r/r- methods of coal and coal ash...
TRANSCRIPT
CHAPTER-2
METHODS OF COAL AND COAL ASH ANALYSIS
INTRODUCTION:
Analytical methods used in trace and toxic
elements analysis of coal and its ash may be separated in
to two categories. There are certain methods which can
not be easily used for multi-element analysis on an
individual sample. Certain trace elements are volatile.
Atomic absorption spectrscopv, potentiometrv, voltmetrv
and absorption spectrometry, require Sample preparation
for coal and fly ash matrices. Precision depends largely
on the individual analyst's Skill. [1] [2] [3] [4]. Several
organisations have published individual summaries of
procedures used in their laboratories. [5] [6] [7] [8], The
present trend is towards development of multielemental
instrumental procedures to cover quantitatively as many
elements as are possible. Because any particu la r
analytical discipline is better suited for certain elements
than for others for var ious inherent reasons. A
combination of methods is usually necessary to determine
[5(3
all elements of interest.
The below mentioned block diagram describes
the methods used in coal analysis by U.S. Geological
Survey [9],
Table N o .l
Methods used in Coal analysis by U.S. Geological Survey.
Coal as received
IAir dry (298"K)
Then ground to 80 mesh.
1
Ashing at 798V’K
1M ethod-1 - A.A.S. fror Mg, Li,
iNa,^Mn, Cd, Pb, Cu and Zn.
M ethod -2 - X-rav fluorescence
for Al, Si, Ca, S, Fe, Ti, K, Cl, P.
iM ethod -3- Semi quantitative
spectrographic analysis tor B,
Ba, Be, Co, Cr, Ga, Go, Mo, \i
and V.
— IStorage
IRaw coal
IM ethod -1- Spectrographic
method for As, Sb.
M e th o d -2- Specific ion
electrodes for F.
M ethod-3-X-rav fluorescence
tor Se.
M ethod-4- Xeutron actu ation
analysis for As, Sb, Se, Fe, Be.
Co, Cr, Zn and others
M ethod-5- Flameless A A S
for Hg, Sb, As and Se
The preferences for a particular technique are
often expressed in the literature. Such preferences are the
results of analysts experience equipment available and
m any other subjective factors. A tom ic absorption
spectroscetry and colorimetry have been employed in the
present context.
A n a l y t i c a l p r o c e d u re s for a t o m i c a b s o r p t i o n
spectroscopy :
A.A.S. is a m ethod w ith h igh sensitiv ity;
sensitivity of the method declines in increasing non
metallic character of the element.
Analytical Procedures for A.A.S.
Sample preparation:
The prob lem s encountered in the sample
dissolution are discussed in some details by Slates. [10].
The Bernas procedure [11] is often used for dissolution of
slag, flv ash and soils with very low organic content.
Silicates are decomposed in 30 to 40 minutes at T10°C
without volatilization losses. The decomposition medium
of HF, H 3B 03 and aqua regia provides a salt free matrix
that offers negligible interferences during AAS analysis.
Bernas procedures permits volume measurements in
calibrated glass containers. The dissolution procedure
has been satisfactorily applied to AAS. analysis. [12] [13]
[14]. Results of AAS Method as applied bv Dreher and
Schleicher [15] has been described below\
Table No. 2
Concentration of Trace and Toxic elements
Element CoalAnalytical A. (in n.m.)
Cone in ppm.
S.D.
[1] Pb 283.307 2.8 8.0
[2] Cu 327.396 4.5-69 5.4
[3] Cr 425.435 4.4-33 3.4 .
[4] Mo 317.035 <0.3-30 5.0'
[5] Zn 334.50 7>200■
[6] Mn 257.61 5.27-400 19
For Cd, Gluscoter [16] obtained the following results.
Cd - l (n n i ) 228.80 <0.1 - 29
Wet chemistry has been employed by us for the
sample preparation of conventinal AAS. It is possible to
determine Li, Be, Cr, V, Mn, Co, Ni, Cu, Ag, Cd and Pb
after dry ashing and acid dissolutions. The procedure
employed is that used by Simon and Huffman [17].
Methods of Analysis :
Accordingly to their method coal ash 0.5 to 1
gm. is weighed in to a 100 ml Pt. d ish. 10 ml of
demineralised water, 10 ml H N O , and 10 ml HF are
added to the dish. The dish is covered and allowed to
stand overnight. Then 7 ml of HCIO^ added to the dish.
The dish is placed on a steam bath for 1 hr. and then
placed on hot plate to fume off the acids near to drvness.
25 ml of water and 5 ml of HC1 are added to the dish,
digested in an steam bath for 30 minutes. The solution in
transferred to a 100 ml volumetric flask and diluted with
water up to the 100 ml mark. Aliquots of this sample are
then aspirated in to the air-acetvlene flame on an atomic
absorption spectrometer to determine the elements
namely Na, Mg, Cu, Li, Mn, Zn, Pb and Cd.
O ther comprehensi\’e reviewsand b ib l io
graphies [18] [19] are available in the literature. Several
organizations have published individual summaries ot
procedures used in their laboratories [20] [21]. Atomic
absorption spectroscopy has certain principles, limitations
and areas of applications. Combined use analytical
disciplines give fruitful results. Sample dissolution has
certain problems; it has been discussed in details bv slates
[22], The Bernas procedure [23] is often used for
dissolution of slag, flvash and soils with very low organic
content. [24] [25j Simon and Huffman [26] determined
coal ash bv AAS. Coal ash in weighed. (0.5 to 1 g.) in to
Pt dish. Demineralised water, 10 ml, H X O , 10 ml and
LIP 10 ml are added to the dish. The dish is covered and
allowed to stand overnight, then 7 ml of HCIO, is added
to the dish. The dish is covered, placed on a steam bath
for 1 hour to fume off the acids to drvness. 25 ml of water
and 5 ml of HC1 are added. The dish is covered and
placed on a steam bath and digested for 30 minutes. The
solution is transferred to a 100 ml volumetric flask and
diluted to volume with water. Aliquot is then aspirated
in to air acetylene flame of an A tom ic Absorption
Spectroscope to determine the concentration of the trace
and toxic elements. The sample aliquot used for the
determination of Mg is made to contain 1 % Lanthanides.
Cd and Ca mav also be determined using a heated
graphite atomizer.
For many elements eg. Cd and Ca, solvent
extraction offers a means for increasing the sensitivity of
the determinations bv isolation and concentration of the
metals of interest. A procedure developed for detection
Cd and Pb bv Cavallaro et.al. [27] using the extraction of
iodide complexes of Pb and Cd in to methvi isobutvl
Ketone. The preparation of coal samples for Cr, Cu, Mn
and Ni was the same as employed for Cd and Pb. Below
mentioned table shows the recommended instrument
parameters for AAS.
Table No. 3.
Recommended instrument parameters for A.A.S.
S.N. Flement Ain run.
SpectraCurrent(M.A.)
Lamp Fuel Support
1. Cu 324.8 0.5 3.5 c =h 4 Air
2. Cr 337.9 0.2 / C :H 4 Air
3. Cd 337.9 0.2 3.5 c :h 4 Air
4. Zn 337.9 1.0 5 Air
5. Pb 405.78 0.7 4 c ;h 4 Air
6. Be 234.9 4-?/ c :h 4 Air
Detection limits for elements in coal ash [28] is as
belovv:-
Table No. 4
Elements Sampleweight
Lower limit of 1
detection in \xg/g.
Na 0.5 100
Mg 0.5 100
Li 0.5 5 j
Mn 0.5 15 i
Zn 0.5 10
Pb 1.0 1Cd 1.0 1.
SPECT RO PH O T O M ET RIC D E T E R M IN A T IO N S
OF SOM E TRACE A N D T OXIC
ELEMENTS IN C O A L .
[1] Z i n c :
For spectrophotometric determination of Zn
following procedure has been employed-[l] Zn
solutions containing 5 to 25 ppm of Zn were
prepared from the stock s o lu t io n .[220 mg
ZnS04. 7H20 /500 ml].
[2] Zn was estimated spectrophotometrically using
dithiozone. [29], Powdered coal sample was
treated 10 ml concentrated H N 0 3 (A.R. Grade).
Solution wras heated in a steam bath. W hen
digestion is complete, the solution was heated
to dryness. Diluted with w'ater to 20 m l with
water.
[3] Dithiozone was dissolved ( lm g /m l) in 0.1 M
NaOH solution.
[4] The pH of the sample was adjusted between 5.5
to 6 by adding 1:15 v /v N H 4OH solution. One
ml. of sample solution was pipetted out, 0.1 ml
of dithiozone solution added. The solution was
suitably diluted to obey lamberts and Beers law.
Absorbance was read at 555 nm. By extrapolation
concentration of the unknow n solution was
obtained.
[2] C d :
Cd was estimated by dithiozone method.[30] 25
ml of 1:10 H 2S 0 4 (v / v ) was added to the powdered coal.
The solution was heated to dryness and repeated if
digetsion is not complete.
The solution was neutralized by N H 4O H (1:12
v /v ) . Then 4 ml of l :1 0v /v HC1 was added and the
volume was made to 100. The pH of the solution was
adjusted to 6 by add ing N H 4O H . The so lution was
filtered in a whatman 42 filter paper. 1 ml of the
sample solution was pipetted out. 0.2 1 of dithioxone
solution was added and concentration of Cd estimated
spectrophotometricallv.
Stock solution of Cd was prepared bv dissolving
l).8 (.ig Cd/m l. Standard solution was obtained b\' dilution
method to contain 0.2 to 0.8 ppm. of Cd.
[31 ESTIMATION OF Cr :
Chromium was estimated spectrophotometricallv
using diphenvl carbazide [31], To the powdered coal, 10
ml of IN H,SO, was added. Then 0.5 ml of 0.5 N KMnO - t
solution was added. Heated in steam bath till sample is
digested completely. Excess of KMnO was decolorised
by add ing 5°o sodium azide solution at the rate of 1
drop per second. Flask was shaken after adding each drop
till brownish tint was destroyed. The solution was
filtered in whatman 42 filter paper. To 1 ml of above
sample, 1 ml of 0.25% d iphenvl carbazide solution
(in acetone) was added. [10]. It was diluted with 10 ml
with water. The absorbance was read at 540 nm.
The standard Cr so lution was prepared by
dissolving 50 mg of K-,Cr.,0, in 1000 ml of water. 1 his
solution contains 10 m g /m of Cr.
Standard solution containing 2fig to 20 fig of Cr
was prepared and standard curve was obtained.
Cu was determined by method described in ref. [32]A.
[4] DET ERM IN AT ION OF Mo [33]B
1 gm of oven dry coal sample is powdered, taken
in a Pt crucible. 5 c.c. HF and 5 c.c. of H C I0 4 were added.
Heated at 300°C till liquid is evaporate!. When digestion
is complete 5c.c. of HC1 and a little quantitv of water is
added. Heated in an electrical bunsen till drvness. The
aliquot is transferred to 100 ml volumetric flask and
diluted to 100 ml mark. This solution is empolved for
colorimetric determination of Mo.
Reagents required
(1) 5% w /v aqueous solution of KI.
(2) 5°o w /v aqueous solution, freshly prepared.
(3) 10% w /y aqueous solution of tartaric acid.
(4) 10% w /v aqueous solution of thiourea,
freshh' prepared and filtered.
(5) D ithiol solution : To 0.2 gm of melted
dithiol, 100 ml of 1% w /v NaOH solution
is added, mixture is stirred for 15 minutes.
1.8 c.c. thiglycollic solution is added to it.
An aliquot of test solution containing 1 ug/c.c. of
Mo is taken. Treated with excess KI. Liberated L is cleared
by adding ascorbic acid,dropwise. 1 c.c. of tartaric acid
solution and 2 c.c. of thiourea solution were added. Then
4 c.c. of dithiol solution added. The solution was allowed
to stand for 30 minutes. The Mo-dithiol complex was
extracted in to isoamyl acetate. The organic phase is dried
and optical density measured at 680 nni.
[5] DET ERM IN AT ION OF Se
[1] Discussion :
Sill, C.YV. and Peterson, H.E. [34] found that Se
has tendency to accompany 'S'. Bowen and Covvse [35]
were able to separate Se from As, Br, Mn, Na and Zn
and determine the element rapidly with sensitivity of
0.005 jig. The permangnate method of Schrenk and
Browning [36] has been extented to the determination o;
Se [37], A procedure with excellent results have been
reported. [38], No. Tellurium has been found to interfere,
even if its concentration is 1000 times greater. Mellichamp
[39] deve loped a sem iquan tita t ive spectrograhic
procedure for Se. Photometric method based on 3,3'
diamines benzidine and 2,3 diaminonaphthalene base
gained w ide acceptance, in the analysis of Se. The
sensitivity of the reagent has been increased bv EDTA.
[40] [41],A tom ic absorp tion analysis by Rann and
Humbly [36] has been found to be excellent.
Reagents required
[1] S o d i u m selinite solution lml= 2 ug of So.
[2] HC1, (density 1.19 g/c.c.) and diluted to
1:7.
[3] H N O v density 1.5 g/c.c.
[4] N H 1 solution diluted (1:1)
[5] EDTA : 5% and 0.1 M solutions.
[6] H CO O H (1:9) solution.
[7] SnCln solution : 10 gms dissolved in 4ml.
HC1, (density 1.19 g/c.c.). Heated, cooled
& diluted with 16 ml of water. Solution
is to be prepared just before analysis.
[8] Sodium hvpophosphite = 10% solution in
HC1 (1:7)
[9] 5% Carbamide solution.
[10] Citric acid 25% and 10% so lu tion of
Sodium arsenite = 1 ml = 50 mg of As.
[11] Cresol red soln.- 1 % in 20% C H .O H
solution.
[12] 0.5% solution of 3.3’ diaminobenzidine in
C fH^ or Toluene (keep the solution in
Procedure :
The solutions containing 1, 3, 5, 7, 9 (Ag of Se in
50 ml beakers are prepared. 2.5% EDTA solution (1 ml)
and 2ml. of H C O O H acid added in each beaker. pH
adjusted between 2 to 3 with NH^ to get yellow color o
cresol red indicator. Two ml of 0.5 solution of 3,3
diaminobenzidine is added to each beakers. Solution is
allowed to stand. NH^ is added to adjust the pH at 8
(violet color of the indicator is obtained). Transfer the
solutions to 100 ml separating funnel.Add 11 ml of C,H
or C6H-CHr anc extract the coloured complex. Percent
absorbance is measured at 415-420 nm.
Mg is determ ined bv titrimetrv and 'S' bv
Eschka method. [43]
Ox ides ot m inera ls associated w i th b i t u m in o u s
coal ash. [44] are as m en t ioned below:
Table No. 5
Constituent Oxide Percentage
SiO, 20-60
a i a 10-35
SO, 0.1-12
Fe2° , 5-35
CaO 1-20
MgO 0.3-4
Na20 + K 20 1-4
Average concentration ot elements in coal ha\'e
been described below : [4b]
Table No. 6. (Cone, in %)
S.N. Hlement U.S. Average World wide
Bv Spectroscopy By A AS Average
1. s 2 2 15 "I 1
Si 2.b 2.89 2.8
AI 14 1 (i7 1.0 i
4 (/a 0.54 0.72 1.01
5. Mk 0.12 0.25 0.02 !1
6. \'a 0.06 0.091
002 i
K 0.18 0.0(1 0 01
s !:e 1.0 - 10
u Mn 0 01 - 0.005
■ [ 6 ' 1
Concentration of some elements in ppm. [46] has
been mentioned below :
Table No. 7.
(Concentration of trace and toxic elements)
S.N. Element Spectroscopic determ ination W orld w ide average
1. Be 2.0
1 1
1
3 1■
2. Bi 0.7 5.5
3. B 50 75
4. Cd 1.3' ' i
5. Cr 15 10
6. Cu 19 15
7. Pb 16 25
8. Li 0.08 0.07
9. M o 3 r>
10. Se 4.1 3
11. Zn 39 50
M g in coal :
Mg conc. in North Dakota lignite is reported bv
Somer ville and Elder. [47] to be 5039 ppm. Burchett [48]
has reported Mg concentration in eight coal samples
from Nebraska to be in the range of 0.047 to 0.574 raw
coal samples from three Illinois based plants had some
what lower value (0.14 ±0.07%) [49], Cooley and Ellman
[49] studied lignite and subb itum inous coals from
Eastern Montana. They found Mg concentrations in
subbituminous coal samples in western direction. In the
present case Mg concentration was found tobe 4350 ppm.
Mg was estimated titrimetricallv.
Ca Concentration :
Ca concentration in coal occurs around 1% or
smaller. The average concentration of coal in North
Dakoita lignite is reported to be 1.6% [51] Nebraska coal
has 0.25 to 2.4% Ca [52] Raw coals from Illinois basin has
0.12 to 1.77% of Ca [53]. In the present study it was
found between 0.7% and 0.86%. Ca was estimated
titrimetrically.
[5] Cr Concentration :
Cr was determined by Bureau of mines in the
ash of two Pennsylvania bitunimous coals. One ash coal
sample from Washington country contained 0.019% Cr^O,
in the ash. Another sample from Cornbria county,
contained 0.039% 0\ 03 in the ash. [54], Cr concentration
in North Dakota lignite is found to be 65 ppm . [55]
Swanson et.al. [48] 63 have reported Cr concentration in
U.S. coals as mentioned below :
Coal Type Cr. concentration
Anthracite - 20 ppm.
Bituminous coal - 15 ppm.
Sub-bituminous coal - 7 ppm.
Lignite - 20 ppm.
Cu in U.S. coals has on average concentration of
19 ppm. [5b]. 1'he highest concentration of (27 ppm.) is
found in anthracite [57], 'I'he worldwide average is 15
ppm. [58]
Se Concentration :
Se in U.S. coals was discussed in reports bv
Zubovic et.al. [61] and Gluskoter [62]. Se is most stronglv
enriched of all the elements. Se is present in both organic
and inorganic combination in coals. Se in Xorth Dakota
lignite was determined bv Sommerville and Elder [63]
to be 0.85 ppm. (average value for 12 coal samples)
Mo Concentration :
Ternieulen [64] discussed the occurrence of Mo
in coal and some plants. Mo in coal in England, Xew
Castle is 0.033%.
L’nashed coal samples were digested by 11X0,
and analysed for Cd and Zn concentration by atomic
absorption spectroscopy. The results of analysis were.as
mentioned below. [65]
Cd - 0.3 to 28 ppm.
Zn - 18 to 300 ppm.
Schultz el.al. [66] have reported Cd
concentrations in pitts bury seam, coal to be 0.14 ± ppm.
Pb Concentrations :
Sawanson V.E. et.al. [67] have examined samples
of coal and ash deposits from a boiler bv Chemical and
spectroscopic methods, concentration have been reported
to be from 0.0001 to 0.00461 bv Dunn and Bloxam. [68]
Pb contents of coal, coal ash and flyash were
recently discussed bv Block and Dams. [69], simple
gravimetric method and atomic absorption spectroscopv
were emploved in the present work. Pb in U.S. coals came
within the range (in ppm.) 0.37 - 86, 0.78 - 59, 1.4 - 17,
1.5-8 in Appalachian Interior province, N. Great plains
and North Dakota coals. [70] [71],
COAL - UTILIZATION
Combustion converts the organic part of coal to
CO., and water and the non volatile inorganic constituents
to coal ash residues. Loevblad [72] has presented data
for ash, volatile compound and ’S’ content and heat of
combustion of coals of different origin, in the table
below :
Table No. 8
Ash, volatile compounds, 'S1 content and heat of
combustion of various coals.
Name of country Ash °„ Volatile
compound %
S °« Ileat of
l ombustio:'
Norway 7 39 0.78 8.4
England 9 30 1.12 7.4
U.S. - 35 1.02 8.1
West Germany 5 28 0.85 9.7
Poland - - 0.60 7.1
Soviet Union 15-17 34-35 0.70 7.8-8.0
Davison et.al. demonstration that Pb, Ga, Sb, Cd,
Se, As, Zn, Ni, Cr and S were markedly increased with
decreasing particle size of ashes. [73], The concentrations
of Ga, Ge, Hg, Pb showed approximately 3 fold increase
between the coarse ( 50 mm) and fine (2 mm) flv ash of
Australian coal sources. [74] [75],
Schwitzgebel, K., et al [78] [79] reported the effect
of particle size of flvash on the concentration of 17 tract'
elements as .shown in the table below:
Table No. 9.
D istribution of trace and toxic elements in bottom
ash, fly ash and flue gas.
Element Bottom ash
22.2 %
Flv ash
77.1 %
Flue Gas
A I 22.5 78.8 0.7
Be 16.9 81.0 2.0
Cd 15.7 80.5 3.8
Cr 13.9 73.7 12.4
Cu 12.7 86.5 0.8 :
Element Bottom ash Flv ash Flue Gas
22.2 °o 77.1 °o
Fe 17 71.3 0.8
Pb 10.3 82.2 7.5
Mn 17.3 81.5 1.2
Mg 17.2 82.0 0 bo
Mo 12.8 77.8
■
9.4
Zn 29.4 68.0 2.6
V 15.3 82.3 2.4
Mukherjee and C houdhary [78] have
investigated ash of Indian coals. The major const i tuents
of the ash are SiOn, A l ,O v and Fe. The SiCX/ALO, ratio
in the samples vary between 1.8 and 2.2. Block et al [79]
have studied the concentrations of elements in coal as the
function of ash content of the coal. V and Si increase with
the increasing content of ash. This is not so for Sb and
Cu. Constituents (Wt% of total) of individual ash [Ref.
80] have been described in the table below :
Table No.10
S.N'o. Gravity Fraction SiO, A 1,0, Fe,0, TiO: P A SO-. CaO____ j
1. Overall G.F. 40 18.9 28.8 0.60 0.08 1.63 02 M 1
2. 1.3 G.F. 33.6 18.3 13.6 0.32 0.19 6.19 2.0 4.4
3. 1.3 -1.50 G.F. 45.5 20.2 27.6 0.40 0.23 0.27 - 0.9
4. 1.50-1.80 G.F. 48.6 21.5 22.6 0.62 0.08 0.40 - 0.7
5. 1.80 (Sink) G.F. 53.2 25.8 13.2 0.67 0.07 0.46 - 1.0
(G.F. = Gravity Fraction)
Average trace element content in ash
(Concentration in ppm .) of coals from different U.S.
regions [81] are shown in the table below :
Table No. 11
Elements Alabama E.kentuckv Medlm Ohio Pasvlvania Tencsst ird'.ana ;
Be 88 20 - 9 8 h 2̂ \'
Cr 207 260 140 235 244 200
i
182
Cu 150 156 75 80 125 U p ̂I I
Pb 40 59 10 43 52 “> i i r> S
Li 812 1 Or 4 140 ?u4 r42 - -t
Mo 117 “1 17 -t ~ s. S . 4”
Zn 243 203 200 284 242
Concentrations of trace and toxic elements
(in ppm.) in coal, and ashes are as mentioned in the
table below :
Table No. 12
Concentration of trace and toxic elements.
(Concentration in ppm.)
Element Coal Bottom Flvash from
precipitator
Be 1.5 5 6
Cd <1 <0.7 <1.6
Cr 4 20 60
Cu 14 53 80
Pb 6.3 26 62
Se 2.7 1.5 6.6
Zn 6 <10 100
Li 50 200 200
Ash has acid insoluble fraction and acid soluble
fractions [82] as described below :
Table No. 13.
Acid Insoluble
fraction
Acid soluble
fraction
S iO , 38.38 to 53.48 0.82 to 0.88
A1,0, 10.13 to 21.80 2.61 to 6.32
Fe.O, 0.88 to 1.09 2.74 to 5.03
T i0 2 0.96 to 1.43 0.40 to 0.42
CaO 1.16 to 1.38 9.42 to 21.65
M gO 0.36 to 0.42 2.57 to 2.97
k 2o 0.31 to 0.61 0.02 to 0.04
Total °o 52.81 to 81 S O , 1.11 to 2.30
M g 0.45 to 6.8
Total 47 to 41.58
Chem ical concentration of trace and toxic
elements in flyash [83] is mentioned below :
Table No. 14.
Element % Range
.... . . . . t
Average
A1 0.1 - 17.3 1 1.7
Si 19.1 - 28.6 26.6
Ca 0.11 - 12.6 4.4
Mg 0.04 - 6.02 0.9
Na 0.01 - 0.66 0.6
K 0.19 -3.0 0.8
Fe 1 - 26 4.1
S 0.1 - 0.5 ' 0.2
Element (ppm.)
Be 3 - 7 5.5
Cd 0.7 - 130 1.0
Cr 10 - 690 54
Cu 14 - 1000 63
Pb 7 - 279 48
Li 50 - 1064 70
Mo 7 - 117 10
Se 0.2 - 134 / .6
Zn 36 - 1333 72
. [ SO 1
Results ol soil, water, coal and ash analysis, for
trace elements of Bhadra, Bartarai and Amadand projects
haye been described in Chapter-3. Spectrophotometry
and atomic absorption spectroscopy haye been employed
according to their feasibility and suitability for different
trace and toxic elements.
★ ★ ★ ★ ★
r " _ ”
REFERENCES s________ _ _____ ____>
Averitt, P.; Hatch, J.R.; Swanson, V.E., Breger, I.
A. Gluskoter et.al. (1976) : Minor trace elements
in coal..... Eng. U.S. Geol. Survey Report 76 -
481 pp. (1976).
Ignsiak, B.S., Ignasiak, T.M. and Berkowitz.
(1975) .Advances in coal analysis, Rev. Anal.
Chem., 2, 278, (1975)
Konieczvnski, J. (1969) : Problems of micro
element analysis in coal and its dye products,
Koks Smola, Gaz, 14, 13 (1969).
Hattman, E.A., Schultz. H. and Me. Kinstrv W.E.
(1977) : solid and gaseous fuels, Anal. Chemistn
176, (1977).
Gluskoter, H.J. (1977) : Illinois state Geol survey,
circular 499, Trace elements in coal, occurrence,
distribution (1977), pp. 154.
Korz, C., Jr., Ed. (1978) : Ana. Methods tor coal
and products Acad. Press. New York. (1978)
Pollock, E.N. (1975) : Trace impurities in coal In
wet Chemical methods, Adv. Chem. Ser. 141/23,
(1975)
VVererka, E.M., Williams, J.M. and vvonck, P.l
(1976) : Assessment and control of Env.
Contamination from trace element from ERDA.
Res. Abstr. Mo. LA-UR-76-87 (1976),7.
Simon, F.O. and Huffm an , C., Ana. (1977) :
Methods used by the U.S. Geo. survey .... Am
Chem. Soc. Divpet. Chem. Prep. 22, 580 (1977).
Slates, R.V. (1977) :Methods of analvsis for tract
elements in coal, flvash, soil and plant samples,
ERDA, Energy Abstract. Rev. (1977) .Abstract
Ik1 m as B., A (1968) : new method tor
decomposition and comprehensive analysis ot
silicates bv AAS, Anal.Chem., 40, 1682, (1%S).
Bernas B., A (1968) : new method tor
decomposition and comprehensive analysis ot
silicates bv AAS, Anal.Chem., 40, 1682, (1968).
Rantola, R.T.T. and Loring D.H. (1973) : New
low cost Teflon deco. ressel., Atomic abso. \ew
letter, 12, 97, (1973)
Buckley, D.E. and Cranston, R.E. (1971) : AAS
Analvsis from , single deco. of alumino silicates.
Chem. Geol, 7, 273, (1971).
Dreher, G.B. and Schleicher, J.A. (1975) : Trace
elements in coal bv optical emission spectroscopv,
Adv. Chem. Ser. 141, 35, (1975).
Gluskoter, H.j. (1977) : Illinois state Geo survev,
circular 499, Trace elements in coal, occurrence
and distri. (1977) pp. 154.
Simon, P.O. and Huffman C. (1977) : Analytical
methods used bv Geo. Survey ........ An. Chem.
Soc. Div. Pet. Chem. prop., 22, 580 (1977).
Ignasiak, B.S., Ignasiak, T.M. and Berkowitz, H.
(1975) : Advances in coal analysis, Rev. anal
Chem., 2, 278 (1975).
Konieczvnski, j. (1969) : Problems of micro
elements analysis in coal, KOKs, Smola Gaz, 14,
13 (1969).
Gluskoter, H J. (1977) : Illinois state Geo. Survey
circular 499, Trace elements in coal, occurrence
and distribution (1977). pp. 154.
Carr., C., Jr. (1978) : Ed., Analytical methods for
coal and coal products, Acad, Press, New York
(1978).
Slates, R.Y. (1976) : Methods for analysis of trace
elements in coal, flvash, soil and plant samples.
ERDA, Energy Res. Abstr. (1977). Abs. \o.
25780, Report No. D.P. 1421, (1976), 21.
Bernas, B.A. (1968) : new method for
decomposition and comprehensive analysis of
silicates bv A AS. Anal. Chem. 40, 1682 (1968).
H ubbard , D.P. (1971) : A nnua l reports on
analytical atomic spectroscopy, Vol. 1, Society for
Anal.Chem. London. (1971).
Pollock, E.N. (1973) : Trace impurities in coal,
An Chem. Soc. Div. Fuel. Chem. Prep., 18, 92,
(1973).
Simon, P.O. and Huffman, (1977) : C, Analytical
M ethods used bv the U.S., Geo. Survey cu
determining the chemical compounds of coal
An., Chem. Soc. Div. Petr. Chem. Prop, 22, 580,
(1977).
Cavallaro j.A., Deubrouck A.W., Gibbon. J. et.al.
(1978) : W’ashabilitv and analytical evaluation
of Potential Pollution----- Analytical methods.
Coal, pp. 1, 435, (1978).
Slates R.V. (1977) : Methods for analysis of trace
elements in coal, flvash, soil, plants from E, RDA
Energy Res. Abstract. (1977) No. 25780. Report
No. pp. 1421.
Song. M.K. Adam, N.F. and Rinder Knecht, H
(1976) : A simple and highly sensitive mothod
of colorimetric Estimation of Zn, Am. J.Clin.
Pathology, 5 22 (1976).
Snell, F.D. and Snell, C.T. (1959) : Colorimetric
methods of analysis vol.II A., Nostrand Inc. New.
jersv. p. 91 (1959)
Saltzman, B.E. (1952) : Micro determination of
Cr with diphenyl carbazide by parmangnate
oxidation, Analytical Chem., 34, 1016 (1952).
Silt'll, 1;.D. and Snell, C.T. (1959) : colorimetric
methods of analysis vol.II A., Nostrand Inc. New.
Jt'i-sv. p. 91 (1959)
Vogel, A.I., Determination of Mo, text book of
quantitative Inorg. Analysis, ELBS. London
(19b8)
SiIl,C.\\'. and Peterson, H.E. (1954)
Determination of Se, Mines report No. 5047
(1954). U.S.A.
Bown, H .J.M . and Cowse, P.A. (19b2)
Determination of Se, Analyst 88, 721, (1962).
Schrenk, W.T. and Browning, B.L. (192b) : f Am
Chem. Soc., 48, 2550, (1926).
Barabas, and Cooper W .C . (195b) Se,
Aanalvtical Chem. 28, 129, (1956).
Bara bos, S. and Bonnet, (1963) . St', Anal. Chem.
35, 125 (1963) P.W.
Mellichemp, J.W. (1954) : Spectroscopic,
determination of Se, Applied spectroscopy, Dtmn
S<', 8, 114 (1954)
Dingwall, D. and Williams, W.D. (1961) : Se, J.
Pharm and Pharmacol, 13,12,(1961).
W atk in^on , J.H. (1960) : Use of E D I A for
increasing sensitivity of analysis. Anal Chem.,
32 981, (1960).
Christian, G.D., Knoblock, E.C. and Pardv, W.C.
(1965) : on determination of Se, JAOAC, 48, 877,
(1965).
Workshop on coal survey tech. at Bilaspur. (1996)
CFRI Unit (C.S.I.R.) Ministry of Sc. and Tech.
Govt of India.
[ M ]
Gorman J.Y., W alker, P.L., Major Minerals in coal
Fuel, 52, 71, (1973).
U.S. National committee for Geochem. National
Acad, press. Washington D.C. (1980).
U.S. National committee for Geochem. National
Acad, press. Washington D.C. (1980).
Sommerville , M.FL and Elder, J.L. (1977) :
Comparision of trace element analysis. Report
EPA, 600/7 - 78 - 063 Ayer G.A. and Masoglia
M.F. Eds. Washington D.C., (1977).
Burchett, R.R. (1977) Coal resources of Nebraska,
rep. N.P. 23879, Univ. of Nebraska, Lincoln
(1977).
Wewerka, E.M., W illiam s, J.M. and Vander
borgh, N.E. (1976) : Contaminations in coal and
coal residues, 4th national conf. and Env. LA -
OR, 76 - 2197, Los Alamos. Sri. Lab. NM. (1976), 23.
[50] Cooley, S.A. and Ellman, R.C. (1975) : Analysis
of coal and ash from lignite and Sub. bituminous,
coal from eastern montana, 22nd Annual publ.
Geol. Soc. 1975, 73.
[51 ] Burchett, R.R. (1977) Coal resources of Nebraska,
rep. N.P. 23879, Univ. of Nebraska, Lincoln
(1977).
[52] Burchett R.R. (1977): Coal resources of Nebraska
Rep. N.P., 23879, Univ. of Nebraska, Lincoln
(1977).
[53] Wewerka, E.M., Williams J.M. and Wanek, P.L.
(1976) : Assessment and control of Env. conta.
from trace elements in coal processing vaste.
ERDA, Energy Re. LA /U R - 76- 86, 1976.
Gibson, F.H. and Solving W.A. (1944) : Rare and
uncommon chemical elements in coal, Tech. pap. 669,
US Burcan of miner, Washington, D.C. 1944, 23.
Thiessenn, G. (1945) : Cr determination in coal.
In Chemistry of coal, utilization, Vol. I, J.Wilev
and Sons. New York (1945). 425.
U.S. national committee for geochem.................
related to envi. quality and health, natio. acad.
press. Washington D.C. (1980).
Swanson, W .E., M ed lin J.H. Et.al.(1976) :
collection, chemi. Analysis and evaluation of coal
in 1975, open file rep., 76 -488- US Geo survev,
Reston, Va, (1976), 503.
Sorenson J R., Kober T.E. and Petering H.G.
(1974) : concentration of Cd, Cu, Fe, Ni, Pb, Zn
in Bitu. coals. Am. Ind. Hvg. Assoc. J. 35, 93
(1974).
[59] Somerville, M.H. et.al (1977) : Comparision of
trace elements Ayer. G.A. and Massoglia, M.F.
eds. Proc. Svmp. env. aspects of fuel conser. Tech.
Rep. EPA, 600/7 - 78 - 063. Washington D.C.
(1977).
[60] Somerville, M.H. et.al (1977) : Comparision of
trace elements Ayer. G.A. and Massoglia, M.F.
eds. Proc. Symp. env. aspects of fuel conser. Tech.
Rep. EPA, 600/7 - 78 - 063. Washington D.C.
(1977).
[61] Zubovic, P. Hatch. J.R. and Medlin, J.H. (1979) :
Assessment of the chemi. compo. of coal in proc.
U.N. sympo, world coal prospects katowice, 15-
23-10, (1979) 68.
[62] Gluskoter, H.J. (1977) : Trace elements in coal,
occurrence and distribution, Cir, 499, Illinois
state, G.S. Urbana, p. 154. (1977).
Ondov, I.M., Ragaini R.C. and Bier m a im A.H.
(1979) : Emissions and particle si/.e distributions
of m inor and trace elements ..........
Environmental, sci.. Tech., 13, 946, (1979).
Termeulen, H. (1932) : D is tr ibu t ion of Mo,
Nature, London, 130, 966, (1932).
Thilo, E. (1934) : Results of Analysis of two coal
ashes, Zeit, inorg. Allem., chem. 218, 201, (1934).
Zubovic, P. Hatch J.R. and Medlin. J.H. (1979) :
Assessment of the Chem. compo of coal resources
in proc. U.N. sym. world coal process, Katowice
15-23-10, (1979), 68.
Swanson Y.E., M ed lin J.H. et.al. (1976) &
Collection, Chemical analysis and evaluation of
coal samples in (1975). Geological Survev Reston.
Ya. 1976. 503.
D u n n , |.T. a n d B lo x a m H .C . I , ( l c>32) . I 'he
presence ot Pb in the he rbage a n d soil l a nd s
ad jo in ing coke ovens |. Soc. chem. Ind., 31, 100
T, (1932).
Billings, CM:., Sacco, A.M. Matson, W.R. et.al.
(1973) : Ilg balance on large scale pulverised,
coal. j.A ir Pollution control, Assoc., 23, 733,
(1973).
Gluscoter, H.J. (1977) : Trace elements in coal
occurrence and distribution, Cire, 499, Illinois
state, Geo survey Urbana, P 154 (1977).
Jubovic, P., Hate. J.R. and Medlin J.H. (1979) :
Assessment of the chemi. compo. of coal resources
in proc. U.X. World coal prospects, katowice, 15
- 23, 10 1979, 68.
Loevblad, G. Ed. (1977) : Trace element conc. in
some coal samples ....... in Sweden, Report, IV
L-B-35S (1977).
Davison, R.L. Xatusch, DI;S, Wallace l.R. and
Evans C.A. (1977) : Trace elements in tlvash, env.
sci. tech. Ind. Rs. Bull., 218, 127 (1977).
Swaine, D.J., Trace elements in flvash, XV, Rep.,
Sci., Ind. Res. Bull, 218, 127 (1977).
Swaine, D.J. (1977) : Trace subst., Environment
and health, 11, 107, (1977).
Ondov, J.M., Ragaini R.C. and Bier mann, A.M.
(1979) : Emissions and particle size distributions
of m inor and trace elements ...........
Environmental, sci.. Tech., 13, 946, (1979).
Ondov, J.M., Ragaini R.C. and Biermann, A.El.
(1978) : characterization of trace elements
......... from energv Res. abstr Xo. 29344, (1978)
Report Xo. UCRL - 80412, (1978), 21.
Mukerjee, D.K. and Choudharv P.B. (197b) :
Catalvtic effect of mineral matter constituents in
North Assam coal, Fuel, 55,4, (1976).
Block, C , Dams R. and Floste. ]. (1976) : Chem.
Composition of coal and flvash, Meas, Retect,
control environmental pollution, proc. Int. symp,
international atomic energv Vienna, (1976) 101.
Block, C , Dams R. and Hoste. J. (1976) : Chem.
Composition of coal and flvash, Meas, Retect,
control Environmental pollution, proc. Int. svmp,
international atomic energv Vienna, (1976) 101.
Abernethv, R.F. Peterson, M.J. and Gibson, F.FI.
(1969) : stereochem, ana of coal ash for trace
elements, U.S. Bureau of mines, Rep Invest, 7281,
30, (1969).