ANALYTICAL LABORATORY TECHNIQUES FOR OIL SHALE

8/13/2019 ANALYTICAL LABORATORY TECHNIQUES FOR OIL SHALE

1/7

- -.ANALYTICAL LABORATORY TECHNIQUES FOR OIL SHALE

B. L. Beck ), David Lie der ma n(2 ), R. Bernheimer3)

i

1

\

( 1 ) E nja y Chemical Company, Baytown, Texas

(3) 2 1 Innes Road, E a s t Brunswick, New J e r s e y2) Mobil Research and Development Corp., Pau lsb oro , N e w J e r s e y

I n t r o d u c t i o n

From 1964 t o 1967, t h e U. S. Bureau of Mines o i l s h a l e f a c i l i t i e s a t AnvilP o i n t s n e a r R i f l e , C ol or ad o w e r e r e a c t i v a t e d f o r a c oo pe ra ti ve i n d u s t r i a l o i l s h a l ere se ar ch program. Mobi l O i l C o r p o r a t i o n a c t e d as manager fo r t h i s p r o j e c t wi th f i v eo t h e r m a jo r o i l c om panies a c t i v e l y p a r t i c i p a t i n g .Company, Continental O i l Company, Pan American Petro leum Cor por ati on, P h i l l i p sPetroleum Company, and th e former S i n c l a i r Research, Inc . Tech nical peop le f rom th eseo i l compan ies, suppor t ed by pe r sonne l f rom th e Colo rado Schoo l o f Mines ResearchFounda t ion (CSMRF), ca r r i e d ou t a n in t e ns iv e r e to r t in g and min ing r e s ea rc h program a tt h e t he n named Anvi l Poi nts O i l S h a l e R e se a rc h C e n t e r. T h i s p a p e r d e s c r i b e s t h ea c t i v i t i e s o f t h e a n a l y t i c a l l a b o r a t o r y which s u p po r te d t h e r e s e a r c h pro gra m.a c t i v i t i e s would p r ob a bl y b e t y p i c a l o f a ny s uc h o i l s h a l e l a b o r a t o r y i n a remotel o c a t i o n . Inform at ion on t h e res ea rc h program may be found e lsew here (1 ) .

The pr imary purpose of the a n a l y t i c a l l a b o r a t o r y w a s t se rve t h e r e t o r t i n gand mining research program as o ppo se d t o d oi n g a n a l y t i c a l r e s e a r c h . Some supp le -m e n ta r y r e s e a r c h work a c t u a l l y w a s found necessary and w a s done. However, t h e sco peo f t h i s p ap er i s l i m i t e d t o t h e r o l e o f t h e l a b o r a to r y as a sup por t g roup .

These were Humble O i l and Ref ining

These

The Labora to ry and S ta ff

The Bureau of Mines bui ld ing, l a bor a to ry f u r n i tu re , and much equipment w e r ea v a i l a b l e a n d u s e d .c o mp l et e t h e p h y s i c a l p a r t o f t h e l a b o r a t o r y.equipment and i n s t r u m e n t a t i o n t h a t h ad a s h o r t d e l i v e r y t im e, w a s r e l i a b l e , and wasas s imple as p o s s i b l e . No s k i l l e d l a b o r a t o r y i ns tr um e nt r e p a i r se rv i ce w a s a v a i l a b l eo n s i t e . ,

a n a l y t i c a l c h em i s ts fro m t h e p a r t i c i p a t i n g c om pa ni es . From f o u r t o seven l a b o r a t o r yt e c h n i c i a n s w e r e r e q u ir e d d u r i n g t h e p r o j e c t .l i mi t e d p ro je c t by th e CSMRF and had l im i t e d o r no l ab ora to ry exp e r i enc e .

t e c h n i c a l s t a f f and t h e te c h n i ci a n s . For t h e t e c h n i c a l p eo p le , t h i s came from v i s i t st o t h e Bureau of Mines St a t io n i n Laramie, Wyoming and t o t h e CSMRF i n Golden,Colorado. The te ch ni c i an s w e r e t r a i n e d o n s i t e by t h e c h e m is ts .

Where necessa ry and j u s t i f i a b l e , new equ ipmen t w a s added toOur major concern w a s o b t a i n i n g

T h e s t a f f w a s headed by a s u p e r v i s o r a n d a chemist , b o t h p r o f e s s i o n a l

These w e r e h i r ed s p e c i f i c a l l y f o r t h i s

T r a i n in g i n o i l s h a l e l a b o r a t o r y t e c hn i qu e s w a s r e q u i r e d f o r b ot h t h e

Analyt ica l Methods

A v a r i e t y o f m e t h o d s w a s u se d t o a n a l y z e t h e s a mp l es g e n e r a t e d by t h ere se ar ch program. These are l i s t e d i n Ta bl e I . Many a r e or a r e s imi l a r t o ASTMmethods and a re so noted. Others are descr ibed below.

F i sche r Assay

One of t h e most i mport ant t e s t s w a s t he F i sc he r Assay o n . r a w and spen ts h a l e . A semiautomated apparatus w a s d es ig ne d u s i n g t h e b a s i c p r i n c i p l e s o f t h emethods repor ted by the Bureau of Mines ( 2 ) , and t h e CSMRF (3 ) .

One c o n t r o l u n i t o f t h e s i x - u n i t a p p a r a t u s i s shown i n F igure 1. This

c o n t r o l c i r c u i t p r ov id ed t h e d e s i r e d h e a t i n g r a t e wi th an uppe r t empera tu re l i m i t


2/7

cu t o ff and ind i ca t o r. Temperatu re was mon ito red wi th the pyromete r, and hea t in gpower with the ammeter. All s i x c o n t r o l u n i t s were mounted on an aluminum panel

4i n by 66 in .

When an assay w a s s t a r t e d , t h e v a r i a b l e t r an sf or me r w a s s e t a f u l l power(normal ly about 13.5 amperes) , and t h e h i g h s e t p o i n t o f t h e p y ro m et er a t 510C.When the t empera tu re r eached 500 C , th e va r i ab le t r ans fo rmer was a d j u s t e d t o a pre -d e te r m in e d s e t t i n g t o m a i n t a i n t h e f i n a l 5OO0C t e m p e ra t u r e. A f t e r r e t o r t i n g w a scomple te , t he m a i n s w i t c h w a s opened.

A comple te de sc r i p t io n of th e F i s che r Assay method i s found i n t he Bureauof Mines paper.

Carbon and Hydrogen

Pre cis io n car bon and hydrogen de ter mi nat ion s were made us ing th e conven-t i on a l h igh t empera tu re ox id a t iv e combus t ion t echn ique fo l lowed by we igh ing theCO and H 0 formed. The app ara tus was sp e c i f i c a l l y des igned and assembled f o r our2n e ed s . d r e e f u r n ac e s w er e u s ed a ro u nd a 19 mm'by 36 i n Vycor co mbu sti on tu be ,packed accordi ng to Steyermark (4) . Temperatures of th e fur na ces were:

i n Sample Furnace

1 2 i n Middle Furnace - 680 10C8 i n E x i t F ur na ce - 190 _ 10C

- O i l and Organic Standards 700 _ 1 0 CG a s , Sha le , and Ino rga nic Standar ds 950 10C

F or a l l bu t g a s s a m p le s , t h e s am pl e f u r n a c e w a s motor dr iv en t o a l low anhour fo r movement f r a n i t s i n i t i a l p o s i t i o n t o i t s f i n a l p o s i t i o n n e xt t o t h e m id dl efu rna ce . When the f i n a l po s i t i on was r eached , a t imer was ac t iva t ed t o g ive 45minutes a dd i t io na l combust ion t ime be for e an end-of- run a larm sounded.

For gas samples , t h e sample fu rnac e w a s p o s i t i o n e d n e x t t o t h e middlefu rnace . A r o l l of c o pp e r g a u z e w a s i n s e r t e d i n p l a c e o f t h e c o m bu st io n b o a t a nda s p e c i a l a d a p t e r ( F i g u r e 2 ) added to t he combus tion tube i n l e t . A 25% br in es o l u t i o n was u se d t o d i s p l a c e t h e g a s s a m p l e from a 1 - l i t e r gas sample tube inabout 40 minute s . The combust ion tub e was the n oxygen purged fo r an ad di t i on al 20minu tes .

Gas Chromatography of G a s Samples

2 , 02 N2, CH4, CO, and He t o r t g a s e s w e r e r o u t i n e l y a n a l y z e d f o r CO A2F i s c h e r Gas P a r t i t i o n e r Model 25V wi th two columns i n se r i e s w a s used. Column 1 was30 i n of hexam ethylp hospho ramid e on 60-80 mesh Columpak; Column 2 was 6.5 f t of42-60 mesh ac t i va te d 13X molec ular s i ev e .mv range plug recorded th e chromatographic peaks . Both ins t rumen ts provided th er em ot e l a b o r at o r y w i t h t h e h i g h r e l i a b i l i t y r e q ui r e d.gas f o r de t e rmin ing a l l components excep t hydrogen; n i t r og en w a s used f o r de t e rmin inghydrogen.

A Sargent Model SR-25 recorder with a 1.0-

Helium was used as c a r r i e r

A na lyz ed s t a n d a r d g a s m i x t u r e s we re u s ed f o r c a l i b r a t i o n .

To ob t a in a compos i t e sample fo r an expe r imen ta l r e t o r t run , a cont inuoussample was s e n t t o a br ine -d i sp lacemen t gas -ho lde r a t t h e l abo ra to ry. Approxima te ly3 cu f t o f g a s were c o l l e c t e d v i a a h e a t - t r a c e d l i n e .o b t a i n e d , i t w a s t hen rou ted th rough a d r y in g tu be d i r e c t l y t o a 0. 5 m l sample loopa t t he ch romatograph .

After a complete sample was

Water Analysis

R e t o r t wa t er p ro du ce d by t h e r e t o r t i n g o f o i l s h a l e w a s analyzed becauseof i n t e r e s t i n co r r os i o n, p o l l u t i o n , d i s p o s a l , and p o ss i b le f u t u r e u t i l i z a t i o n .Analyses were made for NH C 1 , C 0 2 , sol ids , ash , and pH.

3 'S h a l e R ic h ne s s D i s t r i b u t i o n

S h a l e r i c h n e s s , o r a s s a y, c a n be p r e d i c t e d f rom i t s dens i ty. Consequen t lyt h e r i c h n es s d i s t r i b u t i o n o f a s am pl e c a n b e d e t er m i ne d f r om t h e d e n s i t y d i s t r i b u -t i o n . S ev en s o l u t i o n s of ca rbon t e t r a ch lo r i de and t e tr ab romoe thane were p repa redt o cove r th e den s i t y r ange o f i n t e r e s t , 1 .6 to 2 .4. The volumes o f measured sh a l e

J

i

I

1

I

, \

1

i

I

I


3/7

33

s am pl es f l o a t i n g i n g r a d u a t e s o f t h e v ar i o u s s o l u t i o n s were n o r m a li z e d t o 1 00 %f ol lo w ed by a p p l i c a t i o n o f a r i c h n e s s - d e n si t y r e l a t i o n s h i p 5 ) .

Sampling

O b t a i n i n g r e p r e s e n t a t i v e s a m p l e s o f raw a n d s p e n t s h a l e , a n d l i q u i d a n dgaseous r e t o r t prod ucts were a lways of major concern . Crushed sha le , e s p e c i a l l yraw s h a l e , s hows v a r i a t i o n s i n r i c h n e s s w i t h p a r t i c l e s i z e . L i q u i d p r o d u ct fromr e t o r t s i s a m i x tu r e o f o i l , water, a n d s o l i d s .e n t r a i n e d o i l , s o l i d s , and w a te r .

s epa ra t ed , measu red , and then ana lyzed ind i v id ua l ly.

The Fischer Assay and other t e s t s on raw s h a l e s a m p l e s w e r e t h e b a s e s o f mater ia l

b a l an c e s f o r e ac h e x p e ri m e n t al r e t o r t r un .S e v e ra l s t e p s of s i z e r e d u c t i o n t a k e p l a c e f ro m t h e t o n s of r a w s h a l e

mined t o t he 100 grams of raw s h a l e ch arg ed t o t h e l a b o r a t o r y r e t o r t f o r P i s ch e rAssay. However, th e minus eight -mesh sh al e fed t o t he l a b o r a t o r y r e t o r t mu st b er e p r e s e n t a t i v e of t h e s am p le o f i n t e r e s t . When r aw s h a l e i s c r u s he d , t h e l e a n e r ,m o r e b r i t t l e mater ia l c o nc e nt ra t es i n t h e f i n e r p a r t i c l e s , w h i le t h e r i c h e r , toughermate r i a l r e s i s t s c r us h in g and co n c e nt r a te s i n t h e l a r g e r p a r t i c l e s . To dr am at iz et h i s e f f e c t , F i s ch e r Ass ays w e r e ru n on v a ri o u s p a r t i c l e s i z e s o f a crushed sample .The r e s u l t s are shown i n Table 11.

q u a n t i t y a nd p a r t i c l e s i z e b e f o r e a n a l y s es c o ul d b e made.procedure w a s d ev el op ed t o re du ce t h e i n i t i a l q u a n t i t y r e c ei v e d t o a b a s i c 775 t o8 2 5 gram por t ion .a n o t h e r s p e c i f i c s p l i t t i n g a nd c o mb in in g pr oc ed u re w a s used t o r ed uc e t h i s q u a n t i t yt o t h e a mounts r e q u i r e d f o r t h e i n d i v i d u a l t e s t s .

G ase ou s p r o d u c t f r om r e t o r t s h a s

The va r io us phases o f t he l i q u i d and gaseous samples w e r e norma l ly

Sampling and sample s i z e r edu c t ion o f t h e raw s h a l e w er e v e r y i m p o r t a n t .

A l l s h a l e s a m pl es s u b mi t te d t o t h e l a b o r a t o r y n ee d ed t o b e re du c ed i nA r i g o r o u s s p l i t t i n g

Thenh i s p o r t i o n w a s c rushed to pass an e igh t -mesh s c reen .

Records

As p r e v i o u s l y n o t e d , t h i s p r o j e c t i n v ol ve d t h e U. S. Bureau of Mines , t h eCSMRF and s i x o i l companies.r e c o r d s o f s am p le s and t h e i r a n a l y s e s w e r e e s s e n t i a l .l abo ra to ry were s e qu en t i a l l y numbered and r eco rded i n bound no tebooks. The i ri d e n t i t y , d a t e r e c e i v e d , d a t e a n a l y s e s co m pl et ed , a nd a n a l y s e s made w ere a l s orecorded.o r i g i n a l b a s i c d a t a w ere a v a i l a b l e i f r e q u ir e d .

Nine fo rms f o r da t a workup and r ep o r t i ng were deve loped f o r con s i s t e ncya n d s i m p l i f i c a t i o n . A l l o f t h e s e w e r e c o l o r co ded f o r ease o f i d e n t i f i c a t i o n .

Before the completed analyses on any sample w e r e o f f i c i a l l y r e l e a s e df rom t h e l ab o ra to r y, t hey were checked by one o f t he an a l y t i c a l ch emis t s . Thep h i l o so p h y m a i n t a i n e d by t h e l a b o r a t o r y w a s t o r e p o r t no r e s u l t i n p r ef er en c e t o aq u e s t i o n ab l e r e s u l t .

Under t he se c i r cums tances , ac cu ra t e and comple t eA l l samples r ece ived by the

Bound ca l c u l a t io n books were used and r e t a i ne d f o r each t e s t so t h a t t h e

Quality Control and Crosscheck Programs

A p la n ne d an d e f f e c t i v e q u a l i t y c o n r o l p ro gram w a s main ta ined th roughou tt h e r e s e a rc h p r o j e c t .each

wast o r u n o n t h e q u a l i t y c o n t r o l

sampleseach week.

they submi t t ed a form w i t h t h e i r r e s u l t s .v a r i a t i o n s n o t e d and i n v e s t i g a t e d .

program w e r e updated .shown i n Table 111

A s c h e d u l e w a s p o s t e d f o r the t e chn ic i ans showing A a t t e s t s

A t the end of t h e weekThese were recorded and any abnormal

E ve ry t h r e e m on ths s t a n d a r d d e v i a t i o n s f o r a l l t e s t s i n t h e q u a l i t y c o n t r o lF i n a l s t a t i s t i c s f o r some o f t h e k ey t e s t s i n t h e program a r e

The number of q u a l i t y c o n t r o l t e s t s run depended upon the


4/7

31.

f requency of each t e s t normal ly requested and i t s importance .5 of th e normal work l oad .

The i n t e r n a l q u a l i t y c o n t r o l pro gram to o k c a r e o f t h e p r e c i s i o n o f t h et e s t s . However any l ab ora to r y, e s pe c i a l ly a r emote and r e l a t i v e l y inexpe r i encedl a b o r a t o r y, i s a l s o c o n c e r n e d a b o u t t h e a b s o l u t e a c c u r a c y o f i t s r e s u l t s . S t a n d a r d sand syn the t i c samples were used where p o s s i b l e . I n a d d i t i o n , d u r i n g t h e p ro gra ms e v e r a l s a m p l e s were c r o s s c h e c k e d w i t h o t h e r l a b o r a t o r i e s .were made wi th th e Bureau of Mines a t Laramie . Data were a l so exchanged wi th theCSMRF Mobil , and Humble . Some of th e t y p i c a l crossch eck d a t a are shown i n Tab le I V.The F i sche r Assay da ta are a v e r a g e s o f s e v e r a l d e t e r m i n a t i o n s .s a t i s f a c t o r y t o e x ce l le n t.

a n a l y s e s f o r which t h i s l a b o r a t o r y was no t equ ipped .s p e c tr o m e te r g a s a n a l y s e s , an d d e t a i l e d a n a ly se s o f o i l and d i s t i l l a t i o n f r a c t i o n s .

They averaged aboutFi sc he r Assays were run most f r e q u e n t l y.

Most of t h e compar isons

Agreements w e r e from

P a r t i c i p a t i n g o i l company l a b o r a t o r i e s were a l s o r e q u e s te d t o p e rf or mExamples of th es e were mass

C o r r e l a t i o n s h o n g A n al ys es

D u ri ng t h e c o u r s e o f a n a l y z i n g s e v e r a l h u nd r ed s a m p le s , some c o r r e l a t i o n sMost o f t he se were wi th t hemong t h e r e s u l t s f ro m s e v e r a l m e th o ds w e r e developed.

F i sche r Assay o f r a w s h a l e .e q ua t io n s f o r t h e r e l a t i o n s h i p s , a s w e l l a s t h e c o r r e l a t i o n c o e f f i c i e n t and s t an d a rdd e v i a t i o n .

A compute r r eg res s ion ana lys i s p rogram deve loped the

T h e s e d a t a a r e g i v e n i n Ta bl e V.

T he se r e l a t i o n s h i p s c om par ed w e l l w i t h t h o s e p r e v i o u s l y o b t a i n e d b y t h eBureau of Mines, and were v e ry u s e f u l t o i n t e r n a l l y chec k a n a l y t i c a l r e s u l t s f o rc o n s i s t e n c y.

Terminat io n o f Program

The Anvi l Points O i l Sha le Resea rch Cen te r Labora to ry was i n o p e ra t i o nt h r e e y e a r s , a n d s a t i s f a c t o r i l y p er fo rm ed i t s f u n c t i o n as a suppor t group. A t t h eend of t h e program, a l l equ ipmen t and supp l i e s were a p p r o p r i a t e l y d e a c t i v a t e d ,s t o r e d , o r o t h e r wi s e d is po se d o f . A l l notebooks and records were f i l e d and a f i n a lsummary re p or t was prepar ed. With t h i s exper i ence and newer ins t rum en tat iona v a i l a b l e , a la bo ra to ry today could be s i g n i f i c a n t l y improved. Undoubtedly much oft h e s u c c e s s o f t h e l a b o r a t o r y w a s d ue t o t h e h i gh s t a f f r a t i o of two a n a l y t i c a lc h e m i st s t o f o u r -t o - s ev e n t e c h n i c i a n s f o r m o s t l y r o u t i n e a n a l y s e s . The c h e m i st s w er ea b l e to c l os e l y supe rv i se the r ou t i ne work and deve lop and improve methods . Ina d d i t i o n , they were s t i l l a b l e t o ke ep f a m i l a r w i t h a nd c o n t r i b u t e t o t h e r e s ea r c hprogram.

Acknowledgment

The a u t h o r s a p p r e c i a t e t h e p e r m is s io n g r a n t e d by t h e s i x p a r t i c i p a t i n gc om pa ni es t o p u b l i s h t h i s r e p o r t .

1


5/7

\

3)

Refe rences

Lawson, J . E . , e t . a l . , Gas Combustion Reto r t i ng Performance i n a Large Demon-s t r a t i o n Retor t This Symposium. .

Hubbard, A. B . , Automated Modif ied Fis ch er Re to r t s f o r Assaying O i l Sha le andBituminous Materials, U. S . Bureau of Mines Report o I n v e s t i g a t i o n s No. 6676,(1965) .

Reeves, W. H. . Inv es t ig a t i on o f Methods f o r t h e De te rmina t ion o f Crude Sha leO i l i n - O i l S h a l e s, C o lo r ad o S c h oo l of Mines Research Foundation, Report No. 64-1,(1964).

Steyermark, A , , Qu an t i t a t i ve Organ ic Mic r oan a lys i s , pp. 221 , Academic P re s s , New

York, 2nd edi t ion , (1961) .

Smith , J . W. , A p p l i c a b i l i t y o f a S p e c i f i c G ra v i t y -O i l Yi e l d R e l a t i o n s h i p t oGreen River O i l Sha le , Ind . Engr. Chem, 3, 306 (1958).

TABLE I

ANALYTICAL METHODS

Name

Ash Content of O i lAsh Content of Sha leB en ze ne E x t r a c t a b l e s i n S h a l eC and H ( t o t a l ) i n Sh a le , O i l , o r GasDens i ty of Sha leD i s t i l l a t i o n o f O i l (10 lam.)Fischer Assay o S h a l eGas Analys is by Gas ChromatographyG r a v i t y of O i lMinera l CO Conten t o f Sha leMois tu re ,Content o f S h a l eNi t rogen (Kje ldah l ) i n Sha l e and O i lP a r t i c l e S i z e D i s t r i b u t i o n of S h a l ePour Point of O i lRamsbottom Carbon Residue of O i lS a y b o l t Vi s c o s i t y of O i l

S h a l e R i c h n e s s D i s t r i b u t i o nWater Ana lys i sWater i n O i lWater and Sediment i n O i l

s method used s i m i l a r t o ASTM method

2

Procedure

ASTM D 482950C with a i rASTM D 473 sS e e TextLoose, packed, solidASTM D 1160S e e TextSee TextASTM D 287ASTM D 1756 sVo l a t i l e s a t 105CASTM E 258 sS i e v e a n a l y s i sASTM D 97ASTM D 524ASTM D 88

See TextS e e TextASTM D 95ASTM D 1796 s

TABLE I1

VARIATION OF RICHNESS OF R AW SHALE WITH SIZE

S iz e (mesh) Gal/Ton (F is ch er Assay)

+4 31.8-4, +8 30.6- 8 , +20 28.6 .

- 2 0 , +48 28.0.-48, +lo0 23.9

-100, zoo 20.8-200 19.6


6/7

M a t e r i a l

Raw Sha le

S h a l e O i l

R e t o r t Gas

TABLE 111

INTERNAL QUALJTY CONTROL PROGRAM STATISTICS

Te s t Level 95% Confidence L i m i t

F i sche r Assay 28 g a l / t o n17 W t69 W t

M i n e r a l COAshMois tu re 0 .2 W tCarbon 16 W tHydrogen 2 W t

2

Carbon

HydrogenN i t r o g e n

CarbonHydrogen

Te s t

Fischer Assay

S p e c i f i c G r av i ty ( O i l )Carbon (Raw Shale)

(Spen t Sha le )( O i l )

Hydrogen (Raw S h a l e )( S p e n t S h a l e )( O i l )

Mine ra l CO (Raw Shale)

Ash (Raw Shale)(Spent Shale)

(Spent Shale)

84 w t

11W t

2 W t

10 lb/MSCF0.3 lb/MSCF

TABLE I V

SUMMARY OF CROSSCHECK DATA

0.480.320 .190.0340.160.063

0.35

0.550.11

0 .480.13

Labora to ryAnvi l Po in t s B of M Humble

26.730.70.917

1 6 . 36.778 3 . 91 . 7 00 . 3 011.11 6 . 51 4 . 968 .282 .7

27 .030.40.917

16 .26 .788 4 . 81 .700.27 ,11 .61 6 . 21 4 . 568.48 2 . 8

TABLE V

CORRELATIONS AMONG ANALYSES

E q ua t io n s o f R e l a t i o n s h i p s C o r r e l a t i o nR - Raw Sha le S - S pe n t S h a l e ) C o e f f i c i e n t

R Total Carbon = (0.404)(FA) 5.58 0.9 7R Organic Carbon = (0.444)(FA) 0 .25 0.97R Hydrogen = (0.0499)(FA) 0.39 0.9 3R Ash = (-0.372)(FA) 77.70 0.9 2R I g n i t i o n L o s s - CO = (0 .511)(FA) 1 ,085 0 .92S Minera l CO = (-0.809)(Ash) 82.20 0.992

6.77

8 4 . 01 . 7 20.2811 .4

S tanda rdDev ia t ion

0.150.160 .030.240 .330.23


7/7

S H STRIP HEATING ELEMENTS: 12OV2 5 0 W

R H RING HEATING ELEMENT: IZOV 5 0 0 WT THERMOCOUPLEA A M M E T E R : 0 25 AMP- AC

SH V VARIABLE TRANSFORMER: IZOV, 25AMF R REL A Y: ZOAMP SPOT, NC .S HSH S CIRCUIT BREAKER: 2 0 A M PR H L INDICATOR LAMPS

F I S C H E R ASSAY CONTROL CIRCUITF I G U R E I

1 6mm 0 0 . V

GLASS WOOL

S SILICONE STOPPER

C %s CAP

T 3-WAY CAPILLARY STOPCOCK

V VYCOR COMBUSTION TU B E

FROM SAMPLE TUBE C H ADAPTER -FIGURE 2

GAS A N ALY SI S

ANALYTICAL LABORATORY TECHNIQUES FOR OIL SHALE

Documents

Transcript of ANALYTICAL LABORATORY TECHNIQUES FOR OIL SHALE