Sei sulla pagina 1di 25

1400-Fm 9/9/99 7:37 AM Page ii

McGraw-Hill Higher Education


A Division of The McGraw-Hill Companies

MODERN ANALYTICAL CHEMISTRY

Copyright © 2000 by The McGraw-Hill Companies, Inc. All rights reserved. Printed in
the United States of America. Except as permitted under the United States Copyright Act of
1976, no part of this publication may be reproduced or distributed in any form or by any
means, or stored in a data base or retrieval system, without the prior written permission of the
publisher.

This book is printed on acid-free paper.

1 2 3 4 5 6 7 8 9 0 KGP/KGP 0 9 8 7 6 5 4 3 2 1 0

ISBN 0–07–237547–7

Vice president and editorial director: Kevin T. Kane


Publisher: James M. Smith
Sponsoring editor: Kent A. Peterson
Editorial assistant: Jennifer L. Bensink
Developmental editor: Shirley R. Oberbroeckling
Senior marketing manager: Martin J. Lange
Senior project manager: Jayne Klein
Production supervisor: Laura Fuller
Coordinator of freelance design: Michelle D. Whitaker
Senior photo research coordinator: Lori Hancock
Senior supplement coordinator: Audrey A. Reiter
Compositor: Shepherd, Inc.
Typeface: 10/12 Minion
Printer: Quebecor Printing Book Group/Kingsport

Freelance cover/interior designer: Elise Lansdon


Cover image: © George Diebold/The Stock Market
Photo research: Roberta Spieckerman Associates

Colorplates: Colorplates 1–6, 8, 10: © David Harvey/Marilyn E. Culler, photographer;


Colorplate 7: Richard Megna/Fundamental Photographs; Colorplate 9: © Alfred Pasieka/Science
Photo Library/Photo Researchers, Inc.; Colorplate 11: From H. Black, Environ. Sci. Technol.,
1996, 30, 124A. Photos courtesy D. Pesiri and W. Tumas, Los Alamos National Laboratory;
Colorplate 12: Courtesy of Hewlett-Packard Company; Colorplate 13: © David Harvey.

Library of Congress Cataloging-in-Publication Data

Harvey, David, 1956–


Modern analytical chemistry / David Harvey. — 1st ed.
p. cm.
Includes bibliographical references and index.
ISBN 0–07–237547–7
1. Chemistry, Analytic. I. Title.
QD75.2.H374 2000
543—dc21 99–15120
CIP

INTERNATIONAL EDITION ISBN 0–07–116953–9


Copyright © 2000. Exclusive rights by The McGraw-Hill Companies, Inc. for manufacture
and export. This book cannot be re-exported from the country to which it is consigned by
McGraw-Hill. The International Edition is not available in North America.

www.mhhe.com
438 Modern Analytical Chemistry

self-absorption
much higher, background interferences due to molecular emission are less prob-
In atomic emission, the decrease in lematic. Emission from the plasma’s core is strong but is insignificant at a height
emission intensity when light emitted by of 10–30 mm above the core, where measurements normally are made.
excited state atoms in the center of a
flame or plasma is absorbed by atoms in
the outer portion of the flame.
Minimizing Chemical Interferences Flame emission is subject to the same
types of chemical interferences as atomic absorption. These interferences are
minimized by adjusting the flame composition and adding protecting agents,
releasing agents, and ionization suppressors. An additional chemical inter-
ference results from self-absorption. Since the temperature of a flame is
greatest at its center, the concentration of analyte atoms in an excited state is
greater at the center than at the outer edges. If an excited state atom in the
center of the flame emits radiation while returning to its ground state, then
ground state atoms in the cooler, outer regions of the flame may absorb the
radiation, thereby decreasing emission intensity. At high analyte concentra-
tions a self-reversal may be seen in which the center of the emission band de-
creases (Figure 10.52).
Chemical interferences with plasma sources generally are insignificant.
The higher temperature of the plasma limits the formation of nonvolatile
species. For example, the presence of PO 4 3– in solutions being analyzed
for Ca2+, which is a significant interferant for flame emission, has a negligi-
ble effect when using a plasma source. In addition, the high concentration
of electrons from the ionization of argon minimizes the effects of ionization
interferences.

Standardizing the Method Equation 10.34 shows that emission intensity is


Baseline
Figure 10.51 proportional to the population of the excited state, N*, from which the emis-
Method for background correction in flame sion line originates. If the emission source is in thermal equilibrium, then
atomic emission. the excited state population is proportional to the total population of analyte
atoms, N, through the Boltzmann distribution (equation 10.35).
Calibration curves for flame emission are generally linear over two to
three orders of magnitude, with chemical interferences due to ionization limiting
linearity for lower concentrations of analyte, and self-absorption limiting linear-
ity for higher concentrations of analyte. Plasma sources, which suffer from fewer
chemical interferences, often yield calibration curves that are linear over four to
five orders of magnitude and that are not affected significantly by changes in the
matrix of the standards.
When possible, quantitative analyses are best conducted using external stan-
dards. Emission intensity, however, is affected significantly by many parameters,
including the temperature of the excitation source and the efficiency of atomiza-
tion. An increase in temperature of 10 K, for example, results in a 4% change in
the fraction of Na atoms present in the 3p excited state. The method of internal
standards can be used when variations in source parameters are difficult to con-
trol. In this case an internal standard is selected that has an emission line close to
that of the analyte to compensate for changes in the temperature of the excita-
tion source. In addition, the internal standard should be subject to the same
(a) (b) chemical interferences to compensate for changes in atomization efficiency. To
Figure 10.52 accurately compensate for these errors, the analyte and internal standard emis-
Atomic emission line at (a) low concentration sion lines must be monitored simultaneously. The method of standard additions
of analyte, and (b) high concentration of also can be used.
analyte showing the effect of self-absorption.
TEXTBOOK OF
QUANTITATIVE
CHEMICAL
ANALYSIS
FIFTH EDITION

G.H. JEFFERY • J. BASSETT • J. MENDHAM • R. C. DENNEY


Longman Scientific & Technical
Longman Group UK Limited
Longman House, Burnt Mill, Harlow
Essex CM20 2JE, England
and Associated Companies throughout the world
Copublished in the United States with
John Wiley and Sons Inc, 605 Third Avenue, New York NY 10/58
© Longman Group UK Limited 1978, 1989
All rights reserved; no part of the publication
may be reproduced, stored in a retrieval system,
or transmitted in any form or by any means, electronic,
mechanical, photocopying, recording, or otherwise,
without the prior written permission of the Publishers, or a
licence permitting restricted copying in the United Kingdom issued by
the Copyright Licensing Agency Ltd, 33-34 Alfred Place, London WCIE 7DP.
First published in 1939
New impressions 1941, 1942, 1943, 1944, 1945, 1946, 1947, 1948
Second edition 1951
New impressions 1953, 1955, 1957, 1958, 1959, 1960
Third edition 1961 (published under the title A Text-book of Quantitative Inorganic Analysis
Including Elementary Instrumental Analysis)
New impressions 1962, 1964, 1968, 1969, 1971, 1974, 1975
Fourth edition 1978
New impressions 1979, 1981, 1983, 1985, 1986, 1987
Fifth edition 1989

British Library Cataloguing in Publication Data


Vogel, Arthur Israel
Vogel's textbook of quantitative chemical
analysis. - 5th ed.
1. Quantitative analysis
I. Title II. Jeffery, G. H.
545
ISBN 0-582-QQb93-7
Library of Congress Cataloguing in Publication Data
Vogel, Arthur Israel
[Textbook of quantitative chemical analysis]
Vogel's textbook of quantitative chemical analysis. - 5th ed.,'
revised by ... G. H. Jeffery ... [et aI.]
p. em.
Rev. ed. of: Vogel's textbook of quantitative inorganic analysis.
4th ed. 1978.
Includes bibliographies and index.
ISBN 0-470-21517-8
1. Chemistry, Analytic-Quantitative. 2. Chemistry, Inorganic.
I. Jeffery, G. H. 1909- . II. Vogel, Arthur Israel. Vogel's
textbook of quantitative inorganic analysis. III. Title.
QDlO1.2.V63 1989
545-dc20 89-12296
CIP

Set in lO/llpt Lasercomp Times New Roman


Printed in Great Britain
by Bath Press, Avon
FLAME EMISSION SPECTROSCOPY 21.13

(a)

Lamp
emission
v Low current
« 5 rnA)

High current
(15 rnA)

t
Sample
absorption

Fig. 21.12

of hollow cathode lamps may be shortened, particularly those incorporating


the more volatile elements.

21.13 FLAME EMISSION SPECTROSCOPY


There are now two main methods used for flame emission spectroscopy. The
original method, known as flame photometry, is now used mainly for the analysis
of alkali metals.
At present, however, the usual flame emission method is obtained by simply
operating a flame atomic absorption spectrometer in the emission mode (see
Fig. 21.3).
Flame photometers. A flame photometer can be compared with a photoelectric
absorptiometer and the intensity of the filtered radiation from the flame is
measured with a photoelectric detector. The filter, interposed between the flame
and the detector, transmits only a strong line of the element. The simplest and
least expensive detector is a barrier-layer cell (Section 17.6): if sufficient energy
reaches the cell no amplification or external power supply is necessary, and only
a sensitive galvanometer is required. The barrier-layer cell has a high temperature
coefficient: it must, therefore, be placed at a cool part of the photometer. In
some cases the precision is improved by the use of an internal standard and
two filters and, in general, two photocells (one for the standard and one for the
unknown) are utilised; the electronic circuit can be devised to give a direct
reading of the ratio ofline intensities. Flame photometers are intended primarily
for analysis of sodium and potassium and also for calcium and lithium,
i.e.elements which have an easily excited flame spectrum of sufficient intensity for
detection by a photocell. The layout of a simple flame photometer is shown
in Fig. 21.13. Air at a given pressure is passed into an atomiser and the suction
this produces draws a solution of the sample into the atomiser, where it joins

797
© BIOS Scientific Publishers Limited, 2002

First published 2002 (ISBN 1 85996 189 4)

This edition published in the Taylor & Francis e-Library, 2005.

“To purchase your own copy of this or any of Taylor & Francis or Routledge’s
collection of thousands of eBooks please go to www.eBookstore.tandf.co.uk.”

All rights reserved. No part of this book may be reproduced or transmitted, in any form or
by any means, without permission.

A CIP catalogue record for this book is available from the British Library.

ISBN 0-203-64544-8 Master e-book ISBN

ISBN 0-203-68109-6 (Adobe eReader Format)


ISBN 1 85996 189 4 (Print Edition)

BIOS Scientific Publishers Ltd


9 Newtec Place, Magdalen Road, Oxford OX4 1RE, UK
Tel. +44 (0)1865 726286. Fax +44 (0)1865 246823
World Wide Web home page: http://www.bios.co.uk/

Distributed exclusively in the United States, its dependent territories, Canada, Mexico, Central
and South America, and the Caribbean by Springer-Verlag New York Inc, 175 Fifth Avenue,
New York, USA, by arrangement with BIOS Scientific Publishers, Ltd, 9 Newtec Place,
Magdalen Road, Oxford OX4 1RE, UK
Section E – Spectrometric techniques

E4 F LAME ATOMIC EMISSION


SPECTROMETRY

Key Notes
Principles When the atoms of samples are excited to higher electronic energy levels
in flames they emit radiation in the visible and UV regions of the
electromagnetic spectrum. Emission intensities may be measured to
analyze for metals, especially alkali and alkaline earth elements.

Instrumentation A flame atomic emission spectrometer or flame photometer incorporates


a burner, monochromator, or filters, a detector and a method of
introducing the sample solution into the flame.

Applications The technique is used primarily for the quantitative determination of


alkali and alkaline earth metals in clinical, biological and environmental
samples.

Related topics Inductively-coupled plasma Atomic absorption and atomic


spectrometry (E5) fluorescence spectrometry (E7)

Principles When the salts of some metals are introduced into a flame, they impart charac-
teristic colors to it. For example, sodium salts give an intense yellow-orange
color. This is the basis of the ‘flame test’ used in qualitative analysis. The
thermal energy of a gas-air flame is quite low, since the temperature is usually
less than 2000 K and only those transitions of low energy are excited.
Early atomic emission instruments used electric arc or spark excitation. The
higher energy of these sources produced a very great number of emission lines
throughout the visible and UV regions. However, simultaneous measurement of
a large number of elements was possible.
With flame excitation, electronic transitions in alkali and alkaline earth
metals, as listed in Table 1 are the most important.

Table 1. Flame excited lines of some metals


Metal Wavelength/nm Color
Lithium 670 Red
Sodium 589a Orange–yellow
Potassium 766a Red
Rubidium 780a Dark red
Magnesium 285 UV
Calcium 622b Orange
Strontium 461 Red
Barium 554 Green
Thallium 535 Green
Copper 513 Green
a
These lines are doublets. bThis line is due to emission from a calcium hydroxide band.
E4 – Flame atomic emission spectrometry 207

Table 2. Gas mixtures used in flame atomic emission spectrometry


Fuel Oxidant Maximum flame temperature (K)
Natural gas Air 1800
Propane Air 1900
Hydrogen Air 2000
Acetylene Air 2450
Acetylene Nitrous oxide 2950
Acetylene Oxygen 3100

The flame may be produced by burning various gas mixtures, some of which
are listed in Table 2.
The structure of the flame comprises an inner cone, which is the primary
reaction zone for combustion, and the outer cone or mantle where secondary
reactions occur. For the best results, the optical axis is arranged to pass through
the flame at the junction of the inner and outer cones. The supply of fuel and
oxidant is adjusted to give an optimum burning velocity.
The processes that occur to transfer the sample to the flame may be summa-
rized as follows:
(i) production of an aerosol from solution (nebulization)
(ii) removal of solvent MA(aq) Æ MA (solid)
(iii) vaporization of sample MA(solid) Æ MA(vapour)
(iv) atomization MA Æ M• + A•
(v) excitation M• Æ M*
(vi) emission M* Æ M•
Ionization may also occur to give the M+ ion.
These stages each depend on the experimental parameters used in the
instrument. For example:
● the viscosity of the solvent, which affects the aerosol production;
● the nature of the solvent, which may affect the vaporization;
● the rate of fuel flow, which can change the nebulization and the time the
atoms spend in the flame;
● the flame temperature, which controls the evaporation, the atomization and
the extent of ionization; and
● the nature of the flame.
Because of the chemical reactions taking place in the flame, various species such
as OH radicals, CO, water and other combustion products are present, and may
give a background emission throughout the UV-visible range. Compensation for
this background must be made.

Instrumentation Flame atomic emission spectrometers have similar optical systems to those of
UV-visible spectrometers, but the source of radiation is provided by the sample
itself. A flame photometer is a simpler instrument employing narrow bandpass
optical filters in place of a monochromator (Fig. 1). The sample is prepared as a
solution, which is drawn into a nebulizer by the effect of the flowing oxidant
and fuel gases. The fine droplets produced pass into the flame where sample
atoms are progressively excited. The emitted radiation passes through the
monochromator or filter and is detected by a photocell or photomultiplier tube.
208 Section E – Spectrometric techniques

Photo
Flame detector
Filter Readout

410.0

Amplifier
Gas inlet

Constant Nebulizer
head drain
Mixing chamber

Waste

Air

‘U’ tube

Fig. 1. Schematic of a flame photometer. Reproduced with permission from Sherwood


Scientific Ltd.

Applications Flame atomic emission spectrometry (FAES) and flame photometry are used
widely for the determination of alkali and alkaline earth metals. The rapid
determination of Na, K and Ca in biological and clinical samples is one of the
most important applications; for example, calcium in beer, milk or biological
fluids. The usual solvent is water, but organic solvents may be used to enhance
the intensity, since they produce smaller droplets, and have a smaller cooling
effect on the flame.
The instrument is calibrated with standard solutions of the elements to be
determined and the intensity of the emission recorded at each characteristic
wavelength. A calibration graph is constructed after correcting for background
(blank) emission.
Interferences may affect the linearity of the calibration and are chiefly due to
the emission lines produced by other species close to those of the analyte. They
may be minimized by selecting a different spectral line for the analysis, or by
altering the spectral resolution or filter. The presence of anions that form very
stable compounds with the metal ions, such as sulfate and phosphate may
interfere with some determinations.
At high analyte concentrations, the concentration of atoms in the flame may
be high enough to cause self-absorption. That is, the emission is reabsorbed by
the ground state atoms in the cooler outer layers of the flame. This sometimes
causes a loss in sensitivity at higher concentrations.
The advantages of FAES and flame photometry are that the instrumentation
is relatively simple and measurements can be made quickly. A disadvantage is
the sensitivity of the emission intensities to changes in flame temperature due to
variations in gas flow, or cooling by the solvent.
Library of Congress Cataloging-in-Publication Data

Kenkel, John.
Analytical chemistry for technicians / by John V. Kenkel. — 3rd ed.
p. cm.
Includes index.
ISBN 1-56670-519-3 (alk. paper)
1. Chemistry, Analytic. 1. Title.

QD75.22 .K445 2002


543—dc21 2002029654

This book contains information obtained from authentic and highly regarded sources. Reprinted material is quoted with
permission, and sources are indicated. A wide variety of references are listed. Reasonable efforts have been made to publish
reliable data and information, but the author and the publisher cannot assume responsibility for the validity of all materials
or for the consequences of their use.

Neither this book nor any part may be reproduced or transmitted in any form or by any means, electronic or mechanical,
including photocopying, microfilming, and recording, or by any information storage or retrieval system, without prior
permission in writing from the publisher.

The consent of CRC Press LLC does not extend to copying for general distribution, for promotion, for creating new works,
or for resale. Specific permission must be obtained in writing from CRC Press LLC for such copying.

The United States Federal Government retains a nonexclusive, nontransferable, irrevocable, royalty-free license to exercise
or have exercised for or on behalf of the United States throughout the world all the exclusive rights provided by copyright.
Such license does not include the right to see copies or photocopies of this work.

This material is based upon work supported by the National Science Foundation under Grant Nos. DUE9751998 and
DUE9950042.

Direct all inquiries to CRC Press LLC, 2000 N.W. Corporate Blvd., Boca Raton, Florida 33431.

Trademark Notice: Product or corporate names may be trademarks or registered trademarks, and are used only for
identification and explanation, without intent to infringe.

Visit the CRC Press Web site at www.crcpress.com

© 2003 by CRC Press LLC


Lewis Publishers is an imprint of CRC Press LLC

No claim to original U.S. Government works


International Standard Book Number 1-56670-519-3
Library of Congress Card Number 2002029654
Printed in the United States of America 2 3 4 5 6 7 8 9 0
Printed on acid-free paper

Copyright © 2003 CRC Press, LLC


Atomic Spectroscopy 265

WORKPLACE SCENE 9.3

T
he determination of trace metallic ele-
ments is important to material process-
ing, recovery, environmental sampling,
and remediation programs at Los Alamos
National Laboratory. Samples are received in
the liquid or solid state and are prepared and
analyzed according to approved Environmental
Protection Agency (EPA) methods or proce-
dures. This analysis procedure involves the
standardization and calibration of the induc-
tively coupled plasma atomic emission (ICP-
AES) system with known concentrations of
analytes of interest. The calibration and stan-
dardization data obtained are then used to
determine the concentration of trace metallic
elements (analytes) in the samples. During the
treatment, preparation, segregation, and anal- MaryAnn Abeyta, a technician with the Los Alamos
ysis of samples using the ICP-AES system, sig- National Laboratory, analyzes samples using an IRI-
nificant quantities of residue and chemical SICP-AES spectrometer.
waste are generated. Thus the proper disposal
of waste and residue according to waste disposal
is also an important part of this effort.

FIGURE 9.22 The standard curve for ICP quantitative


analysis: intensity vs. concentration. C

ICP has been coupled with another analytical technique known as mass spectrometry. This technique,
as well as the technique coupling it with ICP, will be described in Chapter 10.

9.6 Miscellaneous Atomic Techniques

9.6.1 Flame Photometry


Flame photometry is the name given to the technique that measures the intensity of the light emitted by
analyte atoms in a flame. It is the oldest of all the atomic techniques. It is not highly applicable because
of the low temperature of the flame. Only a handful of elements can be measured with this technique,
including sodium, potassium, lithium, calcium, strontium, and barium. The technique was formerly used

Copyright © 2003 CRC Press, LLC


266 Analytical Chemistry for Technicians

by hospital and clinical laboratories for measuring these elements in body fluids, but has been supplanted
by the use of ion-selective electrodes (see Chapter 14). Instruments designed for flame atomic absorption
can be used as flame photometers. It is a mode of operation in which the hollow cathode is not used
and the detector measures the flame emissions. Advantages are simple, inexpensive instruments and
acceptable sensitivities for the metals listed. Disadvantages include less sensitivity than other techniques.
The standard curve for quantitative analysis is intensity vs. concentration, as shown in Figure 9.22 for ICP.

9.6.2 Cold Vapor Mercury


Mercury is the only metal that is a liquid at ordinary temperatures. It is therefore also the only metal
that has a significant vapor pressure at ordinary temperatures. For this reason, it is possible to obtain
mercury atoms in the gas phase for measurement by atomic absorption without the use of thermal energy.
It is a matter of chemically converting mercury ions in the sample into elemental mercury, getting it in
the gas phase, and channeling it into the path of the light of an atomic absorption instrument.
Reducing agents typically used for the conversion of mercury ions in solution to elemental mercury
include stannous chloride (SnCl2) and sodium borohydride (NaBH4). Elemental mercury, the product
of the reduction, is converted to the gas phase by simply bubbling air through the solution. The mercury–
air mixture is channeled to a quartz absorption cell, a long-path-length tube positioned in the path of
the light from a mercury hollow cathode lamp, and the absorption is measured. The gas phase mixture
is ultimately channeled to waste. The sensitivity is far greater than what can be achieved with flame AA.

9.6.3 Hydride Generation


A useful technique for the otherwise difficult elements of arsenic, bismuth, germanium, lead, antimony,
selenium, tin, and tellurium is the hydride generation technique. This technique is similar to the cold
vapor mercury technique in that a reducing agent, in this case sodium borohydride, is used to convert
ions of these metals to a more useful state—in this case, to hydrides, such as AsH3. Hydrides of the
metals listed above are volatile and can be channeled to an absorption cell using moving air, as in the
cold vapor mercury technique. Once in the absorption cell, however, the gaseous mixture must be heated
in order to achieve atomization. Heating can be accomplished with a low-temperature flame or with an
electrical heating system. As with cold vapor mercury, the vapor in the cell is ultimately channeled to
waste. Absorbance is measured and Beer’s law applies.
Advantages include a very acceptable method for the elements listed when other techniques for these
elements fail. Sensitivity for these elements is also very good.

9.6.4 Spark Emission


A technique that utilizes a solid sample for light emission is spark emission spectroscopy. In this technique,
a high voltage is used to excite a solid sample held in an electrode cup in such a way that when a spark
is created with a nearby electrode, atomization, excitation, and emission occur and the emitted light is
measured. Detection of what lines are emitted allows for qualitative analysis of the solid material.
Detection of the intensity of the lines allows for quantitative analysis.

9.6.5 Atomic Fluorescence


Molecular fluorescence, described in Chapter 8, has a counterpart in atomic spectroscopy called atomic
fluorescence. In order for atoms to emit light of a different wavelength than that which was absorbed,
they must detour to an intermediate excited state before returning to the ground state. This can occur
when the light absorbed elevates the atoms to a higher excited state than the first excited state, so that
the route back to the ground state includes the first excited state and thus a fluorescence—light of less
energy being emitted. The light must be measured at right angles, as with the molecular instruments.
This technique is not popularly used.

Copyright © 2003 CRC Press, LLC


ISSN: 0975-8585

Research Journal of Pharmaceutical, Biological and Chemical


Sciences
Comparison of sodium and potassium content in ORS powders by Flame
photometric method

Priyadatta Mishra, Manoj Kumar Mahapatra*

Royal College of Pharmacy and Health Sciences, Andhapasara Road, Berhampur-760002, Odisha, India.

ABSTRACT

A study was carried out to determine the content of Na and K in two different brands of ORS powder by
Flame photometric method. The Na content was found to be higher in Govt. supplied sample and K content was
higher in the private sample.
Keywords: ORS powder, Flame photometry, Sodium, Potassium.

*Corresponding author:

July – September 2016 RJPBCS Volume 2 Issue 3 Page No. 262


ISSN: 0975-8585

INTRODUCTION

Fluid and electrolyte balance is vital for good health at all ages. In dehydration
associated with diarrhoea, gastroenteritis, cholera and dysentery the body is devoid of water
and electrolytes. ORT (oral rehydration therapy) is the simple treatment which involves
administering a solution of salts and sugars for replenishing electrolyte and water content of
the body. Sodium is the major cat-ion found in the extracellular fluid. It regulates the water
content of the body and is critical for generation of electrical signals. Similarly, Potassium is the
major cat-ion found inside the cells. It is required for regulation of heart beat and function of
the muscles. The Sodium and Potassium concentration of ORS must be sufficient to replace
their loss and correct hyponatremia/hypokalemia but not so high as to cause or worsen
hypernatremia/hyperkalemia which can itself occasionally result in death.

Therefore, it is important to quantify the amount of Sodium and Potassium present in


the ORS powder. Flame photometry is a branch of Atomic emission spectroscopy. It is suitable
for quantitative and qualitative determination of several cat-ions, [1] especially for metals that
are easily excited to higher energy level at a relatively low flame temperature (mainly Na, K, Ca,
Rb, Cu, Ba, Cs). A simple Flame photometric method is described in this paper for the
determination of Sodium and Potassium content of the ORS powder.

MATERIALS AND METHODS

Instrument- SYSTRONICS Flame Photometer 128

Chemicals- Sodium chloride, Potassium chloride, ORS powder


Two different brands of ORS sachets (WALYTE and Govt. supplied ORS) were purchased
and analyzed for their Sodium and Potassium content.

ORS sample 1- WALYTE (Oral Rehydration Salts, I.P): 21 gm


Composition: Sodium chloride- 2.6 gm, Potassium chloride- 1.5 gm, Sodium citrate- 2.8 gm,
Dextrose- 13.4 gm, Excipient- q.s

ORS sample 2- ORS: 21 gm


Composition: Sodium chloride- 2.6 gm, Potassium chloride- 1.5 gm, Sodium citrate- 2.9 gm,
Anhydrous dextrose- 13.5 gm, Excipient- q.s

Preparation of standard Sodium chloride solution

2.54 gm of Sodium chloride was dissolved and the volume was made up to 1L with
double distilled water. 1ml of the solution was diluted up to 10 ml with double distilled water to
get a conc. of 105µg/L (i.e, 100 ppm).

July – September 2016 RJPBCS Volume 2 Issue 3 Page No. 263


Available online www.jocpr.com

Journal of Chemical and Pharmaceutical Research

J. Chem. Pharm. Res., 2016, 3(6):1097-1102


ISSN No: 0975-7384
CODEN(USA): JCPRC5

Determination of Estimation of Potassium Ion in Dry Fruits by


Flame Photometry and Their Proximate Analysis
Venkatesh K. Mutalik*, Jagadish G. Baragi, Somaraddi B. Mekali, C. Veeresh Gouda and
N.B. Vardhaman

Department of Chemistry, J.S.S. College, Vidyagiri, Dharwad, Karnataka(India)

ABSTRACT
Studies were carried out on dry fruits Almond, Cashewnut, Pepper, Pistachious, Drydates,
Raisin(black), Raisin(common), Amla, Acrota, Apricot to determine the Potassium ion
concentration in them. Chemical analysis of the extracts of the fruits revealed that moisture was
4.2% in pepper, to 22.7% in raisin black. The ash value ranged from 1.80% in acrota to 4.05%
in apricot, while dry matter ranged from 77.3% in raisin black to 95.8% in Pepper. Fruits with
low moisture content could store for longer time without spoilage. Potassium was found to be the
most abundant with a level as high as 125.1 mg/100g in apricot and as low as 21.84 mg/100g in
Chinese beans. The results showed that the fruits have safe and adequate dietary nutrients if
consumed in right proportion. Present work to determine Potassium is based on flame
photometry and it is very simple, inexpensive and less time consuming. This method is properly
validated using standard chemicals and it can be applied to formulation.

Key words: Fruits, Potassium, Flame photometry, Dry fruits, Dry matter.

INTRODUCTION

Fruits are generally acceptable as good source of nutrient and supplement for food in a world
faced with problem of food scarcity. They are known to be excellent source of nutrients such as
minerals and vitamins [1]. Mineral ions are of prime importance in determining the fruit
nutritional value. Potassium, calcium and magnesium are the major ones. In the tissue of many
fruits, calcium is one of the mineral believed to be an important factor governing fruit storage
quality [2]. It has been reported to delay ripening and senescence [3] and to reduce storage
disorder [4]. The importance of minerals such as potassium, calcium, sodium etc. to human
health is well known. Required amounts of these elements must be in human diet to pursue good
healthy life [5]. The content of mineral elements in plants depends to a high degree on the soils
abundance, including the intensity of fertilization [6]. Dry fruits contain substantial quantities of

1097
Venkatesh K. Mutalik et al J. Chem. Pharm. Res., 2016, 3(6):1097-1102

essential nutrients in a rational proportion. They are excellent source of minerals, vitamins and
enzymes. They are easy to digest and clean the blood and the digestive area [7]. Dried fruits
retain most of the nutritional value of fresh fruits, and so are included with fresh fruit in dietary
recommendations by U. S.[8] and world health agencies. The specific nutrient content of the
different dried fruits reflect their fresh counterpart and the processing method (e.g. traditional
dried fruits versus sugar infused dried fruit). In general, all dried fruits provide essential nutrients
and an array of health protective bioactive ingredients, making them valuable tools to both
increase diet quality and help reduce the risk of chronic disease. The combination of nutritional
value and enjoyable taste is the reason dried fruits have been popularly considered a healthy food
for millennia. Because they are naturally resistant to spoilage, easy to store and transport and
relatively low in cost, dried fruits are a convenient way to increase the number of servings of
fruit in the diet. One of the most important parts of prevention is good nutrition. Making sure that
you regularly consume the standard recommended daily intake levels of the vitamins, mineral
and other nutrients your body needs is the first vital step in keeping a healthy physic and mind
[13].

But because of today's lifestyle and diet, it is very hard therefore to intake the proper daily
amount of potassium necessary for a normal life. For this concern, nutritional supplements are
the solution.

Potassium (K) is the major cation found inside of cells [14]. The proper level of Potassium is
essential for normal cell function. An abnormal increase of potassium (hyperkalemia) or
decrease of potassium (hypokalemia) can profoundly affect the nervous system and heart, and
when extreme, can be fatal. The normal blood potassium level is 3.5 - 5.0 millimoles/liter
(mmol/l).

Potassium also plays an important role to mental function as well as to physical processes. It
helps to promote efficient cognitive functioning by playing a significant role in getting oxygen to
the brain [15].

In view of the nutritional and health benefits of dry fruits, their daily need in our diet and the
effects of anti nutritional factors, this study was designed to determine the Potassium ion in
highly nutritive dry fruits such as almond, cashewnut, pepper, Pistachious, drydates, raisin(black),
raisin(common), amla, acrota, apricot by Flame photometry method.

Flame photometry is a highly empirical, rather than an absolute, method of analysis such as
gravimetry. That is, we must calibrate the method carefully and frequently. Many different
experimental variables affect the intensity of light emitted from the flame and that finding its
way to the detector. Therefore, careful and frequent calibration is required for good results.

EXPERIMENTAL SECTION

Sample Preparation:
Eleven dry fruits namely almond, cashewnut, pepper, pistachious, drydates, raisin (black),
raisin(common), amla, acrota, apricot and kheerbhez were obtained commercially from market.
They were washed with distilled water and external moisture is removed with a dry cloth. The
individual fruit was separated, dried in hot air oven at 50 0C for 1 h. The dried samples were then
powdered in blander [16] and sieved with a 2 mm rubber and 2 g of each of fruit sample powder
was weighed and subjected to dry ashing in a well-cleaned silica crucible at 5500C in a muffle
furnace for about 5 h [17]. The resultant ash was dissolved in 5 mL HNO 3 / HCl / H2O (1:2:3),

1098
Venkatesh K. Mutalik et al J. Chem. Pharm. Res., 2016, 3(6):1097-1102

fruits may have high nutritive value. Low values of %RSD highlighted the reproducibility of the
results.

Analyses can be made far more rapidly by the flame photometer compared to the best
gravimetric and volumetric methods. With flame photometry, results can be produced promptly
because of the direct analysis which is not possible with chemical methods. While both time and
material may be saved by the use of the flame photometer, the responsibility of the operator is in
no way reduced.

Once the range has been established and remains stable, it is often possible to take many
successive readings which are reproducible and constant over a long period of time. In Table 2,
the results of potassium content in standard solution are given. Validation data obtained with
standard solutions are shown in Table.3, which demonstrate that the method is suitable for the
analysis of potassium in several dry fruit extracts. The reproducibility of the results was evident
from low % RSD values.

The applicability of the proposed method was examined by analyzing the content of potassium in
different dry fruits and the corresponding results are shown in Table 4. The amounts of
potassium in fruits like cashew nut, dry date and apricot were found to agree with of methods
[18-20]. Potassium was found to be the most abundant with a level as high as 125.1 mg/100g in
apricot and as low as 21.84 mg/100g in Chinese beans.

Table.1: Proximate composition of fruits

S.
No. Fruit Sample Moisture* (%) %RSD Ash*, % %RSD Dry matter* (%) %RSD
Kheer BeeZ
1. 7.2 1.65 2.74 1.67 92.8 2.12
(Chinese beans)
2. Almond 7.4 1.78 2.81 1.98 92.6 2.05
3. Cashew 6.9 2.05 2.64 1.54 93.1 1.76
4. Pepper 4.2 2.12 3.51 1.49 95.8 1.98
5. Pistachious 7.3 2.04 2.78 2.11 92.7 1.58
6. Dry Dates 9.1 1.99 1.88 1.89 91.9 2.14
7. Raisin(Black) 22.7 1.64 2.18 2.15 77.3 2.02
8. Raisin(Common) 21.2 2.15 1.87 2.08 78.8 1.74
9. Amla 10.7 1.87 2.68 2.03 89.3 1.59
10. Acrota 4.7 1.66 1.80 1.56 95.3 2.04
11. Apricot 11.09 1.89 4.05 1.96 88.9 2.13
* Average of 5 determinations

Table.2: Data for Standard Potassium solution Analysis

S. No. Potassium (K+)


Standard Solution Amount Present Amount* Found % Found %RSD
1 20 mg/L 0.512 0.510 99.6 2.16
2 40 mg/L 1.024 1.021 99.7 2.22
3 60 mg/L 1.536 1.528 99.5 2.04
4 80 mg/L 2.048 2.050 100 2.34
5 100 mg/L 2.56 2.54 99.22 1.87
* Average of 5 determinations

Table.3: Statistical Validation for the analysis of Standard Potassium solution


Component Mean value* % RSD* %Error*
+
Potassium(K ) 100.0 99.12 1.48 0.88
* Average of 5 determinations

1100
J. Akademika Kim. 5(3): 127-132 August 2016
ISSN 2302-6030 (p), 2477-5185 (e)

PENGARUH EKSTRAK SELEDRI (Apium graveolens L.) TERHADAP


KELARUTAN KALSIUM DALAM BATU GINJAL

Effect of Celery (Apium graveolens L.) Extract Against the Solubility of


Calcium Kidney Stones

*Evie Kurnia Maya Dewi, Daud K. Walanda, dan Sri Mulyani Sabang
Pendidikan Kimia/FKIP - Universitas Tadulako, Palu - Indonesia 94118
Received 10 June 2016, Revised 11July 2016, Accepted 11 August 2016

Abstract
Celery (apium graveolens L.) contains chemicals that can be used as traditional medicine for various
treatments. The research objective is to determine the effect of celery (apium graveolens L.) extractsin
dissolving calcium kidney stones and calcium to determine the relationship between the concentration of
extract of celery (apium graveolens L.) with the solubility of calcium in the kidney stones. Determination
of the solubility of calcium in an extract of celery is by flame fotometer. The concentration of the extract
was varried into 1%, 5%, 10%, 15% and 20%. To a concentration of 1% can dissolve the calcium as
much as 15.104%; concentration of 5% can dissolve the calcium as much as 18.708%; concentration
of 10% can dissolve the calcium as much as 23.683%; concentration of 15% can dissolve the calcium
as much as 28.869%; and to a concentration of 20% can dissolve the calcium as much as 35.048%. It
can be concluded that celeries extract can dissolve calcium of kidney stones.
Keywords: Celery (apium graveolens L); calcium; kidney stone; solubility

Pendahuluan
Pemanfaatan tumbuhan sebagai obat sudah mahal, sedangkan kebanyakan masyarakat
seumur dengan peradaban manusia. Tumbuhan memiliki tingkat ekonomi menengah ke
itu sendiri memiliki banyak manfaat termasuk bawah, sehingga tidak semua penderita dapat
untuk obat berbagai penyakit. Penggunaan melakukan pengobatan yang bereaksi dengan
bahan alam sebagai obat cenderung mengalami cepat tersebut. Adanya pengobatan tersebut
peningkatan dengan adanya back to nature membuat obat tradisional menjadi ketinggalan
dan krisis ekonomi berkepanjangan yang zaman, namun kenyataan membuktikan bahwa
mengakibatkan turunnya daya beli masyarakat obat tradisional mempunyai banyak sekali
terhadap obat-obat modern yang relatif mahal keunggulan selain murah dan mudah didapat,
harganya (Ismadi, 1978). yang lebih penting adalah tidak memiliki efek
Seiring dengan kemajuan dunia kesehatan samping yang nyata, seperti yang ditimbulkan
dan teknologi, cara pengobatan penyakit batu oleh pengobatan alternatif yang lain. Agar
ginjal banyak memberikan alternatif, baik peranan obat tradisional dapat ditingkatkan,
dengan obat-obatan (obat sintesis maupun maka diperlukan upaya pengenalan, penelitian
obat tradisional), operasi dan penyinaran dan penggujian khasiat serta keamanannya
khusus untuk batu ginjal. Banyaknya alternatif (Ismadi, 1978). Terapi medis (penggunaan
pengobatan tersebut para penderita penyakit diuretik dan oabat-obatan lainnya), penggunaan
batu ginjal lebih memilih mengkonsumsi obat- lebih dari obat sintetik yang menghasilkan
obat sintesis, melakukan operasi, dan penyinaran insiden yang lebih tinggi dari reaksi obat yang
yang memiliki daya reaksi yang cepat. Namun merugikan telah memotivasi masyarakat untuk
pengobatan tersebut bukanlah pengobatan kembali ke alam untuk obat yang aman (Rajat
yang murah melainkan pengobatan yang sangat dkk., 2011).
*Correspondence: Tumbuhan seledri (Apium graveolens L)
Evie Kurnia Maya Dewi merupakan salah satu tanaman berkhasiat yang
Program Studi Pendidikan Kimia, Fakultas Keguruan dan banyak digunakan oleh masyarakat, juga sebagai
Ilmu Pendidikan, Universitas Tadulako
email: evieekurnia@gmail.com penyedap dalam makanan (Rukmana, 1995).
Published by Universitas Tadulako 2016 Seledri berkhasiat memacu enzim pencernaan
127
Volume 5, No. 3, 2016: 127-132 Jurnal Akademika Kimia

sebagai berikut : kalsium standar secara berturut-turut yaitu


Tabel 2. Data Serapan Variasi Ekstrak Seledri 11,10 ; 32,30 ; 55,30 ; 81,60 ; 105,10 ; dan
Terhadap Konsentrasi Kalsium 131,50.
Selanjutnya melakukan uji kelarutan batu
ginjal, dimana sebelum diujikan dengan batu
ginjal, terlebih dahulu diujikan dengan kalsium
fosfat karena kalsium fosfat salah satu komposisi
batu ginjal. Selain itu juga agar batu ginjal yang
dibutuhkan tidak terlalu banyak, mengingat
karena batu ginjal sulit diperoleh. Dalam uji
kelarutan batu ginjal ini sampel dibuat menjadi
beberapa variasi konsentrasi yaitu konsentrasi
1%, 5%, 10%, 15%, dan 20%. Hal ini
Tabel 3.Data Peningkatan Ca Pada dilakukan untuk mengetahui tingkat kelarutan
Ekstrak Seledri Setelah Pengocokan dengan kalsium dalam batu ginjal, maka perlakuannya
PenambahkanKalsium Fosfat dibuat sama pada setiap sampel hanya saja
konsentrasinya dibedakan. Setelah membuat
konsentrasi ekstrak seledri, selanjutnya
dilakukan dua kali perlakuan dimana
perlakuan pertama sampel belum ditambahkan
kalsium fosfat, sedangkan perlakuan kedua
sampel telah ditambahkan 0,1 gram kalsium
fosfat kemudian dikocok selama 24 jam
menggunakan magnetik stirer. Tujuannya
adalah untuk mendapatkan kondisi seperti
yang terjadi dalam tubuh, khususnya dalam
Berdasarkan Tabel 3. dapat dibuat kurva organ ginjal yang kemudian bergerak kesaluran
hubungan antara konsentrasi seledri terhadap kemih sebagai tempat biasa ditemukannya batu
peningkatan kadar Ca (%) sebagai berikut ginjal itu sendiri (Lusiyanah, 2011). Setelah
itu larutan didiamkan, selanjutnya disaring
sehingga diperoleh filtratnya kemudian diukur
absorbansinya dengan menggunakan flame
fotometer.
Berdasarkan Tabel 3 dan kurva pada
Gambar 1 diperoleh informasi bahwa dengan
meningkatnya konsentrasi ekstrak seledri
maka semakin banyak kalsium dari batu ginjal
yang terlarut dinyatakan dalam peningkatan
kadar Ca (%), maka dari data pada Tabel 3
ini dapat dilihat bahwa pada konsentrasi 1%
Gambar 1. Kurva Hubungan Antara hingga 20% peningkatan kadar Ca bertambah.
Konsentrasi Seledri (%) Terhadap Peningkatan Meningkatnya konsentrasi ekstrak seledri
Kadar Ca (%). tersebut juga meningkatkan absorbansinya,
dimana kadar kalsium yang terlarut dalam
ekstrak seledri dapat dilihat dari selisih antara
Larutan standar yang digunakan yaitu konsentrasi kalsium sebelum dan sesudah
larutan kalsium standar 1000 ppm, dibuat penambahan batu ginjal (Lusiyanah, 2011).
deret baku dengan konsentrasi 0 ppm, 20 ppm, Nilai selisih konsentrasi yang diperoleh pada
40 ppm, 60 ppm, 80 ppm, dan 100 ppm. masing-masing konsentrasi dapat dilihat pada
Konsentrasi larutan standar yang bervariasi ini Tabel 3, dimana dari Tabel 3 dapat dibuat
dilakukan agar nantinya diperoleh suatu grafik kurva perbandingan antara konsentrasi seledri
yang memiliki garis linear yang mengikuti (%) terhadap peningkatan kadar Ca (%).
hukum Lambert-Beer yaitu absorbansi Setiap konsentrasi ekstrak seledri yang
berbanding lurus dengan konsentrasi uap atom belum ditambah kalsium posfat dan yang telah
dalam nyala. Absorbansi yang diperoleh dari ditambah kalsium fosfat dianalisis kalsiumnya

130
Evi Kurnia Pengaruh Ekstrak Seledri (Apium graveolens L.) ................

dengan mengunakan flame fotometer, pihak yang telah membantu dalam pelaksanaan
dari hasil absorbansi yang diperoleh dapat penelitian.
menentukan konsentrasi kalsium pada masing-
masing konsentrasi sampel baik yang sebelum Referensi
ditambah kalsium posfat dan yang telah
ditambah kalsium posfat seperti tertera pada Ankur, C., Amarchand, P., Aadarsh, C., &
Tabel 3. Deepa, I. (2010). Potential of medicinal
plants in kidney, gall and urinary stones.
Kurva pada Gambar 1 menunjukan bahwa International Journal of Drug Development
ektrak seledri dapat melarutkan kalsium and Research, 2(2), 431-447.
dalam kalsium posfat, dimana semakin besar
konsentrasi ekstrak seledri maka semakin Coe, F. L., Evan, A., & Worcester, E. (2005).
banyak kalsium yang terlarut, ini dapat dilihat Kidney stone disease. Journal Clin Inverst,
dari nilai selisih konsentrasinya. Ini disebabkan 115, 2598-2608.
karena adanya efek dari ion sekutu dan ion Dalimartha, S. (2000). Atlas tumbuhan obat
asing. Ion sekutu adalah suatu ion yang indonesia jilid II. Jakarta: PT. Trubus
juga merupakan salah satu bahan endapan. Agriwidya.
Umumnya dapat dikatakan bahwa kelarutan
suatu endapan dapat berkurang jika salah satu Dalimartha, S. (2002). Resep tumbuhan obat
ion sekutu terdapat dalam sampel. Dalam untuk penderita osteoporosis. Jakarta: Penebar
hal ini kalsium merupakan ion sekutunya Swadaya.
karena terdapat pada ekstrak seledri sebelum
maupun sesudah penambahan kalsium posfat, Hardi, S. (2005). Hancurkan batu ginjal dengan
namun karena adanya ion asing pada ekstrak ramuan herbal. Jakarta: Puspa Swara.
seledri tersebut, sehingga dapat meningkatkan
kelarutan kalsium pada kalsium posfat
(Lusiyanah, 2011). Hidayati, A., Yusrin, & Anggraini, H. (2009).
Salah satu faktor yang mempengaruhi Pengaruh frekuensi penggunaan teh daun
kelarutan kalsium yaitu adanya kalium yang tempuyung kering (sonchus arvensis)
terkandung dalam ekstrak seledri. Ion-ion terhadap daya larut kalisum oksalat
kalium yang cukup tinggi, dapat menjaga (CaC2O4). Jurnal Kesehatan, 2(2), 30-37.
keseimbangan elektrolit pada ginjal. Kalium
inilah yang membuat batu ginjal terurai, Hutapea, J. R. (1994). Inventaris tanaman obat
karena kalium akan menyingkirkan kalsium indonesia edisi III. Jakarta: Departemen
dan bergabung dengan senyawa kalsium fosfat Kesehatan Republik Indonesia Badan
yang merupakan pembentuk batu ginjal dengan Penelitian dan Pengembangan Kesehatan.
membentuk senyawa garam yang mudah larut
dalam air, sehingga batu ginjal itu akan
terlarut secara perlahan-lahan dan ikut keluar Ismadi. (1978). Kuliah penyegaran nefrologi.
bersama urine dengan reaksi kimia sebagai Yogyakarta: Fakultas Kedokteran Universitas
berikut (Hidayati dkk., 2009). Gadjah Mada.

Lusiyanah. (2011). Pengaruh konsentrasi ekstrak


akar dari akar kucing (acalypha indica)
terhadap kelarutan kalsium pada batu ginjal.
Kesimpulan
Ekstrak seledri memiliki efek melarutkan Palu: Universitas Tadulako.
kalsium dalam batu ginjal jenis kalsium oksalat-
fosfat. Kelarutan kalsium dalam batu ginjal Maharani, E. T., Mukamorah, A. H., & Susilo,
berbanding lurus dengan konsentrasi ekstrak J. (2012). Analisis kalium dan prosentase
seledri. Sehingga semakin tinggi konsentrasi daya larut kalsium oksalat oleh kalium
ekstrak seledri maka kelarutan kalsium semakin dalam air teh daun sukun (artocarpus altilis).
besar. Semarang: Fakutas Farmasi Universitas
Muhammadiyah Semarang.
Ucapan Terima Kasih
Penulis mengucapkan terimakasih sebesar-
besarnya kepada kepala laboran laboratorium Mursito, B. (2003). Ramuan tradisional untuk
Agroteknologi Fakultas Pertanian dan semua gangguan ginjal. Jakarta: Penebar Swadaya.

131
J. Akad. Kim. 3(2): 93-97, May 2014
ISSN 2302-6030
ANALISIS KADAR MINERAL NATRIUM DAN KALIUM PADA DAGING
BUAH NANAS (ANANAS COMOSUS (L) MERR) DI KOTA PALU

The Analysis of Sodium Mineral Level and Potassium in Pineapple Flesh (Ananas
comosus (L) Merr) in Palu City.
*Nurjayanti Abdullah Sada, Nurdin Rahman dan Supriadi
Pendidikan Kimia/FKIP - Universitas Tadulako, Palu - Indonesia 94118
Recieved 10 April 2014, Revised 09 May 2014, Accepted 12 May 2014

Abstract
Mineral is inorganic component which is in the human body. The needs of mineral for the body
can be obtained by consuming fruits. Pineapple (Ananas comosus (L) Merr) is one of fruits contains
mineral such as potassium (K) and sodium (Na). the objective of the research was to analysis the mineral
level (Na and K) contained in pineapple flesh that spread out in Palu City. The analysis of Na and K
mineral level used flame photometry analysis. The research result show that pineapple Cayenne varieties
(common pineapple) contains sodium mineral as much 3.71 mg/kg and potassium as much at 376 mg/
kg. The pineapple Queen varieties (Bogor pineapple) contains mineral sodium as much as 2.41 mg/kg
and potassium as much as 198 mg/kg.
Keywords : Queen Pineapple, Cayenne Pineapple, Flame Photometry, Sodium, and Potassium

Pendahuluan
Nanas (ananas comosus (L) merr) 0,04 mg, niasin 0,24 mg dan vitamin A 5,3 IU
merupakan salah satu jenis buah yang umum ( Irfandi, 2005 ; Khamidah, 2009)
dikenal dan dikonsumsi oleh masyarakat Kalium dan natrium merupakan contoh
Indonesia (Sembayang, 2006) dan merupakan mineral yang terdapat dalam nanas. Kalium
suku Bromeliaceae (Dewi, 2013). Buah ini bersama-sama dengan klorida berfungsi
banyak digunakan pada beberapa industri membantu menjaga tekanan osmotik dan
olahan pangan seperti selai, sirup, sari buah, keseimbangan asam basa dalam menjaga
serta buah dalam botol atau kaleng (Widiawati, cairan intraseluler dan sebagian terikat dengan
2009). Menurut sejarah tanaman ini berasal protein. Kalium juga membantu mengaktivasi
dari Brasil dan dibawa ke Indonesia oleh para reaksi enzim, seperti piruvat kinase yang dapat
pelaut Spanyol dan Portugis sekitar tahun 1599
(Hidayat, 2008). Anatomi nanas berbentuk menghasilkan asam piruvat dalam metabolism
semak, dengan daun panjang berbentuk karbohidrat. Mereka yang mendapatkan asupan
pedang, tebal dan liat serta mempunyai duri kalium lebih tinggi cenderung memiliki tekanan
yang menempel dibagian pinggirnya. Buah darah lebih rendah dan orang dengan tingkat
yang sudah masak berwarna kuning/oranye darah rendah kalium yang sedang menjalani
(Pracaya, 2011). operasi jantung berisiko lebih tinggi untuk
Kandungan gizi, vitamin dan mineral dalam mengembangkan aritmia jantung. Asupan
100 g buah nanas sebagai berikut : air 86 g, kalori natrium yang berlebihan dapat meningkatkan
218 kj, protein 0,5 g, lemak 0,2 g, karbohidrat kebutuhan tubuh kalium (Andarwulan, 2011)
3,5 g, serat 0,5 g, dan abu 0,3 g. Kandungan Natrium menjaga keseimbangan asam basa
mineralnya sebagai berikut: kalsium 18 mg, di dalam tubuh dengan mengimbangi zat–
besi 0,3 mg, magnesium 12 mg, pospor 12 mg, zat yang membentuk asam. Berperan dalam
kalium 98 mg, dan natrium 1 mg. Kandungan transmisi saraf dan kontraksi otot. Natrium
vitamin C 10 mg, tiamin 0,09 mg, riboflavin berperan pula dalam absorpsi glukosa dan
*Korespondensi: sebagai alat angkut zat–zat gizi lain melalui
Nurjayanti Abdullah Sada membran, terutama melalui dinding usus
Program Studi Pendidikan kimia, Fakultas Keguruan dan sebagai pompa natrium (Almatsier, 2005).
Ilmu Pendidikan, Universitas Tadulako
email: nur232377@gmail.com Menurut Pardede (2012) perubahan kadar
© 2014 - Program Studi Pendidikan Kimia Universitas Tadulako natrium dapat mempengaruhi tekanan darah
93
Volume 3, No. 2, 2014: 93-97 Jurnal Akademika Kimia

tetapi tidak dengan sendirinya menyebabkan mengukur konsentrasinya dengan Fotometri


tekanan darah tinggi. Meskipun demikian, Nyala. Sebelum dilakukan pengukuran natrium
terdapat cukup banyak bukti yang mendukung dan kalium pada sampel, terlebih dahulu alat
anggapan bahwa mengurangi asupan natrium fotometri nyala di kalibrasi dengan air suling
dapat menurunkan tekanan darah. Kadar sehingga bacaan alat menunjukkan angka nol
natrium yang dibutuhkan tubuh sehari adalah (0.0) (Imelda, 2006). Data konsentrasi sampel
1600 mg. Penelitian ini bertujuan menganalisis yang diperoleh akan dianalisis.
kadar mineral natrium dan kalium pada daging
buah nanas yang beredar di Kota Palu. Hasil dan Pembahasan
Unsur mineral merupakan salah satu
Metode komponen yang sangat diperlukan makhluk
Alat dan Bahan hidup di samping karbohidrat, lemak, protein
Alat-alat yang digunakan dalam penelitian dan vitamin, juga dikenal sebagai zat anorganik
ini adalah: fotometri nyala, cawan porselin, atau kadar abu (Arifin, 2008). Penentuan
neraca analitik, oven listrik, stopwatch, furnace, kadar mineral natrium dan kalium sampel
gelas ukur, kertas saring, corong, gelas kimia, harus didestruksi atau dihancurkan, dalam hal
batang pengaduk, pipet tetes. Sedangkan ini dilakukan pengabuan kering. Pada tahap
bahan-bahan yang akan digunakan adalah : pengabuan ini, sampel dipotong kecil-kecil dan
daging buah nanas masak, HNO3 10% dan di ovenkan untuk menguapkan semua bahan
aquades. – bahan organik yang ada dalam sampel. Suhu
yang digunakan sewaktu pengeringan tidak
Prosedur Penelitian terlalu mempengaruhi kadar abu, meskipun
Pengambilan Sampel demikian sampel biasanya digunakan untuk
Sampel yang digunakan dalam penelitian keperluan lain seperti analisis protein, serat
ini adalah daging buah nanas varietas Queen dan lain-lain. Kemudian diabukan dengan
(nanas Bogor) dan varietas Cayenne (nanas menggunakan tanur, hingga terbentuk abu
biasa) yang beredar di kota Palu Sulawesi putih. Abu merupakan residu anorganik dari
Tengah. proses pembakaran atau oksidasi komponen
organik bahan pangan. Kadar abu dari suatu
Penyiapan Sampel bahan menunjukkan kandungan mineral yang
Daging buah nanas dibersihkan kemudian terdapat dalam bahan tersebut, kemurnian
dirajang halus; Daging buah nanas yang telah serta kebersihan suatu bahan yang dihasilkan
dirajang kemudian ditimbang sebanyak 50 (Andarwulan, 2011)
g, lalu diangin-anginkan selama 15 menit Proses destruksi bertujuan untuk
dan kemudian dikeringkan di dalam oven menghilangkan, merombak dan memutuskan
60oC selama 1 hari; Sampel ditimbang lagi ikatan-ikatan senyawa organik yang terdapat
dan dihitung berat keringnya; Setelah dingin dalam sampel sehingga yang tinggal hanya
sampel dimasukkan kedalam furnace pada suhu senyawa anorganik saja. metoda yang sangat
100oC dan perlahan-lahan naik hingga 550oC tepat digunakan untuk penentuan kadar
minimal 8 jam, hingga menjadi abu keputih kalium dan natrium karena unsur-unsur ini
– putihan; Sampel yang berupa abu putih lalu merupakan logam golongan IA yang sangat
didinginkan, kemudian ditimbang abu putih mudah tereksitasi dengan memancarkan sinar
nya dan dimasukkan ke dalam gelas kimia 100 yang karakteristik dengan intensitas yang cukup
mL; Ditambahkan 10 mL HNO3 10% pekat tinggi untuk diukur dengan fotosel. Kalium
dan aquades (1 : 1), kemudian disaring dan akan menghasilkan intensitas yang tinggi pada
filtratnya ditampung dalam labu takar 100 ml. panjang gelombang 766,5 nm sedangkan
residu yang tertinggal didalam kertas saring natrium pada panjang gelombang 589,0 nm
dibilas dengan larutan HNO3 dan aquades (1 : (Rasyid, 2011)
1) agar residu larut semua; Diencerkan dengan Penambahan HNO3 pekat dalam proses
aquades hingga tanda batas. pengabuan bertujuan mengoksidasi semua
karbon dan melarutkan garam-garam yang
Tahapan Analisis terdapat dalam sampel. Tujuan penelitian ini
Penentuan Na dan K menggunakan untuk menganalisis kadar Na dan K dalam
Fotometri Nyala. Kadar mineral Na dan K daging buah nanas (ananas comosus (L) Merr)
dalam larutan sampel ditentukan dengan cara di kota Palu

94

Potrebbero piacerti anche