon rail t applies to theighly refined (ULSD) with

een an upsurgen the fuel sits were organve been shownrganic mixture

njector depositcase that e system, s of such

ms such as umption, s in injector ith direct

onventional posits there aren developed

usses the variens and the chemistries in

ce emissions g introduced ind the Bharat ulations ng marine and has seen fuelgher pressureswhilst the fuetheir product

s

ere ern

e

h e

nic n es ts

re to

ety

n

n

l s el

wreousyna ThinexbeFu27de Thre

stu D Dnuthinva[1Fi Thin(Ctipthimof

with for exampefinery producutcome of thisystem. In this parrow field of

he causes of dn Figure 1 andxample has beeing adulterateurther with die700 to 3000 baeposits will in

he purpose of eported by our

Figu

udy of fuel de

iesel Deposits

iesel depositsumerous studiheir origin [2-5n a modern comarious parts of19,21]. A typicigure 2.

he majority ofnjectors. The ICEC F-98-08)ps. Internal d

he focus of recmportant problf IDID observ

Fuel acolour

le reduced sulcts such as FAs is a rise of depaper we will diesel and ga

diesel fuel systcontinue to b

een vehicle proed with vegetaesel injectors ar the opportucrease.

f this paper is trselves [2] and

re 1. Sources of

eposits and the

s

have been anes to characte

5, 12-15,16-20mmon-rail engf the injector scal common ra

f work carriedIndustry Standis designed to

iesel injector dcent work and lem in the indued can be categeing depositsr.

lphur whilst bAME or ethano

eposits througl be concernedasoline system

tem deposits abe pertinent. Ooblems as a reable oil in Argnow being at

unities for form

to add to the kd others [3,4]

f Diesel Depos

eir causes.

nd remain the erise them and0]. The diesel gine has seen system and in rail schematic

d out has centrdard engine teo assess foulindeposits (IDIDare regarded

dustry at preseegorised as: ts: tacky brow

blending non-ol. The ghout the fuel d with the

ms.

are described One recent esult of diesel gentina [1]. pressures of

mation of

knowledge in the

its.

subject of d understand

fuel system deposits in filters is shown in

red on the est procedure ng of injector D) have been as the most nt. The types

n or black in

Carbarom

Metsalts

Ampolymol

Deposits are has investiga

Figure

Diesel Inject The introducprocedure (Ctendency of fadditives hasto combat the

Figure 3. Oengine tests o

Engine tests DW10B engitest fuel) havadditives as s08 test proceneodecanoatebrief outline used the 199the DI type wsystem and µoperated on tcycle consisttotal cycle timrepeated to g

bonaceous: blmatic graphitetal Carboxylats of sodium.

mide lacquer deymeric in natulecular weight

also found onated the inside

e 2. A Typical C

tor Tip Depo

ction of the IndCEC F-98-08) fuels dosed ws led to the intese deposits e

bserved power on fuel containi

deposit co

conducted usiine using RF-

ve shown the eshown in Figu

edure the fuel we to give 1mgof the procedu7cm3, 4-cylin

with a high preµ-sac six-hole the engine testing of 12 steame of 3600 se

give a total tes

lack particulate/ene precursotes: off white

eposits: thin fiure linked to pt PIBSI specie

n fuel filters ane of the comm

Common-Rail S

sits

dustry Standarto assess the iith different d

troduction of neffectively.

data from DWing Zn neodecantrol additive.

ing the CEC F06-03 (Europeffectiveness oure 3. As per was adulterate/kg of zinc in ure is given hder, turbo-chaessure commoinjectors. Tht bench accord

ady state condeconds. The cyt time of 32 h

tes containingors. carboxylate

ilms of deposipoor quality loes.

nd recent woron-rail itself.

Schematic

rd test injector foulin

deposit controlnew chemistri

10B keep cleananoate plus nove

F-98-08 ean certificatiof these novelthe CEC F-98ed with zinc the fuel. A

here. The testarged, engine on-rail fuel he engine was ding to a test itions to give ycle was ours.

g

its, ow

rk

ng l ies

n el

ion l 8-

t of

a

Thshreth

Fit

InL PomPIpuinun RcacosuThwcacoininjanuthsp TiSIstcoinioPI

hese novel dephown to be effesulting in a rahe additive afte

igure 4. Observests on fuel con

nternal Dieselacquers

olymeric amidmolecular weig

IBSI) has beenublications [13nvestigated an nknown prove

ecent work [2arried out on aommercial lowuccinimide samhe paper descr

which in the CEaused injector ontrol additiven the same testn addition to thammed injectoumber of analyhe needle surfapectroscopy (F

ime of Flight IMS) showed,arting materiaommercial) wanjector depositon C4H2O2N

- wIBSI (non-com

posit control afective in cleanapid restoratioer 32 hours. T

ved power data fntaining Zn neo

control ad

l Injector Dep

de lacquer depght polyisobuten investigated3-20]. In manyill characteris

enance.

] on these depa well charactew molecular wmple, (LMW Pribed a non-coEC F-98-08 Pesticking. A co

e (DCA) was ft and also prevhe low molecuor needles fromytical tests. Thace was confirFTIR).

Single Ion Ma, by spectral cal, that the LMas present in at. This is showwhich is commmmercial) and

additives haveaning up existion of power onThis is shown

from DW10B codecanoate plusdditive.

posits – Polym

posits and theitene succinimid in a number ny cases these sed LMW PIB

posits saw engerised, lab pre

weight polyisoPIBSI (non-coommercial LMeugeot DW10ommercial PIBfound not to cvented stickinular weight mm the test werhe presence ormed by infra

ass Spectromecomparison wiMW PIBSI (noa lower layer own in Figure 5mon to both thd the injector d

e also been ing deposits n addition of in Figure 4.

clean up engines novel deposit

meric Amide

ir link to low ides (LMW of have

BSI of

gine testing epared, non-obutylene ommercial)).

MW PIBSI 0B engine BSI deposit cause sticking ng when used aterial. The

re subject to af amide on -red

etry (Tof-ith the

on-of the 5 using the he LMW deposit.

e

e

Figure 5. Toffrom

No Industry IDID. CEN TC19/WG24(Coordinatintest committefor IDID cau Although an studies there the understanOxidation Tequalification fuel. This teca number of investigativeinfra-red techthe test can information. Thtesting with anoted work oJFTOT and adeposition onused to illustcharacterisatiJFTOT benchshown in Fig

Figure

f SIMS Depth Puse of LMW P

Standard test (Committee E

4 Injector Depng European Cees are workin

used by LMW

engine test wis also a need

nding of depoester (JFTOT)test for the th

chnique has begroups [13-15

e bench test fohniques we hanform regardihe recent puba LMW PIBSon the lab prepa reference fuen the JFTOT ttrate the use oion tool for sah test. The inf

gure 6.

e 6. Infra-red MTube

Profile Study ofPIBSI (non-com

is currently avEuropean de Nposit Task ForcCouncil) TDFGng to develop PIBSI.

will be the finad for a bench tsits. The Jet F) is the Industrhermal stabiliteen extended t5 ] including or IDID. Usin

ave extended ting the chemislication [2] deI (non-commepared sample uel. This resulttube. This samf infra-red micamples generafra-red map of

icroscope Map Deposit.

f „stuck“ injecto

mmercial).

vailable for Normalisation)ce and CEC G-110 engine an engine tes

l arbiter in anytest to assist inFuel Thermal ry Standard ty of aviation to diesel fuel bourselves as ang mapping the degree thastry of depositetailing engineercial) also using the ted in

mple will be croscopy as a

ated by the f the deposit is

of JFTOT

or

)

st

y n

by n

at t e

a

s

Thtrathatim~1fudedishLMwge InC Incaveis InDBCEthstan TeendousreneouthstwcopeexThfosoteco

Figure 7. Infra

he spectra weransition can b

he tube, amidet ~1670cm-1. Tmide of the PIB1705cm-1. Theuel. It may be eposit on diffeifferences in showed both anMW PIBSI (n

with what was fenerated needl

nternal Dieselarboxylates

nternal diesel iarboxylate souestigation. As currently no I

n the US, CRCIESEL Perforench/Rig/InveEN TC19/WG

he CEC TDFGandard enginend dodecenyls

ests were condngine to assessosed with sodising RF-06-03eceived and theodecanoate. ut as describedhe exhaust gasarted the exha

were recorded dompleted 8 teseriod after whxhaust gas temhis is referred

or a further 8 hoak period befmperatures re

ontinued until

ared spectra froJFTOT tube

re collected albe seen in Figu is predomina

The further aloBSI comes to e amide is formspeculated thaerent parts of tolubilty in the

n imide and annon-commercifound previoule [2].

l Injector Dep

injector deposurces have alsofor the polymIndustry Stand

C committee surmance Groupestigation sub G24 Injector DG-110 panel, are test using a “succinic acid (

ducted using ts the injector sium salts. The3 (European cee fuel was notThe engine te

d above with atemperatures

aust gas tempeduring 15 minst cycles followich the engine

mperatures for to as 8 hour d

hours of test cyfore being re-secorded to giv

32 hours of te

om varoius poine deposit.

long the tube ure 7. At the bant with a stroong the tube othe fore with med from the at the two matthe tube becaue fuel. Thus a n amide specieial) deposit. Tusly on the eng

posits – Meta

sits (IDID) froo been the sub

meric amide ladard engine teub panel on ID

p - Deposit Papanel), and in

Deposit Task Fare working to“fuel soluble”(DDSA).

the CEC F-98sticking tende

he tests were certification tet adulterated west procedure wadditional mos. When the eeratures for eanutes. The engwed by a 4 hoe was re-starter each cylinderdata. The eng

cycles followestarted and the

ve 16 hour dataest cycles had

nts along the

and a beginning of ng vibration

one travels thea band at acids in the

terials use of bench test

es exist in a This agrees gine test

al

om sodium bject of in-

acquers, there est method. DID (CRC nel n Europe, Force, and develop a

” sodium salt

-08 DW10B ency of fuels arried out st fuel) as with zinc was carried

onitoring of ngine was

ach cylinder gine then our soak ed and the r recorded.

gine then ran d by a 4 hour e exhaust a. This

d been

e

completed orsignified seri Previous worsodium 2-ethdodecenylsucsticking afterdid not causefuel sodium 2solution in 2-out to determadditives wersodium carbo

The change iFigure 8. Thfailed to starthours of runn

Figure 8. Obsfuels conconvent

A commerciaadditive comadded at 2X Na (as Na 2-The test ran finjector stick

Figure 9. Exhon fuel co

co

Next generatalso been sho

r until the engious injector s

rk has shown hylhexanoate iccinic acid (Dr 8 cycles. Soe injector stick2-ethylhexano-ethylhexanol

mine if commere effective inoxylate depos

in observed pohe sodium 2-ett following thning.

served power dantaining Na 2-etional and nove

ally available mmonly found

treat rate to thethylhexanoatfor the full 32

king. This is s

haust gas temperontaining Na 2-onventional dep

tion novel depown to be effe

gine failed to ssticking.

the use of fuein conjunction

DDSA) to cauodium 2-ethylhking. To aid soate was addel. Further worercial deposit cn preventing thits within the

ower for each thylhexanoatee first soak pe

ata from DW10ethylhexanoate/l deposit contro

conventional in diesel fuel

he fuel containte) and 10 mg

2 hours withoushown in Figu

ratures from DW-ethylhexanoate

posit control add

posit control aective in preve

start, which

el soluble n with use injector hexanoate alonsolubility in thd as a 10 %w/rk was carriedcontrol he formation oinjectors.

test is shown e/DDSA test eriod after 8

0B engine tests DDSA, plus ol additives.

deposit controglobally was

ning 0.5 mg/kgg/kg DDSA. ut signs of ure 9.

W10B engine tee, DDSA and ditive.

dditives have enting injector

ne he /w

d

of

in

. on

rol

kg

est

r

stfufuanwFi

D

ThthPrw

Inimlafebebedeco Awfrwcuthre11 Thsusu3

icking in the puel. A novel Duel containing nd 10 mg/kg D

without signs oigure 10.

Figure 10. Exhtest on fuel co

n

iesel Commo

he work abovhe common-rareliminary wo

will now be des

n a diesel fuel mportant partsator where the eeds fuel to theeen investigateeen studied. Hescribing the common-rail in

A common-railwhich had suffe

om the field inwith ULSD untut up and one he inner surfacesin and subjec1, 12 and 13.

he surface shourface of the purface. There to 25 microns

presence of soDCA was adde

0.5 mg/kg NaDDSA. The tef injector stick

aust gas temperontaining Na 2-enovel deposit co

on-Rail Depos

e has been limil diesel fuel i

ork on analysisscribed.

injection systis the commofuel is stored

e injector systed [10] until n

Here we presencorrosion that n field use.

from a mediuered a failed inn the USA. Ittil injector failside of the pip

ce of the rail. Tct to SEM ana

owed general cpipe with rust d

was also pittins.

odium speciesed at 1X treat ra (as Na 2-ethest ran for theking. This is

ratures from DWethylhexanoateontrol additive.

sits

mited to the injinjection systes of a diesel c

tem one of theon-rail, a pressat high pressu

tem. Though inow the rail itnt preliminaryhas occurred

um duty diesenjector was ret had been sublure. The compe removed toThis was thenalysis as show

corrosion acrodeposits seen ing observed t

added to the rate to the

hylhexanoate) full 32 hours shown in

W10B engine , DDSA and

jector part of em. ommon-rail

e most sure accumu-ure which injectors have self has not

y data in a

el engine ecovered bjected to use

mmon-rail was o investigate n mounted on wn in Figures

oss the inner across the

to a depth of

Figur

Figure 12. SE

Figure 13. SE

The presenceaspects. One ULSD on a m

re 11. Inner Sur

EM Micrographwith pits 25

EM Micrographwith pits 8-1

e of such corrois that it show

metal fuel syst

Inside surfacecommon rail

rface Common-

h of Common-r5 microns deep.

h of Common-r10 microns deep

osion is of intws the corrosivtem surface bu

8 microns

e of

rail Pipe.

rail Inner Surfac.

rail Inner Surfacp.

erest from twove effect of ut also the pits

25 microns

10 microns

ce

ce

o

s

fosyinth Fulic

D

Fuanobdedobltha Cefde

c

ThanmtefrfrFi InreasCprteit

ormed are activystem [11]. Thngress, biodieshe corrosion in

urther investigcation.

iesel Fuel Fil

uel filters are nd as such canbserved in theeposits. Filteroped with zinclack deposits. he addition of reduction in thlearly these noffective in preveposits throug

Figure 14. Fucontaining Zn n

he applicationnalysis of dies

many years [22chnology has om the filter som a Europeaigure 15.

n addition to bed shows a domsymmetric COOO symmetriresence of carbchnique, the cis analysed sh

ve sites for fuhe corrosion msel componentnhibitor additiv

gations will be

ter Deposits

designed to ren accumulate s

injectors or prs removed aftc neodecanoat Filters taken novel deposit hese deposits ovel deposit cventing not onhout the fuel s

el filters from Deodecanoate wi

control ad

n of infra-red ssel filter sampl]. The advent made possibl

surface routinean diesel filter

ands associateminating band

OO stretch andc stretch at 14boxylate saltscaveat that onlhould always b

uel degradationmay be the rests [12] or disaive.

e reported in a

emove particlesimilar deposiprecursors to tfter DW10B tete showed a bfrom tests co

t control additias shown in F

control additivnly injector desystem.

DW10B engineith and withoutdditive.

spectroscopy les has been ct of diamond Ale direct acquie. An examplr spectrum is s

ed with dieseld at 1565 cm-1

d in conjunctio446 cm-1, suggs. Although a vly the surface be borne in m

n in the fuel sult of water

armament of

a future pub-

es from fuel its to those those esting of fuel uild up of nducted with ives showed Figure 14. ves are eposits but

e test on fuel t novel deposit

to the carried out forATR istion of data le of a filter shown in

l, the infra-1 assigned to on with a gests the very useful of the depos-

mind.

r

-

Figure 15. Eu

The work ondeposits are iing the deposshould also bcommon-railHence our prpreliminary w Gasoline Inj It would be nto one fuel syof recent repoinjector depoeconomy conpushing gasoinjection gasmarket share20% of the wpapers and pprevention hathese have fostudies of thethe body of ta gasoline dir

Figure 16. SE

The SEM of deposit arounanlaysis of th

uropean Field DSpe

n diesel has shoimportant, undsits formed is be noted that tl diesel systemrevious work owork on the co

jector Deposi

naïve to believystem alone anorts regarding

osits [5, 6]. Thnsumer satisfaoline engine moline engine t

e of this type oworld market batents on depoas also increa

ocussed on inje chemistry ofthe injector. Hrect injection

EM Image of GT

the injector tnd the tip and he deposit by X

Diesel Filter Directrum.

own that althoderstanding ananalytically c

there are otherm which requiron diesel filteommon-rail d

its

ve that depositnd there have

g direct injectihe drivers of vaction and emimanufacturers technology, wof powertrain tby 2020. The osit formationsed [5-8]. Thector design of the deposits

Here we report injector which

Gasoline Direct ITip.

tip, Figure 16,the injector hX-ray fluoresc

rect Surface AT

ough injector nd characteris

challenging. Itr parts of the re investigatiors [22], and th

described herei

ts are restrictebeen a numbe

ion gasoline vehicle fuel issions are toward direct

with estimates oto be around number of

n or its e majority of or fuels, and at the tip and initial work o

h had failed.

Injection Inject

showed holes. The cence element

TR

s-t

on. he in.

ed er

t of

in on

tor

tal

anmvise

Thanan

Thacluwspprtowde InhaguThpu C Thcoteun

nalysis (EDAXmetals, just trac

isual morpholoeveral differen

Figure

he injector hond an examplenalyses showe

F

he injector necross the ball aube oil constitu

were found. Depring but againresent. In sumo be different i

with a more cryeposits are ma

nitial data fromas shown the dum, intermedihis study will ublication.

onclusions

his work has soupled with inchniques can nderstanding I

X) did not shoces of molybdogy of the dep

nt chemical sp

e 17. SEM Imag

les where all be is shown in Fed a lack of me

Figure 18. Inje

edle, Figure 1and shaft. In thuent metals (feposits were aln no significan

mmary, the depin nature to deystalline naturainly organic.

m SEM and Indeposit to be cates and carbobe fully descr

shown that thenfra-red spectrbe regarded a

IDID formatio

ow significantdenum and calposits would s

pecies being pr

ge of Injector H

blocked to a cFigure 17. Agetals being pr

ector Needle.

18, had deposithis case, tracefor example mlso noted on tnt amounts of

posit on the neeposits found re being obser

nfra-red microcomplex, withonaceous deporibed in a futu

e bench JFTOroscopic mappas a useful teston.

t amounts of lcium. The suggest resent.

Hole.

certain degree gain, EDAX esent.

it present e amounts of molybdenum)the injector f metals were eedle appears elsewhere,

rved. The

oscopy studiesh both fuel osits present. ure

OT test ping t for

s

The challenge of removing injector tip, IDID and fuel filter deposits has been met by the development of a new generation of DCAs for which successful engine test data is described. Initial investigations of a diesel common-rail has shown corrosion levels to be high with concommitant pitting of the surface producing active sites which have potential to act as fuel degradation sites. The current factors causing deposits in diesel systems are also to be found in other fuel systems such as gasoline. The analytical techniques developed for diesel systems are useful to characterise and understand these deposits. Further it would be naive to think that deposits in the future will be restricted to these two fuel systems. The challenges remain to the DCA producers to keep injectors clean, and to the analytical community to apply techniques to understand the deposits formed. Regarding the latter, work on the application of Focussed Ion-Beam Scanning Electron Microscopy (FIB-SEM), Transmission Electron Microscopy (TEM), Atomic Force Microscopy (AFM) and Raman Spectroscopy, to diesel deposits will be the subject of a future publication. References [1] Rzeznik, M., ASTM Indianapolis 2014. [2] Barker, J., Reid, J., Snape, C., Scurr, D. et al., SAE Technical Paper 2014, doi:10.4271/2014-01-2720. [3] Dallanegra, R. and Caprotti, R., SAE Technical Paper / Journal Article, 2014, doi:10.4271/2014-01-2728. [4] Barbour, R., Quigley, R., and Panesar, A., SAE Technical Paper, 2014, doi:10.4271/2014-01-2721. [5] Dearn, K., Xu, J., Ding, H., Xu, H. et al. SAE Int. J. Fuels Lubr. 7(3):2014, doi:10.4271/2014-01-2722. [6] Smith, S. and Imoehl, W., SAE Technical Paper 2013-01-2616, 2013, doi:10.4271/2013-01-2616. [7] Kinoshita, M., Saito, A., Matsushita, S., Shibata, H. et al., SAE Technical Paper 1999-01-3656, 1999, doi:10.4271/1999-01-3656. [8] Rogerson, J. S. and Dawson, J.E., EP2145940A1P. [9] Graupner, O., Mundt, M., Schutze, A., Jacobus, J. et al. US78901470B2. [10] Karamangil, M.I. and Taflan, R.A., Journal of The Energy Institute 2012, 85, 4, 209-219.

[11] Venkataraman, R. and Esar, S., Chemistry Central Journal 2008, 2:25 doi:10.1186/1752-153X-2-2 [12] Farzal, M.A., Haseeb, S.M.A., and Masjuki, H.H., Fuel Process Technology 2010, 91,1308-15. [13] Reid, J. and Barker, J., SAE Technical Paper 2013-01-2682, doi:10 4271/2013-01-2682. [14] Ullmann, J. and Stutzenberger, H., TAE Fuels 9th International Coloquium, January 2013. [15] Bohenke, H., Gaiol, H., Benoist, G., Guillo, S. et al., JSAE 20145121, 2014. [16] Ullmann, J., Geduldig, M., Stutzenberger, H., Caprotti, R. et al., Diesel Injector Deposits, TAE 7th International Colloquium Fuels, Esslingen, 2009. [17] Schwab, S., Bennett, J., Dell, S., Galante-Fox, J. et al., SAE Int. J. Fuels Lubr. 3(2):865-878, 2010, doi:10.4271/2010-01-2242. [18] Lacey, P., Gail, S., Kientz, J., Milovanovic, N. et al.,SAE Int. J. Fuels Lubr. 5(1):132-145, 2012, doi:10.4271/2011-01-1925. [19] Lacey, P., Gail, S., Kientz, J., Benoist, G. et al., SAE Int. J. Fuels Lubr. 5(3):1187-1198, 2012, doi:10.4271/2012-01-1693. [20] Barbour, R., Quigley, R., Panesar, A., Payne J. et al., TAE 9th International Colloquium Fuels, Esslingen,2013. [21] Barker, J., Richards, P., Goodwin, M., Wooler, J., SAE Technical Paper 2009-10-1877.