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Quantitative Interpretation of X-ray Diffraction Patterns of Mixtures. I. Matrix-Flushing Method for Quantitative Multicomponent Analysis
By FRANK H.CHUNG
Sherwin-Williams Research Center, Chicago, lllinois 60628, U.S.A. (Received 11 June 1973 ; accepted 5 July 1973) A matrix-flushing method for quantitative multicomponent analysis by X-ray diffraction is reported. It is simpler and faster than, yet as reliable as, the conventional internal-standard method. In this new method, the calibration-curve procedure is shunted; a more fundamental 'matrix-flushing' concept is introduced. The matrix-flushing theory gives an exact relationship between intensity and concentration free from matrix effect. Contrary to most theoretical methods the working equation is very simple, no complicated calculations are involved. The matrix-flushing theory and the analytical procedure are presented. Eight illustrative examples are drawn to demonstrate how this theory is applied to multicomponent analysis and amorphous-content determination. A novel 'auto-flushing' phenomenon of binary systems was observed which appears to make the analysis of any binary system a simple matter.
Besides broad routine analysis X-ray diffraction is often the only technique available for distinguishing polymorphic structures and analyzing solid solutions. The results obtained are in terms of materials as they occur in the sample, not in terms of elements or ions present. The pigment industry is especially concerned about polymorphic forms and solid solutions. For example, the best red pigment quinacridone (Chung & Scott, 1971) has four polymorphic forms, only two of which have commercial value; the corrosion inhibiting pigment zinc molybdate (Kirkpatrick & Nilles, 1972) is composed of a solid solution of zinc oxide and molybdenum oxide. However, the only analytical technique, X-ray diffraction, dealing with these situations is hampered by a matrix effect. So far, the best method of quantitative X-ray diffraction analysis is still the internal-standard method developed before 1948 (Alexander & Klug, 1948). It involves the usual procedure of constructing a calibration curve from standards, which is rather tedious since each component sought needs a calibration curve, each calibration curve needs at least three standards, and each standard must contain exactly the same percentage of pure reference material chosen. A new X-ray diffraction method for quantitative multicomponent analysis has been developed. It is much simpler and faster than, yet as reliable as, the conventional internal-standard method. Since 1970, the Joint Committee on Powder Diffraction Standards has published a set of Reference Intensities (I/Ic) (Berry, 1970) of binary mixtures made with a pure material and synthetic corundum (~-A1203) by one-to-one weight ratio, where I and Ic are the intensities of the strongest lines of the pure material and corundum respectively. These Reference Intensities are intended for 'rough quantitative X-ray diffraction analysis of mixtures'. Occasionally there is a need for
a rapid quantitative X-ray diffraction analysis with moderate accuracy in our industrial analytical laboratories; therefore, attempts were made to utilize these Reference Intensities. This thought led to a new X-ray diffraction method for quantitative multicomponent analysis. In this new method, the conventional calibration-curve procedure is shunted and a more fundamental 'matrix-flushing' concept is introduced. The matrixflushing concept gives an exact relationship between intensity and concentration since neither assumption nor approximation is made. Contrary to most theoretical methods, the working equation of this matrixflushing method is very simple, no complicated calculations are involved. It is felt that one can utilize this method without understanding its theoretical basis. The matrix-flushing theory and the analytical procedure are presented below. Experimental data are collected to demonstrate how this theory is applied to multicomponent analysis and amorphous-content determination. A novel 'auto-flushing' phenomenon of binary systems emerged which makes the analysis of any binary system a simple matter.
In contrast with X-ray emission analysis, X-ray diffraction analysis has two factors favoring a more fundamental approach. Firstly, the primary and the diffracted X-rays are monochromatic and of the same wavelength. Secondly, the matrix effect consists of absorption only, no enhancement. When the monochromatic primary X-rays impinge on a fiat powder specimen, the intensities of diffracted rays are related to the percentage composition by equation (1) as derived by Klug & Alexander (1959), Xi/O~ Xdei
I~ = K~
stability and availability./xt / . Even/zt. it is free from matrix effect. In the mean time. including component i. However. ¢z. the ratio 1f~-t can be obtained °/1° through the Reference Intensities.A constant which depends upon the geometry of the diffractometer and the nature of component i.= Density of component i. which may be any pure compound not present in the sample. it is an exact deduction. So the best way of approaching this problem is to flush all these ¢z factors out of the intensity-concentration equation. Klug & Alexander. Consequently k f = k c = l . It represents a straight line passing through the origin with a slope equal to Xc/k. Let the weight fraction of the flushing agent and original sample be designated X s and Xo respectively. has not been accurately measured. let k. we get: 1 °) = ( k . (4) l°s" We have: b = x f uf lit st (10. all the matrix factors in equation (5) can be flushed out completely as shown below.. it is convenient to choose the same corundum as a flushing agent for the same good ieasons.. ) (pP))" kf (9) Substituting equation (9) into equation (5) we have: Xf) Xi = Xs ( kf I. For a binary mixture of compound i and corundum e with one-to-one weight ratio. 1 (7) Since I °. Since it uses intensity ratios of the same scan. and we obtain: (5) Ii This is the working equation for quantitative multicomponent analysis. Ic then equation (6) becomes I i = Intensity of X-rays diffracted by a selected plane (hkl) of component i. that is ( I°~1 °] and similarly: i = 1 \ktl tlxt] Pc . stand for the Reference Intensity ratio: (2) It fit io =Xt /xt where: 1. First. I For the sake of simplicity. ~o. Yet one more simplification can be realized. lc and 1~. is added into a sample of n components. we have (lO)--( ). = ( xs " ' )~s )( ] x. Any pure compound which is not a component of the sample can be used as the flushing agent. lines of the X-ray diffraction patterns of respective pure materials.are the intensities of the strongest °.= 1. Note that the working equation (12) not only comprehends the internal-standard method (Alexander & Klug. Xt = Weight fraction of component i. Since corundum (~-A1203) has been chosen for Reference Intensities by the Powder Diffraction File for its purity. 1° m (6) . (lO) Xf+Xo=Xf+ Then from equation (2): ~ X. I ° = Intensity of X-rays diffracted by a selected plane (hkl) of pure compound i. Thirdly. Intensity ratios from the same scan are the experimental data needed. In order to achieve this. K . a flushing agent. where the subscripts f and c stand for flushing agent and for corundum.= Mass absorption coefficient of pure component i. It is free from matrix factors. This equation (1 l) can be used for quantitative multicomponent analysis. internal standard and reference material added. which are constants from the same diffractometer. neither assumption nor approximation was made to reach the conclusion. the errors due to instrumental drift and sample preparation are minimized. No previous information as to the approximate concentration ranges of various components sought is required. the mass absorption coefficient of pure compound i. if any. The/xi and Pt in equation (2) are called the 'absorption effect' which complicates X-ray diffraction analysis. it gives a simple relationship between intensity and concentration. 1=1 (3) It =Xt Io /~t . Secondly. 1948. /-zt= Mass absorption coefficient of the total specimen exposed to primary X-rays. 1959) but also The individual values of I~9 and 1 ° are dependent upon the atomic positions in their respective crystal structures. similar to equation (5). =kt . all absorption factors are neatly flushed out. Equation (11) is a very important conclusion. .520 Hence we have: X-RAY DIFFRACTION P A T T E R N S OF M I X T U R E S .
)(1_- . The rutile and anatase titanium dioxide were pigment-grade samples containing 99. all samples were ground for about 20 min with an automatic mortar grinder (Fisher Scientific Co.if the specimen is made of exactly 50. the quantitative composition of a binary system can be easily calculated from the intensity ratio of the strongest diffraction peak from each component in a single diffraction scan. k. graphite-monochromatized Cu Ks radiation. One component automatically serves as a flushing agent for the other component and vice versa. of each of these systems was acquired through a calibration curve of standards. a novel 'auto-flushing' phenomenon exists.0 micron.).00% of corundum. calcite in aragonite CaCOa (Azaroff & Buerger. Equation (15) affords a means to check experimentally the correctness of the matrix-flushing theory. C H U N G 521 Xc+ ~ L=I. the free-falling method of sample preparation recommended by NBS Monograph 25 (1971) was employed. A constant-time (40 s) counting technique was used for each peak and each background. the slope of the straight line. we get: H. The flushing agent. Nevertheless. Mathematically. equation (19) represents a straight line passing through the origin with a slope k=kl/k2 when 11/12 is plotted against XI/X2. The chemicals used were certified reagent grade or better. we get" Reference intensities The relative intensities of peaks in an X-ray diffraction pattern of a crystalline compound vary slightly depending on the diffractometer design and instrumental conditions.7% rutile and 99. 1957). applying equation (12) to equation (3). No flushing agent is needed. It is interesting to observe that this linear relationship of binary systems of polymorphic crystals was recognized quite a long time ago. etc.X ~ = X o. (16) (17) i=1 Ii =I~ k1 For a binary system. it can be used for amorphous-content determination. If quantitative results are required. which means quantitative analysis can be done by merely grinding the original sample and scanning it. and pulse-height analyzer. Experimental Eight synthetic samples were prepared to illustrate the application of the matrix-flushing theory. i=1 (13) .-A1203 (l.8% anatase respectively. similar to the derivation of equation (10) we have" xl+x2= 1 ] 11 = kl XI • (18) 12 k2" Xz Solving these two simultaneous equations. 1 kl 12" (19) 1+ k2" 11 Therefore. 1948). The intensity data were collected by use of a Norelco diffractometer equipped with a solid-state scintillation counter.00% original sample and 50. The accumulated counts range from 20 000 to 250 000 counts for the period of 40 s after background correction. Duplicate readings were taken for each peak and each background.FRANK prescribes the slope of calibration curve for every component in the sample. and to predict and assay the presence of amorphous materials in a sample. To avoid preferred orientation. (14) (15) x~+x~ ~=1 k1 =1 ~Ii I¢ i=l k~ X~ ~ Ii = ( X ° ) I c " I . The new way of acquiring the slope k for any binary system and the procedure of quantitative analysis for multicomponent systems are presented in the experimental section below. then equations (12) and (15) are reduced to the following rather interesting relations: 1 Ii XI= 2ki (Ic) Note that this auto-flushing phenomenon is true for any binary system. the Reference Intensities in the Powder Diffraction File are quoted to only two digits. Furthermore. Union Carbide). thus it is not necessary to actually work out these calibration curves. As no restriction is imposed by the theory upon the weight fraction of flushing agent X s in equation (I 1) and X~ in equations (12) and (15). Prime examples are the determination of anatase in rutile TiO2 (Spurr & Myers. quartz in cristobalite SiO2 (Alexander & Klug. This is because in such special cases Pl =P2 and inherently there are no matrix effects whatsoever in the polymorphic systems. to appraise the reliability of intensity data. was Linde semiconductor-grade v. When corundum is chosen as the flushing agent. 1958). it is necessary to determine the Reference Intensities of materials concerned using the same diffractometer under the same instrumental conditions. integrated-circuit control panel. synthetic corundum. In order to ensure optimum particle size and sample homogeneity. Let the weight fraction of the two components of a binary mixture be X~ and )(2. A strip-chart trace of the X-ray diffraction pattern of each sample was recorded for later reference. Consequently. The Reference Intensities (I/Ic) obtained from different laboratories hardly agree beyond two significant figures.
I Reference intensities by counting Intensity (c. 40 mA 839 V 128 1"0 V 3.93 43.36 It ~ k~ X0 Ic x~" 2 3 4 5 Composition (g) ZnO KC 1 LiF A1203 Flushing ZnO KC1 LiF A1203 Flushing ZnO TiO2 (R) CaCO3 A1203 Flushing ZnO TiO2 (R) CaCO3 A1203 Flushing ZnO CaCO3 SiOz (Gel) A1203 Flushing 6 7 8 ZnO TiO2 (R) TiO2 (R) TiO2 (A) KCI LiF 1. which was t h e n g r o u n d to a h o m o g e n e o u s fine powder. T h e i n s t r u m e n t a l c o n d i t i o n s o f the diffractometer are given in Table 2.9197 0.4147 0.62 3.39 2. T h e w o r k i n g e q u a t i o n (12) was applied to each c o m p o n e n t .9037 0"7351 0.96 77. a n d the intensity of the strongest line of each c o m p o n e n t was measured.017.23 22.0633 1.0 V 40 s Copper X-ray tube.1 4 % ( E x p e r i m e n t ) 41. 1.79 39. Sample 1 Intensity and composition data Intensity (c.× 599 = 2736 (Theory).5 3. 0. Idl~ By counting PDF 4. a n d the c o m p o s i t i o n f o u n d are listed in T a b l e 3.35 2"60 2-57 78.8901 1"0128 0"8348 0.6759 0. A k n o w n q u a n t i t y of flushing a g e n t ( ~ 1 6 % cx-Al203) was a d d e d into this s a m p l e Xo Xc " Ic = 82"04 -1-7"96. S a m p l e 1 consisted of three c o m p o nents Z n O .70 56-20 57"30 74. give fairly g o o d accuracy.80 42.5341 0.3 Six chemical c o m p o u n d s were used for the following illustrative examples. All s u b s e q u e n t intensity d a t a were collected u n d e r the same i n s t r u m e n t a l conditions.57 16-28 40.87 + 1.95 21"44 71.49 41.32 18.98 2.49 % (True V a l u e ) .41 28"00 26"20 16.13 15.36 17.s.96 4.26 1"38 1.f l u s h i n g t h e o r y to m u l t i c o m p o n e n t analysis.4317 1.96 18.8181 0"9532 0"6601 0-8972 2"5114. T h e i r Reference Intensities (I/1c) a n d relevant d a t a were d e t e r m i n e d a n d are listed in T a b l e 1. It is f o u n d t h a t even the intensities read directly f r o m the p a t t e r n on a strip-chart. Fig.78 27.9 1.07 28.32 1.40 17.) 5968 2845 810 599 2856 1651 765 1719 2408 931 2558 420 120 139 4756 352 4661 2298 0 631 6259 1461 1373 2386 5371 604 % Composition Known Found 41.35 4.8219 2721 2736 1662 1719 1767 1761 1677 1711 1842 2312 .1276 21-1272 2. rutile TiOz anatase PDF card 5 -664 4-587 4-857 5-586 21 . All the p e a k s in the diffraction p a t t e r n of this m i x t u r e were clearly resolved.) I~ Ic 8178 1881 4740 1223 3283 2487 4437 1491 2728 1040 3573 1054 Reference intensity. T a b l e 3.522 X-RAY DIFFRACTION T a b l e 1.87 3.32 Diffractorneter conditions 50 kV. T h e true c o m p o s i t i o n .3 ZnO KC 1 LiF CaCO3 TiO. broad focus Scintillation detector Gain Baseline Window Constant time Multicornponent analysis F o u r samples were p r e p a r e d to d e m o n s t r a t e the app l i c a t i o n of the m a t r i x . KCI a n d LiF.p.0 3"4 4.s.1309 0.14 22.90 74"64 25-10 25. for example: Xz.4234 0.4253 0. PATTERNS OF MIXTURES.p. T h e correctness of the m a t r i x .22 72.04 18.f l u s h i n g t h e o r y is f u r t h e r scrutinized by e q u a t i o n (15): Ii 5968 2845 810 = 2721 ( E x p e r i m e n t ) ki = 4"35 + 3. T a b l e 2.06 34-43 36.7418 0-9518 2.35 x 5968 599 = 4 1 . the intensity data.36 15.5759 0.98 19-10 13.4530 0.15 12"41 17"87 16"86 50"00 24-38 25.5629 1.36 19.0335 0.
or better is typical with the solid-state scintillation counter.5% by weight should be detectable. The intensity of the next strongest line of AlzO3 was measured. Generally 0. It is apparent that the same working equation (12) can be applied regardless of the concentration range. Exactly 50.. . . a good agreement between experimental values and true values is obtained and the interesting relationship that the sum of It/k~ should be equal to the intensity of corundum Ic is fulfilled. It also shows that the matrix-flushing effect is independent of the amount of flushing agent used. . . Sample 4 was prepared to check the sensitivity and detection limit of the method. .p. is limited only by the minimum size of the peak above background which is usually taken as three standard deviations of the background intensity. . . and this is used to calculate the intensity of the strongest line of AI203 with reference to the pattern of pure AlzO3 obtained by use of the same diffractometer under the same conditions. . . . The X-ray diffraction patterns of (a) Sample 1 where all peaks are resolved. 1. Very good agreement between the experimental values and the true values is shown in Table 3. C H U N G 523 before. (b) Sample 3 where there are some overlapping peaks. and 80 % CaCO3 with 17 % AlzO3 as flushing agent. A CaCO3 line interferes with the strongest line of A1203. the TiOz peak in this case Key A : A 1203 C : CaCOs K: KCI L: LiF T:TiO 2 Z: ZnO Z C & z T K II & T A C .FRANK This proves that the relationship between X-ray intensity and concentration derived from the matrixflushing theory is real.s. (d) the ZnO-KC1 binary system for slope determination. Sample 2 is composed of the same three components in different quantities. The precision of intensity measurement is always in our favor. Sample 3 is made of ZnO. not all of the strongest lines are resolved. . . 25 . TiOz and CaCO3 with about 20 % flushing agent ~-AlzO3. i i i r 35 (a) 40 0 20 25 in ... 3'5 . 2 % TiOz. . . For example. .a. In such situations. Two other CaCO3 lines overlap the first and second strongest lines of ZnO. i 30 J . . (c) Sample 5 which contains amorphous material. more AI203 should be added to bring the concentration of the major component down. i . The intensity of the third strongest line of ZnO was counted to calculate the intensity of the strongest line of ZnO as H. Note that the scintillation counter might be flooded if the concentration of a strongly diffracting component is extremely high (such as 90 %). however. It contains about 1% ZnO. A sensitivity of 5 c. 25 30 35 (¢) 40 0 20 25 30 S5 (a) 40 0 20 Fig. (b) 4'0' ' ' 62'6 Z A A C K A ~ l . The detection limit depends upon the nature of the sample.. In this example. Again. .00% ~-AlzO3 was incorporated into the sample. while the Reference Intensities are obtained at 50% concentration.. The lower concentration level.
(15). kz . There is no matrix effect whatsoever in such a system. The percentage composition can be obtained from a regular scan of the binary mixture.7 %.g. . Xl x2 = k .13 % silica gel actually put in.5583 Note that" kl 1-32 . quartz and cristobalite SiO2 (Alexander & Klug. l. 1967) is 1. . [ ILw ~ _ 1846 =0"331 k = \ IKc~I 50/50 . which is quite good in normal analysis. Fascinatingly. Comparing this with the 16. Three examples are cited to depict the features of the auto-flushing phenomenon. Sample 5 contains three components ZnO. (18) and (19).87 These results compare very favorably with the true values as shown in Table 3. It is composed of rutile and anatase TiO2.95 % amorphous material is found..62 6259 1+ 4-35" i461 : 27"93 % . hence a linear relationship between In conclusion. Fig. eO/'o = . 5371 1 +0"331 × 604 Similarly for a ZnO-KCI binary system: Izno) k = . . Other polymorphic binary systems have been discussed in the literature. I X-ray intensity and concentration exists for each component: I1 = k .. Auto-flushing For any binary system..341 kz 3-87 XLiF .. .. the recovery is felt to be very good. Sample 7 is a special case of a binary system. The general nature of this linear relationship and the simplest way to obtain the slope was not discussed in the cited references.. x2 gives 7394 counts with a background of 1824 counts in a fixed time of 40 s. . Since duplicate readings were taken the relative standard deviations (Jenkins & DeVries. CaCO3 and SiOz (silica gel. . . a polymorphic binary system.. = 1 25"36% . e.13. Each component automatically serves as flushing agent for the other component. .Rb _~ 100 1/~ 1/185+46 ]/'2 x 40 185-46 1"7% 11 /2 - kl k2 X1 X~ (18) Amorphous-content determination Traditionally. 0.. 1948). XZnO= 4"35 1461 =72"07% 1+-2"62"6259 1 1"20 X'TiO2 = 2. . However. A normal scan of this sample.. . . which is what Alexander & Klug have demonstrated. It was previously shown that all p factors are flushed out of the basic intensity-concentration equations (12). . . . 100 V'2 ~/T ~Rv+Rb R v . .35 4747 3956 =1. . Sample 6 is a binary system of ZnO and TiOz which represents a general case. No flushing agent is needed. The slope of this line is equal to a singular value which is simply the corresponding intensity ratio of a 50/50 mixture of the two components. . The slope k is simply the corresponding intensity ratio of a 50/50 mixture of the same two components. Substituting the intensity ratio of the strongest line of ZnO to that of TiO2 into equation (19). .IKcl/s0/s0 while kl 4. etc.. the plot of weight ratio to X-ray intensity ratio is always a straight line passing through the origin. The linear intensity-concentration relationship of all polymorphic systems was recognized and determined by calibration curves. The difference here is that k~' and k~ do contain absorption factors (p) while the ratio (kl/kz) does not. An interesting feature of this matrix-flushing method is that it can be used to detect and determine the total amorphous material in a sample.524 X-RAY DIFFRACTION P A T T E R N S OF M I X T U R E S . X-ray diffraction analysis provides information about crystalline components in the sample. By the use of equation (12) and material balance. . amorphous). calcite and aragonite CaCO3 (Azaroff & Buerger. a general rule of auto-flushing for binary systems can be pronounced as follows: For any binary system. The presence or absence of amorphous materials is generally ignored.3. does not indicate the presence of amorphous material. 15. In this case I~ Xo Xc ~k< z which indicates the presence of amorphous materials. 1958). . the matrix-flushing method shows a large intensity imbalance as shown in Table 3. the kl and kz in equation (18) derived from the matrix-flushing theory are indeed the Reference Intensities. we have: 1 Note that k~' and k~ are not the Reference Intensities. . . They are unknown constants and have to be determined by calibration curves. an auto-flushing phenomenon emerges. Sample 8 is made of LiF and KCI to illustrate the simpler way to determine the slope k =kJk2 in equation (19) without using the Reference Intensities at all.
& SCOTT. If it can be regarded as a binary system of CaCO3 and A1203. The author wishes to thank Mr. (1973). F. any line obeys this rule as long as the same line is used consistently. H. P. (1970). p. 886889. KIRKPA'rRICK. NBS Monograph 25 (1971). Appl.. CHUNG. 225-230. J. & BUERGER. the following three factors deserve attention: ALEXANDER. Therefore.783. Joint Committee on Powder Diffraction Standards. New York: Springer-Verlag. The level of perfection or imperfection is revealed by the width of their diffraction lines. Appl. Note 18. 20. A. CHUNG. The minor components contribute only 4 % by weight. Chem. The extreme case is the newly developed X-ray diffraction method for the determination of crystallinity of polymers (Chung & Scott. Sherwin-Williams Company. & ALEXANDER.. (2) No previous information about the approximate concentration range is required. H.S.1%. closer results could be obtained. AZAROFF. p. R. p. R. This rule. & DE VRIES. . (1967). (1948).677. However. The features of this matrix-flushing method are multifold. hence the errors due to instrumental drift and sample preparation are eliminated. Standard X-Ray Diffraction Powder Patterns. (1958). p. The application of this rule of auto-flushing is not confinetl to stricqy binary systems. 412. KLUG. References XAIzO3= 1+ 1 4756 =18"1% 2"98 352 (True value 17. neither component needs to be a good crystalline material as long as the perfection or imperfection in crystal structure of the component sought is of the same order as that of the reference material used to determine the slope k. 1 =81"9% . It was found that the slope of the straight line in this reference is another proof of equation (20). p. Inorganic Index to the Powder Diffraction File. L. J. 3. T. (2) The grinding of the sample must be thorough enough to ensure optimum particle size and sample homogeneity. C. 760762. 4756 (True value 79.9 x 96 % = 78. 205. New York: McGraw-Hill. H. 4. New York: John Wiley. All the matrix factors are flushed out of the intensity-concentration equation.6 %) . (1971).1 x 9 6 % = 17. (1957). R. & NILLES. 96. (3) The loading of the sample into the sample holder must be free-falling as recommended by NBS Monograph 25 (1971) to avoid preferred orientation and induced packing. F.0 % . C H U N G 525 Ix =kX~ I1 k = i2 at ork= xl ~-~=1 (20) (/1) h s0/50 = slope. Pennsylvania. 29. the more important ones are: (1) No calibration curve is needed. Anal. concise and precise.S. L. overlapping peaks do not present a problem. (3) All the intensity data are obtained from a single scan. Cryst. Anal. Richard W. M. BERRY. If the percentage of the minor components is approximately known. 1189. A case in point is Sample 4 which contains four components when AlzO3 is counted as an unknown. Cryst. R.98 x In order to attain high precision and high accuracy of X-ray diffraction analysis by the matrix-flushing method. ~ KLUG. this sample has only two major components CaCO3 and AI2Oa. J.J.: U. (1959). & SCOTT. (4) It can be used for amorphous-content determination as well as multicomponent analysis.4%). H.--352 1 + 2. (1972). Government Printing Office. 6. Scott for his stimulating discussion and warm encouragement. X-Ray Diffraction Procedures. (5) The general rule of auto-flushing puts the analysis of any binary systems on its shortest route. makes the quantitative X-ray diffraction analysis of any binary system a very simple matter. L. then 1 (1) The material used to determine the Reference Intensity must have the same level of perfection or imperfection in crystal structure as the component sought. (6) It is a most general method in its simplest form embracing the three cases of quantitative analysis put forth by Klug & Alexander (1959). Discussion Xc"c°s=.C. W. J. Furthermore. L. It is not necessary to choose the strongest line of the diffraction pattern. JENKINS. Fairly good results can be obtained this way and thus eliminate the addition of a flushing agent. E. Chem. & MYERS. SPURR.FRANK In simple mathematics: H. The Powder Method in X-Ray Crystallography. Washington D.. 506-51 I. Practical X-Ray Spectrometry. J. U. Patent 3. Note 81. H. W. V. 1973) where one component is amorphous while the other component is a poor crystalline material.
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