### Disclaimer

This report was prepared as an account of work sponsored by the National Biodiesel Board and the Cold Flow Consortium. Neither National Biodiesel Board, the Cold Flow Consortium nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the National Biodiesel Board, the Cold Flow Consortium or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the National Biodiesel Board, the Cold Flow Consortium or any agency thereof.

## Col d Fl o w Consorti um Commi ttee

M a r a t h on A s hland Mr. Rick Stanko Mr. Steve Hoehne

F lint Hills Resources Mr. B r ett W e bb

Magel l a n Mi d s trea m Partn ers Mr. Rod L a wren ce

BP Mrs. Sherr y B o ldt

ADM Mr . Pe te r Re ime r s

Bake r Co m m odit ie s Mr. F r ed W e llons

West Cent ral Soy Mr. M y ron Danz er Mr. Don I r men

FPPF Dr. Gar y P e arl

National Renew a ble En ergy L a b o ratory Mr s. Te r e s a Alle ma n

F a rm er ’ s U n io n M a r k et ing a nd P r o cessing Association – F U M P A Mr. C h arl e s Ne ec e

K a ne b P i pe line Mr. Paul Heinz

Tesoro Ref i ning Com p any Mr. J ohn B e r g er

S c h a ef f

er Man u f a ctu r i n g Com p an y Mr. Hoon Ge CANME T – Natu ral Re sou rces C a nada Mr. Ed Ho g a n

M u r phy Oil USA Inc Mr. Ba rr y J e ffe r y

SOY M OR Mr . J im B l a i r

Sm it hfie ld Bi oenergy LLC Mr. J im B oushka

Non-Voting Members:

National Biodiesel Boar d Mr. Paul Naz z aro Mr. S t eve Howel l

University of Minnesota Mr. Ken B i ckel

M i nne sot a D e par t m e nt of C o m m e r c e Mr. J im Hedman

ii

## Executiv e Summa r y I n cre a sed use o f biodiese l has cre a ted some ha ndli n g ch allen g es fo r brin g i n g blend e d fuels to the c onsume r . The mo st imme dia t e ha ndling c o nc e r n f o r

ble nder s is a ssur a nc e th a t die s e l fuels and biodiesel c a n b e bl ended uniforml y and in a sing le phas e . More s p ecificall y , blenders ne ed g u idelines and param e ters fo r bl end i ng di esel fu el a nd biodie s el in colder climates. Neat biodiesel has a much hi g h er cloud point than conventional diesel fuels and
t h i s can i m p act handl i n g procedur es. Thi s conc ern becam e a pri o ri t y fol l o w i ng t h e pass a g e of

a

bill in Minne sota tha t r e quir e d a ll on- hi g h w a y die s e l f u e l s to c onta i n a t le a s t 2% biodiesel as earl y as J u l y 1, 2005.

I n response to the n eed i n Minnesota, the Na tiona l B i odiesel B o ard establi s hed a B i odies el Cold F l ow Consortium t o stud y the blendin g prop erties of biodiesel. Memb ers of the consortium included petr oleum marketers, biodi es el produce r s, fuel blend e r s , and other

e x pe r t s a nd inte r e ste d par tie s. The me mbe r s d e si gned a proje c t to investig a t e this cold flow problem. The proje c t g o a l was to define ope ra tin g paramete rs for blendin g biodiesel with di esel fuel at a v a ri et y of t e m p erat ur es, i n cl udi ng t hose seen in the winterti me in Minnesota.

To achieve this g o al, a small blending test r i g was de sig n e d to simula te sp la sh a nd proportional blending at the te rminal. Unadditiz ed No. 1 and No. 2 diesel fu els were selected, alon g with thr e e biodiesels with a ran g e o f cold flow prop erties. T h e test
te mpe r a t ure s we re de termine d using Minne sota winte r c lima te da ta

. All te sting f o c u se d on preparin g 2 volume p e rc ent biodiesel blends.

Splash blending tests wer e based on visual obse r va tion of wax cr y s t a l fo rm a t i on and are thus qua lita tive

. To e n sure qua ntita tive da ta w a s o b ta ine d, dif f

e re ntia l pr e s s u r e dr op

m easurem ent s w e re col l e ct ed. These m easur em ent s com p ared t h e p r essur e drop of neat die s e l f u e l thr o u g h a f ilte r with the pr e ssure dr op cr e a t e d b y B 2 ble nds a t v a r i ous t e m p erat ur es.

Results from the testing s howed that the biodies el must be kept at least 10o F above its cloud point to suc c e ssf ull y ble n d with die s e l f u e l s in c o ld c lima te s. B e c a u se ge ner i c , una dditize d f u e l s we re use d in this proje c t , the a c t ua l te mp e r a t ur e s of the f u e l s will ne ed to be determined on an individ u al basis.

iii

## Tabl e of Contents Cold F l ow Consor tium C o mmitte e

.......................................................................................... i Ex e c u tive Summa ry

............................................................................................................... iii I n tr odu c tion

............................................................................................................................. 1 Scope

............................................................................................................................... ........ 1 Ex perimental Apparatus

.......................................................................................................... 1 Test Procedur es

....................................................................................................................... 2 Test F u els

............................................................................................................................... . 3 Results and Discussion

............................................................................................................ 3 Conclusions

............................................................................................................................. 5 Small Group Steering Co mmittee Members

........................................................................... 6 Appendix A. P&I D of Sp lash B l endin g Rig

. .......................................................................... 7 Appendix B

. P&I F o f M odified Test Rig

................................................................................ 8 Appendi x C

. S t ep-b y

- st e p Anal y t i c al P r ocedu r es

................................................................... 9 Appendix D. Certificate of Anal y s i s for #1 Di es el Fuel

....................................................... 11 Appendix E. Certificate of Anal y s i s for #2 Di es el Fuel

........................................................ 13 Appendix F

. Certificate o f Anal y s is for So y B i odie s el

......................................................... 15 Appendi x G. C e rt i f i cat e of Anal y s i s for Y e l l o w G r ease Bi odi esel

...................................... 16 Appendix H. Certificate of Anal y s i s for Tal l o w B i odi esel

................................................... 17 Appe ndix I

. Qua lita tive B l e ndin g Da ta

................................................................................. 18 Appendix J

. L i stin g of C onsor tium Me mbe r s Comme nts

..................................................... 22

iv

## I n tr oducti on I n response to the rec e nt passa g e of Minnesot a ’s b ill requiring 2% biodies el in all diesel fuels starting as ea rl y as J u l y 1, 2005, the N a ti onal B i odiesel B o ard conv en ed a Cold F l ow Consor tium. The Consor tium wa s ta ske d with i nve stig ating th e blendin g of biodiesel into die s e l f u e l a t te mper a t ur es simila r to those e x pe r i e n c e d in the Minne sota wi nte r , with the objective of de fining p a r a meters fo r succ e ssfull y preparin g homo g en eous sing le-ph a se blends. The Consortium was composed of fuel pr oviders, markete r s, blend e rs, and other inte r e ste d pa r tie s. E a c h me mbe r ha d an equal voi ce in the Consortium.


## Scope
Thi s st ud y was desi g n ed t o accur a t e l y det e rm i n e t h e t e m p erat u r e wh ere bi o d i e sel and No. 1 and No. 2 diesel could be blended at 2 volume per cent (2%) biodies el, while meetin g standards for bl end pre c ision and homog en eit y

. T h e approa ch taken was t o fabri c at e a sm al l

sc a l e ble ndin g s y ste m to simula te spla sh and prop ortional blending . Th e s y stem has the

c a p a b ilit y to ble nd biodiese l a t dif f

e re nt r a te s with dif f

e r e nt gr a d e s o f die s e l f u e l a t dif f

e r e nt temperatur es. This stud y focused on pr eparin g 2 % biodiesel (B 2 ) ble nds ex cl usi v el y

. The blending s y stem was s e lf -contained to in clude tan k s, pumps, motors, and necessa r y appurtenan ces. The s y ste m included the abilit y to heat and/or cool the biodi esel as ne eded and cool the diesel as n e e d ed.


## Experimental A p paratus The te st unit wa s de si g n ed to be tota ll y por ta ble to a llow f o r

f

u ture te sting at va r i ous locations. The desi g n of t h e test skid was speci f i call y size d f o r

te sting B 2 a s ma nda te d in the
sta t e of Minne sota . The t e st skid inc l ude d a n e nvironme n ta l c h illing c h a m b e r , c a p a b le of cooling fu el to near -60o F in a re asonabl y s hort p e riod of time. A photo g ra ph of the blending unit is in F i g u r e 1. E ach process and t e st w a s re co rded manuall y and with v i deo equipment along with the blendin g e quipment records of volu m e amounts. To assist in recordin g the results of these tests, the finished product tank inc l uded interior lig htin g , viewing po rts, and sample ports. The finishe d produc t tank was manu factur ed of a clea r materi al to offer the best possible opportunit y for evalu a tin g the format ion of cr y s tals.

The de si g n f o r

the f i r s t se r i e s of te stin g simu lated splash blending into a cl ear blendin g

c onta i ne r ma inta ine d a t ambie n t te mpe r a t ur e

. A proc e ss a nd instr u me nta tio n dia g ra m (P&I D ) of this test bench config u r ation is containe d in Appendix A. F o r pro portional blending , a flow loop wa s creat ed to allow the fue l s to circulate throu g h the piping while inside the cooling ch amb e r. The pipin g loop in clu d ed a filter and diffe renti a l pressure across the f ilte r wa s e m plo y e d t o monitor f

u e l visc osit y cha nge s a nd de t e r mine if t h e f u e l s wer e plugg in g the f ilte r s or stra ine r s. L a rg e inc r e a s e s in visc osit y or f

ilte r plu g g i ng would indicate the formation of wax or biodiesel cr y s tals. A P&I D of this con f ig u r ation is shown in Appendix B

.

1Figur e 1

. P hotogr a ph of Sma ll S c a l e T e s t Unit for B l e nding Biodie s e l a nd Die s e l Fue l



## Test Procedures Sequential Blending into Visible Container . The s e te sts simula te d splash bl ending

. F our scenari o s w e re t e st ed: 1. Cold No. 1 diesel was loaded into the containe r. The first t y p e of biodiese l was added to the top to c r eate a B 2 bl end. This pr ocedure was r e peat ed for each t y pe of biodiesel. 2. Cold No. 2 diesel was loaded into the containe r. The first t y p e of biodiese l was added to the top to c r eate a B 2 bl end. This pr ocedure was r e peat ed for each t y pe of biodiesel. 3. Bi odi esel was l o ad ed i n t o t h e cont ai ner first. The No. 1 diesel fuel w a s loaded on top to cre a te th e B 2 blend. This sc enario was rep eated fo r e a ch t y pe of biodiesel. 4. Bi odi esel was l o ad ed i n t o t h e cont ai ner first. The No. 2 diesel fuel w a s loaded on top to cre a te th e B 2 blend. This sc enario was rep eated fo r e a ch t y pe of biodiesel.

Proportional Blending. The bi odi esel and di esel fuel s wer e blended throu g h propo rtional blending . To a ccomplish this, four gallons of cold No. 1 or No. 2 diesel fu el were circulat ed thr oug h the f ilte r s a nd th e pr e ssure dr op ac r o ss th e f ilte r s me a s ure d. B i odie s e l wa s the n proportionall y blend e d at 2% and an y c h an g e in th e filter pressu re drop mo nitored. This procedur e was repe at ed wi t h each of t h e t h ree bi o d i e sel s . S t ep-b y

- st ep pro cedures are g i v e n in Appendix C.

2

## Test Fuel s A local truck r ack op erat or provided the dies el fue l s for t h i s proj ect . The fu el s were

una dditize d c o mme r c ia l g r a d e s of No. 1 a nd No. 2 die s e l f u e l s. The c e r tif i c a t e s of a n a l y s is are in Appendix D and E, respectivel y

. Th e biodie s els were so y

- , y e llow g r ease-, and tallow-derived fu els. The certific ates of an al y s is ar e in Appendices F

, G, an d H, respectivel y

. W e st Centr a l So y provided the so y b i odiesel. Rothsa y / L a ur en co provided the
y e l l o w g r eas e and t a l l o w bi odi esel s.

The biodiesels wer e sent to a test facilit y to me asu r e the cloud and pou r poi nts of the neat biodie s e l s a nd the B 2 blends. B e ca use the un a dditize d die s e l f u e l ( A ppe ndi c e s D a nd E ) wa s not available, a t y pical n o. 2 diesel was used to m a ke the blends fo r cloud point and pour point determination. The results of th is testing ar e shown in Table 1.

T a b l e 1. M easu red L o w T e mp erat u r e Pro p e rt ies o f F u e ls Us ed in t h is St u d y Cloud P o int P our P o int Fue l

° C ° F ° C ° F N o

. 2 Dies e l

- 2 3

- 9

- 2 7

- 1 7 So y B i o d ies e l 2 3 5 0 3 2 Yel l o w G r eas e Bi odi es e l 5 4 1 3 3 7 T a llo w Bio d i e s e l 1 4 5 7 1 8 6 4 2% S o y Bi od ies e l

- 2 1

- 5

- 2 7

- 1 7 2% Yel l o w G r e a s e B i o d ies e l

- 21

- 5

- 27

- 17 2% T a llo w B i od ies e l

- 20

- 4

- 27

- 17



## Results and D i scu ssion The initia l te sting use d vi sua l obse r va tion to de te rmine if shoc k c r y s ta lliza tion oc c u r r e d. Testing r e veal ed seve ral drawba cks with this method. F i rst, the fuel w a s p u shed throug h th e apparatus with nitro g en gas. B ubbles of nitro g en r e mained suspended in th e fuels impedin g visual observation. To all o w for visual observ a tion, the clear bl ending v e sse l was ex posed to ambient temperatur es. Al thoug h the fu el was pr ec onditioned to the test temperatur es and the plumbing was insulated, the ambient air wa rm ed t h e fuel s and t h e t e st t e m p erat ur e was unknown. Due to the qua litative nature of the dat a , no conclusions could be drawn f r om the visual data, howeve r the y are included in App e ndi x I

.
To resolve these issues, v a ne pumps wer e used to push the fuel rathe r than nitrog en gas. Tem p erat ur e m oni t o ri ng was used t o ensur e t h e p u m p s were not he at i n g t h e fuel s. The cl ea r bl endi ng vess el was r e pl aced wi t h a st e e l bl e ndi n g vess el . The st eel bl endi ng vess el was pl aced i n an envi ronm ent a l cham ber d e si g n ed t o k eep t h e app a rat u s at t h e d e si red
t e m p erat ur e. These chan g e s no l o n g er al l o wed fo r visual observation of the blending r e sults.

A qua ntita tive me a s ure o f c h a n g e s in the bl e nd was ne e d e d. Swage l ok SS- 8TF 2 f ilte r s of

va r y in g p o r o sitie s we re u s e d in c onjunc tion with dif f

e r e ntia l p r e ssur e ga u g es to indic a t e chan g e s in viscosit y o r s o lid formation. The diese l fuels were circul ated thr oug h a 15 micron filter to determin e the baseline p r essure d r op. Results of this baseline testing are listed in Table 2. The dur ation is the amount of time needed to dispens e 1 g a llon of fuel.

Ta ble 3 shows the re sults of te sting with the t h re e bi odi esel s. The fuel s we r e ci rcul at ed

3

### throug h the pump ri g fo r 180 seconds. The dif f

er e n tial pressure w a s measu r ed at va rious intervals throug hout the t e sting

. F o r the lo w and m i ddle cloud point fuels, the 100 mesh strainer was clean at the end of the cir c ul ation per i od. F o r the hi g h cloud p o int fuel, the
str a ine r wa s 50 % plu g g e d with solids. The 15 mic r on f ilte r did not a llow f o r

usa b le da ta
, a s the biodiesels ex ceeded t h e gau g e r a n g e and b y pa ssed the loop throug h the relief valv e.

T a b l e 2. Bas e lin e T est in g w i t h F u e ls t o Det e rmin e P r essu re Dro p A c ro ss V a ri o u s Siz e F ilt ers
an d St ra in er s Fue l S t r a in e r Flow Ra te , GP M T e mp erat u r e, oF Dur a tion,

sec Differential Pre ssu r e , PSI # 2 N o n e 1 6 4 6 0 0 # 2 N o n e 3

. 3 6 4 1 8 0 # 2 1 0 0 m e s h 3

. 3 6 8 1 8 7

. 5 # 2 1 5 m i c r o n 1

. 9 6 8 3 1 8 2 # 2 1 0 0 m e s h 1

. 4 6 8 4 2 1 # 2 1 5 m i c r o n 0

. 8 5 6 8 7 1 3 5 # 1 1 0 0 m e s h 3

. 3 5 0 1 8 3 #1 15 m i c r on 2.1 50 29 not m eas ur ed #1 100 m e s h 1.5 51 39 not m eas ur ed #1 15 m i c r on 1.1 51 37 not m eas ur ed

T a b l e 3. Bas e lin e T est in g w i t h Bio d i esel F u e ls t o D e t e rmin e P r es su re Dro p A c ro s s 10 0 M esh Filter. Sha ded l i nes ind i c a t e bi od ies e l w a s at or b e lo w its c l o ud p o i n t. Biodie s e l Cloud Point, oF Flow Ra te , GP M T e mp erat u r e, oF T est T i me,
sec Differential Pre ssu r e , PSI 3 2 3

. 3 5 0 6 0 5 3 2 3

. 3 5 1 9 0 5 3 2 3

. 3 5 1 1 2 0 5 3 2 3

. 3 5 1 1 5 0 5 3 2 3

. 3 5 1 1 8 0 5 4 3 3

. 3 5 0 6 0 6 4 3 3

. 3 5 1 9 0 6 4 3 3

. 3 5 1 1 2 0 6 4 3 3

. 3 5 1 1 5 0 6 4 3 3

. 3 5 1 1 8 0 6 58 3.3 51 60 17 58 3.3 51 90 16 58 3.3 51 120 16 58 3.3 51 150 16 58 3.3 52 180 14



### The diesel fuel w a s filter e d through the 15 micron filter then switc hed to th e 100 mesh
st rai n er. The di f f

er ent i a l pressure w a s m easu r ed b e fore, du ring

, and a f ter bl ending with biodiesel at a constant te mperat ure. Th e final dif f

e rential pr e ssure r eadin g was taken throu g h the 15 mic r on f ilte r a nd compa r e d to the die s e l b a se line r e sults to de te r mine the r i se in
pressure o f the blend (T a b le 4).

4T a b l e 4. Dif f e ren t i a l Pre s s u re Re su lt s o f Bio d i esel Blen d i n g in t o Die sel F u e l s T he s haded li nes i n d i c a te t hat t he b i o d ies e l t e m per atur e is at or be lo w its c l o ud p o int

. T e s t T y p e of D i e s el F u el D i e s el F u el Te m p

. F Bio d i e s e l Clou d P o i n t, F Bio d i e s e l Te m p

. F % Bio d i e s e l

in T e s t Sam p le Unbl end ed F uel D P

PSI B2 D P PSI DP Ri s e i n

PSI Com m ents

1 R R # 2 1 0 3 2 5 8 1

. 7 7 0 7 5 5

2 K e r o s e n e 1 0 3 2 5 0 2 4 0 4 0 0
3 # 2 1 0 4 3 5 0 1

. 9 7 5 8 0 5
4 K e r o s e n e 1 0 4 3 5 0 1

. 9 4 5 4 5 0
5 #2 10 58 56 1.8 75 82 7
6 Ker o s e n e 10 58 58 1.7 40 42 2
7 Ker o s e n e 0 3 2 5 0 1

. 7 3 3 3 5 2
8 K e r o s e n e

- 1 0 3 2 5 0 1

. 8 5 0 5 5 5
9 K e r o s e n e

- 1 0 4 3 5 0 1

. 8 4 5 4 5 0
1 0 Ker o s e n e 0 4 3 5 0 1

. 9 3 2 3 5 3
11 Ker o s e n e 0 58 53 1.9 40 45 5
12 Ker o s e n e

- 10 58 53 2 35 45 10 Ble nd U n su cce ssf u l
A l l above t e st s w e re perf o rm ed u s i ng a 15 m i c r on Fi l t er and 2 % B i odi es el B l ends. A l l s a m p l e s w e re t op s a m p l e s

.



### Unde r the c o n d itions use d in this stud y , re se ar c h er s de te r mine d tha t the bio d ie se l must be a t least 10oF w a rmer than it s cloud point when it is blended in cold diesel fu el. Althoug h some testing was conducted b e low the cloud point of the biodiesels, there is not enoug h d a ta to draw de finite conclusion s and the re co mmendatio n above is a cons ervative estimate. Una dditize d die s e l f u e l s we r e d e libe r a t e l y c hose n f o r

this stud y

. Due to v a rious f u e l properties en counter ed in the real wo rld, the tar g et temperatur es will need t o be determined on an individual basis based on the fuels in use.

The r e sults wer e shar e d with the Consor tium me mbe r s. A r e c o r d of th e i r c o mme nts is in Appendix J

. 

## Concl u si ons This stud y wa s de si g n e d to simula te dif f

e r e nt t y pe s of blending for biodiese l and diesel f u e l s. A sma ll te st r i g w a s c onstr uc te d to simula te r e a l wor l d ble ndin g sce n a r ios. The orig inal tests used visual observation to dete rmine when the blends w e re su ccessful. This method did not provide objective data. A modifi c a tion to the test methodolo g y w a s made – f ilte r s a nd dif f

e r e ntia l pre ssur e g a u g e s wer e use d to de te r mine the c h a n g e i n dif f

e r e ntia l pressure b e tween th e bas e fuel and the B 2 blends.

B a sed on t e sts with the fuels descri bed above, the stud y findin g s ar e:

• Qua lita tive visua l obse r v a tions of se que ntia l ble n ding with die s e l a nd biodiesel fuels showed cl ouding and po ssible c r y s talliz ation of the fuel.

o This may be a c o n c e r n in Nor t he r n a nd Midw e s t sta t e s whe r e biodie s e l will be blended into colder di esel fuel that ma y r e sult i n c r y s ta l f o r m a tion witho u t

a d e qua te mix ing

.

5

### • A t y pic a l rack bl ending s y s t em is “ onc e throu g h o n l y ” without cir c ulation throug h a pump.

o Circulating diesel o r bi odiesel fuels throu g h a pum p does not match up with real world r ack blendin g s y stems.

o I n this stud y , test run ble nding used circulation th roug h a pump that may ha ve pr ovide d a dditiona l she a r in g a nd mix ing tha t he lpe d to e limina t e “shock” or wax cr y s talliz ation.

I n this stud y , succ essful B 2 blends we re mad e wh en the biodiesel was 10° F above its cloud point. Una dditize d die s e l f u e l wa s de liber a t e l y c h ose n f o r

this stud y a nd the thr e e biodie s e l s

were s e lected to span a r a nge of cloud points and are not meant to be repr e s entative of all fuels encounte r ed. B e cau se of the vari et y o f fuel p r operties, the targ e t te mp e r a t ure s f o r ble nding will ne e d to b e de te r mine d on a n individ u a l ba sis based on the fu els and actual winter temper atures at th e terminal. I t will be important for blenders to req u est cloud point i n form at i on from suppl i e rs for co ld w eathe r consi d erations.



## Small Gr oup Stee ri ng Commi ttee M e mber s Steve Howell-Ma rc I V C onsulting Group Paul Naz z a ro-Advanc ed F u el S y st ems Cha r le y Se lve d g e -F lint Hills Re sour c e s Rick Stanko-Marathon A s hl and Petroleum Compan y Rod L a w r enc e - M a g e llan Midstream L P

6

## A p pendi x A

. P&I D of Sp l ash Blendi ng Ri g.

7

## A p pendi x B. P&I F of M odi fi ed Tes t R i g

8

## A p pendix C. Step- b y - step A n al y t ical Procedure s

The st ep-b y

- st ep anal y t i c al procedu r es fol l o w.

B a sel i ne D e te rm inat ion 1. T u rn on the die s e l fu el p u m p. Set the tem p era t ur e con t r o ll er to t h e t e s t t e m p eratu r e

. 2. Assure tha t F l ow Cont ro l Va lv e #1 (FC V 1 ) i s cl osed, i. e. no f u el is pass ing th roug h the D i ff ere n t i a l P r e ssu re G a ug e (D P G ). 3. Allow t h e sy st em to run for XX m i nutes . (Ca l cu la ted v a lue bas e d on the v o lum e of dies el fue l i n th e t a nk and t h e f l ow ra te ; v o lum e pum p e d > v o lum e in t h e t a nk .) 4. A ssure the tem p era t u r e ha s stab il iz ed. R e c o rd the tem p era t ur e. 5. Open FCV 1 and s t a r t tim er. 6. At 1 m i nute int e rv als re cor d the rea d ing on t h e DPG. 7. I f the DP incr eas es to ov er 10? m m H g , record the tim e and turn of f th e pum p. 8. At 10 m i n rec o rd the rea d in g on the DPG as the F i na l D i ff ere n t i al Pre ssu re (FD P )

. 9. Repeat st eps 1 – 8. 10. Record the re sul t s from the tw o run s and rep o r t th e av e r ag e.

Bi o d i e s el Bl en d Filt e r a b il ity De t e r m i n a t io n 1. T u rn on the die s e l fu el p u m p. Set the con t ro ll er to t h e t e st tem p era t ur e. 2. Assure tha t FC V 1 is c l os ed

. 3. Allow t h e sy st em to run for XX m i nutes 4. Load th e de si red am ount o f biod ies e l int o th e in je cto r

. 5. Record the in jec t or tem p era t ure

. 6. A ssure the di ese l fu el tem p era t ur e has st abi liz ed. R eco rd th e t e m p eratu r e. 7. Open FCV 1 and a l low th e dies el fue l t o f l ow th roug h t h e DPG for 1 m i nute. 8. R ecord the D P

. 9. I n j ect the bio d ie se l 10. I f the DP incr eas es to ov er 10? m m H g , record the tim e and turn of f th e pum p. 11. At 10 m i nute s re cor d th e re ading on t h e DPG as the F D P. 12. Repeat st eps 1 – 11, w ith n e w die s el fue l an d bi odi ese l

. 13. Record the re sul t s from the tw o run s and rep o r t th e av e r ag e.

B i odi ese l S o lubi li ty D e te r m ination 1. T u rn on d i e s el fue l pum p. Set t h e tem p erat ure con t ro ll er t o th e t e st tem p era t ur e. 2. Assure tha t FC V 1 is c l os ed

. 3. Allow t h e sy st em to run for XX m i nutes 4. Load th e de si red am ount o f biod ies e l int o th e in je cto r

. 5. Record the in jec t or tem p era t ure

. 6. A ssure the di ese l fu el tem p era t ur e has st abi liz ed. R eco rd th e t e m p eratu r e. 7. I n j ect the bio d ie se l 8. Circu l a t e the b l en ded fue l f o r 10 m i nut es. 9. Open FCV 1 and a l low th e blend e d f u el to flow thr oug h the DPG. 10. Record the DP ev ery one m i nut e. 11. I f the DP incr eas es to ov er 10? m m H g , record the tim e and turn of f th e pum p. 12. At 10 m i nute s re cor d th e re ading on t h e DPG as the F D P. 13. Repeat st eps 1 – 11, w ith n e w die s el fue l an d bi odi ese l

. 14. Record the re sul t s from the tw o run s and rep o r t th e av e r ag e.



### 9T h e ab il ity to u s e the rig an d the p r oc edu r es abov e to a sses s th e co ld tem p erat ure prope rt ies of bl ends bel o w th e cl oud p o int of d i e s el fue l de pend s on the rep e a t ab il ity of the r a te o f f

i l t e r plug g i ng , because a t thes e t e m p eratur es, the fi lt er is g o ing to pl ug

.



### 10

## A ppen d ix D. Cert ificate of A n al y s is for #1 Dies el Fuel

11

## Laboratory Analysis Report

Date Printed: 5/20/2005

Report To: Submitted By:

cc: Rod Lawrence Magellan Analytical Services 1090-A Sunshine Rd Kansas City KS 66115 - Paul Hinkle Additive Systems Inc 407 S Main Broken Arrow OK 74012 True

Sample ID: KS04100778 Type of Sample: Diesel Fuel

Tank: Sample Description: Jet Fuel
Sample Notes: D9

Method Results
D 86 - Distillation 165.6 °C IBP 185.8 °C 10% 191.8 °C 20% 210.9 °C 50% 250.0 °C 90%

272.9 °C FBP 97.6 mL Volume
1.0 mL Loss 1.4 mL Residue D 93 - Flash-Point by Pensky-Martens Closed Cup Tester 37 °C
D 5453 - Total Sulfur by Ultraviolet Fluorescence 920 ppm (wt/wt)
D 4737 - Cetane Index 44.9
D 5773 - Cloud Point -54 °F
D 5949 - Pour Point -70 °F

Results in boxes do not meet ASTM D975 specifications. 10/20/2004

Page 1 of 1

KS04100778 1090-A Sunshine Road, Kansas City, KS 66115 913-621-3603

## A p pendix E. Ce rt if icate of A n al y s is for #2 Diese l Fuel

13

## Laboratory Analysis Report

Date Printed: 5/20/2005

Report To: Submitted By:

cc: Rod Lawrence Magellan Analytical Services 1090-A Sunshine Rd Kansas City KS 66115 - Paul Hinkle Additive Systems Inc 407 S Main Broken Arrow OK 74012 True

Sample ID: KS04100777 Type of Sample: Diesel Fuel

Tank: Sample Description: # 2 LSD
Sample Notes: D9

Method Results
D 86 - Distillation 181.8 °C IBP 213.3 °C 10% 224.2 °C 20% 262.1 °C 50% 324.6 °C 90% 351.8 °C FBP 97.8 mL Volume
1.0 mL Loss 1.2 mL Residue D 93 - Flash-Point by Pensky-Martens Closed Cup Tester 50 °C
D 5453 - Total Sulfur by Ultraviolet Fluorescence 292 ppm (wt/wt)
D 4737 - Cetane Index 47.3
D 5773 - Cloud Point 6 °F
D 5949 - Pour Point -10 °F

Results in boxes do not meet ASTM D975 specifications. 10/20/2004

Page 1 of 1

KS04100777 1090-A Sunshine Road, Kansas City, KS 66115 913-621-3603

## A p pendix F. Certif icate of A n al y s is for So y Biodiesel

15

## A p pendix G. Ce rt ificate of A n al y s is for Ye llo w G r ease Biodiesel

16

## A p pendi x H. Certi f i cate of A n al y s i s for Tall o w B i odi es el

17

## A p pendi x I

. Quali t ati v e Bl endi ng Data

Ble nd Ty p e Diese l Ty p e Diese l Te m p , F Biodie s e l Cloud Point, F Biodie s e l Te m p , F Te m p Diffe r e ntia l Comments

Rati o N o

. 2 4 0 3 2 7 2 3 2 Mix ed we l l Rati o N o

. 2 3 0 3 2 7 2 4 2 Mix ed we l l Rati o N o

. 2 2 0 3 2 7 2 5 2 Mix ed we l l Rati o N o

. 2 1 0 3 2 7 2 6 2 Mix ed we l l

Rati o N o

. 2 0 3 2 7 2 7 2 Mix ed we ll, Si gns of ic i ng r e ve al ed p a r a f f i n dr opo ut,

c l ogg ed 8 0 M s t r a in er s on #2 F u e l

. Rem o ved s t r a i ner s an d r e t e s t. Rati o N o

. 2

- 5 3 2 7 2 7 7 Mix ed we l l Rati o No. 2

- 5 32 72 77 Mix ed W e ll, No ic i ng Rati o No. 2

- 10 32 72 82 Mix ed W e ll, No ic i ng Rati o No. 2

- 10 32 72 82 Mix ed W e ll, No ic i ng Rati o No. 2

- 15 32 72 87 Mix ed W e ll, S o m e ic ing Rati o No. 2

- 17 32 72 89 #2 s l us h y

. Bi o b l e nde d thr o ugho ut t hou gh.

Rati o N o

. 2

- 2 0 3 2 7 2 9 2 #2 s l us h y , Par t ia ll y f r o z e n

. Bio di d n o t b l e nd t h r oug hou t Rati o N o

. 2

- 2 5 3 2 7 2 9 7 # 2 F r o z e Rati o No. 2

- 10 32 55 65 Mix ed W e ll, No ic i ng Rati o No. 2

- 10 32 50 60 Mix ed W e ll, No ic i ng Rati o No. 2

- 10 32 45 55 Bio Cr y s ta ll i z in g o n c ont ac t
, Mix i ng but not bl end ing

. Rati o N o

. 2

- 1 5 3 2 5 0 6 5 Sm all am ounts of bio Cr y s t a ll i z in g o n c ont ac t, M i xi ng bu t no t bl en d i n g

. Rati o No. 2

- 15 32 55 70 Mix ed W e ll, No ic i ng Rati o N o

. 2 0 4 3 6 0 6 0 Mix ed W e l l Rati o N o

. 2

- 5 4 3 6 0 6 5 Mix ed we l l Rati o No. 2

- 5 43 55 60 Mix ed W e ll, No Cr y s ta ls Rati o No. 2

- 10 43 55 65 Mix ed W e ll, No Cr y s ta ls Rati o No. 2

- 10 43 50 60 Mix ed W e ll, No Cr y s ta ls , H a z y F u e l Rati o No. 2

- 15 43 45 60 Mix ed W e ll, No Cr y s ta ls , H a z y F u e l Rati o No. 2

- 15 43 40 55 Mix ed thor o ugh l y , Ver y Cl o u d y Rati o No. 2

- 15 43 35 50 Bio ic i ng, Cr eat ing lar g e c r ys tals , Di d n o t B l e nd Rati o No. 2

- 15 43 30 45 Bio ic i ng, So li ds Pr es e n t, D i d n o t Ble nd Rati o No. 2

- 5 43 35 40 Mix ed T hor o ugh l y , Cr y s ta ls f o r m ing on c o n t ac t. Rati o No. 2

- 5 43 40 45 Mix ed W e ll, No ic i ng Rati o No. 2 0 43 35 35 Mix ed we ll but s t a y e d h a z y , c l oud y



### 18Ble nd Ty p e Diese l Ty p e Diese l Te m p , F Biodie s e l Cloud Point, F Biodie s e l Te m p , F Te m p Diffe r e ntia l Comments

Rati o No. 1

- 30 32 45 75 Ic ing, m i x ed f a ir Rati o No. 1

- 30 32 50 80 Ic ing, m i x ed f a ir Rati o No. 1

- 30 32 60 90 Ic ing, m i x ed f a ir Rati o No. 1

- 25 32 60 85 Ic ing, m i x ed f a ir Rati o N o

. 1

- 2 0 3 2 6 0 8 0 M i x ed we l l Rati o No. 1

- 20 32 55 75 Ic ing, m i x ed f a ir Rati o N o

. 1

- 1 5 3 2 5 5 7 0 M i x ed W e l l Rati o No. 1

- 15 32 50 65 Ic ing, m i x ed f a ir Rati o N o

. 1

- 1 5 3 2 5 3 6 8 M i x ed we l l Rati o N o

. 1

- 1 0 3 2 5 0 6 0 M i x ed W e l l Rati o No. 1

- 10 32 45 55 Mix ed W e ll, No ic i ng Rati o No. 1

- 10 32 50 60 Mix ed W e ll, No ic i ng Rati o N o

. 1

- 5 3 2 4 5 5 0 Ble n d ed wel l Rati o N o

. 1

- 5 3 2 4 0 4 5 Ble n d ed wel l Rati o No. 1 0 32 35 35 Ic ing, m i x ed f a ir Rati o N o

. 1

- 1 5 4 3 4 0 5 5 M i x ed we l l Rati o N o

. 1

- 2 0 4 3 4 0 6 0 M i x ed we l l Rati o No. 1

- 25 43 40 65 Sl ight Ic in g of bi o Rati o N o

. 1

- 3 0 4 3 4 0 7 0 I c ing of b i o Rati o N o

. 1

- 1 5 4 3 3 5 5 0 B l e n d ed wel l Rati o N o

. 1

- 1 0 4 3 3 5 4 5 I c ing of b i o Rati o No. 1

- 25 43 45 70 Mix ed W e ll, No ic i ng Rati o N o

. 1

- 3 0 4 3 4 5 7 5 I c i n g Rati o N o

. 1

- 3 0 4 3 5 0 8 0 I c i n g Rati o N o

. 1

- 2 5 4 3 5 0 7 5 B l e n d ed wel l Rati o N o

. 1

- 3 0 4 3 5 5 8 5 B l e n d ed wel l Rati o N o

. 1

- 3 5 4 3 5 5 9 0 I c i n g Rati o N o

. 1

- 3 5 4 3 6 0 9 5 B l e n d e d



### 19Ble nd Ty p e Diese l Ty p e Diese l Te m p , F Biodie s e l Cloud Point, F Biodie s e l Te m p , F Te m p Diffe r e ntia l Fir s t Pr oduc t: Comme nts

Seq uent ia l No. 2 0 32 50 50 Bio : M i x ed W e ll Seq uent ia l No. 2 0 32 50 50 No. 2: Mix e d W e ll Seq uent ia l No. 2

- 5 32 45 50 Bio : M i x ed W e ll Seq uent ia l No. 2

- 5 32 45 50 No. 2: Mix e d W e ll Seq uent ia l No. 2

- 10 32 45 55 Bio : M i x ed W e ll Seq uent ia l No. 2

- 10 32 45 55 No. 2: Mix e d W e ll Seq uent ia l No. 2

- 10 32 40 50 Bio : Ic in g Seq uent ia l No. 2

- 10 32 40 50 No. 2: Mix e d W e ll Seq uent ia l No. 2

- 10 32 45 55 Bio : M i x ed W e ll Seq uent ia l No. 2

- 15 32 55 70 Bio : M i x ed W e ll Seq uent ia l No. 2

- 15 32 55 70 No. 2: Mix e d W e ll Seq uent ia l No. 2

- 15 32 50 65 Bio : M i x ed W e ll Seq uent ia l No. 2

- 15 32 50 65 No. 2: Mix e d W e ll Seq uent ia l No. 2

- 15 32 45 60 Bio : M i x ed F a ir / Sl o w er D i s per s i ng Seq uent ia l No. 2

- 15 32 40 55 Bio : Ic in g/ Sti l l m i x ed f a ir Seq uent ia l No. 2 0 32 45 45 No. 2: S lig ht Ic i ng Seq uent ia l No. 2 0 43 50 50 Bio : M i x ed W e ll Seq uent ia l No. 2 0 43 50 50 No. 2: Mix e d W e ll Seq uent ia l No. 2

- 5 43 45 50 Bio : M i x ed W e ll Seq uent ia l No. 2

- 5 43 45 50 No. 2: Mix e d P oor l y Seq uent ia l No. 2

- 10 43 45 55 Bio : M i x ed W e ll Seq uent ia l No. 2

- 10 43 45 55 No. 2: Mix e d P oor l y Seq uent ia l No. 2

- 10 43 40 50 Bio : Ic in g Seq uent ia l No. 2

- 10 43 40 50 No. 2: B i o b l o b b i ng, no bl e ndi ng a t a ll Seq uent ia l No. 2

- 10 43 45 55 Bio : M i x ed W e ll Seq uent ia l No. 2

- 15 43 55 70 Bio : M i x ed W e ll Seq uent ia l No. 2

- 15 43 55 70 No. 2: S l o w t o b l e nd b u t d i d m i x w i th agi tat i on

. Seq uent ia l No. 2

- 15 43 50 65 Bio : M i x ed W e ll Seq uent ia l No. 2

- 15 43 40 55 No. 2: B i o b l o b b i ng, no bl e ndi ng a t a ll Seq uent ia l No. 2

- 15 43 45 60 Bio : B l e nde d w e ll Seq uent ia l No. 2

- 15 43 40 55 Bio : B l e nde d W e ll, but Cr y s tals F o r m ing Seq uent ia l No. 2 0 43 45 45 No. 2: S l o w t o b l e nd b u t d i d m i x

.



### 20Ble nd Ty p e Diese l Ty p e Diese l Te m p , F Biodie s e l Cloud Point, F Biodie s e l Te m p , F Te m p Diffe r e ntia l Fir s t Pr oduc t: Comme nts

Seq uent ia l K e r o s e n e

- 2 0 3 2 6 0 8 0 Ker o s e n e : M i x e d W e l l Seq uent ia l K e r o s e n e

- 1 5 3 2 5 5 7 0 Bio : M i x ed W e l l Seq uent ia l K e r o s e n e

- 1 5 3 2 5 5 7 0 Ker o s e n e : M i x e d W e l l Seq uent ia l K e r o s e n e

- 1 0 3 2 5 0 6 0 Bio : M i x ed W e l l Seq uent ia l Ker o s e n e

- 10 32 50 60 Ker o s e n e : N o t B l e n d i ng Seq uent ia l K e r o s e n e

- 1 0 3 2 4 0 5 0 Bio : M i x ed W e l l Seq uent ia l K e r o s e n e

- 1 0 3 2 4 5 5 5 Bio : M i x ed W e l l Seq uent ia l K e r o s e n e

- 5 3 2 5 5 6 0 Bio : M i x ed W e l l Seq uent ia l K e r o s e n e

- 5 3 2 5 5 6 0 Ker o s e n e : M i x e d W e l l Seq uent ia l K e r o s e n e

- 5 3 2 5 0 5 5 Bio : M i x ed W e l l Seq uent ia l K e r o s e n e 0 3 2 5 0 5 0 Ker o s e n e : M i x e d W e l l Seq uent ia l K e r o s e n e 0 3 2 4 5 4 5 Ker o s e n e : Ic i n g Seq uent ia l K e r o s e n e 0 3 2 4 0 4 0 Bio : B l e nde d W e l l Seq uent ia l Ker o s e n e 0 32 40 40 Ker o s e n e : N o t B l e n d i ng, Ic i ng Seq uent ia l Ker o s e n e

- 30 43 40 70 Bio : S l i ght ic in g of bi o Seq uent ia l Ker o s e n e

- 30 43 40 70 Ker o s e n e : Ic i ng of bio. Po o r Mix Seq uent ia l Ker o s e n e

- 25 43 40 65 Bio : M i nor ic in g of bi o. M i x W e ll Seq uent ia l Ker o s e n e

- 25 43 40 65 Ker o s e n e : M i n o r ic i ng of bi o. M i x Po or Seq uent ia l Ker o s e n e

- 20 43 40 60 Bio : M i x w e ll, no ic in g Seq uent ia l Ker o s e n e

- 25 43 45 70 Bio : M i x w e ll, no ic in g Seq uent ia l K e r o s e n e

- 3 0 4 3 4 5 7 5 Bio : Ic in g Seq uent ia l Ker o s e n e

- 20 43 40 60 Ker o s e n e : Ic i ng of bio. Po o r Mix Seq uent ia l K e r o s e n e

- 1 5 4 3 3 5 5 0 Bio : M i x ed wel l Seq uent ia l Ker o s e n e

- 15 43 35 50 Ker o s e n e : D i d not ble nd w e ll

. Seq uent ia l K e r o s e n e

- 2 5 4 3 5 0 7 5 Bio : M i x ed W e l l Seq uent ia l Ker o s e n e 0 43 50 50 Ker o s e n e : Bl end ed wel l Seq uent ia l K e r o s e n e

- 3 0 4 3 5 5 8 5 Bio : B l e nde d W e l l Seq uent ia l K e r o s e n e

- 3 0 4 3 5 0 8 0 Bio : Ic in g Seq uent ia l K e r o s e n e

- 3 5 4 3 5 5 9 0 Bio : Ic in g Seq uent ia l K e r o s e n e

- 4 0 4 3 6 0 1 0 0 Bio : Ic in g Seq uent ia l K e r o s e n e

- 3 5 4 3 6 0 9 5 Bio : B l e nde d W e l l



### 21

## A p pendi x J. L i sti n g of Consor ti um M e mbe r s Comme nts

Contributors of the Consortium have offe red th e f o l l o wi ng st at em ent s for c onsi d erat i on:

• Optimal biodiesel blending is dep e nda nt on ac cur a te knowled g e o f B 100 a nd Petroleum diesel cold flo w proper tie s to he lp de t e rmine pa r a me ter s

. • The impact of blendin g method t y pe (spl ash, rati o, and sequen tial blendin g ) and mechanic al mix ing on B 2 blend homog en eit y wa s not evaluated in this stud y

. • The impact of B 2 biodies el blends on D975 te st pa rameters w a s not evalu a ted in test runs completed and do cu me nted in this report.

• The impa c t of w a te r c ont a mina tion on wa x /ic e c r y s ta lliza tion wa s not e v a l ua te d within this stud y althou gh desiccant filters wer e u s ed to help prevent moisture contamination of the B 1 0 0 and fuels for t e sting

. • I n man y cas es the pressu re drop of the B 2 blend was g r e a ter than that o f the base diesel fuel. I n no c a se w a s the B 2 blend a l o wer p r essure d r op t h an t h e bas e di esel f u e l . The pote n tia l implic a tions of this f o r users o f B 2 blends mad e durin g cold weather bl ending ar e not known.

• I n s e ve ra l c a s e s the bottoms sa mple s ha d s lig htl y hig h er biodies el conc entr ations tha n the “ bulk” sa mple s. This mig ht indic a t e the ex is te nc e of not c o mple te l y homog enous mix tures for these test conditions.

22