Hindawi Publishing Corporation

Journal of Chemistry
Volume 2013, Article ID 151395, 6 pages
http://dx.doi.org/10.1155/2013/151395

Research Article
Rapid Microwave Digestion Procedures for the Elemental
Analysis of Alloy and Slag Samples of Smelted Ocean Bed
Polymetallic Nodules

Kumari Smita,1 Saurabh Kumar Singh,2 and Brajesh Kumar3

1
Analytical Chemistry Division, National Metallurgical Laboratory, Jharkhand, Jamshedpur 831 007, India
2
Control, Research, and Development Department, Uranium Corporation of India Limited, Turamdih, Sundernagar, Jharkhand,
Jamshedpur 832 107, India
3
P.G. Department of Chemistry, Tata College, Jharkhand, Chaibasa 833 202, India

Correspondence should be addressed to Kumari Smita; k.smita2010@rediffmail.com

Received 9 January 2012; Revised 27 May 2012; Accepted 6 June 2012

Academic Editor: Yoshihiro Kudo

Copyright © 2013 Kumari Smita et al. is is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

e use of microwave digester for digestion of alloy and slag samples of smelted ocean bed polymetallic nodules has permitted the
complete digestion of samples, thereby replacing the tedious classical methods of digestion of samples. e digestion procedure
includes two acid-closed digestions of samples in a microwave oven. Owing to the hazardous nature of perchloric acid, it was
not used in developed digestion procedure. Digested sample solutions were analyzed for concentrations of various radicals and the
effectiveness of the developed digestion methodology was tested using certi�ed reference materials. It was found that the developed
method is giving results comparable with that obtained from conventionally digested samples. In this digestion procedure, time
required for digestion of samples was reduced to about 1 hour only from 8-9 hours of conventional digestion.

1. Introduction its extensive terrestrial deposits [4]. A signi�cant amount

of R&D efforts are in progress around the world towards
Ocean bed polymetallic nodules or manganese nodules developing schemes for extraction of valuable metals from
found on the deep sea�oor have been recognized as an these nodules [5, 6]. Initially, the extraction of only three
alternate source for certain metals, when land deposits get metals, namely, nickel, copper and cobalt from manganese
exhausted. India is one of the eight pioneer investors in the nodules was considered. Aer 1978, manganese extraction
world with exclusive rights over an area of 75,000 sq. Km was added to improve the process economics and to reduce
in the Central Indian Ocean for the exploration and future the amount of waste [3]. e technologies so far developed
exploitation of these mineral deposits [1]. ese nodules for extraction of valuable metals form manganese nodules are
contain metals like copper, nickel, cobalt, manganese, iron, of two types: hydrometallurgical in which metals are leached
lead, zinc, aluminum, and so forth [2]. Generally, these from the nodules by acid or alkaline reagents, and pyromet-
nodules contain a little over 2% of copper, nickel, and allurgical, in which the hydroxides of metals are reduced
cobalt together, ∼10% iron, 20% manganese and around 18% and the melted metals are separated [2, 7, 8]. At National
silica. Metal entities such as Cu, Ni, Co, Mo, and Zn are Metallurgical Laboratory (NML), Jamshedpur, India a pyro-
accommodated in the complex cage of iron and manganese hydrometallurgical route for recovery of valuables from man-
hydroxides. Nickel and copper oxides are distributed and ganese nodules is under development. In this process direct
associated with the manganese oxide phase. Cobalt, present reduction smelting—matte formation—pressure leaching of
as cobaltic oxide, is associated with iron oxide phase [3]. manganese nodules samples were adopted. e process
ough manganese is the major element in ocean nodules, under development at NML, Jamshedpur for processing of
little attempt has been made on its extraction owing to manganese nodules consists of reduction roasting of nodules
2 Journal of Chemistry

followed by direct smelting of roasted nodules in an electric- method, the use of perchloric acid for digestion was com-
arc furnace. In this process a manganese-rich slag and an pleted eliminated.
iron-nickel-cobalt alloy are produced. From the alloy, the
individual metals are recovered through matte formation and
2. Experimental
subsequent pressure dissolution of matte. It was reported
in the literature that similar type of alloy can be used for 2.1. Equipment and Materials. Ethos-1 (Milestone SRL, Italy)
recovery of individual metals and similar type of slag can microwave digester was used for the digestion of smelted
be used for production of silicomanganese [9]. e alloy manganese nodules slag and alloy samples. e digester
and slag obtained aer electrothermal smelting of roasted has TFM (tetra�uoromethoxil) vessels of 75 mL capacity.
manganese nodules are intermediate products in recovery Maximum magnetron of digester is 1500 W and can be
process of valuable metals from manganese nodules. It is programmed according to desired temperature of digestion.
required to analyze the alloy and slag samples to ascertain the Samples were digested in triplicate using three TFM vessels,
overall effectiveness of the roasting and smelting processes. out of which one is the control vessel having temperature
With this, it is essential to know the radical concentrations in and pressure measurement probes to control the digestion
slag and alloy for further improvement and/or modi�cation procedure. In forth vessel reagent blank was taken. e
in extraction methodology. e alloy and slag samples manganese nodule samples were received from National
are analyzed for radicals such as Si, Fe, Mn, Cu, Ni, Co, Centre for Antarctic and Ocean Research (NCAOR), Goa,
CaO, MgO, and Al2 O3 using their appropriate methods of India. e nodule samples were crushed and �nally grounded
analysis. e wet chemical analysis by orthodox conventional to −150 𝜇𝜇 size. e grounded samples were mixed with
method or by advanced instrumental methods needs sample desired amount of Low Diesel (LD) oil (reductant) and
in solution phase for analysis. Conventional wet sample further milled/mixed for 40 minutes. is mixture was
preparation methods for the decomposition of solid samples pelletized using disc pelletizer. e nodule pellets were air
are performed either with a re�ux system or in a beaker dried followed by oven drying at 100∘ C for 6 h. e oven
on a laboratory hot plate. Common to both methods is dried pellets were roasted in a pot furnace at 750∘ C in argon
the temperature limitations as a consequence of the boiling atmosphere. e roasted nodules are then smelted in a 50
point of the solution used for digestion. e conventional KVA electric arc furnace with coke and quartz. Aer smelting
digestion of alloy and slag samples of smelted manganese process a manganese-rich slag and an iron-nickel-cobalt alloy
nodules is carried out using hydrochloric acid (HCl), nitric are produced. ese are used for digestion studies.
acid (HNO3 ), and perchloric acid (HClO4 ). Among these
the fuming of percholric acid itself takes 6-7 hours. So the
2.2. Reagents. e chemicals and reagents used were of
digestion cannot be completed in a single working day. is
analytical reagent grade. HCl (35% m/v), HNO3 (69% m/v)
poses serious problems for laboratories having high sample
and HClO4 (71–73% m/v) (all from Merck India) were used
load. With this, the conventional digestion procedure is prone
during digestion. Deionized water (Millipore System, USA)
to many drawbacks such as long time requirement, high man-
was used where required.
power input, high reagents consumption, and loss of volatile
components during heating.
Recent development in the area of digestion technique 2.�. Certi�ed Reference Materials. Certi�ed reference mate-
resulted into a microwave digester. Microwave digestion rials were used in this paper: Ocean bed polymetallic nod-
technique is a closed vessel digestion technique, which ules No. NML 2388, Manganese ore No. NML 66.2 and
utilizes the added advantage of elevated pressure for quick Ferrosilicon No. NML 31.2. (NML: National Metallurgical
digestion of samples. As microwave heating is internal as Laboratory, Jamshedpur, India).
well as external, the heat conduction stage is avoided because
energy is instantly transferred to the sample by absorptive 2.4. Digestion Procedures. (i) Choice of Acid. In this developed
polarization rather than molecular collisions [10]. Use of protocol, we use nitric and hydrochloric acid. Nitric acid is
microwave digester for sample preparation is gaining sub- a strong oxidizing agent widely used for liberating metals
stantial important day by day. Many researchers used this from various types of matrices as highly soluble nitrate
method for sample preparation and validated the same [11– salts. Hydrochloric acid is used for dissolution of samples
14]. erefore, microwave-assisted closed vessel digestion as it preserves the metals in solution. e classical hot-
was tried for alloy and slag samples of smelted manganese plate dissolution of samples having a matrix similar to our
nodules. Our present study is focused on microwave diges- samples requires perchloric acid dissolution with nitric and
tion and subsequent analysis of digested samples. In our hydrochloric acid. However the perchloric acid handling
paper, we discussed the microwave digestion procedure for requires great care. Combustible materials and most organic
alloy and slag samples obtained during a new extraction compounds contaminated with perchloric acid are highly
process for smelted manganese nodules (under development �ammable [11]. �erchloric acid particularly catches �re with
at NML, India). e microwave digestion method developed easily oxidisable materials. Hence the use of perchloric acid
during our study was validated using CRM. Developed was eliminated in this dissolution protocol.
microwave digestion procedure reduces the time of digestion (ii) Conventional Digestion of Samples. e smelted man-
from 8-9 h to about 1 h only and it substantially reduced ganese nodules alloy and slag samples were grounded sep-
the volume of acid required for digestion. In the developed arately to −75 𝜇𝜇 size using agate-coated planetary ball mill.
Journal of Chemistry 3

T 1: Conditions for Microwave digestion of samples.

Sample weight HCl Digestion time Ventilation

Experiment Number HNO3 (mL) Power (Watt) Temperature (∘ C)
(gram) (mL) (minutes) time (minutes)
M1 0.1 16 2.00 500 150 90 30
M2 0.1 10 3.50 500 150 90 30
M3 0.1 16 2.00 500 150 40 10
M4 0.1 10 3.50 500 150 40 10
Note: M stands for Microwave digestion.

T 2: Concentrations of radicals present in microwave and conventionally digested alloy samples.

S. No. Detail of Experiment Si (%) Fe (%) Mn (%) Cu (%) Ni (%) Co (%)

1 M1 NF 62.60 4.63 12.30 15.82 1.18
2 M2 NF 62.67 4.60 12.40 15.69 1.18
3 M3 NF 62.63 4.68 12.40 15.65 1.22
4 M4 NF 62.50 4.49 12.48 15.66 1.26
5 C NF 62.53 4.42 12.46 15.67 1.22
Note: NF : Not found.

T 3: Concentrations of radicals present in microwave and conventionally digested slag samples.

S. No. Detail of Experiment SiO2 (%) FeO (%) MnO (%) Al2 O3 (%) MgO (%) CaO (%) Cu (%) Ni (%) Co (%)
1 M1 21.95 8.82 44.36 4.12 16.90 1.84 0.57 0.58 0.029
2 M2 21.86 8.89 44.30 4.02 16.99 2.07 0.56 0.63 0.025
3 M3 21.80 8.87 44.22 4.06 16.90 2.10 0.54 0.58 0.029
4 M4 21.92 8.83 44.20 4.20 17.03 1.98 0.56 0.65 0.030
5 C 21.95 8.90 44.25 4.08 17.02 2.06 0.58 0.62 0.028
Note: In both the Tables shown above, C stands for Conventional digestion. All concentrations are in %, w/w. All results are mean value of triplicate
measurement.

T 4: Mass balance of analysis of digested alloy and slag samples.

Alloy sample Slag sample

S. No.
Exp. Detail Mass balance (%) Exp. Detail Mass balance (%)
1 M1 96.53 M1 99.17
2 M2 96.54 M2 99.35
3 M3 96.58 M3 99.10
4 M4 96.39 M4 99.40
5 C 96.30 C 99.49

T 5: Comparison of concentrations of radicals obtained in CRM digested by microwave digester and conventional method.

S. No. Radicals Certi�ed Value Microwave digested sample Conventionally digested sample
1 SiO2 (%) 16.07 16.11 16.18
2 Fe (%) 14.94 15.00 15.07
3 Mn (%) 21.28 21.31 21.37
4 Al2 O3 (%) 1.65 1.64 1.63
5 Ca (%) 1.80 1.79 1.81
6 Cu (%) 0.49 0.49 0.49
7 Ni (%) 0.71 0.71 0.70
8 Co (%) 0.14 0.14 0.14
Note: All results are mean of triplicate measurement. All concentrations are % w/w.
4 Journal of Chemistry

T 6: e Standard Deviations and Relative Standard Deviation of measurement for radical concentrations of microwave and
conventionally digested CRMs.

Microwave Digestion Conventional Digestion

S. No. Radical
Mean Value (%) (𝑛𝑛 𝑛 𝑛) SD RSD (%) Mean Value (%) (𝑛𝑛 𝑛 𝑛) SD RSD (%)
1 SiO2 16.11 0.01 0.06 16.18 0.01 0.06
2 Fe 15.00 0.02 0.13 15.07 0.02 0.13
3 Mn 21.31 0.03 0.14 21.37 0.01 0.05
4 Al2 O3 1.64 0.01 0.61 1.63 0.01 0.61
5 Ca 1.79 0.002 0.11 1.81 0.02 1.10
6 Cu 0.49 0.0002 0.04 0.49 0.002 0.4
7 Ni 0.71 0.0006 0.08 0.70 0.003 0.4
8 Co 0.14 0.0 — 0.14 0.0 —

About 100 g. of each sample was separated from main complexometry using ammoniacal buffer in the presence of
bulk by coning and quartering and used for digestion. For Eriochrome black-T indicator [17]. CaO alone was estimated
conventional digestion of samples, 0.5 g. sample, 40 mL 1 : 1 using EDTA titration in presence of triethanolamine and
HCl, 10 mL HNO3 , and 10 mL HClO4 was used. First of all potassium hydroxide using Patton and Reeder’s indicator
0.5 g. sample was mixed with 40 mL 1 : 1 HCl in a beaker [17].
and covered beaker was kept for digestion on a hot plate for
about 1 h. at about 100∘ C. en 10 mL concentrated HNO3
was added and the whole content was boiled till evolution 3. Results and Discussion
of nitrous fumes ceased (for about 30 minutes). Finally,
10 mL HClO4 was mixed and the whole content of beaker Total four sets of microwave digestion experiments were
was re�uxed for 6-7 h. e content of beaker was extracted carried out for both alloy and slag samples with reagent
with 20 mL 1 : 1 HCl and �ltered with 40 no. �hatman blanks. ese four sets of microwave digestion experiments
�lter paper. e residue was used for estimation of silica were denoted by notation M1 , M2 , M3 , and M4 for experiment
gravimetrically. Aer silica estimation, this residue was fused 1, 2, 3, and 4, respectively (Table 1). e digested samples were
with KHSO4 and with the help of 20 mL 1 : 1 HCl, the fused analyzed for concentrations of desired radicals in triplicate.
mass was added to the �ltrate obtained previously. e �ltrate e alloy and slag samples were also digested by conventional
volume was made 250 mL by adding de ionized water. is route and analyzed for radical concentrations. ese results
�ltrate was used for estimation of other radicals. All digestion of analysis for digested alloy samples are shown in Table 2.
experiments were carried out in triplicate with a reagent Similarly the results of analysis of digested slag samples are
blank. shown in Table 3.
(iii) Microwave Digestion of Samples. For microwave di- Applying law of conservation of mass, the mass balance
gestion, samples were prepared in similar manner described of analysis for all microwave and conventionally digested
earlier. Quantity of sample, reagent volumes, and digestion samples were prepared and shown in Table 4.
parameters used during microwave digestion are tabulated Addition of concentrations of all radicals for digested
in Table 1. All microwave digestions were carried out in alloy sample is coming about 96%. Rest 4% are carbon and
triplicate with a reagent blank. Aer digestion of samples, sulphur which we did not shown in this study. Addition of
preparation of samples for analysis was done in similar concentrations of all radicals for digested slag sample is com-
manner as described in conventional digestion of samples. ing about 99%. From mass balance calculation, it is clear that
(iv) Analysis of Digested Samples. Digested sample were we succeeded to analyze the digested alloy and slag samples
analyzed for Si, Fe, Mn, Cu, Ni, and Co. For analyzing almost completely. From Table 4, it is also clear that the
Cu, Ni, Fe, and Co, �ame atomic absorption spectrometer radical concentrations are almost same in all cases, regardless
(�BC Avanta, Australia) with air-acetylene �ame was used of the method of digestion used. However the most appropri-
[15]. Hollow cathode lamp (HCL) is used as source of light. ate set of digestion conditions for microwave digester must
Analysis of Cu, Ni, Co, and Fe is done at 327.4 nm, 341.5 nm, possess lowest time and reagent volume requirement. On
240.7 nm, and 248.3 nm wavelength, respectively. Si is ana- this criterion, the digestion conditions described at M4 of
lyzed by gravimetric method [16–19]. Al2 O3 , CaO, and MgO Table 1 seem to be most promising. Taking in to account of
are analysed by complexometric titration using EDTA [16– low time of digestion and low reagent volume requirement,
20]. Aluminum is complexed with EDTA by boiling with the digestion conditions described at M4 of Table 1 was
excess of reagent. e excess of reagent is back titrated used to digest Certi�ed Reference Materials (CRMs) in
with standard zinc acetate solution at pH 5 to 5.5 using microwave digester. Aer digestion, the CRMs were analyzed
xyenol orange indicator. A blank is also determined simul- for radical concentrations. e CRMs were also digested by
taneously and from the EDTA used up, Al2 O3 is computed conventional digestion procedure and analyzed separately.
(IBM manual, 1979). CaO+MgO is determined by EDTA e results of analysis were depicted in Table 5.
Journal of Chemistry 5

T 7: Detailed digestion conditions selected for digestion of samples in microwave digester.

Step Power (W) Time (minutes) T1 (∘ C) T2 (∘ C) Pressure (bar)

1 500 5 100 80 10
2 500 10 110 90 10
3 500 25 150 100 10
Note: Ventilation time given = 10 minutes.

T 8: Conventional digestion versus developed microwave digestion.

S. No. Parameter Conventional digestion Microwave digestion

1 Sample weight 0.5 gram 0.1 gram
40 ml 1 : 1 HCl, 10 mL
2 Acid requirement 10 mL HCl and 3.5 mL HNO3
HNO3 and 10 ml HClO4
3 HClO4 requirement Yes No
40 minutes digestion time and 10 minutes ventilation time
required. Additional 20 minutes is required for loading &
4 Digestion time Total 8-9 h.
unloading of digestion vessels in digester.
So, total time required is 1 h. 10 min.
Time required for analysis of Time requirement for analysis of radicals is same irrespective of method of digestion
5
radicals

Statistical treatment was given to the results of analysis digestion was achieved with 10 mL HCl and 3.5 mL HNO3 .
obtained for digested Certi�ed Reference Materials. e In microwave digestion experiments 0.1 gram of samples
standard deviations (SDs) and relative standard deviations was used and the results of analysis of microwave digested
(RSDs) of measurement are given in Table 6. samples are comparable with that of 0.5 gram samples
digested via conventional route. e developed protocol
was validated using CRM. e use of perchloric acid at
3.1. Dissolution Procedure Adopted. From Table 6, it appears
high temperature and high pressure is hazardous due to its
that, the digestion conditions taken for microwave digestion
potentially explosive nature and hence the requirement of
of CRMs are giving satisfactory results. Here we use 0.1 g.
perchloric acid is completely eliminated in our digestion
sample, 10 mL HCl, and 3.5 mL HNO3 . Digestion temper-
methodology.
ature given was 150∘ C with 40 minutes digestion and 10
minutes ventilation time. e detailed digestion program
used for M4 is given in Table 7. For digesting the samples, Acknowledgment
three-staged increment of temperature was adopted. As per
manufacturer’s instruction, this is required for efficient and e authors are thankful to the Director, National Metallur-
trouble-free working of microwave digester. In all steps, the gical Laboratory, Jamshedpur, India for, his kind permission
magnetron power of microwave digester was �xed at 500 W, to publish this work.
while time and temperature were increased progressively. In
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