STATE OF ILLINOIS WILLIAM G. STRATTON, Governor DEPARTMENT OF REGISTRATION AND EDUCATION VERA M. BINKS, Director DIVISION OF THE STATE GEOLOGICAL SURVEY JOHN C. FRYE, Chief URBANA CIRCULAR 197 EFFECT OF DILUENTS ON THE PLASTIC PROPERTIES OF COAL AS MEASURED BY THE GIESELER PLASTOMETER BY O. W. REES and E. D. PIERRON PRINTED BY AUTHORITY OF THE STATE OF ILLINOIS URBANA, ILLINOIS 19 5 5 SURVEY LIBRARY JUN f> . 1955 Digitized by the Internet Archive in 2012 with funding from University of Illinois Urbana-Champaign http://archive.org/details/effectofdiluents197rees EFFECT OF DILUENTS ON THE PLASTIC PROPERTIES OF COAL AS MEASURED BY THE CIESELER PLASTOMETER by O. W. Rees and E. D. Pierron ABSTRACT The effect of some diluents on the plastic properties of two high-volatile bituminous A coals of different maximum -fluidity levels was studied. The diluents, in increments of 10 to 20 percent, were mixed with ' each coal, and plastic properties were determined with the Gieseler plastometer. Data indicate that the duplicability of this method is not satisfactory quanti- tatively but is adequate for qualitative grouping of coals; that use of diluents to improve results is not satisfactory; that addition of increasing amounts of diluents progressively decreases maximum fluidity but not in a linear pattern; and that the chars studied may lower fluidity somewhat more than other diluents. INTRODUCTION The study of plastic properties of coal for fundamental understanding of behavior and for practical application is of definite importance, but there are many experimental difficulties and uncertainties in interpretation. Numerous descriptions of laboratory methods designed for this purpose are available, but it is not the aim of this report to discuss their relative merits There is considerable disagreement as to the best method available, and m as to the measure by which a method may be judged to be useful. There e those who insist that to be useful a method for measuring plastic prop- rties of coal must be quantitative and duplicable from laboratory to laboratory. On the other hand, there are those who believe that a method *hich gives only qualitative or semiquantitative results may be useful in Riding data on the basis of which coals may be grouped and comparisons thai £ T- lab i ° rat0r y we tend to agree with the latter group. We have found nat the Gieseler plastometer yields results which permit useful evaluation coals for certain applications (Reed et al. , 1952). Consequently we have tinued to use it and have studied the variables involved for the purpose of possible improvement of the instrument and for better understanding of the results obtained. [i] ILLINOIS STATE GEOLOGICAL SURVEY 5 > * xl o o o h O 00 co o o o o co . • • • . . • . . . . —< m o o vO LO O t^- ^ o o o vO o O ro CO — » O m i— i I s - lO —• o r— 1 I— 1 i * ~i .— t r-4 cd -n 2 3 u GO IT) o fM ^ o rsj -* o oo ^b o o co fl . • • • • • . • . . • • . CO a — • o o fM vO o o c\J ^ o o ■—I vO o o r— 1 +■> 4-> CU £ cu CO in m f— 1 CU c/> +-> rt h CU -«-» cu g '3 CO 4J O 6 in o in CO 4-> vJD o m d. cu "tf o sO m o ^H CO o . . . c . . . d . . . . . cd i—i PL. u *+H o o o fM cu vO O o CM fM d o r-4 vO o o r— 1 cd £ CM f-H 3 i—i ,d m 43 m i-H I—I cu r-H 2 cu -M 1 o CU aJ +J CO cu 3 cd 3 •l-i Is o -H cd o o CO i-H N 6 o z CO cti -t-> ■i-H r-l •r-t rQ cd o "a o ■ i-t o m d o d cd ,d CO u cu w 00 d o d i—i 2 d CO d o d I—I pq NO d o d m <—* CO d cu o ■— 1 ■^ o ^ I—I d w Q o 43 rd vO o o r» o o H . P. 00 o o ~* m o o — i rg 4-> o s cu CM —4 m m CX> ■M m o o vO CO o vO o o — • J-l ~ cd \ vh* £ v^ £! -d ^ o T3 . • d X o > ih (d £ < S 2 cd " vhI Jtj P- M-. £j ^ *♦■• ^» tJ VM -r-l 73 U O t3 • ' * Ik z < 2 2 o^^ ^H ^ XI *** o -d . . ci « o > *H cd 2 ^ o xJ Q J> -r-l (d z < 2 2 PLASTIC PROPERTIES OF COAL 3 This report covers a study of the effect of diluents on the plastic prop- erties of two high-volatile bituminous A coals of different maximum -fluidity levels as measured with the Gieseler plastometer. The objectives of this work were: 1) to better evaluate the Gieseler plastometer as an instrument for measuring plastic properties of coals, 2) to learn more about the effect of diluents on the plastic properties of coal, 3) to learn whether diluents may be added in definite amounts to badly swelling coals to obtain better plastic property data for them, and 4) to learn whether chars as diluents behave in a distinctive manner. APPARATUS The Gieseler plastometer used in this work was built in the Survey machine shop according to the description published by Soth and Russell (1943) but with certain changes described in a recent publication (Rees and Pierron, 1954). The instrument includes a modification in the head to permit a fixed position of the thruslrtrearing and provision for removal of decomposition gases by suction. Temperature control is accomplished man- ually by means of an auto-transformer to give a rate of heat rise of 3°C. per minute. Temperature readings are obtained by means of a chromel-alumel thermocouple and a Bristol pyrometer calibrated from 250°C. to 500°C. The values determined with the Gieseler plastometer are defined as follows : Softening temperature. - The temperature at which dial pointer movement reaches 0. 5 dial divisions per minute. Fusion temperature. - The temperature at which dial pointer movement reaches 5. dial divisions per minute. Maximum fluid temperature. - The temperature at which dial pointer movement reaches maximum rate. Setting temperature. - The temperature at which dial pointer movement stops. Maximum fluidity. - The maximum rate of dial pointer move- ment in dial divisions per minute. Plastic range. - The temperature range from the softening temperature to the setting temperature, in which the coal is plastic. SAMPLES For this work, coals representing two levels of maximum fluidity were sed, one of > 15000 dial divisions per minute, and the other of 2000 or less dial divisions per minute. The former, or more fluid, coal was from the Hernshaw seam of West Virginia; the other was from the Elkhorn No. 3 seam of eastern Kentucky. Two samples of each coal were obtained at different mes. In the discussion which follows they will be referred to as the base coals. The materials used as diluents were as follows: With the Hernshaw coal - Illinois high-volatile C bituminous coal (HVCB), Illinois high-volatile B bituminous coal ILLINOIS STATE GEOLOGICAL SURVEY (M r~- oo rsj vo co g o r- vo co co oj — ■* O tH ro tji -^ in CO <0 i— t 00 r—t c i i i i i i 1 O o h m oo o <-* o o in I s - — • o m o o a S -d •d •t-i i-H I s •!-t Pa -d 4) a. v Q s u 2 * o M 0) Ph o P5 •i-i *d 4 -. a x £ in o^ io n ^ "^ ^ co in r>^ ^* ^* °° |£2 (NJ M H H H H H O^ 00 r-' O ro ^' -< N ^ , I I I I I ' ' ■ O rM O O O O O O O OfOOOOOOO© o» ~* 00 O -H vO CO . vO » ^ ^ (Vj H H N •-« 2 S I— I >— I o 55 ' I S Ph U < O o M * u i n) I s £ P* ,a J-4 (ti o o PLASTIC PROPERTIES OF COAL 5 (HVBB), Pocahontas No. 3 coal, anthracite, char of ap- proximately 22% volatile matter, char of approximately 16% volatile matter, coke, graphite, and carborundum. With the Elkhorn coal - Illinois high-volatile B bituminous coal, Pocahontas No. 3 coal, anthracite, char of approx- imately 22% volatile matter, char of approximately 16% volatile matter, coke, and graphite. To obtain fresher samples and to minimize oxidation effects, samples of the base coals and some of the diluent coals were obtained at intervals during the course of the work rather than taking the entire sample at the beginning. Because of this, plastic property data for base coals and, to some extent, for certain diluent coals, appear somewhat different in the tabular data. However, samples were never changed within a given series. PROCEDURE The base coals and diluents were each manually stage -ground to pass a 40-mesh sieve. Test portions were prepared by mixing the diluents, in incre- ments of 10 or 20 percent, with each of the base coals. Each portion was thoroughly mixed, and plastic properties were determined with the Gieseler plastometer. Determinations on the base coals were made at the beginning and at the end of each series of tests. All determinations were made in dup- licate. RESULTS Tables 1 and 2 present a study of the duplicability of results for this work. Data obtained for mixtures of diluents 7 with the Hernshaw coal are shown in table 3. Data for mixtures of diluents with the Elkhorn coal are shown in table 4. Graphic representation of the effect of diluents on both base coals is shown on semilogarithmic scale in figures 1 to 9. Table 5 shows per- centage reductions of maximum fluidities of base coals by diluents, arranged according to decreasing volatile -matter content. DISCUSSION Reference to table 1 will give a picture of the duplicability of data. Dup- licate temperature values checked satisfactorily throughout the work. Con- sidering all data, the average difference between duplicate maximum -fluidity values was 15.9% with a range of difference from to 100%. For the Hern- shaw coal with diluents the average difference was 15.1% and the range from to 77.8%. For the Elkhorn coal with diluents the average difference was 19.3% and the range from to 100%. For the base coals only, the duplicability was better, being 6.9% average, with a range from to 13.3%. A comparison of maximum fluidity duplicabilities obtained for mixtures of base coals with the various diluents is shown in table 2. The best duplica- tion was obtained when high -volatile ft' bituminous coal was used as a diluent with Hernshaw coal. Of the diluents that have no Gieseler fluidity, coke and carborundum gave best duplication of results with the Hernshaw coal. For the Elkhorn coal with diluents, the lowest average difference between dupli- ILLINOIS STATE GEOLOGICAL SURVEY o o I— 1 o* I s - r» rg co ^ cg m -^ vo CO o cO m m m o o o CO m r\j m vO 00 m 00 ^ ^ o m in o mj r» o b ^ m O CO u CD X u o o eg oo eg co ^ m oo eg m in o r- eg o oo o — • O^ N rO m vO CO ^ ^ ^ eg eg O CO ^ (M t^- h ro %0 eg m vO O^ ^ ^ tF ^ ^ ^ >-* oo o o Tt* oo Q\ rt ^ vO vO > CO ^f ^ ^ co vo oo oo m m O h cO \fl M N CO "^ "sH ^ •"" • vO -rt (NJ N fO vO r— I "sj* ^1 vO ^ ■^ -^ Tp Tp o r» o "tf eg "* *-* eg -^f I s - I s - vO Tf ^ "^ ^ eg •— • o^ r- o m o eg -tf I s - o r*- Tp tJ< ^ ^ vO o t^ m co -v o eg m o» too TJ< ^ Tt< ^ 2 * o O CO "tf eg sO CO m oo co r- m rg CO O eg in 00 sO 00 O rt ^ f. r- oo CO Th -* ^ O CO ^ -^ ^ oo oo vO I s - h m co o — • ^ oo f«- oo co -^ ^ ^ ro o rg oo vo m o o> ^ ^ co i^ o> CO ^< -* ^ ^ o oo o oo < o h ^ oo 'oc CO ^ ^ ^ ) CO m m o m o o eg CO . o 0* S -6 s 2 PL +J 3 +■» a a ^j cj hh oo M-» o O .PI . 'i3 ^ § «J -^ «J rt en ^ S w S Cm P. S (U rt rt 4-> (U rt « pj 53 op « w **h oi H .a x 5a iid £a^«ft PLASTIC PROPERTIES OF COAL fM id vO O "sF r\) co m oo O ~* O r\j PO sO ro ^ ^ ^ H fO \0 ro ^ f>j o <\] -^ h- rg r*- ^ ^ ^h ^ co N O^ h oo ^h v£> O0 h (js N ^ o «# o r\j ^ n m \0 ^ ^ ^ ^ T*< ^ 00 vO sO O CO ro ■^t* ^f ^ O ro f\J oo in m m ^ r^ co rg o — • ^ r- ro co CO ^t* ^t* ^ s O 00 -tf —i ro -tf r- ^ ^ ^ ^ oo — « o m oo r*- o eg ^ r*- —t r^ M Tt* ^ ^ -H m m oo o r^ ld O •— • Tp 00 vO °° ro "^ ^f "^ CO ^ O *-i ro n m oo n <^ ^ ^t* ^ 00 -* o rg ro -<# I s - O O —• ^f I s - CnJ 00 ^ ^ in in ^O oo r* 00 eg o ^ ^ r- 00 ro ^ xh ^ m H oo vo n m h O h ^ ^ 00 N "^ "^ "^H Tf ro — • (M ^ O O ^ ^ 00 ro -^ ^f ^ O o m oo rg -< ^t* r- o r- ^ ^ ^f s rg ro in o cm r- (> H ^ f^ H 00 ro ^ -^ tF r-* ^ ro s ■— < ro ^ m r- — » 00 ro rjs n r* 00 vO ro - 1 ^ N ro 00 * ^ ^ --. m m m ro o oo o -* •*& oo o oo CO ^ tJ< t*« o r- r- o -h ^ ^ o — * m o co o ro "^ ^ ^ o ro ^ xf 00 m m ^ — i in o o ro Tt< -^ ^ o 00 o rg sO ro oo 00 —• ^ 00 ro o ro Tt* ^ -* oo r^ h- m o so 3 "* oo o o^ f ^ -^ o in rg ^ ^ m m -o r—t o ^ m -r- in t^. Qs i— 1 tH CO ro On o r-t ■tf 00 vO rjs ro -sp ^ ^ 00 ro ^ ^ ^ vO '-i CO O ro 00 vO o ro ^t* ^f ^f vO - O 00 o r-H sO 00 00 00 1— 1 ^ CO o o ro <* ^ ^ r~ ^o t>- o in oo o oo o Tp co o o fO i* ^ ^ r- vo r*» \o <—* co m oo o ro co o o^ fO M* ^ ^ N O N N 00 CO CO o^ h ^ oo o r> en Tf ^ ^ ^ s 0) d a -Ui d >> 00 d. CD d ■p-t 3 '3 a rt d s ■d S 3 h 4-> fi 4-J •rH 0) VH 00 4-1 o u 4-» f4 r— < OJO x' (0 o en O CO rrj +-> 4-> CD CO <: >s cu +j ojo 3 § 3 ^ »—• .. «+H U . +-> X 2 rd "J ^ a 4-» ojo ■h o . ti . 33 » *: \ 3 u. \ E \ o 2 \ \ Fig. 1 V. \ \ \ N X • \ \ • N \ • < \ \ \ \ ""*< ^ V Fig. 2 20 40 60 80 100 20 40 60 80 100 ^» \ 1 \ • \ \ \ • \ \ \ 1 \ i \ \ \ \ \ • \ \ \ \ \ i \ • 10 Fig. 3 \ \ < > \ \ \ \ \ \ • \ N < i \ \ \ • \ \ \ i \ • \ • / 10 Fig. 4 \ 4 V / 20 IOO 20 40 60 80 Percent Diluent Added too 40 60 80 Percent Diluent Added Fig. 1. - Effect of Illinois HVCB coal as diluent on maximum fluidity. Fig. 2. - Effect of Illinois HVBB coal as diluent on maximum fluidity. Fig. 3. - Effect of char (22% V. M.) as diluent on maximum fluidity. Fig. 4. - Effect of Pocahontas No. 3 coal as diluent on maximum fluidity. Solid lines identify the Hernshaw coal, dotted lines the Elkhorn No. 3 coal. PLASTIC PROPERTIES OF COAL 9 cates was found when char of approximately 16% volatile matter was used (14.2%). In this case, however, the range of differences between the lowest and highest was rather large (0 to 43.8%). The lowest range of differences was obtained when Pocahontas coal was used as diluent. It is of interest to note that in no case did the diluents tried improve duplicability of results for base coals. TEMPERATURE VALUES The apparent influence on Gieseler plasticity values of diluents added to base coals is shown in tables 3 and 4. The data indicate that fusion temper- atures increase as increased amounts of Pocahontas coal, both chars, coke, and anthracite are added to the base coals. This is true also for anthracite with the Hernshaw coal, whereas this diluent with the Elkhorn coal shows no marked influence on fusion temperature. Addition of high-volatile B bitumi- nous coal as a diluent to both base coals showed no marked influence. High- volatile C bituminous coal was tried as a diluent with the Hernshaw coal only. The data indicate a gradual increase in fusion temperature as increasing amounts of diluents were added. Carborundum with Hernshaw coal showed no marked influence on fusion temperature up to 70% addition. Temperatures with 80 and 90% addition were higher. With one exception, no striking influence of diluents appears in the max- imum-fluidity temperature data. Increasing additions of Pocahontas coal to both base coals raises maximum -fluidity temperatures. Increasing amounts of all diluents, with the exception of Pocahontas coal, appear to lower setting temperatures for both base coals. MAXIMUM FLUIDITY All diluents used progressively lowered maximum fluidities of both base coals as the amount of diluent added was increased. However, this lowering is not directly proportional to the amount of diluent added (figs. 1 to 9). Fur- thermore, the lowering effect of the diluents varies considerably for each base coal. Table 5 gives data for the percentage reduction of maximum fluidity of base coals by increasing amount of diluents, and shows that percentage re- duction of maximum fluidity of base coals increases rapidly as increasing amounts of diluents are added. The data also indicate considerable differ- ences among diluents in their ability to lower fluidity. Not only is this true for different diluents with the same base coal, but the effect of each diluent on each base coal is different. With regard to this point, there is evidence that additions of 10 to 30% diluent to the Hernshaw coal reduce its maximum fluidity less and less as the volatile -matter content of the diluent decreases. This effect is not evident with the Elkhorn coal; in fact, there is some indica- tion of the reverse. The question arises as to the cause of the difference in behavior of diluents with the two base coals. We cannot answer this question definitely but suspect that there may be a difference in kind as well as quan- tity of constituents, which may affect the plastic properties of the two base coals and lead to the differences shown. 10 ILLINOIS STATE GEOLOGICAL SURVEY o o co c\j CO m •<* o o I s - s - ^* N vO 00 ^ r- N m I s - oo — • c\j no -^ tj< ^ m ^ [v_ ^ r- 1 io I s - ■^ I s - co — • — « vo Tf »^ -^ m o vO ^ m co o 00 a- mm in co ^ ^ S (D 3 vO r-t . s O t^ m o i 1 m I s - O^ rO vO nO 43 CO -* -^ +J •l-l * m H . 0j o —• co in o rsi m m —* ^o (0 CO -* ^ ^ o 43 ,£ o X -u 1— t w 73 o m r- co -^ ^ ^ 7* on •— « co vO rsi I s - J-l CO ^ ^ "* o •d m cd ^ ^ -^ ^ bX) •« 3 x S Oh pu 6 b 5 -g o • 'ft °! CO U* A >* ^ i-i ♦• 3 CO ^ P, a r-1 nJ CO B B B •rH 3 Pj +j S 3 2 '3 00 PI rH i > vO d. B B 0) • ■•-> Pu " "i O 4-> O CO P! ^-4 X R) i— l 00 «M C! . •^ x (U > O CO O . • H ^ 00^ .!: S id "j N 00 s vO ro m oo o ro <* O CO O m O ro vO f\J ■— 1 vO <—* ro CO ro vO LO CO m fM o oo cq ro r^ CO m ^ t> ^ ro vO LO o rg T^ vO ro vO O rvj ^ ^ ^ Tt* ^ ^ ^ ^ N O O^ 00 h vfl o rvj ro vO in so ^ ^f ^ ^ I s - m 00 ro O vO O N rO'O N in ^ ^f ^ ^ O O ro ro vO ro rO "sf ^ sO ro ^ "^ ^H ^ If) H H H Tj< vfl o r\j ^t* I s - I s - so ■^ ^ ^ ^ s£> ^ O Tf ro oo o r\j ^ vO ro m ^ ^ ^ ^ m ro N O \fl h . vo co I s - o (\j m vo Tf m ^f ^ ^ ^* O I s - •-• o o o ~t tj< r^ -^ ^ ^ n< ^ ro <-* o o <-* co o O N ^ N 00 N -* "* "^ ^ ft "^ s O — * ro I s - o — • tj< h- rg so ^ ^ ^ ^ f» 00 I s - ro m 00 r^- ■— i I s - o r\] m ft s ft Tt* I s - o I s - o r—t ro I s - r«- t^- ro "^ ^ ^ in -* ^ <* ^H ro N vO in 't \0 (M O ft r# (>* <\J I s - ^* ^ ^ ^ ro m in ^ oo o ro (> H ^ N O CO ro Tf ^ tJ< o o I s - — i -^ f\j m s — « ^ I s - m I s - ro "^ -^ ^ I s - c\J vO ro s O I s - O *-l T^ I s - vO F»- ^ ^ ^ ^ Qs » S •H \ • \ \ \ « > \ \ \ • > \ \ \ \ ' \ \ \ • \ i Fig. 5 V \ > 1 • ^^ \ \ \ •v > > \ \ \ \ v \ \ \ 1 Fig. 6 • V 20 40 60 80 KX> 20 40 60 80 100 10,000 Q |,000 \ 100,000 10,000 -\ \ \ \ > > 1,000 100 10 v \ \ •x \ \ 1 » \ \ \ \ < » \ \ \ \ \ 1 i \ • \ • V \ \ i v \ \ \ \ • \ \ \ i \ > \ V \ i \ \ • \ Fig. 7 ,\ .1.. Fig. 8 i 1 . 1 20 40 60 80 Percent Diluent Added 40 60 80 Percent Diluent Added Fig. 5. - Effect of char (16% V. M.) as diluent on maximum fluidity. Fig. 6. - Effect of anthracite as diluent on maximum fluidity. Fig. 7. - Effect of coke as diluent on maximum fluidity. Fig. 8. - Effect of graphite as diluent on maximum fluidity. Solid lines identify the Hernshaw coal, dotted lines the Elkhorn No. 3 coal. PLASTIC PROPERTIES OF COAL 13 IOQPOO 10,000 1,000 I 100 E 10 — • — < '— •—, ^ \ < \ \ < \ • Fig. 9 i i 1 20 40 60 Percent Diluent Added 80 100 Fig. 9. - Effect of carborundum as diluent on maximum fluidity. Another interesting point in table 5 is the indication that there is some- thing more than simple dilution involved in the reduction of maximum fluidity by the diluents. If simple dilution alone were involved, then maximum fluid- ities of base coals should be reduced by the same percentage as the percent- age of diluent added. In only one case is this approximated - addition of 10% anthracite to the Hernshaw coal reduced the maximum fluidity 10.6%. Diluents (10% added) of volatile -matter content greater than that of anthracite reduced the maximum fluidity of Hernshaw coal more than can be accounted for by simple dilution, and diluents of less volatile -matter content reduced it less than can be accounted for in this way. In all cases, diluents reduced the max- imum fluidity of the Elkhorn coal more than can be accounted for by simple dilution. We are not certain how this additional reduction, over and above simple dilution, is accomplished. However, inter chemical action between base coal and diluent, solvent effect of one on the other, and difference in wettability of solid diluent particles by melted base coal might be possible factors involved. Whatever the cause may be, it appears that each base coal in admixture with each diluent is a distinct and individual problem. 14 ILLINOIS STATE GEOLOGICAL SURVEY I 1 2 g i—l -H o W o •r-« o DO + ON ^ + ON o -* > > X X (Tt U u d O £\ P. u 1 X\ O m d O O PQ o +j pq Z o (0 4-> > X u ti u u