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KEY I
I
Main outcrops of
Carboniferous limestones
.Motorways f
Trunkroutes,majorroads
Railways
. . . .. . . . . . National Park
boundary
NOTTINGHAM
9 0 1 2 3 4
Fig. 1. Localitymap
2
Borehole
lnsolubles %
1 2 3 4 5
-depth (m)
Collected
- section
Insolubles%
-1 0
..........................
-1 5
. . . . . . .
-20
0
-25
0
0
-30 0
/ Sect ion
ends at 23m
-35
KEY:
-40
. . Pellets
-
Y Y Y Y Y
cI Brachiopod shells
0 0 Crinoid debris
o( Encrusting Algae (includes Girvanella )
-45
A A Algae (Dasycladaceae)
0 0 Chert
SI SI Silicified shell
-50
1-1 Pale limestone
............
.............
*
............
...........
............ Dark limestone
...........................
.........................
.........................
.........................
...........................
.........................
..........................
.........................
.........................
..........................
.........................
-55
k + + + + + + + +
-60
Borehole
completed
at 60.91
m
3
7
-1 0
- 20
-30
-40
Fi
(il
lithostratigraphy. Since the recognition of beds depths of about 61 m (approximately equivalent
l e s s than half a metre thick is of paramount to the depth of the deepest working quarries at
importance in establishing lithological correlations, the time of survey); three deeper boreholes were
p r o b l e m s a r i s e in using sections because of their drilled for stratigraphical purposes, the deepest
irregular geographical distribution and, more being taken to almost 210 m. The combination of
particularly, the occurrence of numerous small relief and the OD level of the topographically
gaps in even the best examples. Other problems lowest borehole resulted in samples being
include the inaccessibility of some cliff and obtained from a vertical interval of about 300 'm.
quarry faces and the danger and cost of handling For limestone resource assessment generally,
the large blocks of stone necessary to obtain the minimum depth to which drilling should be
fresh material. It has been concluded that taken depends on the structure, stratigraphy and
resource assessment should be based upon a topography of the area being assessed, on the
complete succession established by drilling and projected maximum quarrying depth and on the
augmented by samples from sections. The number feasibility of mining; current surveys are based
of boreholes required will depend upon the upon the need to collect data to depths of 100 m
geographical and stratigraphical distribution of from the surface. The variation in structure and
the sections and the structural and sedimentary stratigraphy from one area to another suggests
complexity of the area. that the assessment of a 1:25 000 sheet should be
conducted in two stages. The first should involve
SPACING OF T H E SAMPLING POINTS the drilling of key boreholes (say 5 o r 6 on
Although particular emphasis during this study average) and the collecting and the laboratory
has been placed upon the regional variation of processing of material from natural and quarry
calcium carbonate content within the rocks, other exposures. The need for further drilling, if any,
properties were recorded. For example, in in a second stage will be indicated by the results
addition to lithostratigraphy, insoluble residue of the first.
and loss-on-ignition, which relate directly to
carbonate content, other data recorded include FIELD L O G G I N G
strength index, non- carbonate mineralogy, trace - A preliminary lithological log was prepared on
element content and colour values. To map the site and was used as a reference aid and
distribution of all these properties adequately supplement to the laboratory log. Two simple
would require a different sampling grid for each, strength tests were investigated in the field, a
determined by either a specifically designed point-load strength test and a stamp-mill test,
experiment or prior knowledge of s i m i l a r r o c k s (Franklin and others, 1971; Protodyakonov, 1963;
from comparable areas. For some the frequency Brook and Misra, 1970) and it was concluded that
of sampling required could be prohibitively the former was the more suitable. The structural
expensive. Because of the financial restraints on homogeneity of the limestones was assessed by
a publicly funded resource investigation, the measuring the frequency of naturally occurring
minimum sampling interval compatible with f r a c t u r e s s u c h as joints and bedding planes, which
producing useful results must be established. was expressed quantitatively as a f r a c t u r e -
This has been determined by comparing the spacing index.
r e s u l t s f r o m b o r e h o l e s with spacings ranging
f r o m 1 to 6 km. Fig. 3 shows an optimum Laboratory programme
correlation using irregularly spaced boreholes
and demonstrates that boreholes up to 6 k m a p a r t In the course of the feasibility study, laboratory
may be satisfactorily linkedby means of lithology t e s t s were undertaken to examine the mineralo-
and insoluble residue data. It is concluded that gical, chemical and physical properties of the
the lithological, mineralogical, chemical and limestones. This information was used for
physical variation of the rocks studied would have classification, to determine regional trends and
been adequately detected by boreholes spaced to indicate the suitability of the rocks for particular
approximately 6 kmapart.However,optimum end uses.
conditions rarely apply and a 3-km interval w a s The following procedures were followed:
chosen to provide an increased number of data Petrographical logging
points. From this it follows that 11 o r 1 2 equally Carbonate determination by:
spaced boreholes would be required to cover the a insolubleresiduemeasurements
a r e a of one 1:25 000 sheet (100 km2) with b volumetric determination of carbonate
limestones of similar lithological variation. c loss-on-ignition
Generally, material for lithological, mineralo- Mineralogical examination of the insoluble
gical and insoluble residue determinations was residue using petrographical and X-ray methods
obtained by sampling from every metre in Use of stains to determine carbonate
exposed sections. In the case of a borehole, the mineralogy
core was sawn in two; one half was etched and Automated chemical analyses of powdered
used to prepare a detailed lithological log, and samples
the other was crushed in metre-lengths to provide Measurements of the colour reflectance of
bulk samples for the determination of insoluble powdered samples and etched limestone
residues, chemical analyses, reflectance values Comparison of mechanical testing methods:
and mechanical properties. a point-loadtest
The area studied has a 250 m variation in b stamp-milltest
topography and most boreholes were drilled to c aggregate-impact value test
5
DETAILED PETROGRAPHICAL LOGGING 10-50 per cent Dolomitic limestone
To examine the limestone samples, all m a t e r i a l 51-90 per cent Calcitic dolomite
frQm boreholes and sections was sawn and etched >90 per cent Dolomite rock (commonly referred
in hydrochloric acid to remove s a w marks and to to as dolomite)
clean the surface. This proved to be a highly
satisfactory way of revealing lithology. Acetate
peels were prepared at this stage, for use as a
logging aid and as a r e c o r d of the original samples.
The samples were examined systematically
using a binocular microscope and thin sections SYSTEMATIC CARBONATE DETERMINATION
were made when required. The petrographical Carbonate content is fundamental to a wide range
t e r m s u s e d a r e b a s e d on Folk's classification of limestone uses. A simple method for deter-
(Folk,1959; 1 9 6 1 ) (Table 1). The results were mining the carbonate content of large numbers of
presented as written and graphical logs (Fig. 4) sampleshad,therefore,tobeselected.Ideally
and were the basis of a correlation of the rock the method should be rapid, accurate, easy to
sequence. use (preferably by semi-skilled staff), not subject
If the rock contains significant (>2 5 per cent) to operator error and should be capable of giving
quantities of allochems, which are not mentioned reproducible results.
in the main rock name, they may be shown as
qualifiers before the rock name and have a capital Insoluble residue
letter,egCrinoidalbiosparite.Subordinate This method for the determination of carbonate
diagnostic allochems also precede the main rock content is widely used in industry and has the
name; these are differentiated by use of s m a l l m e r i t of providing samples of the non-carbonate
initial letters, eg algal Brachiopod biosparite. fraction for mineralogical examination. Initially
Folk's grain-size classification has also been in this study, chip samples were taken at metre
adopted and may be incorporated into the rock intervals and the proportion of chert was
type (eg Biosparrudite, Biomicarenite etc). calculated separately by direct measurements on
The pure mineral dolomite (CaMg( C O Q ) ~ ) , the core. It was subsequently decided that
contains 21.9 per cent MgO and 30.4 p e r c e n t sampling would be more representative i f the
CaO(= 54.3 per cent CaC03). Rocks containing core were crushed in metre lengths and sub-
more than 1 0 per cent of dolomite a r e c l a s s i f i e d samples taken for each test using a laboratory
a s follows: splitter.
RESOURCE BLOCK A
Sheet number site ref A
Surface level+ 385.3m (+ 1264 ft) NW 13
Relch (airflush), 74 m dlameter
Harch 1971
Thickness Depth
(metres) (metres)
INSOLUBLE
Tops011
Limestone
Openhole
to 1.1Om. algal
10.0
3.18
1.00
4.18
LITHOLOGY COLOUR MECHANICAL PROPERTIES RESIDUE DATA
PURITY
crinoid
subordlnate an-bris, +, + + + + + +
*+++++++
pyrlte present ln increasing amounts
towards base
Altered
Pale
grey-green, firable at
top
with 1-49 31 -00
Lava
amygdales
pyrite
and
streaks
alteredAmygdalesbecome less commonatdepth 2.16+ 33-16
Lava
33.1h
Borehole completed at
6
Because it w a s established that there is good
agreement (Fig. 5) with the residues calculated CHEMICAL ANALYSES
from conventional chemical analyses, minor Detailed chemical analyses are necessary when
discrepancies falling within the errors of the a range of industrial uses is being considered,
various analytical methods employed, the number Most uses are governed by total carbonate content
of more expensive chemical analyses can be and by the proportions of various other elements
reduced. The distribution of insoluble residues and minerals, which may be beneficial o r
from several boreholes, shown in Fig. 3, deleterious.Forexample,limestonescontaining
indicates the additional usefulness of this method metals that impart colour are unsuitable for use
as a correlation tool. in the manufacture of good quality glass; lead
and arsenic must be monitored in rocks used in
Volumetric determination of carbonate the production of animal feedstuffs o r f o r s u g a r
British Standard 1795 (1965) gives a description refining. The samples selected for full chemical
of this method in which carbonate content is analysis were taken to represent the full range of
determined from powders. This method is m o r e , rock types present, as indicated by the laboratory
rapid than the insoluble residue technique and logs and the carbonate determinations. Analyses
r e s u l t s w e r e found to be reproducible, but the were made using direct electron excitation X-ray
s c o p e f o r o p e r a t o r e r r o r is s i m i l a r in both cases. spectrometry for Na20, MgO,Al2O3, Si02,
P2O5, SO3, K20, CaO, Fez03 and F; other
Loss-on-ignition elements were determined by atomic absorption
Following an established technique (Galle and spectrophotometry (Roberts and Davis, 1 9 7 7 ) .
Runnels, 1 9 6 0 ) , selected powdered samples were These provided a 'background' level of t r a c e -
heated to 550" C to drive off carbonaceous material element chemistry but, because of the relatively
and water, and the temperature then raised to wide spacing of boreholes, localised variations in
1000" C to release C02. The loss of weight during the concentration of industrially significant
the second ignition can be used to calculate the elements w i l l not be recorded. Table 2 shows a
percentage CaC03. The method gives relatively typical analysis for an assessment borehole.
accurate results, even with the darker coloured
rocks, which contain considerable impurities, COLOUR MEASUREMENT
This technique gives reproducible results and is Objective colour measurements are a valuable
simple and rapid. However, it is impractical for aid to correlation between cores. In addition,
the large number of determinations required. colour determines whether powdered limestone
The insoluble residue method has the advantage can be used as a whitening agent. Discs of
of providing information on the nature of the powdered ( < 6 3 ~) v e r y high purity limestone
mineralogy of the non-carbonate fraction, and is (Table 5) were prepared using a Leitz Elrepho
suitable for large batch work. It was therefore press and their reflectance was measured with a
decided to use this method. Recent research reflectancespectrophotometer. A white
(Molinia, 1974) has shown that filtration may be magnesium carbonate standard (percentage
used to determine insoluble residues. Micro- reflectance = 100) was used to calibrate the
cellulose filters are used to trap the residue from equipment. The following three systems of colour
a sample of powdered limestone of known weight measurement were tried using different filters,
which has been dissolved in N / 1 0 hydrochloric 1 Filters approximating to X Y and Z wavelengths
acid. This method combines the advantages of (Kaye and Labey, 1973) were used to calculate
the classical method of insoluble residue deter- the Commission Internationale de LIEclairage
mination with a v e r y high throughput. It has (C. I. E. ) coordinates. Unfortunately, a plot of
therefore been adopted for use in more recent X and Y on the chromaticity chart locates all
surveys. the samples in the same area near the source,
because all the samples are grey o r white in
MINERALOGY OF T H E N O N - C A R B O N A T E colour.
FRACTION 2 The colour index (CI) system was evaluated
Initial mineralogical determination of the insoluble according to the formula
residue was by optical microscopy, followed by
analysis using an X-ray diffractometer. Results Red - Blue x 100 = CI
have indicated the presence of chert, clay-grade Green
quartz, baryte, pyrite and various clay minerals,
a l l of which are important in determining possible This index is used in industry to distinguish
uses for the rock. As t,he insoluble residues are between whites but it was found to be
now retained on filters they can be readily stored incapable of separating shades of grey,
and used for X-ray studieswhen necessary. 3 Tri-colour reflectance measurements using
f i l t e r s with wave-lengths of 660 nm, 520 nm
STAINING and 470 nm were made both of powders and
The staining of limestones to determine their etched rock surfaces.
carbonate mineralogy is a well-established The tri-colour reflectance method gave a
technique (Dickson, 1 9 6 6 ) , which is used primarily s c a t t e r of r e s u l t s which allowed a reasonable
to determine the presence of dolomite, ferro- classification of the samples measured and it was
dolomite and ferrocalcite. This process is concluded that this system was the most suitable
now used only where dolomitis'ation is suggested for limestone assessment work. A s u m m a r y of
by the petrographical study. values obtained by this method on very high purity
7
Table 1. Classification of limestone rocks (based on Folk, 1959)
T LIMESTONES
Intraclasts:
lntramicrite
lntrasparite Intractastic
(rare) micrite
( rare)
Oomicrite Oolites
Oosparite ( rare) Ool i t i c m i c r i t e
(rare)
Fossils: Micrite
Biosparite Biomicrite Fossiliferous
Micrite
Biopelsparite Biopelmicrite
Pel lets:
Pel l e t if erous
Micrite
Pelspa r i t e Pelmicrite
Depth C
(metres)
-
%INSOLUBLE
1
RESIDUE
2 3 4 5 6
0
%INSOLUBLE
RESIDUE
10 10
20 20
3c 30
40 40
50
6C
i A
50
60
1.10 0.01 0.38 0.13 1.54 0.04 0.32 0.02 54.20 tr 0.03 43.33
3.90 0.01 0.34 0.09 1.63 0.03 0.35 0.02 54.35 tr 0.00 43.1 6
5.85 0.00 0.21 0.03 0.45 0.04 0.3 6 0.01 55.20 tr 0.00 43.71
9.00 0.00 0.22 0.05 1.49 0.04 0.32 0.01 54.40 tr 0.01 43.09
11.00 0.00 0.22 0.04 0.98 0.05 0.34 0.01 55.15 tr 0.02 43.51
12.00 0.00 0.23 0.06 1.25 0.05 0.32 0.01 54.75 tr 0.04 43.22
14.00 0.00 0.22 0.03 1.01 0.04 0.32 0.01 55.15 tr 0.00 43.26
16.00 0.00 0.23 0.03 0.83 0.03 0.26 0.01 55.10 tr 0.00 43.49
19.00 0.03 0.25 0.04 1.39 0.04 0.37 0.01 54.65 tr 0.00 43.31
21.00 0.00 0.23 0.04 0.62 0.03 0.30 0.01 55.00 tr 0.01 43.69
22.00 0.00 0.25 0.03 0.63 0.03 0.26 0.01 55.00 tr 0.00 43.74
24.00 0.00 0.20 0.01 0.40 0.03 0.23 0.01 55.10 tr 0.00 43.82
26.00 0.00 0.29 0'. 20 0.55 0.03 0.26 0.02 54.65 tr 0.00 43.73
27.00 0.00 0.31 0.12 1.oo 0.03 0.22 0.01 54.60 tr 0.00 43.52
28.90 0.00 0.27 0.23 0.58 0.03 0.23 0.03 54.40 0.48 0.00 43.43
t r = trace
Maj = Major
I1 11
11 11
9
powders is given in Table 3. this value is defined as the rock impact hardness
number (RIHN) (Brook and Misra, 1970). It was
MECHANICAL TESTZNG METHODS found that the values obtained were reproducible
and could be correlated with particular lithologies
Point-load test (Table 4; Fig. 7). In particular there was a
Samples representing a wide range of limestone strong correlation between grain size of allochems
lithologies were taken at 1-m intervals from and RIHN.
borehole cores and tested diametrally to failure
between conical platens. The point-load strength Table 4. Mean rock impact hardness numbers
index (Is) determined by this method gives a (RIHN) for typical limestone lithologies
m e a s u r e of tensile rock strength. The histogram
(Fig. 6) plotted from all the observations shows L itholo gy Carbonate type Mean RIHN
a slightly skewed normal distribution with a mode
between 4.0 and 4.5 MN/m2, but a mean below 1 Dark Micrite 44.02
4.0 MN/m2. This indicates either that the
limestones have a fairly uniform strengtho r that 2 Pale Micrite 38.90
the testing method is insensitive to lithological
variation. The particular value of t h i s t e s t is 3 Dark Biomicrite 38.26
that it may be carried out easily and cheaply in
the field. Research by the Engineering Geology 4 Sorted Fine
Unit of the Institute has failed to confirm the Calcarenite 31.80
relationship claimed (Franklin and others, 1971)
between Is values and compressive strength. 5 Sorted Medium
However, there a r e indications (Dr N. Brook, Calcarenite 28.80
personal communication) that laboratory tests for
compressive strength have a low reproducibility 6 Pale Biomicrudite 28.00
and are therefore unlikely to produce results
which correlate well with those of other tests. 7 Sorted Coarse
Calcarenite and
200
KEY Fine Rudite 25.42
V H Veryhigh strength
H Hlgh strength
M Medlurn strength
Is Corrected strength index
8 Dolomite 23.44
(after Broch 5 Franklin 19721
150
48-
44-
>
z2 100
40-
w
K
36-
R.I.H.N.
32-
50
28
24
20
M I H VH Is(MN/m2) - 8 7 6 5 4 3 2 1
LITHOLOGIES (TABLE 4)
Stamp-milt test
This test involves the comminution of rock
s a m p l e s in a mortar using a falling weight and
was applied in this study to rock cylinders and Fig. 7. Range of rock impact hard-
chippings. The number of blows needed to produce ness numbers (RIHN) f o r typical
25 per cent fines ( <500/1 ) was determined and limestone lithologies
10
Current research at Leeds University Purity values are determined as follows. The
( D r N. Brook, personal communication) suggests insoluble residue measurements (=non-carbonate
that plant and drill-bit wear can be related to fraction) for individual boreholes and sections
RIHN; theindex is, therefore, important a r e grouped into sets representing limestone
commercially. Values can be converted to samples from the uppermost 10 m of rock and
approximate equivalent values of compressive succeeding 5-m depth increments. For each set
strength; in the samples tested maximum and the mean, the standard deviation and confidence
minimum RIHNls of 15 and 44 correspond to l i m i t s a r e c a l c u l a t e d a t t h e 95 per cent proba-
compressive strengths of 80 and 1 9 6 MN/m2 bility level, assuming a student's It' distribution.
respectively. The sum of the mean and positive confidence
l i m i t is subtracted from one hundred to obtain a
Aggregale-impact value (AIV) conservative ( = worst) estimate of the calcium
The AIV t e s t is determined by measuring the carbonate content for each depth increment. This
percentage fines produced by a given number of value is used to assign the limestone within each
blows. The method is described in B r i t i s h depth increment to one of the five categories.
Standard 812 ( 1975) and is s i m i l a r to that of the
stamp-mill test. The repeatability and RESOURCE M A P
reproducibility of the AIV test makes it suitable Although the scale of map selected for the
for use in a regional assessment and since it is publication of these surveys is 1:25 000, it would
also used widely in industry, it has been adapted be possible. to adapt the field procedures and
in a l l c u r r e n t s u r v e y s cartographical techniques described below to
produce either small-scale reconnaissance maps
Preparation of results for publication omr o rdee t a i l elda r g e - s c a laes s e s s m e n t s .
Base map, including contours, is the Ordnance
Information is continuallyaddedtoexistingSurvey 1:25 000 outlineeditionprinted in grey.
geological data from the detailed study and The geological boundaries a r e shown in green
correlation of boreholes and sections, and an (both on the face of the map and in vertical and
improved geological map results. Facies varia- horizontal sections); faults and other structural
tions are defined spatially and stratigraphically f e a t u r e s a r e shown in red. Mineral veins are
and these in turn are related to the economically indicated by lines of alternating red and black.
important parameters recorded. Drift deposits a r e shown in black shading. Shades
When deciding the form the assessment map of blue are used to indicate the categories of
should take, it was necessary to consider which limestone purity in the top 1 0 m.
properties should be displayed and how best to Mineral resource information is shown in shades
show them in map form. Because the carbonate of blue for limestone and green for dolomite. The
content is of paramount importance when category shown reflects information on purity
considering most industrial uses, it was decided determined from boreholes, sections and spot
that the primary requirement is to illustrate its samples, together with other relevant field
distribution. The categories selected are shown observations (eg, presence or absence of chert);
in Table 5. some data may be weighted, by eg, their area of
Asphalt
Low Purity 85-93.5
11
influence. Where more than one category of horizontal sections (Fig. 10) a r e drawn to indicate
limestone occurs within the uppermost 1 0 m, the limestone purity at depth throughout the area.
ground where they overlap (zone of intermixing) The calculated. average purity to 10m is shown,
is shown by alternating stripes of the appropriate but below this depth the limestones are assigned
colour, bounded by a dotted line (Fig. 8). This categories of purity from an interpretation of
'system is also used where 'solid' non-carbonate structural, stratigraphical and lithological data.
rocks dilute overall purity within 10 m of the A graphical section on the left-hand margin
surface, In areas where dolomites occur shows the thicknesses of the beds and their
extensively, zones of intermixing with limestones stratigraphical correlations. The symbols and
can be shown. conventions used are explained in the right-hand
margin.
BROCH, E. andFRANKLIN,J.A.1972.The
point load strength test. Int. J. RockMech.
Min. Sci.. Vol. 9. m . 669-697.
DICKSON, J. A. D. 1966.Carbonateidentification
and genesis as revealed by staining. J. Sedi-
ment,Petrol., Vol.36, No. 2, pp. 491-505.
FOLK, R. L. 1959. P r a c t i c a lp e t r o g r a p h i c
classification of limestones. Bull. Am. Assoc.
Pet.Geol. , Vol. 43, No. 1, pp.1-38.
GALLE, 0. K. andRUNNELS,R.T.1960.
Determination of C 0 2 in carbonate rocks by
controlled l o s s onignition. J. Sediment.
P e t r o l . , Vol. 30, No. 4,pp.613-618.
I
METRES
0-
NW 86 (S)
338.0 1105
- Borehole site
M.A. U. registration number, IS' indicates section
Surface level in metres and feet above O.D. (Newlyn)
%Carbonateand lithology1
2 Cateior y of Lithological Symbols
limestone
Continuous core
Chert
Openhole C!ay wayb oard
Mineralized core Shale 1mudstone
40 Mean insoluble residue shown for Basalt
increments of 5 metres
50 Gap in data
60
+63- Additional thickness of strata proved
1 . In later maps this will be aggregate impact value (A.I.V.) and lithology.
2. Shown by shades of blue on original
400
200
100
0 500 1000m
Vertical Exaggeration 3 - 5 x
Ordnance
Datum
14