MAPAN-Journal of Metrology Society of India

https://doi.org/10.1007/s12647-019-00326-8

ORIGINAL PAPER

A Modified Acid Digestion Method for Analysis of Gold in Geological

Samples: A Comparative Study
P. Ghosh1*, H. Mandal1, B. Sirisha1, U. Sen2, S. Goswami2 and N. V. R. Kiran1
1
Geological Survey of India, Southern Region, Hyderabad 500068, India
2
Central Chemical Laboratory, Central Headquarter, Geological Survey of India, Kolkata 700016, India

Received: 15 November 2018 / Accepted: 22 May 2019

 Metrology Society of India 2019

Abstract: Quantification of gold in geological samples using fire-assay technique is a well-established and recommended
method worldwide. However, the method is laborious, complicated, sluggish, and health hazardous. Only a well-trained
chemist can perform gold analysis through fire assay routinely. Although classical aqua regia digestion for determination of
gold yields high throughput, this method too has disadvantages of sample nature dependency, thus brings down the
recovery levels. Herein, we report a modified aqua regia digestion method, followed by solvent extraction using methyl
isobutyl ketone for the accurate and precise estimation of Au in variety of geological samples of different genre in broad
concentration range. Roasting of sample was avoided and excess of aqua regia (6 times or higher than of sample weight)
was used to bring all gold in aqueous phase. This method was applied to soil and rock samples and the results obtained
were compared with conventional fire-assay technique. The analytical results for international reference materials of gold
(SRM/CRM) measured by the proposed method were in close agreement with those obtained by fire-assay method and
recommended values. Very low detection limits were achieved in the proposed method (1 ng/g by GF-AAS and 100 ng/g
in F-AAS). This method also works satisfactorily at moderately higher concentration of gold in rock samples, at least up to
15 ppm. Thus fire-assay technique may be substituted by the proposed method for detection of Au in 10 ppb–15 ppm
concentration range in the geological samples mentioned under present study.

Keywords: Analysis of gold; Aqua regia; MIBK; Fire assay; GF/F-AAS; CRM/SRM; Field geological samples

1. Introduction complex matrixes has been a longstanding problem due to

Gold (Au) with a mononuclidic and monoisotopic form is
one the least reactive chemical elements and hence often
occurs in native state as nuggets or grains, in rocks, quartz
veins and even in soil. Gold is distributed in a heteroge-
neous manner as discrete particles and minerals like sili-
cates, arseno-pyrites, or in the form of solid solutions in
sulphides and spinels [1]. The average concentration of
gold is not only very low in crust (4–5 ng/g) but also in the
ores [2]. Although gold is found as nugget in many
instances, it can also be found in complex matrixes, e.g.
sulphides, arseno-pyrites. Determination of gold in such
Electronic supplementary material The online version of this
article (https://doi.org/10.1007/s12647-019-00326-8) contains sup-
plementary material, which is available to authorized users.
Haridas Mandal and B. Sirisha have contributed equally to this work.
*Corresponding author, E-mail: prasung86@gmail.com
extremely low levels of leaching [3, 4]. Thus the accurate
and precise measurement of gold is always challenging to a
chemist. Rapid and accurate estimation of low (ng/g)
concentration of gold is essential for geochemical mapping,
whereas moderately high concentrations (lg/g) of gold in
rocks, ores, and other geological materials are required in
exploration studies. These measurements are also helpful to
solve the most attractive problems of geochemistry, e.g.
understanding of the origin of gold in Earth’s crust, its
concentration processes and formation mechanisms of the
deposits [5–8].
A large quantity of the geological samples is generally
used for consistent and reliable results due to the lower
abundance and heterogeneous distribution of gold. It has
been shown that methods using sample weight of 5–20 g
are appropriate for gold exploration studies [9]. Beside
large sample weights, pre-concentration and separation
step is crucial to reach very low detection limit (ng/g)

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 P. Ghosh et al.

[10, 11]. The classical lead fire-assay method is a pre-
concentration and separation technique, used widely all
over the world from historical time and accepted as the
most dependable analytical method for the determination
of Au, especially in gold ore samples. The fusion flux used
in this method is varied to accommodate different types of
samples. This technique uses Pb as a collector for precious
metals which form Au–Ag–Pb alloy. As in this method,
complete fusion occurs at a temperature well above
1000 C, all silicate matrixes rupture and Au separates
along with the collector [10–12]. The key advantage of the
process is its applicability irrespective of matrix nature of
sample. However, the whole method is associated with
complicated and time-consuming steps as mentioned ear-
lier. As a result, this method cannot be adopted for analysis
of large number of samples.
Another popular technique is digestion of geological
samples with aqua regia followed by the extraction of
chloride complex of gold into methylisobutyl ketone
(MIBK), and the gold content is then measured by either
F-AAS or GF-AAS [12–14]. This method is relatively
simple and fast, therefore can be used in routine analysis.
This process in combination of GF-AAS analysis can yield
excellent detection limit (0.5 ng/g) for Au [11–15]. Severe
limitation of this process is incomplete leaching of Au from
sulphide, arseno-pyrites and some other complex matrixes
[15, 16]. As a result, applicability of this technique to all
kind of geological samples is questionable. This creates a
lot of problems in gold ore samples, where Au is primarily
stuck in complex matrixes. Application of this technique to
these samples yields lower analyte value compared to that
of fire-assay technique.
In this paper, we have addressed this issue by adopting a
modified acid digestion process. The poor leaching of gold
may be resulted from incomplete oxidation of gold due to
insufficient quantity of acid which prevents complete
extraction of Au from the complex matrixes. Herein, we
have optimised the required amount of aqua regia to obtain
maximum leaching of Au in solution. The comparative
results obtained from both lead fire assay and modified acid
digestion are found to be well in line for a wide range of
concentration present in various types of geological sam-
ples. The reported studies [17–19] did not include such
wide range of sample genre and broad concentration range
of Au in geological materials used in present study.
2. Experimental Section
2.1. Instrumentation
For this study, a Model Spectra AA 220 (Varian, Australia)
flame atomic absorption spectrometer and a Model Spectra
AA 880Z with GTA-100 (Varian, Australia) graphite fur-
nace atomic absorption spectrometer with Zeeman back-
ground correction were used. Details of instruments are
given elsewhere [20]. The instrumental parameters
(Tables 1, 2) were optimised for maximum absorbance. All
readings were taken up to 0.5 absorbance in both the cases
to retain the linearity of Lambert–Beer’s law.
2.2. International Geochemical Gold Reference
Materials
Rock, ore and soil samples having certified values for gold
were obtained from various international agencies, and the
details are given in Table 3.
2.3. Reagents
The acids and other reagents used were obtained from
Merck, India. All acids and chemicals were Emparta grade.
1000 lg/mL stock solution in 0.1 N HCl as synthetic gold
standard was of analytical standard grade. Whenever
required, the stock solution was diluted stepwise with 2 N
HCl to obtain the desired concentration. Double-distilled
water (18 XM) was used throughout the investigations.
2.4. Field Geological Samples
All the studied samples were collected from different pla-
ces of India, mainly from Karnataka, Rajasthan and Andhra
Pradesh. Some of them were collected through National
Geochemical Mapping (NGCM) program, and others were
collected through different projects undertaken by Geo-
logical Survey of India (GSI) to uncover gold mines. As a
result, a wide variety samples, e.g. soil, rock, core drill,
trench composite, etc., with a broad range of concentration
were obtained and employed for the present study. All the
samples used in this study are geologically very much
Table 1 Operating parameters for GF-AAS
Background correction Zeeman
Measurement mode Peak height
Argon flow 3 L/min
Sample vol. 10 lL
Wavelength 242.8 nm
Slit width 1 nm
EHT 300 v
Lamp current 4 mA
Sampling mode Automix
Drying 120 C (hold for 60 s)
Ashing 700 C (hold for 10 s)
Atomization 2600 C (hold for 2 s)

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A Modified Acid Digestion Method for Analysis of Gold in Geological Samples: A Comparative…

Table 2 Operating parameters for F-AAS with Zeeman background cooling down to room temperature, the volume was made
correction up to 60 mL with 2 N HCl and left overnight to settle
Wavelength 242.8 nm down. 30 mL of the transparent supernatant was decanted
Lamp Current 4 mA and extracted with 5 mL MIBK using separating funnel.
Slit width 1 nm After rejecting the aqueous layer, the organic layer was
Flame type Air-acetylene washed twice with 2 mL 1 N HCl to remove trace amount
Air-flow rate 3.50 L/min of iron or other base metals which were extracted along
Acetylene flow rate 1.50 L/min with gold [26, 27]. Then gold was again stripped back in
Solvent uptake rate 2.5 mL/min 2 N HCl from MIBK layer and final volume was adjusted
Measurement time 5.0 s to 5 mL. This final solution was aspirated in F-AAS/GF-
Background correction D2 lamp
AAS.
Sampling mode Manual
Caution: For carbonaceous and sulphide sample, a small
quantity of aqua regia should be added carefully to avoid
vigorous effervescence and loss of samples. After complete
different from each other. Matching standards were chosen cease of effervescence, the desired quantity of aqua regia
after critical review of major and minor elements of the should be filled and kept for digestion.
samples. Some other standards (Table 3) were also used in
this study to check the robustness of the analytical method. 2.4.2. Adjustment of amount of aqua regia to be added
Each bulk sample was reduced to 500 g of 200 mesh for
chemical analysis following a standard sampling technique Aqua regia is the oxidising agent in the method applied
[22]. herein. Thus, it is very important to optimise the sample to
aqua regia ratio. Although there are few references in this
2.4.1. Sample Decomposition and Extraction of Gold regard, no elaborate study is available [24, 25]. Moreover,
into MIBK the earlier workers conducted the studies with limited
geostandards and only with a handful of samples. Herein,
Each 10-g sample was transferred into a borosilicate glass we have used a large number of field samples from dif-
beaker followed by addition of small amount of water to ferent parts of India of diverse variety, together with 10
moisten the sample. To it, freshly prepared aqua regia geostandards. We have observed that different quantities of
(60 mL) was added, and the beaker was covered with a lid. aqua regia are required for different types of samples
The mixture was digested at 180 C till the volume was depending on their matrixes. During this study, it was
reduced to 20 mL. It took almost 4 h to reach the required found that different amount of aqua regia is required for
volume. This prolonged heating is very essential to obtain different samples. Therefore, it is indispensable to optimise
complete leaching of gold in solution. With increasing the sample to aqua regia ratio. Amount of aqua regia was
temperature oxidation potential gradually increases and varied keeping all other conditions identical. For the study,
leaching becomes more feasible [23]. At this stage, for- we have chosen three geostandards, namely GTS2, MA3a
mation of pasty mass was desirably avoided as the active and PTM1A. Three field samples of different rock type,
Au3? so formed may convert into other insoluble forms arseno-pyrites, quartz vein with sulphides, and banded iron
like Au2O, which may not come into HCl medium. After formation (BIF) in Schist belts (sample no 9, 14 and 16,

Table 3 Details of international gold geostandards

S. no. Name Rock type Origin

1 WMG1 Mineralised gabbro PGE material Canada

2 WMS1 Massive Sulphide PGE material Canada
3 GTS2a Gold Tailings Canada
4 SARM-7 Felsphatic pyroexnite South Africa
5 PTC-1A Chalcopyrite, Pentlandite, Pyrrhotite Canada
6 PTM-1A Sulphide of Ni and Cu Canada
7 MA-2c Gold ore (Quartz, Feldspar, Dolomite) Canada
8 MA-3a Gold ore (Quartz, Feldspar, Dolomite, Calverite) Canada
9 MA-1b Gold ore (Quartz, Feldspar, Calverite) Canada
10 BND 3401.01 [21] Gold sulphide-bearing quartz vein India

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 P. Ghosh et al.

110 or more leaching of gold from all the samples and geo-
standards used in this study except in BIF. Only 85%
100
leaching was obtained in this case, even increase in aqua
regia could not enhance leaching of gold in this case. In
90
case of BIF, the solution contains a lot of Fe?3. Thus for
Leaching (%) of Au

removal of Fe?3 multiple HCl wash was required which

80
may lead to loss of some Au?3. So we fix the ratio 6 for the
GTS 2
70 MA 3a entire study. This study also indicates that if excess aqua
PTM 1a regia is used then roasting step may be escaped. In roasting
Arsenopyrites step, sulphide structures are broken to some extent via
60 sulfide
BIF Schist belt oxidation which leads to easy leaching of gold. Excess
50 aqua regia can take care of this issue as it can provide very
strong oxidising environment.
2 4 6 8 10

Aqua regia: Sample (v/w)
Fig. 1 Extent of leaching (%) of gold from geological samples with
varying aqua regia sample ratio
respectively, in Table 5) were also used. In case of field
samples, results obtained from fire-assay method were
considered as true value and then compared. All results are
plotted as leaching of gold versus aqua regia/sample ratio
as shown in Fig. 1. All data presented in the graph are
average of four analyses. From the plot, it is evident that
lesser amount of acid was required for geostandards, while
larger amount of acid was required for arseno-pyrites and
other complex matrix samples. For GTS-2 and MA3a
requirement of acid is four times that of sample used
whereas, this factor is 6 for PTM1a. PTM1a is Ni-Cu matt
and contains large amount of sulphides, as a result more
aqua regia is required for complete leaching of Au. Six
times or more quantity are required for complete release of
Au in solution for field samples. This resulted due to higher
degree of complexity in field samples. From the graph, it is
evident that aqua regia/sample ratio 6 is optimum for 95%
2.5. AAS measurement and calibration using synthetic
AuCl3 solution
As Au3? is selectively extracted into MIBK thus effect of
matrix is minimal in this case. Therefore, we have used
synthetic standards for calibration of AAS instrument.
However, during analysis of samples, geostandards of
similar matrix were used as check standards to that of
samples. The operating parameters (Tables 1, 2) were
optimised to get maximum absorbance for gold in the
working concentration range. A representative calibration
curve obtained from GF-AAS and F-AAS is shown in
Fig. 2. For all measurements, absorbance was kept below
0.5 to retain linearity of Lambert–Beer’s law. To obtain
such absorbance final solution was diluted accordingly.
These calibration curves were verified by using appropriate
CRMs. Detection limit of these instruments was calculated
by measuring absorbance of process blanks. For this pur-
pose, ten process blanks were prepared and measured in
GF-AAS and F-AAS, respectively. In GF-AAS, their mean
and SD were 0.41 ppb and 0.053 ppb, respectively, and

(a) (b)
0.5 0.25
Absorbance Absorbance
Linear fitting of absorbance Linear fitting of Absorbance
0.4 0.20
Absorbance
Absorbance

0.3 0.15

0.2 Adj R2: 0.99935 0.10

Intercept: 0.00416 Adj R2: 0.98839
Intercept: 0.01683
0.1 0.05

10 20 30 40 50 1 2 3 4 5 6 7 8 9
[Au] ppb [Au] ppm

Fig. 2 Calibration curve obtained in GF-AAS (a) and F-AAS (b) using synthetic gold standards

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A Modified Acid Digestion Method for Analysis of Gold in Geological Samples: A Comparative…

limit of quantification (LOQ) = Mean ? 10 9 SD = 0.93
ppb & 1 ppb. In F-AAS, their mean and SD were 26 ppb
and 7 ppb, respectively, and LOQ = Mean ? 10 9
SD = 96 ppb & 100 ppb.
3. Results and Discussion
Solvent extraction is a very selective technique and can be
applied to extract particular element from solution even at
a very low concentration. MIBK is an ideal solvent for
extraction of gold from solution. If Au leaches out from
rock/soil samples and remains in Au3? state in solution,
then MIBK can quantitatively extract almost 100% of it
along with some other traces [26, 27]. The gold content of
the organic phase can be accurately determined by atomic
absorption spectrometry. Table 4 represents gold data
obtained on some international gold geochemical reference
samples by MIBK extraction method in comparison with
certified values. These results clearly indicate that the
recovery of certified value is more than 90% in most of the
geostandards. From the list of rock type of geostandards
used in this study, it is obvious that this method is appli-
cable to even most complex nature of matrixes, e.g. gold
sulphide-bearing quartz vein, calverite, chalcopyrite. Ear-
lier good recovery was obtained in these standards only
after digestion of roasted samples. For the first time, we are
reporting such good recovery values without roasting the
samples. This leads to much faster and cheaper analysis of
gold in geological samples.
3.1. Comparison with Pb Fire-Assay Method
Till now, it is clear that our method (without roasting of
samples and high ratio of aqua regia to sample with pro-
longed heating) works very well with different type of
geostandards. However, the scenario may vary completely
in case of actual field samples due to much complex and
inhomogeneous nature of samples. Field samples may be
very unique in nature and not comparable with geostan-
dards. Thus, to establish our methodology, it is essential to
compare our results and those obtained from a well-known
standard procedure. Classical Pb fire-assay method is used
widely all over the world and it is accepted as the most
dependable analytical method for the determination of Au
in geological and, all other kind of Au-alloy samples. This
method was applied to obtain for separation and pre-con-
centration of Au prior to analysis of gold by F-AAS/GF-
AAS. In this method, all kinds of matrixes can be broken at
such a high temperature, and Au comes out as a prill [28].
A comparison of the gold concentrations is obtained by fire
assay followed by F-AAS/GF-AAS techniques. Those
obtained by MIBK extraction method on various field
samples are presented in Table 5. For comparison, the
results obtained from fire assay are considered as true
value. From Table 5, it is evident that our proposed method
works very well within the range of 50 ppb to 21.6 ppm.
This range may vary depending upon the sample nature and
rock type. Recovery factor is quite high for field samples
also, more than 80% in most of the cases. Lower values
were obtained in certain quartz vein with sulphides (sample
15), BIF Schist belt (sample 16). Lower recovery may be
attributed to the inhomogeneity in these samples. In case of
high iron-containing samples (BIF,) multiple wash of
MIBK layer with HCl may be attributed to some loss of
Au. In some cases, result obtained from MIBK extraction
method is higher than that of fire assay. This possibly
resulted due to incomplete reaction which can be avoided
by multiple cupellations [28–30]. Moreover, some gold
might be lost in scorification step also. However, overall
recovery is still on the higher side in our proposed method
and can be used for the rock types mentioned herein.

Table 4 Gold value obtained from different CRMs using proposed method. All results shown here are average of 4 analysis
Standard Certified value Observed value (ppm) Recovery (%) Observed value (ppm) Recovery (%)
(ppm) [MIBK] [MIBK] [FA] [FA]

WMG1 0.11 ± 0.011 0.12 ± 0.014 109.1 0.115 ± 0.012 104.5

WMS1 0.279 ± 0.33 0.258 ± 0.26 92.4 0.267 ± 0.29 95.7
GTS2a 0.272 ± 0.005 0.267 ± 0.006 98.2 0.264 ± 0.006 97.1
SARM-7 0.31 ± 0.015 0.23 ± 0.02 74.0 0.243 ± 0.025 78.4
PTC-1A 1.31 ± 0.11 1.33 ± 0.13 101.5 1.28 ± 0.09 97.7
PTM-1A 3.3 ± 0.2 3.1 ± 0.18 93.9 3.15 ± 0.14 95.5
MA-2c 3.02 ± 0.06 3.01 ± 0.08 99.7 2.8 ± 0.09 92.7
MA-3a 8.56 ± 0.09 8.41 ± 0.11 98.2 8.47 ± 0.10 98.9
MA-1b 17.0 ± 0.3 15.8 ± 0.4 92.9 15.62 ± 0.4 91.9
BND 12.1 ± 0.7 11.5 ± 0.6 95.0 11.6 ± 0.7 95.9
3401.01

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 P. Ghosh et al.

Table 5 Gold concentrations (lg/g) in a few geological samples determined by two different methods. All results shown here are average of 3
analysis
S. no. Sample type Sampling area [Au] ppm MIBK [Au] ppm FA

1. Stream Sediment Thenepennaiyar River, Tamilnadu 0.052 ± 0.005 0.048 ± 0.004

2. 0.054 ± 0.006 0.06 ± 0.004
3. Soil Waynad, Kerala 0.35 ± 0.012 0.36 ± 0.014
4. Trench sample, Laterite soil Karnataka 1.6 ± 0.05 1.8 ± 0.06
5. 2.3 ± 0.08 2.7 ± 0.07
6. Felsic Metavolcanic rock Khera main block, Rajasthan 0.5 ± 0.04 0.6 ± 0.05
7. Metavolcanic Sedimentary rock, Arseno-pyrites Jagpura area, Rajasthan 1.3 ± 0.07 1.1 ± 0.05
8. 9.5 ± 0.3 11.8 ± 0.4
9. 1.8 ± 0.08 1.7 ± 0.08
10. 21.6 ± 0.2 18.6 ± 0.3
11. 7.6 ± 0.3 6.6 ± 0.3
12. Kanara-Shimoga Schist belt Mathurapura-Attigere prospect, Karnataka 14.0 ± 0.5 10.2 ± 0.4
13. 16.5 ± 0.7 14.2 ± 0.5
14. Quartz vein with Sulphides Velligallu, Chittor Dist., Andhra Pradesh 5.6 ± 0.2 5.7 ± 0.2
15. Quartz vein with Sulphides Gani-Kalva area, Andhra Pradesh 9.1 ± 0.5 11.4 ± 0.6
16. Schist belt, BIF Bangaragatti area, Karnataka 10.9 ± 0.4 13.1 ± 0.3
FA fire assay

4. Estimation of measurement uncertainty r r0

U1 ¼ p ¼ 1:240868 and U10 ¼ p ¼ 1:2301
n n
Estimation of uncertainty is very essential to obtain con-
fidence in measured results. There are two major con- All other elements arise from analysis part, e.g. weighing
tributing factors in measurement of uncertainty. First one of sample, error in volume make-up, error in calibration
arises from the method, depending on the digestion tech- curve, etc. [31, 32]. These factors will remain same for
nique leaching of Au may differ which in turn reflected in MIBK and fire assay analysis. Calculation of uncertainty
the recovery factor. Mean and SD of recovery factors are arising due to these terms is given in Table 6.
calculated from Table 4. This part, designated as U1 for Now we can calculate the total uncertainty (Uc) by using
0
MIBK method and U1 for fire assay technique, is most Eq. 1
sffiffiffiffiffiffiffiffiffiffiffiffiffiffi
important in measurement of uncertainty as all the exper- Xn
imental parameters of digestion process is incorporated in Uc ¼ Ui2 ð1Þ
0
this term. During calculation of U1 and U1 , recovery factor i¼1

of SARM 7 was discarded as it stays outlier. Thus degrees Applying Eq. 1, we get Uc (MIBK) = 0.0181 and Uc
of freedom (n) for this data set is 8. (FA) = 0.013, respectively (Supporting information). From

Table 6 Sources and calculation of uncertainty

Source Distribution Degree of Calculation Value
freedom

U2 = mass for Weight of sample Normal ? Standard uncertainty = 0.01/2 = 0.005, 0.0005
Expanded uncertainty for 10 g is 0.01 g U2 = 0.005/10 = 0.0005
Expanded Uncertainty is divided by coverage
factor K = 2 at confidence level of 95%
U3 = uncertainty due to volume make-up, Triangular ? Standard uncertainty = 0.2/H6 = 0.0816 0.00136
vol. = 60 mL, max. calibration error = 0.2 mL H6 U3 = 0.0816/60 = 0.00136
U4 = uncertainty due to volume made max. Triangular ? Standard uncertainty = 0.05/H6 = 0.020412, 0.00408
calibration error for 5 mL = 0.05 mL H6 U4 = 0.04491/5 = 0.00408
U5 = uncertainty due to Calibration of instrument, Rectangular ? Standard uncertainty = 0.01/H3 0.00006
uncertainty = 1% for 0.1–10 ppm range H3 U5 = 0.01/(10 9 H3) = 0.00006

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A Modified Acid Digestion Method for Analysis of Gold in Geological Samples: A Comparative…

and accuracy reach close to that of fire assay method

Modified acid digestion 75
Acid digestion 90
(Fig. 3). Although we have got very encouraging results
Fire Assay 100
Time with sulphide rocks also, the most difficult one, more
detailed study is required for complete understanding of
Modified acid digestion 200 this complex rock. The method described above can be
Acid digestion 180 adapted for both geochemical mapping and assay deter-
Fire Assay 100 Efficiency mination for mining prospects in the geological samples
mentioned here.
Modified acid digestion 90
Acid digestion 70
Fire Assay 100 Accuracy Acknowledgements Authors thank the Additional Director General,
Geological Survey of India, Hyderabad, for permitting the publication
of this paper. National Geophysical Research Institute (Council of
45 Modified acid digestion
Scientific and Industrial Research), Hyderabad is thanked for pro-
50 Acid digestion viding high-grade gold geochemical reference material (BND
Fire Assay 100 Cost 3401.01). Authors are also thankful to the laboratory in-charges of
GSI, SR, Hyderabad and CCL, Kolkata, for their active support to
0 50 100 150 200
complete this work.
Arbitary values (%)

Fig. 3 Comparison of fire assay method, classical acid digestion

method and modified acid digestion method regarding time required,
efficiency, accuracy and cost, for analysis of each sample [33, 34] References

[1] A. A. Levinson, Introduction to exploration geochemistry,

Student’s t-table for 95% confidence, the coverage factor
(K) is 2.306. The expanded uncertainty = Uc 9 K. So
expanded uncertainty for the two methods as follows:
UMIBK = 0.0417 and UFA = 0.0299.
From this calculation, it is clear that uncertainty of two
methods is very close to each other and well within the
acceptable range. At a much lower cost and time, similar
accuracy can be obtained by our method. Figure 3 shows
the comparison of proposed method with two classical
methods regarding all these aspects. From Fig. 3, it is
obvious that proposed modified acid digestion method is
superior in all aspects compared to classical methods.
5. Conclusion
Proposed modified MIBK extraction is advantageous over
conventional fire-assay methods and save labour, material
expense, and does not require specially trained technicians.
The above-described method does not have the step of
roasting of samples. Thus it can save a lot of time of
analyst and overall process becomes cheaper. However, for
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