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CONTROL, ANALYSIS,AND TESTING
CHEMICAL ANALYSIS OF PLATING SOLUTIONS
by Charles RosensteinShellcase Ltd., Jerusalem, Israel
and Stanley HirschLeeam Consultants Ltd., New Rochelle, N.Y.
Plating solutions must be routinely analyzed in order to maintain the recommended bathformulation and to preempt the occurrence of problems related to improper levels of bathconstituents. Contaminant levels in the solutions must also be monitored. Manufacturers ofplating systems establish optimum specifications to ensure maximum solution efficiency anduniformity of deposits. The various factors that cause the concentrations of bath constituentsto deviate from their optimum values are as follows:
1. drag-out;2. solution evaporation;3. chemical decomposition; and4. unequal anode and cathode efficiencies.
A current efficiency problem is recognized by gradual but continuous changes in pH,metal content, or cyanide content (see Table I).
The techniques employed for the quantitative analysis of plating solutions are classifiedas volumetric (titrimetric), gravimetric, and instrumental. Volumetric and gravimetricmethods are also known as “wet” methods. The analyst must select the method that is bestsuited and most cost effective for a particular application.
The wet methods outlined here are simple, accurate, and rapid enough for practically allplating process control. They require only the common analytical equipment found in thelaboratory, and the instructions are sufficiently detailed for an average technician to followwithout any difficulty . The determination of small amounts of impurities and uncommon
Table I . Problems Caused by Unequal Anode andCathode Efficiencies
Problem Cause
High pH High anode efficiencyLow pH High cathode efficiencyHigh metal content High anode efficiencyLow metal content High cathode efficiencyHigh free cyanide Low anode efficiencyLow free cyanide High anode efficiency
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metals should be referred to a competent laboratory, as a high degree of skill and chemicalknowledge are required for the determination of these constituents.
Hull cell testing (see the section on plating cells elsewhere in thisGuidebook) enables theoperator to observe the quality of a deposit over a wide current density range.
VOLUMETRIC METHODS
When titrants composed of standard solutions are added to a sample that contains acomponent whose concentration is to be quantitatively determined, the method is referred toas a volumetric method. The component to be determined must react completely with thetitrant in stoichiometric proportions. From the volume of titrant required, the component’sconcentration is calculated. The simplicity, quickness, and relatively low cost of volumetricmethods make them the most widely used for the analysis of plating and related solutions.
Volumetric methods involve reactions of several types: oxidation-reduction, acid-base,complexation, and precipitation. Indicators are auxiliary reagents, which usually signify theendpoint of the analysis. The endpoint can be indicated by a color change, formation of aturbid solution, or the solubilization of a turbid solution.
Some volumetric methods require little sample preparation, whereas others may requireextensive preparation. Accuracy decreases for volumetric analyses of components found inlow concentrations, as endpoints are not as easily observed as with the components found inhigh concentrations.
Volumetric methods are limited in that several conditions must be satisfied. Indicatorsshould be available to signal the endpoint of the titration. The component-titrant reactionshould not be affected by interferences from other substances found in the solution.
GRAVIMETRIC METHODS
In gravimetric methods, the component being determined is separated from othercomponents of the sample by precipitation, volatilization, or electroanalytical means.Precipitation methods are the most important gravimetric methods. The precipitate is usuallya very slightly soluble compound of high purity that contains the component. The weight ofthe precipitate is determined after it is filtered from solution, washed, and dried. Gravimetricmethods are used to supplement the available volumetric methods.
Limitations of gravimetric methods include the requirement that the precipitatedcomponent has an extremely low solubility. The precipitate must also be of high purity andbe easily filterable.
Species that are analyzed gravimetrically include chloride, sulfate, carbonate, phosphate,gold, and silver.
INSTRUMENTAL METHODS
Instrumental methods differ from wet methods in that they measure a physical propertyrelated to the composition of a substance, whereas wet methods rely on chemical reactions.The selection of an instrument for the analysis of plating solutions is a difficult task. Analystsmust decide if the cost is justified and if the analytical instrument is capable of analyzing forthe required substances with a high degree of accuracy and precision. Instruments coupled tocomputers can automatically sample, analyze, and record results. Mathematical errors areminimized and sample measurements are more reproducible than with wet methods.Instrumental methods are also extremely rapid when compared with wet methods.
Unlike humans, instruments cannot judge. They cannot recognize improper samplepreparation or interfering substances. Erroneous results are sometimes produced by electronicand mechanical malfunctions.
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Analytical instruments frequently used in the analysis of plating solutions can becategorized as spectroscopic, photometric, chromatographic, and electroanalytical. Spectro-scopic methods (flame photometry, emission spectrometry, X-ray fluorescence, mass spec-trometry, and inductively coupled plasma) are based on the emission of light. Photometricmethods (spectrophotometry, colorimetry, and atomic absorption) are based on the absorptionof light. Chromatographic methods (ion chromatography) involve the separation of substancesfor subsequent identification. Electroanalytical methods (potentiometry, conductometry,polarography, amperometry, and electrogravimetry) involve an electric current in the courseof the analysis.
The instrumental methods, comprehensively reviewed below, are most applicable toplating environments.
SPECTROSCOPIC METHODS
Spectroscopy is the analysis of a substance by the measurement of emitted light. Whenheat, electrical energy, or radiant energy is added to an atom, the atom becomes excited andemits light. Excitation can be caused by a flame, spark, X-rays, or an AC or DC arc. Theelectrons in the atom are activated from their ground state to unstable energy shells of higherpotential energy. Upon returning to their ground state, energy is released in the form ofelectromagnetic radiation.
Because each element contains atoms with different arrangements of outermost elec-trons, a distinct set of wavelengths is obtained. These wavelengths, from atoms of severalelements, are separated by a monochromator such as a prism or a diffraction grating.Detection of the wavelengths can be accomplished photographically (spectrograph) or viadirect-reading photoelectric detectors (spectrophotometers). The measurement of intensityemitted at a particular wavelength is proportional to the concentration of the element beinganalyzed.
An advantage of spectroscopy is that the method is specific for the element beinganalyzed. It permits quantitative analysis of trace elements without any preliminary treatmentand without prior knowledge as to the presence of the element. Most metals and somenonmetals may be analyzed. Spectroscopic analysis is also useful for repetitive analyticalwork.
Disadvantages of spectroscopic analysis include the temperature dependence of intensitymeasurements, as intensity is very sensitive to small fluctuations in temperature. The accuracyand precision of spectrographic methods is not as high as some spectrophotometric methodsor wet analyses. Spectrographic methods are usually limited to maximum element concen-trations of 3%. Additionally, sensitivity is much smaller for elements of high energy (e.g.,zinc) than for elements of low energy (e.g., sodium).
Applications of spectroscopy include the analysis of major constituents and impurities inplating solutions, and of alloy deposits for composition.
Flame PhotometryIn flame photometry (FP), a sample in solution is atomized at constant air pressure and
introduced in its entirety into a flame as a fine mist. The temperature of the flame(1,800–3,100˚K) is kept constant. The solvent is evaporated and the solid is vaporized andthen dissociated into ground state atoms. The valence electrons of the ground state atoms areexcited by the energy of the flame to higher energy levels and then fall back to the groundstate. The intensities of the emitted spectrum lines are determined in the spectrograph ormeasured directly by a spectrophotometer.
The flame photometer is calibrated with standards of known composition and concen-tration. The intensity of a given spectral line of an unknown can then be correlated with theamount of an element present that emits the specific radiation.
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Physical interferences may occur from solute or solvent effects on the rate of transportof the sample into the flame. Spectral interferences are caused by adjacent line emissionswhen the element being analyzed has nearly the same wavelength as another element.Monochromators or the selection of other spectral lines minimize this interference. Ionizationinterferences may occur with the higher temperature flames. By adding a second ionizableelement, the interferences due to the ionization of the element being determined areminimized.
An advantage of FP is that the temperature of the flame can be kept more nearly constantthan with electric sources. A disadvantage of the method is that the sensitivity of the flamesource is many times smaller than that of an electric arc or spark.
FP is used for the analysis of aluminum, boron, cadmium, calcium, chromium, cobalt,copper, indium, iron, lead, lithium, magnesium, nickel, palladium, platinum, potassium,rhodium, ruthenium, silver, sodium, strontium, tin, and zinc.
Emission SpectrometryIn emission spectrometry (ES), a sample composed of a solid, cast metal or solution is
excited by an electric discharge such as an AC arc, a DC arc, or a spark. The sample is usuallyplaced in the cavity of a lower graphite electrode, which is made positive. The uppercounterelectrode is another graphite electrode ground to a point. Graphite is the preferredelectrode material because of its ability to withstand the high electric discharge temperatures.It is also a good electrical conductor and does not generate its own spectral lines.
The arc is started by touching the two graphite electrodes and then separating them. Theextremely high temperatures (4,000–6,000˚K) produce emitted radiation higher in energy andin the number of spectral lines than in flame photometry. Characteristic wavelengths fromatoms of several elements are separated by a monochromator and are detected by spectro-graphs or spectrophotometers. Qualitative identification is performed by using availablecharts and tables to identify the spectral lines that the emission spectrometer sorts outaccording to their wavelength. The elements present in a sample can also be qualitativelydetermined by comparing the spectrum of an unknown with that of pure samples of theelements. The density of the wavelengths is proportional to the concentration of the elementbeing determined. Calibrations are done against standard samples.
ES is a useful method for the analysis of trace metallic contaminants in plating baths. The“oxide” method is a common quantitative technique in ES. A sample of the plating bath isevaporated to dryness and then heated in a muffle furnace. The resultant oxides are mixedwith graphite and placed in a graphite electrode. Standards are similarly prepared and a DCarc is used to excite the sample and standards.
X-ray FluorescenceX-ray fluorescence (XRF) spectroscopy is based on the excitation of samples by an
X-ray source of sufficiently high energy, resulting in the emission of fluorescent radiation.The concentration of the element being determined is proportional to the intensity of itscharacteristic wavelength. A typical XRF spectrometer consists of an X-ray source, a detector,and a data analyzer.
Advantages of XRF include the nondestructive nature of the X-rays on the sample. XRFis useful in measuring the major constituents of plating baths such as cadmium, chromium,cobalt, gold, nickel, silver, tin, and zinc. Disadvantages of XRF include its lack of sensitivityas compared with ES.
X-ray spectroscopy is also used to measure the thickness of a plated deposit. The X-raydetector is placed on the wavelength of the element being measured. The surface of thedeposit is exposed to an X-ray source and the intensity of the element wavelength is measured.A calibration curve is constructed for intensity against thickness for a particular deposit.Coating compositions can also be determined by XRF.
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Mass SpectrometryIn mass spectrometry (MS), gases or vapors derived from liquids or solids are bombarded
by a beam of electrons in an ionization chamber, causing ionization and a rupture of chemicalbonds. Charged particles are formed, which may be composed of elements, molecules, orfragments. Electric and magnetic fields then separate the ions according to their mass tocharge ratios (m/e). The amount and type of fragments produced in an ionization chamber, fora particular energy of the bombarding beam, are characteristic of the molecule; therefore,every chemical compound has a distinct mass spectrum. By establishing a mass spectrum ofseveral pure compounds, an observed pattern allows identification and analysis of complexmixtures.
The mass spectrum of a compound contains the masses of the ion fragments and therelative abundances of these ions plus the parent ion. Dissociation fragments will alwaysoccur in the same relative abundance for a particular compound.
MS is applicable to all substances that have a sufficiently high vapor pressure. Thisusually includes substances whose boiling point is below 450˚C. MS permits qualitative andquantitative analysis of liquids, solids, and gases.
Inductively Coupled PlasmaInductively coupled plasma (ICP) involves the aspiration of a sample in a stream of
argon gas, and then its ionization by an applied radio frequency field. The field is inductivelycoupled to the ionized gas by a coil surrounding a quartz torch that supports and encloses theplasma. The sample aerosol is heated in the plasma, the molecules become almost completelydissociated and then the atoms present in the sample emit light at their characteristicfrequencies. The light passes through a monochromator and onto a detector.
The high temperature (7,000˚K) of the argon plasma gas produces efficient atomicemission and permits low detection limits for many elements. As with atomic absorption(AA), ICP does not distinguish between oxidation states (e.g., Cr31 and Cr61) of the sameelement—the total element present is determined. Advantages of ICP include completeionization and no matrix interferences as in AA. ICP allows simultaneous analysis of manyelements in a short time. It is sensitive to part-per-billion levels.
Disadvantages of ICP include its high cost and its intolerance to samples with greaterthan 3% dissolved solids. Background corrections usually compensate for interferences due tobackground radiation from other elements and the plasma gases. Physical interferences, dueto viscosity or surface tension, can cause significant errors. These errors are reduced bydiluting the sample. Although chemical interferences are insignificant in the ICP method, theycan be greatly minimized by careful selection of the instrument’s operating conditions, bymatrix matching, or by buffering the sample.
ICP is applicable to the analysis of major components and trace contaminants in platingsolutions. It is also useful for waste-treatment analysis.
PHOTOMETRIC METHODS
Photometric methods are based on the absorption of ultraviolet (200–400 nm) or visible(400–1,000 nm) radiant energy by a species in solution. The amount of energy absorbed isproportional to the concentration of the absorbing species in solution. Absorption isdetermined spectrophotometrically or colorimetrically.
The sensitivity and accuracy of photometric methods must be frequently checked bytesting standard solutions in order to detect electrical, optical, or mechanical malfunctions inthe analytical instrument.
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Spectrophotometry and ColorimetrySpectrophotometryinvolves analysis by the measurement of the light absorbed by a
solution. The absorbance is proportional to the concentration of the analyte in solution.Spectrophotometric methods are most often used for the analysis of metals with concentra-tions of up to 2%.
Spectrophotometers consist of a light source (tungsten or hydrogen), a monochromator,a sample holder, and a detector. Ultraviolet or visible light of a definite wavelength is usedas the light source. Detectors are photoelectric cells that measure the transmitted (unabsorbed)light. Spectrophotometers differ from photometers in that they utilize monochromators,whereas photometers use filters to isolate the desired wavelength region. Filters isolate awider band of light.
In spectrophotometric titrations, the cell containing the analyte solution is placed in thelight path of a spectrophotometer. Titrant is added to the cell with stirring, and the absorbanceis measured. The endpoint is determined graphically. Applications of this titration include theanalysis of a mixture of arsenic and antimony and the analysis of copper with ethylenediamine tetra acetic acid (EDTA).
The possibility of errors in spectrophotometric analyses is increased when numerousdilutions are required for an analysis.
Colorimetry involves comparing the color produced by an unknown quantity of asubstance with the color produced by a standard containing a known quantity of thatsubstance. When monochromatic light passes through the colored solution, a certain amountof the light, proportional to the concentration of the substance, will be absorbed. Substancesthat are colorless or only slightly colored can be rendered highly colored by a reaction withspecial reagents.
In the standard series colorimetric method, the analyte solution is diluted to a certainvolume (usually 50 or 100 ml) in a Nessler tube and mixed. The color of the solution iscompared with a series of standards similarly prepared. The concentration of the analyteequals the concentration of the standard solution whose color it matches exactly. Colors canalso be compared to standards via a colorimeter (photometer), comparator, or spectropho-tometer.
The possible errors in colorimetric measurements may arise from the following sources:turbidity, sensitivity of the eye or color blindness, dilutions, photometer filters, chemicalinterferences, and variations in temperature or pH.
Photometric methods are available for the analysis of the following analytes:
Anodizing solutions: Fe, Cu, MnBrass solutions: FeCadmium solutions: Fe, Ti, Zn, Cu, NiChromium solutions: Cr, Fe, Ni, Cu, SeAcid copper solutions: Cl, FeAlkaline copper solutions: Fe, SeGold solutions: Au, Ni, In, Co, Cu, Fe, PO4
Iron solutions: Mn, NH3Lead and tin-lead solutions: PbNickel solutions: Cr, Cu, Zn, Fe, Co, NH3Palladium solutions: Pd, Cr, NH3Platinum solutions: PtRhodium solutions: RhSilver solutions: Ni, Cu, SbAcid tin solutions: Fe, CuAlkaline tin solutions: Cu, Pb, Zn
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Acid zinc solutions: Cu, FeAlkaline zinc solutions: Cu, FeWastewater: Cr61, Ni, Cu, Fe, Zn, Pb, Al, B, NO3, NO2, PO4, Cl, CN, wetting agents.
Atomic AbsorptionMetals in plating and related solutions can be readily determined by AA spectropho-
tometry. Optimum ranges, detection limits, and sensitivities of metals vary with the variousavailable instruments.
In direct-aspiration atomic absorption(DAAA) analysis, the flame (usually air-acetylene or nitrous oxide-acetylene) converts the sample aerosol into atomic vapor, whichabsorbs radiation from a light source. A light source from a hollow cathode lamp or anelectrodeless discharge lamp is used, which emits a spectrum specific to the element beingdetermined. The high cost of these lamps is a disadvantage of the AA method. A detectormeasures the light intensity to give a quantitative determination.
DAAA is similar to flame photometry in that a sample is aspirated into a flame andatomized. The difference between the two methods is that flame photometry measures theamount of emitted light, whereas DAAA measures the amount of light absorbed by theatomized element in the flame. In DAAA, the number of atoms in the ground state is muchgreater than the number of atoms in any of the excited states of the spectroscopic methods.Consequently, DAAA is more efficient and has better detection limits than the spectroscopicmethods.
Spectral interferences occur when a wavelength of an element being analyzed is close tothat of an interfering element. The analysis will result in an erroneously high measurement.To compensate for this interference, an alternate wavelength or smaller slit width is used.
When the physical properties (e.g., viscosity) of a sample differ from those of thestandard, matrix interferences occur. Absorption can be enhanced or suppressed. To overcomethese interferences, matrix components in the sample and standard are matched or a releaseagent, such as EDTA or lanthanum, is added.
Chemical interferences are the most common interferences encountered in AA analysis.They result from the nonabsorption of molecularly bound atoms in the flame. Theseinterferences are minimized by using a nitrous oxide-acetylene flame instead of anair-acetylene flame to obtain the higher flame temperature needed to dissociate the moleculeor by adding a specific substance (e.g., lanthanum) to render the interferant harmless.Chemical interferences can also be overcome by extracting the element being determined orby extracting the interferant from the sample.
The sensitivity and detection limits in AA methods vary with the instrument used, thenature of the matrix, the type of element being analyzed, and the particular AA techniquechosen. It is best to use concentrations of standards and samples within the optimumconcentration range of the AA instrument. When DAAA provides inadequate sensitivity,other specialized AA methods, such as graphite furnace AA, cold vapor AA, or hydride AA,are used.
In graphite furnace AA(GFAA), the flame that is used in DAAA is replaced with anelectrically heated graphite furnace. A solution of the analyte is placed in a graphite tube inthe furnace, evaporated to dryness, charred, and atomized. The metal atoms being analyzedare propelled into the path of the radiation beam by increasing the temperature of the furnaceand causing the sample to be volatilized. Only very small amounts of sample are required forthe analysis.
GFAA is a very sensitive technique and permits very low detection limits. The increasedsensitivity is due to the much greater occupancy time of the ground state atoms in the opticalpath as compared with DAAA. Increased sensitivity can also be obtained by using largersample volumes or by using an argon-hydrogen purge gas mixture instead of nitrogen.Because of its extreme sensitivity, determining the optimum heating times, temperature, andmatrix modifiers is necessary to overcome possible interferences.
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Interferences may occur in GFAA analysis due to molecular absorption and chemicaleffects. Background corrections compensate for the molecular absorption interference.Specially coated graphite tubes minimize its interaction with some elements. Gradual heatinghelps to decrease background interference, and permits determination of samples withcomplex mixtures of matrix components.
The GFAA method has been applied to the analysis of aluminum, antimony, arsenic,barium, beryllium, cadmium, chromium, cobalt, copper, iron, lead, manganese, molybdenum,nickel, selenium, silver, and tin.
Cold vapor atomic absorption(CVAA) involves the chemical reduction of mercury orselenium by stannous chloride and its subsequent analysis. The reduced solution is vigorouslystirred in the reaction vessel to obtain an equilibrium between the element in the liquid andvapor phases. The vapor is then purged into an absorption cell located in the light path of aspectrophotometer. The resultant absorbance peak is recorded on a strip chart recorder.
The extremely sensitive CVAA procedure is subject to interferences from some organics,sulfur compounds, and chlorine. Metallic ions (e.g., gold, selenium), which are reduced to theelemental state by stannous chloride, produce interferences if they combine with mercury.
Hydride atomic absorption(HAA) is based on chemical reduction with sodiumborohydride to selectively separate hydride-forming elements from a sample. The gaseoushydride that is generated is collected in a reservoir attached to a generation flask, and is thenpurged by a stream of argon or nitrogen into an argon-hydrogen-air flame. This permitshigh-sensitivity determinations of antimony, arsenic, bismuth, germanium, selenium, tellu-rium, and tin.
The HAA technique is sensitive to interferences from easily reduced metals such assilver, copper, and mercury. Interferences also arise from transition metals in concentrationsgreater than 200 mg/L and from oxides of nitrogen.
Ion ChromatographyIn ion chromatography (IC), analytes are separated with an eluent on a chromatographic
column based on their ionic charges. Because plating solutions are water based, the solublecomponents must be polar or ionic; therefore, IC is applicable to the analysis of plating andrelated solutions.
Ion chromatographs consist of a sample delivery system, a chromatographic separationcolumn, a detection system, and a data handling system.
IC permits the rapid sequential analysis of multiple analytes in one sample. The variousdetectors available, such as UV-visible, electrochemical, or conductivity, allow for specificdetection in the presence of other analytes. IC is suitable for the analysis of metals, anionicand cationic inorganic bath constituents, and various organic plating bath additives. It is alsoused for continuous on-line operations.
Interferences arise from substances that have retention times coinciding with that of anyanion being analyzed. A high concentration of a particular ion may interfere with theresolution of other ions. These interferences can be greatly minimized by gradient elution orsample dilution.
IC has been applied to the analysis of the following analytes in plating and relatedsolutions:
Metals: Aluminum, barium, cadmium, calcium, trivalent and hexavalent chromium,cobalt, copper, gold, iron, lead, lithium, magnesium, nickel, palladium, platinum, silver, tin,zinc.
Ions:Ammonium, bromide, carbonate, chloride, cyanide, fluoborate, fluoride, hypophos-phite, nitrate, nitrite, phosphate, potassium, sodium, sulfate, sulfide, sulfite.
Acid Mixtures:Hydrofluoric, nitric, and acetic acids.Organics:Brighteners, surfactants, organic acids.
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ELECTROANALYTICAL METHODS
Electroanalytical methods involve the use of one or more of three electricalquantities—current, voltage, and resistance. These methods are useful when indicators for atitration are unavailable or unsuitable. Although trace analysis may be done quite well byspectroscopic or photometric methods, electroanalytical methods offer ease of operation andrelatively lower costs of purchase and maintenance.
PotentiometryPotentiometry involves an electrode that responds to the activity of a particular group of
ions in solution. Potentiometric methods correlate the activity of an ion with its concentrationin solution.
In potentiometric titrations, titrant is added to a solution and the potential between anindicator and reference electrode is measured. The reaction must involve the addition orremoval of an ion for which an electrode is available. Acid-base titrations are performed witha glass indicator electrode and a calomel reference electrode. The endpoint corresponds to themaximum rate of change of potential per unit volume of titrant added.
Advantages of potentiometric titrations include its applicability to colored, turbid, orfluorescent solutions. It is also useful in situations where indicators are unavailable.
The sensitivity of potentiometric titrations is limited by the accuracy of the measurementof electrode potentials at low concentrations. Solutions that are more dilute than 1025 Ncannot be accurately titrated potentiometrically. This is because the experimentally measuredelectrode potential is a combined potential, which may differ appreciably from the trueelectrode potential. The difference between the true and experimental electrode potentials isdue to the residual current, which arises from the presence of electroactive trace impurities.
The direct potentiometric measurement of single ion concentrations is done with ionselective electrodes (ISEs). The ISE develops an electric potential in response to the activityof the ion for which the electrode is specific. ISEs are available for measuring calcium,copper, lead, cadmium, ammonia, bromide, nitrate, cyanide, sulfate, chloride, fluoride, andother cations and anions.
Cation ISEs encounter interferences from other cations, and anion ISEs encounterinterferences from other anions. These interferences can be eliminated by adjusting the samplepH or by chelating the interfering ions. ISE instructions must be reviewed carefully todetermine the maximum allowable levels of interferants, the upper limit of the single ionconcentration for the ISE, and the type of media compatible with the particular ISE.
Some of the solutions that can be analyzed by potentiometric methods are:
Anodizing solutions: Al, H2SO4, C2H2O4, CrO3, ClBrass solutions: Cu, Zn, NH3, CO3
Bronze solutions: Cu, Sn, NaOH, NaCN, Na2CO3
Chromium solutions: Cr, ClCadmium solutions: Cd, NaOH, NaCN, Na2CO3
Acid copper solutions: ClAlkaline copper solutions: NaOH, NaCN, Na2CO3
Gold solutions: Au, Ag, Ni, CuLead and tin/lead solutions: Pb, Sn, HBF4
Nickel solutions: Co, Cu, Zn, Cd, Cl, H3BO3
Silver solutions: Ag, Sb, NiAcid tin solutions: Sn, HBF4, H2SO4
Alkaline tin solutions: Sn, NaOH, NaCO3, ClZinc solutions: Zn
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ConductometryElectrolytic conductivity measures a solution’s ability to carry an electric current. A
current is produced by applying a potential between two inert metallic electrodes (e.g.,platinum) inserted into the solution being tested. When other variables are held constant,changes in the concentration of an electrolyte result in changes in the conductance of electriccurrent by a solution.
In conductometric titrations, the endpoint of the titration is obtained from a plot ofconductance against the volume of titrant. Excessive amounts of extraneous foreignelectrolytes can adversely affect the accuracy of a conductometric titration.
Conductometric methods are used when wet or potentiometric methods give inaccurateresults due to increased solubility (in precipitation reactions) or hydrolysis at the equivalencepoint. The methods are accurate in both dilute and concentrated solutions, and they can alsobe used with colored solutions.
Conductometric methods have been applied to the analysis of Cr, Cd, Co, Fe, Ni, Pb, Ag,Zn, CO3, Cl, F, and SO4.
PolarographyIn polarography, varying voltage is applied to a cell consisting of a large mercury anode
(reference electrode) and a small mercury cathode (indicator electrode) known as a droppingmercury electrode (DME). Consequent changes in current are measured. The large area of themercury anode precludes any polarization. The DME consists of a mercury reservoir attachedto a glass capillary tube with small mercury drops falling slowly from the opening of the tube.A saturated calomel electrode is sometimes used as the reference electrode.
The electrolyte in the cell consists of a dilute solution of the species being determined ina medium of supporting electrolyte. The supporting electrolyte functions to carry the currentin order to raise the conductivity of the solution. This ensures that if the species to bedetermined is charged, it will not migrate to the DME. Bubbling an inert gas, such as nitrogenor hydrogen, through the solution prior to running a polarogram, will expel dissolved oxygenin order to prevent the dissolved oxygen from appearing on the polarogram.
Reducible ions diffuse to the DME. As the applied voltage increases, negligible currentflow results until the decomposition potential is reached for the metal ion being determined.When the ions are reduced at the same rate as they diffuse to the DME, no further increasesin current occur, as the current is limited by the diffusion rate. The half-wave potential is thepotential at which the current is 50% of the limiting value.
Polarograms are obtained by the measurement of current as a function of appliedpotential. Half-wave potentials are characteristic of particular substances under specifiedconditions. The limiting current is proportional to the concentration of the substance beingreduced. Substances can be analyzed quantitatively and qualitatively if they are capable ofundergoing anodic oxidation or cathodic reduction. As with other instrumental methods,results are referred to standards in order to quantitate the method.
Advantages of polarographic methods include their ability to permit simultaneousqualitative and quantitative determinations of two or more analytes in the same solution.Polarography has wide applicability to inorganic, organic, ionic, or molecular species.
Disadvantages of polarography include the interferences caused by large concentrationsof electropositive metals in the determination of low concentrations of electronegative metals.The very narrow capillary of the DME occasionally becomes clogged.
Polarographic methods are available for the following solutions:
Anodizing solutions: Cu, Zn, MnBrass solutions: Pb, Cd, Cu, Ni, ZnBronze solutions: Pb, Zn, Al, Cu, NiCadmium solutions: Cu, Pb, Zn, Ni
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Chromium solutions: Cu, Ni, Zn, Cl, SO4Acid copper solutions: Cu, ClAlkaline copper solutions: Zn, Fe, Pb, CuGold solutions: Au, Cu, Ni, Zn, In, Co, CdIron solutions: MnLead and tin-lead solutions: Cu, Cd, Ni, Zn, SbNickel solutions: Cu, Pb, Zn, Cd, Na, Co, Cr, MnPalladium solutions: Pd, Cr31, Cr61
Rhodium solutions: RhSilver solutions: Sb, Cu, CdAcid tin solutions: Sn41, Cu, Ni, ZnAlkaline tin solutions: Pb, Cd, Zn, CuAcid zinc solutions: Cu, Fe, Pb, CdAlkaline zinc solutions: Pb, Cd, CuWastewater: Cd, Cu, Cr31, Ni, Sn, Zn
AmperometryAmperometric titrations involve the use of polarography as the basis of an electrometric
titration. Voltage applied across the indicator electrode (e.g., DME or platinum) and referenceelectrode (e.g., calomel or mercury) is held constant and the current passing through the cellis measured as a function of titrant volume added. The endpoint of the titration is determinedfrom the intersection of the two straight lines in a plot of current against volume of titrantadded. Polarograms are run to determine the optimum titration voltage.
Amperometric titrations can be carried out at low analyte concentrations at whichvolumetric or potentiometric methods cannot yield accurate results. They are temperatureindependent and more accurate than polarographic methods. Although amperometry is usefulfor oxidation-reduction or precipitation reactions, few acid-base reactions are determined bythis method.
Some of the reactions that can be analyzed by amperometric methods are given inTable II.
ElectrogravimetryIn electrogravimetry, the substance to be determined is separated at a fixed potential on
a preweighed inert cathode, which is then washed, dried, and weighed. Requirements for anaccurate electrogravimetric analysis include good agitation, smooth adherent deposits, andproper pH, temperature, and current density.
Table II. Reactions That Can Be Analyzed by Amperometry
Analyte Titrant Supporting Electrolyte
Fluoride Lead nitrate Potassium chlorideGold Hydroquinone Sulfuric acidNickel Dimethylglyoxime ChlorideLead Sodium fluoride ChlorideBromide Silver nitrate Nitric acidCalcium EDTA AmmoniaCadmium EDTA AmmoniaChloride Silver nitrate Nitric acidIndium EDTA Weak acid
EDTA, ethylene diamine tetra acetic acid.
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Advantages of electrogravimetry include its ability to remove quantitatively mostcommon metals from solution. The method does not require constant supervision. Disadvan-tages include long electrolysis times.
Some of the metals that have been determined electrogravimetrically are cadmium,cobalt, copper, gold, iron, lead, nickel, rhodium, silver, tin, and zinc.
SAMPLING
Analyses are accurate only when the sample is truly representative of the solution beinganalyzed. Each tank should have a reference mark indicating the correct level for the solution,and the bath should always be at this level when the sample is taken. Solutions should bestirred before sampling. If there is sludge in the tank, the solution should be stirred at the endof the day and the bath allowed to stand overnight, taking the sample in the morning.
Solutions should be sampled by means of a long glass tube. The tube is immersed in thesolution, the thumb is placed over the upper open end, and a full tube of solution is withdrawnand transferred to a clean, dry container. The solution should be sampled at a minimum of 10locations in the tank to ensure a representative sample. A quart sample is sufficient foranalysis and Hull cell testing, and any remaining solution can be returned to its tank.
STANDARD SOLUTIONS, REAGENTS, AND INDICATORSFOR WET METHODS
Standard solutions, reagents, and indicators can be purchased ready-made from labora-tory supply distributors. Unless a laboratory has the experience and high degree of accuracythat is required in preparing these solutions, it is recommended that they be purchased asprepared solutions. Preparations for all the solutions are given here to enable technicians toprepare or recheck their solutions.
A standard solution is a solution with an accurately known concentration of a substanceused in a volumetric analysis. Standardization of standard solutions requires greater accuracythan routine volumetric analyses. An error in standardization causes errors in all analyses thatare made with the solution; therefore, Primary Standard Grade chemicals should be used tostandardize standard solutions.
The strengths of standard solutions are usually expressed in terms of normality ormolarity. Normalities of standard solutions and their equivalent molarities are listed in TableIII. The methods to standardize all the standard solutions required for the analysis of platingand related solutions are listed in Table IV.
Table III. Molarities and Normalities of Standard Solutions
Standard Solution Formula Normality Molarity
EDTA C10H14O8N2Na2·2H2O 0.2 0.1Ferrous ammonium sulfate FeSO4(NH4)2SO4·6H2O 0.1 0.1Hydrochloric acid HCl 1.0 1.0Iodine I2 0.1 0.1Potassium dichromate K2Cr2O7 0.1 0.02Potassium iodide-iodate KI-KIO3 0.1 0.0167Potassium permanganate KMnO4 0.1 0.02Potassium thiocyanate KSCN 0.1 0.1Silver nitrate AgNO3 0.1 0.1Sodium hydroxide NaOH 1.0 1.0Sodium thiosulfate Na2S2O3·5H2O 0.1 0.1
EDTA, ethylene diamine tetra acetic acid.
532
Indicators are added to solutions in volumetric analyses to show color change or onset ofturbidity, signifying the endpoint of a titration. The indicators required for all of the analyses andtheir preparations are listed in Table V. Analytical Grade chemicals should be used in preparinganalytical reagents (Table VI) and Reagent Grade acids should be used (Table VII). Whenchemicals of lesser purity are used, the accuracy of the results will be diminished.
Tables VIII through XII provide specific methods for testing the constituents ofelectroplating, electroless, and anodizing baths, as well as acid dips and alkaline cleaners.
SAFETY
As with any laboratory procedure, the accepted safety rules for handling acids, bases, andother solutions should be followed. Acids are always added to water, not the reverse. Mouthpipettes should not be used for pipetting plating solutions. Safety glasses should always beworn, and care should be exercised to avoid skin and eye contact when handling chemicals.A fume hood should be used when an analytical method involves the liberation of hazardousor annoying fumes. Laboratory staff should be well versed in the first-aid procedures requiredfor various chemical accidents.
DETERMINATION OF CATHODE EFFICIENCY
The procedure for determining cathode efficiency, using the setup pictured in Fig. 1, isas follows:
1. Connect the copper coulometer in series with the test cell.2. The copper coulometer solution should contain 30 oz/gal copper sulfate pentahydrate
and 8 oz/gal sulfuric acid.3. Use the same anodes, temperature, and agitation in the test solution that are used in
the plating bath.4. Plate at 0.4 A (30 A/ft2) for a minimum of 10 minutes.5. Rinse both cathodes, dry in acetone, and weigh.
% Cathode Efficiency5weight in grams of test metal3 valence of test metal in bath3 3177
weight in grams of copper metal3 atomic weight of test metal
Fig. 1. Test setup for determination of cathode efficiency. Use 500-ml beakers and 13 2-in.brass cathodes. The anodes for the test solution should match that used in the plating bath.Use copper anodes for the coulometer.
533
Tab
leIV
.S
tand
ardi
zatio
nof
Sta
ndar
dS
olut
ions
So
lutio
nR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
e
Ca
lcu
latio
ns
(ml,
N,
M-t
itra
nt;
wt-
sam
ple
ing
ram
s)
0.1
ME
DT
A37
.0g
Na 2
ED
TA
·2H
2O
per
liter
H2O
5.0
gC
aCO 3
diss
olve
din
1:3
HC
land
dilu
ted
to50
0m
lin
avo
lum
etric
flask
.P
ipet
te20
-mls
ampl
e,ad
d10
0m
lH 2O,,a
10m
lpH
10bu
ffer,
and
EB
Tpo
wde
r.
ED
TA
Red
-blu
eM
ED
TA
5(w
tC
aCO 3
3m
lsam
ple)
/(m
lED
TA
350
.05)
0.1
NH
Cl
9m
l36%
HC
lper
liter
H2O
0.2
gN
a 2C
O3,
125
mlH
2O
,an
dbr
omoc
reso
lgre
en.
HC
lB
lue-
gree
nN
HC
l5
(wt
Na 2
CO
3)/
(ml3
0.05
299)
1.0
NH
Cl
89m
l36%
HC
lper
liter
H2O
2.0
gN
a 2C
O3,
125
mlH
2O
,an
dbr
omoc
reso
lgre
en.
HC
lB
lue-
gree
nN
HC
l5
(wt
Na 2
CO
3)/
(ml3
0.05
299)
0.1
NI 1
12.7
gI 2,
24.0
gK
lpe
rlit
erH 2
O
0.2
gA
s 2O
3,
20m
l1.0
NN
aOH
,ge
ntly
heat
until
As
2O
3di
ssol
ves,
cool
,ad
dph
enol
phth
alei
n,1.
0N
HC
ladd
edfr
ompi
nkto
colo
rless
,10
0m
lH2O
,1
mlc
onc.
HC
l,2
gbi
carb
onat
ead
ded
slow
ly,
and
star
chso
lutio
n.
I 2C
olor
less
-blu
eN
I 25
(wt
As 2
O3/
(ml3
0.04
946)
0.01
NH
g(N
O 3) 2
1.08
3g
HgO
,5
ml
50%
HN
O 3pe
rlit
erH
2O
7.5
gK
Cld
isso
lved
inH 2
Oan
ddi
lute
dto
1,00
0m
lin
avo
lum
etric
flask
.P
ipet
te2-
mls
ampl
e,ad
d10
0m
lH 2O,
and
15m
l20%
tric
hlor
oace
ticac
id.
Hg(
NO
3) 2
Col
orle
ss-p
urpl
eN
Hg(
NO 3)
25
(wt
KC
l3
mls
ampl
e)/(
ml
Hg(
NO
) 3) 2
374
.56)
0.1
NK
I-K
IO3
3.6
gK
IO3,
1.0
gN
aOH
,10
.0g
KI
per
liter
H2O
In50
0-m
lfla
skad
d0.
20g
Sn,
100
mlc
onc.
HC
l,2
drop
sS
bCl
3
solu
tion,
let
stan
dat
room
tem
pera
ture
tilld
isso
lved
.A
dd18
0m
lH
2O
,5-
in.
fold
ed“U
”-sh
aped
nick
elst
rip,
and
5.0
gre
duce
diro
npo
wde
r.S
topp
erfla
skw
ithru
bber
stop
per
fitte
dw
ith1 ⁄4-in
.gl
ass
tube
imm
erse
din
toa
satu
rate
dN
aHC
O3
solu
tion.
Hea
tso
lutio
non
hot-
plat
eto
boil
for
20m
inut
esan
dth
enpl
ace
inco
olin
gta
nkan
dal
low
toco
olto
room
tem
pera
ture
.M
ake
sure
glas
sou
tlet
tube
isim
mer
sed
inth
eN
aHC
O 3.R
emov
est
oppe
ran
dad
dst
arch
solu
tion.
KI-
KIO
3C
olor
less
-blu
eN
KI-
KIO
35
(wt
Sn)
/(m
l30.
0593
45)
534
Tab
leIV
.S
tand
ardi
zatio
nof
Sta
ndar
dS
olut
ions
(co
nt.)
So
lutio
nR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
e
Ca
lcu
latio
ns
(ml,
N,
M-t
itra
nt;
wt-
sam
ple
ing
ram
s)
0.1
NK
MnO
4
3.2
gK
MnO
4pe
rlit
erH
2O
Hea
tK
MnO
4so
lutio
nto
near
boili
ngfo
r30
min
utes
and
let
stan
dov
erni
ght.
Filt
erth
roug
ha
sint
ered
glas
scr
ucib
le.
The
n,to
stan
dard
ize:
add
0.2
gN
a2C
2O
4,
200
mlH
2O
,30
ml2
0%H 2
SO
4,
heat
to18
5–19
5˚F
.
KM
nO4
Col
orle
ss-p
ink
NK
MnO
45
(wt
Na 2
C2O
4)/
(ml3
0.06
70)
0.1
NK
SC
N9.
7g
KS
CN
per
liter
H2O
0.3
gA
g,15
ml5
0%H
NO 3
,10
0m
lH2O
,an
dF
AS
.K
SC
NC
olor
less
-red
NK
SC
N5(w
tA
g)/
(ml3
0.10
787)
0.1
AgN
O3
17.0
gA
gNO 3
per
liter
H2O
0.2
gN
aCl,
125
mlH
2O
,an
dK 2
CrO
4.
AgN
O3
Yel
low
-red
NA
gNO 3
5(w
tN
aCl)/
(ml3
0.05
845)
0.1
NN
aOH
4.0
gN
aOH
per
liter
H2O
0.5
gpo
tass
ium
hydr
ogen
phth
alat
e(K
HC
8H
4O
4),
125
mlH
2O
,an
dph
enol
phth
alei
n.N
aOH
Col
orle
ss-p
ink
NN
aOH5
(wt
KH
C8H
4O
4)/
(ml3
0.20
422)
1.0
NN
aOH
40.0
gN
aOH
per
liter
H2O
4.0
gpo
tass
ium
hydr
ogen
phth
alat
e(K
HC
8H
4O
4),
125
mlH
2O
,an
dph
enol
phth
alei
nin
dica
tor.
NaO
HC
olor
less
-pin
kN
NaO
H5(w
tK
HC
8H
4O
4)/
(ml3
0.20
422)
0.1
NN
a 2S 2
O3
25.0
gN
a 2S 2
O3·5
H2
Ope
rlit
erH 2
O
Add
0.1
gN
a 2C
O3
toN
a 2S 2
O3
solu
tion
and
let
stan
dfo
r24
hour
s.T
ost
anda
rdiz
e:ad
d0.
12g
KIO 3,
2g
KI,
25m
lH2O
,an
d8
ml
10%
HC
l.T
itrat
eto
light
yello
ww
ithN
a 2S2O
3an
dad
d2
mls
tarc
hso
lutio
n.
Na 2
S 2O
3B
lue-
colo
rless
NN
a 2S2O
35
(wt
KIO
3)/
(ml3
0.03
567)
0.1
NT
h(N
O 3) 4
14.0
gT
h(N
O3) 4
·4H
2O
per
liter
H2O
5.0
gN
aFdi
ssol
ved
inH 2O
and
dilu
ted
to1,
000
mli
na
volu
met
ricfla
sk.
Pip
ette
10-m
lsam
ple,
add
100
mlH 2O
,al
izar
inin
dica
tor,
2%H
NO
3,
drop
wis
efr
ompi
nkto
yello
w,
and
3m
lflu
orid
ebu
ffer.
Th(
NO
3) 4
Yel
low
-pin
kN
5(w
tN
aFpe
rlit
er)/
(ml3
4.19
98)
ED
TA
,et
hyle
nedi
amin
ete
tra
acet
icac
id.
a Use
deio
nize
dor
dist
illed
wat
erfo
ral
lsol
utio
ns.
535
Table V. Indicators for Analyses
Alizarin 1.0 g sodium alizarin sulfonate, 1,000 ml H2O.Bromocresol Green 0.4 g bromocresol green, 1,000 ml H2O, 0.5 ml 1.0 N NaOH.Bromocresol Purple 0.4 g bromocresol purple, 1,000 ml H2O, 1.0 ml 1.0 N NaOH.EBT Powder 2.0 g Eriochrome Black T, 198 g NaCl.EBT Solution 5.0 g Eriochrome Black T, 150 ml methanol, 100 ml triethanolamine.FAS 50 g ferrous ammonium sulfate, 950 ml H2O, 10 ml conc. HNO3.K2CrO4 20 g K2CrO4, 980 ml H2O.Methyl Orange 1.0 g methyl orange (sodium salt), 1,000 ml H2O.Murexide 2.0 g murexide, 198 g NaCl.PAN 1.0 g peroxyacetal nitrate, 1,000 ml methanol.Phenolphthalein 1.0 g phenolphthalein, 500 ml ethanol, 500 ml H2O.Starch Solution 10.0 g starch, 1,000 ml hot H2O, 0.5 ml formaldehyde.Sulfo Orange 100 ml sulfo orange, 100 g NaCN, 845 ml H2O.
Note: Use deionized or distilled water for preparation of all solutions.
Table VI. Reagents for Analyses
Ammonium Oxalate Solution 40 g ammonium oxalate, 960 ml H2O.Dimethylglyoxime Solution 10 g dimethylglyoxime, 1,000 ml ethanol.Fluoride Buffer Dissolve 40 g monochloroacetic acid in 400 ml H2O and divide the
solution in two equal parts. Add phenolphthalein to one part andtitrate with 1.0 N NaOH from colorless to pink. Mix both partsand add H2O to 1,000 ml.
KF Solution 100 g KF dissolved in 1,000 ml H2O. Neutralize to pH 7.0 with1.0 N NaOH.
NaCN Solution 100 g NaCN, 900 ml H2O.Na2SO4 Solution 135 g Na2SO4, 950 ml H2O.pH 10 Buffer 350 ml conc. NH4OH, 54 g NH4Cl, 625 ml H2O.Reducing Solution 100 ml conc. HCl, 250 ml conc. HC2H3O2, 200 ml ethanol,
450 ml H2O.Rochelle Solution 200 g Rochelle salts, 800 ml H2O.SbCl3 Solution 2.0 g SbCl3, 100 ml 50% HCl.Silver Nitrate Solution 10 g AgNO3, 95 ml H2O.Sodium Sulfite Solution 100 g sodium sulfite, 950 ml H2O. Adjust to pH 9.0 with 1.0 N
NaOH or 1.0 N HCl. Solution has a 1-week shelf life.Tartaric Acid Solution 150 g tartaric acid, 950 ml H2O.
Note: Use deionized or distilled water for preparation of all reagents.
Table VII. Properties of Reagent Grade Acids
Acid Formula Wt % Specific Gravity (60˚F) Pounds/Gallon
Acetic HC2H3O2 99.0 1.050 8.76Fluoboric HBF4 48.0 1.365 11.38Formic HCHO2 98.0 1.220 10.17Hydrobromic HBr 48.0 1.490 12.43Hydrochloric HCl 36.0 1.183 9.87Hydrofluoric HF 70.0 1.256 10.48Nitric HNO3 70.0 1.420 11.84Phosphoric H3PO4 85.0 1.690 14.09Sulfuric H2SO4 93.0 1.835 15.30
536
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Bra
ssC
uCN
(Met
hod
I)2
ml
15m
lcon
c.H
NO 3,
heat
tobl
ueco
lor,
100
mlH
2O
,aco
nc.
NH 4
OH
tode
epbl
ue,
heat
to14
0˚F
,an
dad
dP
AN
.
0.1
ME
DT
AP
urpl
e-gr
een
CuC
N(o
z/ga
l)52.
985
3M
3[2
3C
uCN
ml2
0.8
3Z
n(C
N) 2
ml]
CuC
N(M
etho
dII)
2m
l10
0m
lH2O
,15
mlc
onc.
HN
O 3,
heat
tobl
ueco
lor
and
disa
ppea
ranc
eof
brow
nfu
mes
,N
H 4O
Hto
deep
blue
,ac
etic
acid
tolig
htbl
ue,
5g
KI.
Titr
ate
with
Na 2
S 2O
3to
pale
yello
w,
add
5m
lsta
rch
solu
tion,
cont
inue
titra
ting
toco
lorle
ss.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
uCN
(oz/
gal)5
ml3
5.97
13
N
Zn(
CN
) 25
ml
100
mlH
2O
,10
mlp
H10
buffe
r,E
BT
pow
der,
and
15m
l10%
form
alde
hyde
.0.
1M
ED
TA
Red
-blu
eZ
n(C
N) 2(o
z/ga
l)5
ml3
3.13
13
M
NaC
Nor
5m
l10
0m
lH2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dN
aCN
(oz/
gal)5
ml3
2.61
43
NK
CN
KC
N(o
z/ga
l)5
ml3
3.47
33
N
NaO
Hor
5m
l25
mlH
2O
and
5m
lsul
fo-o
rang
e.1.
0N
HC
lO
rang
e-ye
llow
NaO
H(o
z/ga
l)5
ml3
1.06
73
NK
OH
KO
H(o
z/ga
l)5
ml3
1.49
63
N
Na 2
CO
3or
10m
l10
0m
lhot
H 2O
,35
ml1
0%B
a(N
O 3) 2
,al
low
tose
ttle,
filte
r,w
ash
filte
rtw
ice
with
hot
H2O
,tr
ansf
erfil
ter
pape
ran
dpr
ecip
itate
toa
beak
er,
add
100
mlH 2O
,an
dm
ethy
lora
nge.
1.0
NH
Cl
Ora
nge-
pink
Na 2C
O3
(oz/
gal)
5m
l30.
707
3N
K2C
O3
K2C
O3
(oz/
gal)
5m
l30.
921
3N
537
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
KN
aC4H
4O
6·4
H2O
5m
l25
ml2
0%H 2
SO
4,
filte
r,w
ash
flask
and
filte
rpa
per
twic
eea
chw
ithH 2O
,an
dbo
ilth
eco
llect
edfil
trat
e5
min
utes
.
0.1
NK
MnO
4C
olor
less
-pin
kK
NaC
4H
4O
6·4
H2O
(oz/
gal)
5m
l31.
250
3N
Bro
nze
Cu
(Met
hod
I)2
ml
15m
lcon
c.H
NO 3,
heat
tobl
ueco
lor,
100
mlH
2O
,co
nc.
NH 4
OH
tode
epbl
ue,
heat
to14
0˚F
and
add
PA
N.
0.1
ME
DT
AP
urpl
e-gr
een
Cu
(oz/
gal)5
ml3
4.23
63
M
Cu
(Met
hod
II)2
ml
100
mlH
2O
,15
mlc
onc.
HN
O 3,
heat
tobl
ueco
lor
and
disa
ppea
ranc
eof
brow
nfu
mes
,N
H 4O
Hto
deep
blue
,ac
etic
acid
tolig
htbl
ue,
5g
KI.
Titr
ate
with
Na 2
S 2O
3to
pale
yello
w,
add
5m
lsta
rch
solu
tion,
cont
inue
titra
ting
toco
lorle
ss.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
u(o
z/ga
l)5m
l34.
236
3N
Sn
5m
l10
0m
lH2O
,50
mlc
onc.
HC
l,3.
0g
iron
pow
der
in50
0-m
lfla
sk.
Sto
pper
flask
with
stop
per
fitte
dw
itha
glas
stu
beim
mer
sed
ina
beak
erfil
led
with
satu
rate
dbi
carb
onat
eso
lutio
n.H
eat
gent
lytil
liro
ndi
ssol
ves.
Coo
lto
room
tem
pera
ture
,m
akin
gsu
reou
tlet
tube
isim
mer
sed
inbi
carb
onat
eso
lutio
n.A
dd10
mls
tarc
hso
lutio
nan
dbi
carb
onat
edu
ring
titra
tion.
0.1
NK
I-K
IO3
Cle
ar-b
lue
Sn
(oz/
gal)5
ml3
1.58
33
N
NaC
Nor
5m
l10
0m
lH2O
and
10m
l10K
I.0.
1N
AgN
O 3C
lear
-tur
bid
NaC
N(o
z/ga
l)5m
l32.
614
3N
KC
NK
CN
(oz/
gal)
5m
l33.
473
3N
NaO
Hor
5m
l25
mlH
2O
and
5m
lsul
fo-o
rang
e.1.
0N
HC
lO
rang
e-ye
llow
NaO
H(o
z/ga
l)5
ml3
1.06
73
NK
OH
KO
H(o
z/ga
l)5
ml3
1.49
63
N
538
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Na 2
CO
3or
K2C
O3
10m
l10
0m
lhot
H 2O
,35
ml1
0%B
a(N
O 3) 2
,al
low
tose
ttle,
filte
r,w
ash
filte
rtw
ice
with
hot
H2O
,tr
ansf
erfil
ter
pape
ran
dpr
ecip
itate
toa
beak
er,
add
100
mlH 2O
and
met
hylo
rang
e.
1.0
NH
Cl
Ora
nge-
pink
Na 2C
O3
(oz/
gal)
5m
l30.
707
3N
K2C
O3
(oz/
gal)
5m
l30.
921
3N
KN
aC4H
4O
6·4
H2O
5m
l25
ml2
0%H 2
SO
4,
filte
r,w
ash
flask
and
filte
rpa
per
twic
eea
chw
ithH 2O
,an
dbo
ilth
eco
llect
edfil
trat
e5
min
utes
.
0.1
NK
MnO
4C
olor
less
-pin
kK
NaC
4H
4O
6·4
H2O
(oz/
gal)
5m
l31.
250
3N
Ca
dm
ium
Cya
nid
eC
d2
ml
100
mlH
2O
,10
mlp
H10
buffe
r,E
BT
pow
der,
and
15m
l10%
form
alde
hyde
.0.
1M
ED
TA
Red
-blu
eC
d(o
z/ga
l)5m
l37.
493
3M
Tot
alan
d5
ml
100
mlH
2O
,15
mlc
onc.
NH 4
OH
,an
d10
ml1
0%K
I.0.
1N
AgN
O3
Cle
ar-t
urbi
dT
otal
NaC
N(o
z/ga
l)5m
l32.
614
3N
Fre
eN
aCN
Fre
eN
aCN
(oz/
gal)5
Tot
alN
aCN
21.
744
3C
dN
aOH
5m
l25
mlH
2O
and
5m
lsul
fo-o
rang
e.1.
0N
HC
lO
rang
e-ye
llow
NaO
H(o
z/ga
l)5
ml3
1.06
73
N
Na 2
CO
310
ml
100
mlh
otH 2
O,
35m
l10%
Ba(
NO 3
) 2,
allo
wto
settl
e,fil
ter,
was
hfil
ter
twic
ew
ithho
tH
2O
,tr
ansf
erfil
ter
pape
ran
dpr
ecip
itate
toa
beak
er,
add
100
mlH 2O
and
met
hylo
rang
e.
1.0
NH
Cl
Ora
nge-
pink
Na 2C
O3
(oz/
gal)
5m
l30.
707
3N
Ca
dm
ium
Flu
ob
ora
teC
d2
ml
100
mlH
2O
,10
mlp
H10
buffe
r,E
BT
pow
der,
and
15m
l10%
form
alde
hyde
.0.
1M
ED
TA
Red
-blu
eC
d(o
z/ga
l)5m
l37.
493
3M
539
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
NH
4B
F 45
ml
50m
lH2O
,bo
iling
chip
s,50
ml2
0%N
aOH
inK
jeld
ahlf
lask
.A
ttach
flask
toth
edi
still
atio
nap
para
tus
with
the
colle
ctio
ntu
befr
omth
eco
nden
ser
imm
erse
din
abe
aker
cont
aini
ng10
0m
lsa
tura
ted
H 3BO
3so
lutio
n.B
oilf
lask
till
20m
lrem
ain
inst
ill.
Rem
ove
beak
eran
dad
dm
ethy
lora
nge.
0.1
NH
Cl
Yel
low
-red
NH 4
BF 4
(oz/
gal)
5m
l32.
795
3N
Ca
dm
ium
Su
lfate
Cd
2m
l10
0m
lH2O
,10
mlp
H10
buffe
r,E
BT
pow
der,
and
15m
l10%
form
alde
hyde
.0.
1M
ED
TA
Red
-blu
eC
d(o
z/ga
l)5m
l37.
493
3M
H2S
O4
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
100%
H2S
O4
(oz/
gal)
5m
l30.
654
3N
Ch
rom
ium
CrO
3(C
r61
)10
mlo
fst
ock
10-m
lsam
ple
into
500-
mlv
olum
etric
flask
.P
ipet
te10
mlo
fst
ock,
add
100
ml
H2O
,2
gam
mon
ium
biflu
orid
e,15
ml
conc
.H
Cl,
10m
l10%
KI,
and
star
chso
lutio
n.(S
eeT
able
XIII
for
alte
rnat
em
etho
ds.)
0.1
NN
a 2S 2
O3
Blu
eto
colo
rless
CrO 3
(oz/
gal)
5m
l322
.219
3N
Cr3
110
mlo
fst
ock
10-m
lsam
ple
into
500
mlv
olum
etric
.P
ipet
te10
mlo
fst
ock,
add
200
mlH 2
O,
0.25
gN
a 2O
2,
boil
gent
ly30
min
utes
,m
aint
ain
volu
me
at20
0m
lwith
H 2O.
Coo
l,ad
d2
gam
mon
ium
biflu
orid
e,15
mlc
onc.
HC
l,10
ml1
0%K
I,an
dst
arch
solu
tion.
0.1
NN
a 2S 2
O3
Blu
eto
colo
rless
Cr31
(oz/
gal)
5(m
l322
.219
3N
2C
r61
)3
0.52
0
540
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
SO
425
ml
100
mlH
2O
,10
0m
lred
ucin
gso
lutio
n,bo
il30
min
utes
,re
mov
efr
omhe
at,
add
50m
l10%
Ba(
NO 3
) 2,
100
mlh
otH 2
O.
Allo
wso
lutio
nto
stan
dfo
r3–
4ho
urs,
heat
solu
tion
tobo
iling
.F
ilter
inta
red
Goo
chcr
ucib
le,
was
hpr
ecip
itate
with
hot
H2O
,dr
yin
oven
at11
0˚C
,co
olin
desi
ccat
oran
dw
eigh
.
SO
4(o
z/ga
l)5
(wei
ght
ingr
ams
ofpr
ecip
itate
)32.
195
F5
ml
100
mlH
2O
,1.
0N
NaO
Hto
pH7.
5,us
ing
apH
met
erpr
evio
usly
stan
dard
ized
topH
7.0.
Add
10%
AgN
O 3so
lutio
nun
tilth
edi
sapp
eara
nce
ofth
eye
llow
colo
raf
ter
settl
ing
ofth
epr
ecip
itate
,fil
ter,
was
hpr
ecip
itate
,sa
vefil
trat
e.A
ddA
lizar
inin
dica
tor,
2%H
NO 3
tillc
olor
ofso
lutio
nch
ange
sfr
ompi
nkto
yello
w.
Add
3m
lflu
orid
ebu
ffer.
0.1
NT
h(N
O 3) 4
Yel
low
-pin
kF
(oz/
gal)5
ml3
0.50
73
N
Co
pp
er
Cya
nid
eC
uCN
(Met
hod
I)2
ml
15m
lcon
c.H
NO 3,
heat
tobl
ueco
lor,
100
mlH
2O
,co
nc.
NH 4
OH
tode
epbl
ue,
heat
to14
0˚F
,an
dad
dP
AN
.
0.1
ME
DT
AP
urpl
e-gr
een
CuC
N(o
z/ga
l)5m
l35.
971
3M
CuC
N(M
etho
dII)
2m
l10
0m
lH2O
,15
mlc
onc.
HN
O 3,
heat
tobl
ueco
lor
and
disa
ppea
ranc
eof
brow
nfu
mes
,N
H 4O
Hto
deep
blue
,ac
etic
acid
tolig
htbl
ue,
5g
KI.
Titr
ate
with
Na 2
S 2O
3to
pale
yello
w,
add
5m
lsta
rch
solu
tion,
cont
inue
titra
ting
toco
lorle
ss.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
uCN
(oz/
gal)5
ml3
5.97
13
N
541
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
NaC
Nor
5m
l10
0m
lH2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dN
aCN
(oz/
gal)5
ml3
2.61
43
NK
CN
KC
N(o
z/ga
l)5
ml3
3.47
33
N
NaO
Hor
5m
l25
mlH
2O
and
5m
lsul
fo-o
rang
e.1.
0N
HC
lO
rang
e-ye
llow
NaO
H(o
z/ga
l)5
ml3
1.06
73
NK
OH
KO
H(o
z/ga
l)5
ml3
1.49
63
N
Na 2
CO
3or
K2C
O3
10m
l10
0m
lhot
H 2O
,35
ml1
0%B
a(N
O 3) 2
,al
low
tose
ttle,
filte
r,w
ash
filte
rtw
ice
with
hot
H2O
,tr
ansf
erfil
ter
pape
ran
dpr
ecip
itate
toa
beak
er,
add
100
mlH 2O
,an
dm
ethy
lora
nge.
1.0
NH
Cl
Ora
nge-
pink
Na 2C
O3
(oz/
gal)
5m
l30.
707
3N
K2C
O3,
etc
K2C
O3
(oz/
gal)
5m
l30.
921
3N
KN
aC4H
4O
6·4
H2O
5m
l25
ml2
0%H 2
SO
4,
filte
r,w
ash
flask
and
filte
rpa
per
twic
eea
chw
ithH 2O
,an
dbo
ilth
eco
llect
edfil
trat
e5
min
utes
.
0.1
NK
MnO
4C
olor
less
-pin
kK
NaC
4H
4O
6·4
H2O
(oz/
gal)
5m
l31.
250
3N
Co
pp
er
Flu
ob
ora
teC
u(M
etho
dI)
2m
l10
0m
lH2O
,co
nc.
NH 4
OH
tode
epbl
ue,
heat
to14
0˚F
,an
dad
dP
AN
.0.
1M
ED
TA
Pur
ple-
gree
nC
u(o
z/ga
l)5m
l34.
236
3M
Cu(
BF 4
) 2(o
z/ga
l)5
Cu
33.
73
Cu
(Met
hod
II)2
ml
100
mlH
2O
,N
H4O
Hto
deep
blue
,ac
etic
acid
tolig
htbl
ue,5
gK
I.T
itrat
ew
ithN
a 2S 2
O3
topa
leye
llow
,ad
d5
ml
star
chso
lutio
n,co
ntin
uetit
ratin
gto
colo
rless
.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
u(o
z/ga
l)5m
l34.
236
3N
HB
F 410
ml
100
mlH
2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-g
reen
100%
HB
F4
(oz/
gal)
5m
l31.
171
3N
Co
pp
er
Pyr
op
ho
sph
ate
Cu
(Met
hod
I)2
ml
100
mlH
2O
conc
.N
H 4O
Hto
deep
blue
,he
atto
140˚
Fan
dad
dP
AN
.0.
1M
ED
TA
Pur
ple-
gree
nC
u(o
z/ga
l)5m
l34.
236
3M
542
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Cu
(Met
hod
II)2
ml
100
mlH
2O
,N
H4O
Hto
deep
blue
,ac
e-tic
acid
tolig
htbl
ue,
5g
KI.
Titr
ate
with
Na 2
S 2O
3to
pale
yello
w,
add
5m
lsta
rch
solu
tion,
cont
inue
titra
ting
toco
lorle
ss.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
u(o
z/ga
l)5m
l34.
236
3N
Tot
alP 2
O7
5m
l10
0m
lH2O
,1.
0N
HC
ldro
pwis
eto
pH3.
8(u
sepH
met
erst
anda
rdiz
edat
pH4.
0),
back
-titr
ate
with
1.0
NN
aOH
ifpH
3.8
isov
ersh
ot,
stir
5m
inut
esan
dm
ake
sure
pHis
3.6–
3.8,
add
50m
l20%
ZnS
O 4(a
djus
ted
topH
3.8)
and
stir
10m
inut
es.
Titr
ate
slow
lyw
ithst
irrin
gus
ing
1.0
NN
aOH
topH
3.8
(not
eth
ese
mlN
aOH
used
for
calc
ulat
ion)
.
1.0
NN
aOH
Tot
alP 2O
7(o
z/ga
l)5
ml3
2.32
3N
1C
u3
1.37
Rat
io5
[Tot
alP 2
O7
(oz/
gal)]
/Cu
(oz/
gal)
NH
310
ml
200
mlH
2O
,bo
iling
chip
s,50
ml2
0%N
aOH
inK
jeld
ahlf
lask
.A
ttach
flask
toth
edi
still
atio
nap
para
tus
with
the
colle
ctio
ntu
befr
omth
eco
nden
ser
imm
erse
din
abe
aker
cont
aini
ng10
0m
lsa
tura
ted
H 3BO
3so
lutio
n.B
oilf
lask
and
dist
illov
er10
0m
l.R
emov
ebe
aker
and
add
met
hylo
rang
e.
0.1
NH
Cl
Yel
low
-red
29%
NH 3
(oz/
gal)
5m
l30.
803
N
Co
pp
er
Su
lfate
Cu
(Met
hod
I)2
ml
100
mlH
2O
,co
nc.
NH 4
OH
tode
epbl
ue,
heat
to14
0˚F
,an
dad
dP
AN
.0.
1M
ED
TA
Pur
ple-
gree
nC
u(o
z/ga
l)5m
l34.
236
3M
CuS
O 4·5
H2O
(oz/
gal)
5C
u3
3.93
Cu
(Met
hod
II)2
ml
100
mlH
2O
,N
H4O
Hto
deep
blue
,ac
etic
acid
tolig
htbl
ue,5
gK
I.T
itrat
ew
ithN
a 2S 2
O3
topa
leye
llow
,ad
d5
ml
star
chso
lutio
n,co
ntin
uetit
ratin
gto
colo
rless
.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
u(o
z/ga
l)5m
l34.
236
3N
543
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Cu
(Met
hod
III)
(See
Tab
leX
IV)
H2S
O4
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-g
reen
100%
H2S
O4
(oz/
gal)
5m
l30.
654
3N
Cl
50m
l50
mlH
2O
,25
ml5
0%H
NO 3
,5
drop
s0.
1N
AgN
O3.
Not
e:F
orch
lorid
ean
alys
is,
carb
on-t
reat
the
solu
tion
prio
rto
anal
ysis
.
0.01
NH
g(N
O 3) 2
Tur
bid-
clea
rC
l(pp
m)5
ml3
709.
13
N
Aci
dG
old
Au
20m
l25
mlc
onc.
H 2S
O4,
heat
tow
hite
fum
es,
cool
,ad
d10
ml3
0%H 2O
2,
heat
tow
hite
fum
es.
Rep
eat
H 2O2
and
heat
ing
until
Au
spon
geco
agul
ates
and
solu
tion
clea
rs.
Coo
l,ad
d10
0m
lH2O
,he
atat
140˚
Ffo
r5
min
utes
.F
ilter
thro
ugh
Goo
chcr
ucib
leco
ntai
ning
fiber
glas
sfil
ter
pape
r,w
ash
Au
spon
gew
ithho
tH 2O
,dr
ycr
ucib
lein
oven
at11
0˚C
,co
olin
desi
ccat
oran
dw
eigh
.
Au
(g/L
)5
(wei
ght
ofgo
ldpr
ecip
itate
)350
.0
Go
ldC
yan
ide
Au
20m
lP
roce
dure
asab
ove
for
acid
gold
.A
sab
ove
for
acid
gold
.
NaC
Nor
5m
l10
0m
lH2O
,10
ml1
0%K
I.0.
1N
AgN
O 3C
lear
-tur
bid
NaC
N(g
/L)5
ml3
19.6
053
NK
CN
KC
N(g
/L)
5m
l326
.048
3N
Na 2
CO
3or
K2C
O3
10m
l10
0m
lhot
H 2O
,35
ml1
0%B
a(N
O 3) 2
,al
low
tose
ttle,
filte
r,w
ash
filte
rtw
ice
with
hot
H2O
,tr
ansf
erfil
ter
pape
ran
dpr
ecip
itate
toa
beak
er,
add
100
mlH 2O
,an
dm
ethy
lora
nge.
1.0
NH
Cl
Ora
nge-
pink
NaC
O 3(g
/L)
5m
l35.
303
3N
K2C
O3
(g/L
)1
ml3
6.90
83
N
544
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Ind
ium
Cya
nid
eIn
2m
l10
0m
lH2O
,50
mlR
oche
lleso
lutio
n,10
mlp
H10
buffe
r,he
atto
140˚
F,
and
add
EB
Tpo
wde
r.
0.1
ME
DT
AR
ed-b
lue
In(o
z/ga
l)5m
l37.
655
3M
Tot
alK
CN
5m
l10
0m
lH2O
,20
ml2
0%N
aOH
,an
d10
ml1
0%K
I.0.
1N
AgN
O3
Cle
ar-t
urbi
dT
otal
KC
N(o
z/ga
l)5m
l33.
473
3N
Fre
eK
CN
5m
l10
0m
lH2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dF
ree
KC
N(o
z/ga
l)5m
l33.
473
3N
KO
H5
ml
25m
lH2O
and
5m
lsul
fo-o
rang
e.1.
0N
HC
lO
rang
e-ye
llow
KO
H(o
z/ga
l)5
ml3
1.49
63
N
Ind
ium
Flu
ob
ora
teIn
2m
l10
0m
lH2O
,50
mlR
oche
lleso
lutio
n,10
mlp
H10
buffe
r,he
atto
140˚
F,
and
add
EB
Tpo
wde
r.
0.1
ME
DT
AR
ed-b
lue
In(o
z/ga
l)5m
l37.
655
3M
NH
4B
F 45
ml
50m
lH2O
,bo
iling
chip
s,50
ml2
0%N
aOH
inK
jeld
ahlf
lask
.A
ttach
flask
toth
edi
still
atio
nap
para
tus
with
the
colle
ctio
ntu
befr
omth
eco
nden
ser
imm
erse
din
abe
aker
cont
aini
ng10
0m
lsa
tura
ted
H 3BO
3so
lutio
n.B
oilf
lask
till
20m
lrem
ain
inst
ill.
Rem
ove
beak
eran
dad
dm
ethy
lora
nge.
0.1
NH
Cl
Yel
low
-red
NH 4
BF 4
(oz/
gal)
5m
l32.
795
3N
Iro
nC
hlo
rid
eF
e21
5m
l10
0m
lH2O
,25
ml2
0%Z
nSO 4
,an
d50
ml1
0%H 2
SO
4.
0.1
NK
MnO
4C
olor
less
-pin
kF
e21
(oz/
gal)
5m
l31.
489
3N
545
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Tot
alF
e5
ml
100
mlH
2O
,5
gC
dfla
kes,
boil
5m
inut
es,
cool
and
deca
ntliq
uid
into
500-
mlf
lask
,w
ash
Cd
resi
due
with
H2O
and
add
tofla
sk,
add
25m
l20%
ZnS
O4,
and
50m
l10%
H 2S
O4.
0.1
KM
NO
4C
olor
less
-pin
kT
otal
Fe
(oz/
gal)5
ml3
1.48
93
NF
e31
(oz/
gal)
5T
otal
Fe
2F
e21
HC
l25
ml
100
mlH
2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
36%
HC
l(oz
/gal
)5
ml3
0.54
03
N
Iro
nF
luo
bo
rate
Fe2
15
ml
100
mlH
2O
,25
ml2
0%Z
nSO 4
,an
d50
ml1
0%H 2
SO
4.
0.1
KM
nO4
Col
orle
ss-p
ink
Fe21
(oz/
gal)
5m
l31.
489
3N
Tot
alF
e5
ml
100
mlH
2O
,5
gC
dfla
kes,
boil
5m
inut
es,
cool
and
deca
ntliq
uid
into
500-
mlf
lask
,w
ash
Cd
resi
due
with
H2O
and
add
tofla
sk,
add
25m
l20%
ZnS
O4,
and
50m
l10%
H 2S
O4.
0.1
NK
MnO
4C
olor
less
-pin
kT
otal
Fe
(oz/
gal)5
ml3
1.48
93
N
Fe3
1(o
z/ga
l)5
Tot
alF
e2
Fe2
1
NaC
l5
ml
100
mlH
2O
,5
ml3
0%H 2
O2,
boil
for
10m
inut
es,
filte
r,w
ash
prec
ipita
tew
ithho
tH
2O
,an
dad
dK 2
CrO
4to
filtr
ate.
0.1
NA
gNO
3Y
ello
w-r
edN
aCl(
oz/g
al)5
ml3
1.55
83
N
Le
ad
Flu
ob
ora
teP
b1
ml
100
mlH
2O
,25
mlR
oche
lleso
lutio
n,20
mlc
onc.
NH 4
OH
,an
dE
BT
solu
tion.
0.1
ME
DT
AR
ed-b
lue
Pb
(oz/
gal)5
ml3
27.6
253
M
HB
F 410
ml
100
mlH
2O
.1.
0N
NaO
HC
lear
-tur
bid
100%
HB
F4
(oz/
gal)
5m
l31.
171
3N
Bla
ckN
icke
lZ
n2
ml
100
mlH
2O
,10
mlp
H10
buffe
r,E
BT
pow
der,
and
15m
l10%
form
alde
hyde
.0.
1M
ED
TA
Red
-blu
eZ
n(o
z/ga
l)5m
l34.
358
3M
546
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Ni
2m
l10
0m
lH2O
,10
mlc
onc.
NH 4
OH
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
(mlE
DT
Afo
rN
i2
ml
ED
TA
for
Zn)
33.
914
3M
NaS
CN
10m
l10
0m
lH2O
,15
ml2
0%H 2
SO
4,
and
FA
Sin
dica
tor.
0.1
NA
gNO
3R
ed-c
olor
less
NaS
CN
(oz/
gal)5
ml3
1.08
13
N
Nic
kelF
luo
bo
rate
Ni
2m
l10
0m
lH2O
,10
mlc
onc.
NH 4
OH
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
ml3
3.91
43
M
H3B
O3
10m
l25
mlH
2O
,5.
0g
man
nito
l,an
dbr
omoc
reso
lpur
ple.
1.0
NN
aOH
Gre
en-p
urpl
eH 3B
O3
(oz/
gal)
5m
l30.
824
3N
Nic
kelS
trik
eN
i2
ml
100
mlH
2O
,20
mlc
onc.
NH 4
OH
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
ml3
3.91
43
M
HC
l10
ml
100
mlH
2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
36%
HC
l(fl
oz/g
al)
5m
l31.
115
3N
Nic
kelS
ulfa
ma
teN
i2
ml
100
mlH
2O
,20
mlc
onc.
NH 4
OH
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
ml3
3.91
43
M
NiB
r 25
ml
100
mlH
2O
and
K 2C
rO4.
0.1
NA
gNO 3
Yel
low
/gre
en-r
edN
iBr 2
(oz/
gal)
5m
l32.
914
3N
NiC
l 2·6
H2O
20m
l10
0m
lH2O
and
K 2C
rO4.
0.1
NA
gNO 3
Yel
low
/gre
en-r
edN
iCl 2·6H
2O
(oz/
gal)
5m
l30.
792
3N
H3B
O3
10m
l25
mlH
2O
,5.
0g
man
nito
l,an
dbr
omoc
reso
lpur
ple.
1.0
NN
aOH
Gre
en-p
urpl
eH 3B
O3
(oz/
gal)
5m
l30.
824
3N
547
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
SO
410
ml
100
mlH
2O
,5
ml5
0%H
Cl,
25m
lB
a(N
O3) 2
,al
low
solu
tion
tost
and
4ho
urs,
filte
rin
tare
dG
ooch
cruc
ible
,w
ash
prec
ipita
tew
ithH 2O
,dr
yin
oven
at11
0˚C
,co
olin
desi
ccat
or,
and
wei
gh.
SO
4(o
z/ga
l)5
(wei
ght
ingr
ams
ofpr
ecip
itate
)35.
488
Wa
tts
Nic
kel
Ni
2m
l10
0m
lH2O
,20
mlc
onc.
NH 4
OH
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
ml3
3.91
43
M
NiC
l 2·6
H2O
1m
l10
0m
lH2O
,1
mlK
2C
rO4
(ifpH
isbe
low
4.0,
add
1.0
gC
aCO 3).
0.1
NA
gNO
3Y
ello
w/g
reen
-red
NiC
l 2·6
H2O
(oz/
gal)5
ml3
15.8
473
N
NiS
O4·6
H2O
(oz/
gal)
54.
5(N
i20.
247
3N
iCl 2
·6H
2O
)
H3B
O3
10m
l25
mlH
2O
,5.
0g
man
nito
l,an
dbr
omoc
reso
lpur
ple.
1.0
NN
aOH
Gre
en-p
urpl
eH 3B
O3
(oz/
gal)
5m
l30.
824
3N
Nic
kel-Ir
on
Ni
2m
l10
0m
lH2O
,20
mlc
onc.
NH 4
OH
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
ml3
3.91
43
M
Fe2
15
ml
100
mlH
2O
,25
ml2
0%Z
nSO 4
,an
d50
ml1
0%H 2
SO
4.
0.1
NK
MnO
4C
olor
less
-pin
kF
e21
(oz/
gal)
5m
l31.
489
3N
Tot
alF
e5
ml
100
mlH
2O
,5
gC
dfla
kes,
boil
5m
inut
es,
cool
and
deca
ntliq
uid
into
500-
mlf
lask
,w
ash
Cd
resi
due
with
H2O
and
add
tofla
sk,
add
25m
l20%
ZnS
O4,
and
50m
l10%
H 2S
O4.
0.1
KM
NO
4C
olor
less
-pin
kT
otal
Fe
(oz/
gal)5
ml3
1.48
93
NF
e31
(oz/
gal)
5T
otal
Fe
2F
e21
H3B
O3
10m
l25
mlH
2O
,5.
0g
man
nito
l,an
dbr
omoc
reso
lpur
ple.
1.0
NN
aOH
Gre
en-p
urpl
eH 3B
O3
(oz/
gal)
5m
l30.
824
3N
548
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Pa
llad
ium
Pd
10m
l10
mlc
onc.
HN
O 3,he
atun
tilsy
rupy
,10
mlc
onc.
HN
O 3,
heat
toon
set
ofbo
iling
.A
dd25
0m
lH2O
,co
ol,
slow
lyad
d40
mld
imet
hylg
lyox
ime
solu
tion,
allo
wso
lutio
nto
stan
dat
leas
t2
hour
s,fil
ter
thro
ugh
No.
3po
rosi
tyta
red
cruc
ible
,w
ash
prec
ipita
tew
ithH 2O
.D
ryin
oven
at11
0˚C
,co
olin
desi
ccat
or,
and
wei
gh.
Pd
(g/L
)5(w
eigh
tin
gram
sof
prec
ipita
te)3
31.6
7
Pla
tinu
mP
t10
ml
10m
lcon
c.H
Cl,
heat
until
syru
py,
100
mlH
2O
,5
gso
dium
acet
ate,
1m
lcon
c.fo
rmic
acid
,he
atat
140˚
Ffo
r5
hour
s,fil
ter,
was
hpr
ecip
itate
with
hot
H 2O.
Pla
cefil
ter
pape
ran
dP
tpr
ecip
itate
inta
red
porc
elai
ncr
ucib
le,
dry
slow
lyw
ithB
unse
nbu
rner
,ch
arfil
ter
pape
r,dr
yP
tpr
ecip
itate
athi
ghte
mpe
ratu
refo
r30
min
utes
.C
ooli
nde
sicc
ator
and
wei
gh.
Pt
(g/L
)5(w
eigh
tin
gram
sof
prec
ipita
te)3
100.
0
Rh
od
ium
Rh
25m
l2
gM
gtu
rnin
gs,
conc
.H
Cld
ropw
ise.
Whe
nal
lMg
diss
olve
s,ad
d0.
5g
Mg
turn
ings
and
HC
ldro
pwis
eto
ensu
reco
mpl
ete
prec
ipita
tion
ofR
h.F
ilter
solu
tion
inta
red
Goo
chcr
ucib
leco
ntai
ning
fiber
glas
sfil
ter
pape
r,w
ash
prec
ipita
tew
ithho
tH 2
O,
dry
inov
enat
110˚
C,
cool
inde
sicc
ator
and
wei
gh.
Rh
(g/L
)5(w
eigh
tin
gram
sof
prec
ipita
te)3
40.0
H2S
O4
or
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
100%
H2S
O4
(g/L
)5
ml3
4.90
43
NH
3P
O4
100%
H 3P
O4
(g/L
)5
ml3
9.80
03
N
549
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Ru
the
niu
mR
uthe
nium
cann
otbe
easi
lyde
term
ined
byvo
lum
etric
orgr
avim
etric
met
hods
.It
isus
ually
dete
rmin
edby
emis
sion
spec
tros
copy
and
itsan
alys
issh
ould
bere
ferr
edto
aco
mpe
tent
labo
rato
ry.
Silv
er
Cya
nid
eA
g5
ml
15m
lcon
c.H 2
SO
4,
5m
lcon
c.H
NO 3
,he
atun
tilth
edi
sapp
eara
nce
ofor
ange
fum
es,
cool
,ad
d10
0m
lcol
dH 2O
,an
dF
AS
indi
cato
r.
0.1
NK
SC
NC
olor
less
-red
Ag
(oz/
gal)5
ml3
2.87
73
NA
gCN
(oz/
gal)
5A
g3
1.24
1
NaC
Nor
5m
l10
0m
lH2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dN
aCN
(oz/
gal)5
ml3
2.61
43
NK
CN
KC
N(o
z/ga
l)5
ml3
3.47
33
N
Na 2
CO
3or
10m
l10
0m
lhot
H 2O
,35
ml1
0%B
a(N
O 3) 2
allo
wto
settl
e,fil
ter,
was
hfil
ter
twic
ew
ithho
tH
2O
,tr
ansf
erfil
ter
pape
ran
dpr
ecip
itate
toa
beak
er,
add
100
mlH 2O
and
met
hylo
rang
e.
1.0
NH
Cl
Ora
nge-
pink
Na 2C
O3
(oz/
gal)
5m
l30.
707
3N
K2C
O3
K2C
O3
(oz/
gal)
5m
l30.
921
3N
Tin
Flu
ob
ora
teS
n21
2m
l10
0m
lH2O
,25
ml5
0%H
Cl,
10m
lst
arch
solu
tion,
add
bica
rbon
ate
durin
gtit
ratio
n.
0.1
NK
I-K
IO3
Col
orle
ss-b
lue
Sn21
(oz/
gal)
5m
l33.
956
3N
550
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Sn4
12
ml
In50
0-m
lfla
skad
dsa
mpl
e,10
0m
lco
nc.
HC
l,2
drop
sS
bCl
3so
lutio
n.A
dd18
0m
lH2O
,5-
in.
fold
ed“U
”-sh
aped
nick
elst
ripan
d5.
0g
redu
ced
iron
pow
der.
Sto
pper
flask
with
rubb
erst
oppe
rfit
ted
with
1⁄4-
in.
glas
stu
beim
mer
sed
into
asa
tura
ted
NaH
CO
3
solu
tion.
Hea
tso
lutio
non
hot
plat
eto
boil
for
20m
inut
esan
dth
enpl
ace
inco
olin
gta
nkan
dal
low
toco
olto
room
tem
pera
ture
.M
ake
sure
glas
sou
tlet
tube
isim
mer
sed
inth
eN
aHC
O 3.R
emov
est
oppe
ran
dad
dst
arch
solu
tion.
0.1
NK
I-K
IO3
Col
orle
ss-b
lue
Sn41
(oz/
gal)
5m
l33.
956
3N
2S
n21
HB
F 410
ml
100
mlH
2O
and
met
hylo
rang
e.1.
0N
NaO
HC
lear
-tur
bid
100%
HB
F4
(oz/
gal)
5m
l31.
171
3N
Fre
eH 3
BO
310
ml
100
mlH
2O
,10
mlN
a 2S
O4
solu
tion.
Titr
ate
topH
7.0,
usin
ga
pHm
eter
prev
ious
lyst
anda
rdiz
edto
pH7.
0.A
dd5
gm
anni
tol,
titra
tefr
ompH
7.0
topH
8.0
(mlN
aOH
requ
ired
for
this
step
are
used
for
the
calc
ulat
ion)
.
1.0
NN
aOH
H 3B
O3
(oz/
gal)
5m
l30.
824
3N
551
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Tin
Sta
nn
ate
K2S
nO3·3
H2O
5m
l10
0m
lH2O
,50
mlc
onc.
HC
l,3.
0g
iron
pow
der
in50
0-m
lfla
sk.
Sto
pper
flask
with
stop
per
fitte
dw
itha
glas
stu
beim
mer
sed
ina
beak
erfil
led
with
satu
rate
dbi
carb
onat
eso
lutio
n.H
eat
gent
lytil
liro
ndi
ssol
ves.
Coo
lto
room
tem
pera
ture
,m
akin
gsu
reou
tlet
tube
isim
mer
sed
inbi
carb
onat
eso
lutio
n.A
dd10
mls
tarc
hso
lutio
nan
dbi
carb
onat
edu
ring
titra
tion.
0.1
NK
I-K
IO3
Col
orle
ss-b
lue
K 2SnO
3·3
H2O
(oz/
gal)5
ml3
3.98
63
NN
a 2S
nO3·3
H2O
Na 2
SnO
3·3
H2O
(oz/
gal)
5m
l33.
556
3N
KO
H5
ml
25m
lH2O
and
5m
lsul
fo-o
rang
e1.
0N
HC
lO
rang
e-ye
llow
KO
H(o
z/ga
l)5
ml3
1.49
63
NN
aOH
NaO
H(o
z/ga
l)5m
l31.
067
3N
Tin
Su
lfate
SnS
O 45
ml
100
mlH
2O
,25
ml5
0%H
Cl,
10m
lst
arch
solu
tion,
add
bica
rbon
ate
durin
gtit
ratio
n.
0.1
NK
I-K
IO3
Col
orle
ss-b
lue
SnS
O 4(o
z/ga
l)5
ml3
2.86
33
NS
n21
(oz/
gal)
5S
nSO 4
30.
553
Sn4
12
ml
In50
0-m
lfla
skad
dsa
mpl
e,10
0m
lco
nc.
HC
l,2
drop
sS
bCl
3so
lutio
n.A
dd18
0m
lH2O
,5-
in.
fold
ed“U
”-sh
aped
nick
elst
ripan
d5.
0g
redu
ced
iron
pow
der.
Sto
pper
flask
with
rubb
erst
oppe
rfit
ted
with
1⁄4-
in.
glas
stu
beim
mer
sed
into
asa
tura
ted
NaH
CO
3
solu
tion.
Hea
tso
lutio
non
hot-
plat
eto
boil
for
20m
inut
esan
dth
enpl
ace
inco
olin
gta
nkan
dal
low
toco
olto
room
tem
pera
ture
.M
ake
sure
glas
sou
tlet
tube
isim
mer
sed
inth
eN
aHC
O 3.R
emov
est
oppe
ran
dad
dst
arch
solu
tion.
0.1
NK
I-K
IO3
Col
orle
ss-b
lue
Sn41
(oz/
gal)
5m
l33.
956
3N
2S
n21
552
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
H2S
O4
10m
l10
0m
lH2O
,25
mla
mm
oniu
mox
alat
eso
lutio
n,an
dm
ethy
lora
nge.
1.0
NN
aOH
Red
-or
ange
/yel
low
100%
H 2S
O4
(oz/
gal)
5m
l30.
654
%v
H2S
O4
5m
l30.
279
3N
Tin
-Le
ad
Flu
ob
ora
teS
n21
100
ml
H 2O
,25
ml5
0%H
Cl,
10m
lsta
rch
solu
tion,
add
bica
rbon
ate
durin
gtit
ratio
n0.
1N
KI-
KIO
3C
olor
less
-blu
eS
n21
(oz/
gal)
5m
l33.
956
3N
Sn4
12
ml
In50
0-m
lfla
skad
dsa
mpl
e,10
0m
lco
nc.
HC
l,2
drop
sS
bCl
3so
lutio
n.A
dd18
0m
lH2O
,5-
in.
fold
ed“U
”-sh
aped
nick
elst
ripan
d5.
0g
redu
ced
iron
pow
der.
Sto
pper
flask
with
rubb
erst
oppe
rfit
ted
with
1⁄4-
in.
glas
stu
beim
mer
sed
into
asa
tura
ted
NaH
CO
3
solu
tion.
Hea
tso
lutio
non
hot-
plat
eto
boil
for
20m
inut
esan
dth
enpl
ace
inco
olin
gta
nkan
dal
low
toco
olto
room
tem
pera
ture
.M
ake
sure
glas
sou
tlet
tube
isim
mer
sed
inth
eN
aHC
O 3.R
emov
est
oppe
ran
dad
dst
arch
solu
tion.
0.1
NK
I-K
IO3
Col
orle
ss-b
lue
Sn41
(oz/
gal)
5m
l33.
956
3N
2S
n21
Pb
2m
l5
mlc
onc.
HN
O 3,
heat
tills
yrup
y,co
olan
dad
d:25
mlR
oche
lleso
lutio
n,15
ml
conc
.N
H 4O
H,
15m
l10%
NaC
Nan
dE
BT
solu
tion.
0.1
ME
DT
AR
ed-b
lue
Pb
(oz/
gal)5
ml3
13.8
133
M
HB
F 410
ml
100
mlH
2O
.1.
0N
NaO
HC
lear
-tur
bid
100%
HB
F4
(oz/
gal)
5m
l31.
171
3N
553
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Fre
eH 3
BO
310
ml
100
mlH
2O
,10
mlN
a 2S
O4
solu
tion.
Titr
ate
topH
7.0,
usin
ga
pHm
eter
prev
ious
lyst
anda
rdiz
edto
pH7.
0.A
dd5
gm
anni
tol,
titra
tefr
ompH
7.0
topH
8.0
(mlN
aOH
requ
ired
for
this
step
are
used
for
the
calc
ulat
ion)
.
1.0
NN
aOH
H 3B
O3
(oz/
gal)
5m
l30.
824
3N
Tin
-Le
ad
Me
tha
ne
Su
lfon
ate
Sn1
25
ml
100
mlH
2O
,25
ml5
0%H
Cl,
10m
lst
arch
solu
tion,
add
bica
rbon
ate
durin
gtit
ratio
n.
0.1
NK
I-K
IO3
Col
orle
ssbl
ueS
n21
(g/L
)5
ml3
11.8
693
N
Sn4
15
ml
In50
0-m
lfla
skad
dsa
mpl
e,10
0m
lco
nc.
HC
l,2
drop
sS
bCl
3so
lutio
n.A
dd18
0m
lH2O
,fo
lded
“U”-
shap
edni
ckel
strip
and
5.0
gre
duce
diro
npo
wde
r.S
topp
erfla
skw
ithru
bber
stop
per
fitte
dw
ith1⁄4-
in.
glas
stu
beim
mer
sed
into
asa
tura
ted
NaH
CO 3
solu
tion.
Hea
tso
lutio
non
hot-
plat
eto
boil
for
20m
inut
esan
dth
enpl
ace
inco
olin
gta
nkan
dal
low
toco
olto
room
tem
pera
ture
.M
ake
sure
glas
sou
tlet
tube
isim
mer
sed
inth
eN
aHC
O 3.
Rem
ove
stop
per
and
add
star
chso
lutio
n.
0.1
NK
I-K
IO3
Col
orle
ss-b
lue
Sn41
(g/L
)5
ml3
11.8
693
N(S
n21
)
Pb
25m
l75
mlH
2O
,3
mlH
2O
2,
50m
lRoc
helle
solu
tion,
25m
lpH
10bu
ffer,
EB
Tso
lutio
n,15
ml1
0%fo
rmal
dehy
de.
0.1
ME
DT
AR
ed-b
lue
Pb
(g/L
)5m
l38.
288
3M
Met
hane
sulfo
nic
acid
(MS
A)
10m
l10
0m
lH2O
,ph
enol
phth
alei
n.1.
0N
NaO
HC
olor
less
-pin
k10
0%M
SA
(g/L
)5
ml3
9.61
3N
554
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Tin
-Nic
kel
Sn
2m
l10
0m
lH2O
,25
ml5
0%H
Cl,
10m
lst
arch
solu
tion,
add
bica
rbon
ate
durin
gtit
ratio
n.
0.1
NK
I-K
IO3
Cle
arbl
ueS
n(o
z/ga
l)5m
l33.
956
3N
Ni
2m
l25
mlH
2O
,1
ml3
0%H 2
O2,
heat
gent
lyto
boil,
cool
,ad
d10
mlt
arta
ricac
idso
lutio
n.N
eutr
aliz
ew
ithco
nc.
NH 4O
Hto
abl
ueco
lor,
add
20m
lpH
10bu
ffer,
150
mlH
2O
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
ml3
3.91
43
M
NH
4H
F 210
ml
200
mlH
2O
,bo
iling
chip
s,50
ml2
0%N
aOH
inK
jeld
ahlf
lask
.A
ttach
flask
toth
edi
still
atio
nap
para
tus
with
the
colle
ctio
ntu
befr
omth
eco
nden
ser
imm
erse
din
abe
aker
cont
aini
ng10
0m
lsa
tura
ted
H 3BO
3so
lutio
n.B
oilf
lask
and
dist
illov
er10
0m
l.R
emov
ebe
aker
from
colle
ctio
ntu
bebe
fore
rem
ovin
ghe
atso
urce
.A
ddm
ethy
lora
nge.
0.1
NH
Cl
Yel
low
-red
NH 4
HF 2
(oz/
gal)
5m
l30.
761
3N
Zin
cC
hlo
rid
e
Zn
2m
l10
0m
lH2O
,10
mlp
H10
buffe
r,E
BT
pow
der,
and
15m
l10%
form
alde
hyde
.0.
1M
ED
TA
Red
-blu
eZ
n(o
z/ga
l)5m
l34.
358
3M
Cl
1m
l10
0m
lH2O
,1
mlK
2C
rO4.
0.1
NA
gNO 3
Yel
low
-red
Cl(
oz/g
al)5
ml3
4.72
73
N
Zin
cC
yan
ide
Zn
2m
l10
0m
lH2O
,10
mlp
H10
buffe
r,E
BT
pow
der,
and
15m
l10%
form
alde
hyde
.0.
1M
ED
TA
Red
-blu
eZ
n(o
z/ga
l)5m
l34.
358
3M
555
Tab
leV
III.
Tes
tM
etho
dsfo
rE
lect
ropl
atin
gS
olut
ions
(co
nt.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Tot
alN
aCN
1m
l10
0m
lH2O
,20
ml2
0%N
aOH
,an
d10
ml1
0%K
I.0.
1N
AgN
O3
Cle
ar-t
urbi
dT
otal
NaC
N(o
z/ga
l)5m
l313
.069
3N
NaO
H5
ml
25m
lH2O
,5
mls
ulfo
-ora
nge.
1.0
NH
Cl
Ora
nge-
yello
wN
aOH
(oz/
gal)
5m
l31.
067
3N
Na 2
CO
310
ml
100
mlh
otH 2
O,
35m
l10%
Ba(
NO 3
) 2,
allo
wto
settl
e,fil
ter,
was
hfil
ter
twic
ew
ithho
tH
2O
,tr
ansf
erfil
ter
pape
ran
dpr
ecip
itate
toa
beak
er,
add
100
mlH 2O
,an
dm
ethy
lora
nge.
1.0
NH
Cl
Ora
nge-
pink
Na 2C
O3
(oz/
gal)
5m
l30.
707
3N
ED
TA
,et
hyle
nedi
amin
ete
tra
acet
icac
id;
PA
N,
pero
xyac
etyl
nitr
ate.
a Use
deio
nize
dor
dist
illed
wat
erfo
ral
lsol
utio
ns.
556
Tab
leIX
.T
est
Met
hods
for
Ele
ctro
less
Pla
ting
Sol
utio
ns
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Co
pp
er
Cu
20m
l10
0m
lH2O
,aco
nc.
NH 4
OH
tode
epbl
ue,
heat
to14
0˚F
,an
dad
dpe
roxy
acet
alni
trat
e.
0.1
ME
DT
AP
urpl
e-gr
een
Cu
(g/L
)5m
l33.
177
3M
NaO
H5
ml
150
mlH
2O
.T
itrat
eto
pH10
.5,
usin
ga
pHm
eter
prev
ious
lyst
anda
rdiz
edto
pH10
.0.
0.1
NH
Cl
NaO
H(g
/L)5
ml3
8.0
3N
HC
HO
5m
l10
0m
lH2O
.A
djus
tpH
to9.
0,us
ing
apH
met
erpr
evio
usly
stan
dard
ized
topH
10.0
.A
dd25
mls
odiu
msu
lfite
solu
tion,
stir
1m
inut
e.T
itrat
eto
pH9.
0(t
hese
ml
are
used
for
the
calc
ulat
ion)
.
0.1
NH
Cl
HC
HO
(g/l)
5m
l316
.232
3N
Nic
kel
Ni
5m
l10
0m
lH2O
,20
mlc
onc.
NH 4
OH
,an
dm
urex
ide
pow
der.
0.1
ME
DT
AO
rang
e-pu
rple
Ni(
oz/g
al)5
ml3
1.56
63
M
NaH
2P
O2·H
2O
5m
lU
segl
ass-
stop
pere
dio
dine
flask
.A
dd5
mlc
onc.
H 2S
O4
and
50m
l0.1
Nio
dine
solu
tion.
Sw
irlto
mix
,st
oppe
rfla
sk,
and
plac
ein
dark
for
30m
inut
es,
then
add
star
chso
lutio
n.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssN
aH2P
O2·H
2O
(oz/
gal)
5(m
lI2
3N
-I2
2m
lN
a 2S 2
O3
3N
-Na 2
S 2O
3)
31.
413
Tin
Sn2
12
ml
100
mlH
2O
,25
ml5
0%H
Cl,
10m
lst
arch
solu
tion,
add
bica
rbon
ate
durin
gtit
ratio
n.
0.1
NK
I-K
IO3
Cle
ar-b
lue
Sn
(oz/
gal)5
ml3
3.95
63
N
ED
TA
,et
hyle
nedi
amin
ete
tra
acet
icac
id.
a Use
deio
nize
dor
dist
illed
wat
erfo
ral
lsol
utio
ns.
557
Tab
leX
.T
est
Met
hods
for
Ano
dizi
ngS
olut
ions
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Ch
rom
icC
rO3a
10m
lof
stoc
k10
mls
ampl
ein
to50
0m
lvol
umet
ric.
Pip
ette
10m
lof
stoc
k,ad
d10
0m
lH
2O
,b2
gam
mon
ium
biflu
orid
e,15
ml
conc
.H
Cl,
15m
l10%
KI,
and
star
chso
lutio
n.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
rO 3(o
z/ga
l)5
ml3
22.2
193
N
Fre
eC
rO3
25m
l10
0m
lH2O
.T
itrat
eto
pH3.
05,
usin
ga
pHm
eter
prev
ious
lyst
anda
rdiz
edto
pH4.
0.
1.0
NN
aOH
Col
orle
ss–p
ink
Fre
eC
rO 3(o
z/ga
l)5
ml3
0.53
33
N
Su
lfuric
Tot
alH
2S
O4
5m
l10
0m
lH2O
and
phen
olph
thal
ein.
1.0
NN
aOH
Col
orle
ss-p
ink
Tot
alH
2S
O4
(oz/
gal)
5m
l31.
308
3N
Fre
eH 2
SO
45
ml
100
mlH
2O
,10
mlK
Fso
lutio
n,an
dph
enol
phth
alei
n.1.
0N
NaO
HC
olor
less
-pin
kF
ree
H 2SO
4(o
z/ga
l)5
ml3
1.30
83
N
Al
Al(
oz/g
al)5
(mlN
aOH
for
Tot
alH
2S
O4
2m
lNaO
Hfo
rfr
eeH 2
SO
4)
30.
240
3N
a See
also
alte
rnat
em
etho
din
Fig
.2.
b Use
deio
nize
dor
dist
illed
wat
erfo
ral
lsol
utio
ns.
558
Tab
leX
I.T
est
Met
hods
for
Aci
dD
ips
and
Ele
ctro
polis
hing
Sol
utio
ns
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
HC
2H
3O
210
ml
100
mlH
2O
aan
dph
enol
phth
alei
n.1.
0N
NaO
HC
olor
less
-pin
k%
wt
HC
2H
3O
2(1
00%
)5(m
l30.
6005
3N
)/s.
g.so
lutio
nH
3C
6H
5O
7·H
2O
(Citr
icac
id)
10m
l10
0m
lH2O
and
phen
olph
thal
ein.
1.0
NN
aOH
Col
orle
ss-p
ink
%w
tH
3C
6H
5O
7·H
2O
5(m
l30.
7005
3N
)/s.
g.so
lutio
nH
BF 4
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
%w
tH
BF
4(1
00%
)5(m
l30.
8781
3N
)/s.
g.so
lutio
nH
Cl
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
%w
tH
Cl(
100%
)5
(ml3
0.36
463
N)/
s.g.
solu
tion
HF
2g
100
mlH
2O
and
phen
olph
thal
ein.
(Not
e:us
epl
astic
labw
are.
)1.
0N
NaO
HC
olor
less
-pin
k%
wt
HF
(100
%)5
(ml3
2.00
13
N)/
wt
HN
O3
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
%w
tH
NO
3(1
00%
)5(m
l30.
6301
3N
)/s.
g.so
lutio
nH
3P
O4
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
%w
tH
3P
O4
(100
%)5
(ml3
0.98
003
N)/
s.g.
solu
tion
H2S
O4
10m
l10
0m
lH2O
and
met
hylo
rang
e1.
0N
NaO
HR
ed-y
ello
w/g
reen
%w
tH
2S
O4
(100
%)5
(ml3
0.49
043
N)/
s.g.
solu
tion
HN
O3
1H
F10
ml
100
mlH
2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
Am
l1
ml
100
mlH
2O
,A
lizar
in,
1.0
NN
aOH
topi
nk,
2%H
NO 3
drop
wis
efr
ompi
nkto
yello
w,
3m
lflu
orid
ebu
ffer.
0.1
NT
h(N
O 3) 4
Yel
low
-pin
kB
ml
%w
tH
NO
3(1
00%
)5[(
Am
l3
N2
103
Bm
l3N
)3
0.63
01]/s
.g.
solu
tion
%w
tH
F(1
00%
)5(B
ml3
20.0
063
N)/
s.g.
solu
tion
H3P
O4
1H
2S
O4
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
Am
lA
ddph
enol
phth
alei
nto
the
solu
tion
abov
e.1.
0N
NaO
HP
urpl
e-re
dB
ml
%w
tH
2S
O4
(100
%)5
[(A
ml
2B
ml)
30.
4904
3N
]/s.g
.so
lutio
n%
wt
H3P
O4
(100
%)5
(Bm
l30.
9800
3N
)/s.
g.so
lutio
nH
2S
O4
1H
2O
2H
2S
O4
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
NaO
HR
ed-y
ello
w/g
reen
%w
tH
2S
O4
(100
%)5
(ml3
0.49
043
N)/
s.g.
solu
tion
559
Tab
leX
I.T
est
Met
hods
for
Aci
dD
ips
and
Ele
ctro
polis
hing
Sol
utio
ns(c
on
t.)
Ba
thS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
H2O
22
ml
100
mlH
2O
and
25m
l20%
H 2SO
4.
0.1
NK
MnO
4C
olor
less
-pin
k%
wt
H 2O
2(1
00%
)5(m
l328
.345
3N
)/s.
g.so
lutio
nC
rO3
1H
2S
O4
CrO
3
10m
lof
stoc
k10
-mls
ampl
ein
to50
0m
lvol
umet
ricfla
sk.
Pip
ette
10m
lof
stoc
k,ad
d10
0m
lH
2O
,2
gam
mon
ium
biflu
orid
e,15
ml
conc
.H
Cl,
10m
l10%
KI,
and
star
chso
lutio
n.
0.1
NN
a 2S 2
O3
Blu
e-co
lorle
ssC
rO 3(o
z/ga
l)5
ml3
22.2
193
N
H2S
O4
25m
l10
0m
lH2O
,10
0m
lred
ucin
gso
lutio
n,bo
il30
min
utes
,re
mov
efr
omhe
at,
add
50m
l10%
Ba(
NO 3
) 2,
100
mlh
otH 2
O.
Allo
wso
lutio
nto
stan
dfo
r3–
4ho
urs,
heat
solu
tion
tobo
iling
.F
ilter
inta
red
Goo
chcr
ucib
le,
was
hpr
ecip
itate
with
hot
H2O
,dr
yin
oven
at11
0˚C
,co
olin
desi
ccat
or,
and
wei
gh.
100%
H 2S
O4
(oz/
gal)
5(w
eigh
tin
gram
sof
prec
ipita
te)3
2.24
1
a Use
deio
nize
dor
dist
illed
wat
erfo
ral
lsol
utio
ns.
560
Tab
leX
II.T
est
Met
hods
for
Alk
alin
eC
lean
ers
So
lutio
nS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
Na 2
O25
ml
100
mlH
2O
aan
dm
ethy
lora
nge.
1.0
NH
Cl
Yel
low
-ora
nge/
red
Na
2O
(oz/
gal)
5m
l30.
165
3N
Na 2
CO
31
NaO
H10
ml
100
mlH
2O
and
sulfo
oran
ge.
1.0
NH
Cl
Ora
nge-
yello
wB
ml
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
HC
lY
ello
w-o
rang
e/re
dA
ml
Na 2
CO
3(o
z/ga
l)5
(Am
l2
Bm
l)30.
707
3N
NaO
H(o
z/ga
l)5B
ml3
0.53
33
NN
aOH
1N
aCN
NaO
H10
ml
100
mlH
2O
and
sulfo
oran
ge.
1.0
NH
Cl
Ora
nge-
yello
wN
aOH
(oz/
gal)
5m
l30.
533
3N
NaC
N10
ml
100
mlH
2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dN
aCN
(oz/
gal)5
ml3
1.30
73
NN
a 2C
O3
1N
aCN
10m
l10
0m
lH2O
and
met
hylo
rang
e.1.
0N
HC
lY
ello
w-o
rang
e/re
dA
ml
10m
l10
0m
lH2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dB
ml
NaC
N(o
z/ga
l)5B
ml3
1.30
73
NN
a 2C
O3
(oz/
gal)
5(A
ml
3N
2B
ml
3N
)3
0.70
7N
a 2C
O3
1N
a 3P
O4
10m
l15
0m
lH2O
and
met
hylo
rang
e.1.
0N
HC
lY
ello
w-o
rang
e/re
dA
ml
Boi
labo
veso
lutio
n5
min
utes
,co
ol,
and
add
phen
olph
thal
ein.
1.0
NN
aOH
Col
orle
ss-p
ink
Bm
l
Na 3
PO
4(o
z/ga
l)5
Bm
l32.
1863
NN
a 2C
O3
(oz/
gal)
5(A
ml
3N
22
3B
ml3
N)
30.
707
Na 3
PO
41
NaC
N1
Na 2
SiO
3·5
H2O
10m
l15
0m
lH2O
and
met
hylo
rang
e.1.
0N
HC
lY
ello
w-o
rang
e/re
dA
ml
Boi
labo
veso
lutio
n5
min
utes
,co
ol,
and
add
phen
olph
thal
ein.
1.0
NN
aOH
Col
orle
ss-p
ink
Bm
l
10m
l10
0m
lH2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dC
ml
Na 3
PO
4(o
z/ga
l)5
Bm
l32.
1863
NN
aCN
(oz/
gal)5
Cm
l31.
307
3N
Na 2
SiO
3·5
H2O
(oz/
gal)
5(A
ml
3N
22
3B
ml3
N2
Cm
l3N
)3
1.41
4
561
Tab
leX
II.T
est
Met
hods
for
Alk
alin
eC
lean
ers
(co
nt.)
So
lutio
nS
am
ple
Siz
eR
ea
ge
nts
(To
be
ad
de
din
ord
er
liste
d)
Titr
an
tC
olo
rC
ha
ng
eC
alc
ula
tion
s(m
l,N
,M
-titr
an
t)
NaO
H1
Na 2
CO
31
Na 3
PO
4
10m
l15
0m
lH2O
and
met
hylo
rang
e.1.
0N
HC
lY
ello
w-o
rang
e/re
dA
ml
Boi
labo
veso
lutio
n5
min
utes
,co
ol,
and
add
phen
olph
thal
ein.
1.0
1.0
NaO
HC
olor
less
-pin
kB
ml
10m
l10
0m
lH2O
and
phen
olph
thal
ein.
1.0
NH
Cl
Pin
k-co
lorle
ssC
ml
NaO
H(o
z/ga
l)5(2
3C
ml2
Am
l)3
0.53
33
NN
a 2C
O3
(oz/
gal)
5(A
ml
3N
2B
ml
3N
2C
ml3
N)
31.
414
Na 3
PO
4(o
z/ga
l)5
Bm
l32.
186
3N
NaO
H1
Na 3
PO
41
NaC
N10
ml
150
mlH
2O
and
met
hylo
rang
e.1.
0N
HC
lY
ello
w-o
rang
e/re
dA
ml
Boi
labo
veso
lutio
n5
min
utes
,co
ol,
and
add
phen
olph
thal
ein.
1.0
1.0
NaO
HC
olor
less
-pin
kB
ml
10m
l10
0m
lH2O
and
10m
l10%
KI.
0.1
NA
gNO 3
Cle
ar-t
urbi
dC
ml
Na 3
PO
4(o
z/ga
l)5
Bm
l32.
186
3N
NaC
N(o
z/ga
l)5C
ml3
1.30
73
NN
aOH
(oz/
gal)5
Am
l3
N2
23
Bm
l3N
2C
ml3
N)
30.
533
a Use
deio
nize
dor
dist
illed
wat
erfo
ral
lsol
utio
ns.
562
Table XIII. Alternate Method for Chromic Acid
Degrees Baumé Oz/gal-CrO3 Degrees Baumé Oz/gal-CrO3
1.50 2.1 19.00 29.02.00 2.8 19.50 29.82.50 3.4 20.00 30.63.00 4.1 20.50 31.53.50 4.8 21.00 32.44.00 5.5 21.50 33.34.50 6.2 22.00 34.25.00 6.8 22.50 35.15.50 7.5 23.00 36.06.00 8.2 23.50 37.16.50 8.9 24.00 38.27.00 9.7 24.50 39.17.50 10.4 25.00 40.08.00 11.1 25.50 40.98.50 11.9 26.00 41.99.00 12.6 26.50 42.99.50 13.4 27.00 44.0
10.00 14.2 27.50 45.010.50 15.0 28.00 46.011.00 15.8 28.50 47.111.50 16.5 29.00 48.212.00 17.3 29.50 49.212.50 18.2 30.00 50.213.00 19.1 30.50 51.513.50 19.8 31.00 52.714.00 20.4 31.50 54.014.50 21.2 32.00 55.215.00 22.0 32.50 56.315.50 22.9 33.00 57.516.00 23.7 33.50 58.716.50 24.5 34.00 60.017.00 25.4 34.50 61.217.50 26.3 35.00 62.318.00 27.2 35.50 63.518.50 28.1 36.00 64.8
Procedure: 1. Cool the solution to room temperature after testing.2. Determine the density of the solution with a Baumé hydrometer.3. Read the oz/gal of chromic acid (CrO3) corresponding to this density.
563
Table XIV. Alternate Method for Copper Sulfate
Baumé
Copper Sulfate1Sulfuric Acid
(oz/gal) Baumé
Copper Sulfate1Sulfuric Acid
(oz/gal)
1.5 2.8 14.5 24.72.0 3.5 15.0 25.72.5 4.3 15.5 26.83.0 5.1 16.0 27.83.5 5.9 16.5 28.84.0 6.7 17.0 29.84.5 7.4 17.5 30.85.0 8.2 18.0 31.85.5 9.0 18.5 32.86.0 9.8 19.0 33.86.5 10.6 19.5 34.97.0 11.5 20.0 35.97.5 12.3 20.5 37.08.0 13.1 21.0 38.18.5 13.9 21.5 39.29.0 14.8 22.0 40.49.5 15.7 22.5 41.6
10.0 16.6 23.0 42.810.5 17.5 23.5 43.911.0 18.3 24.0 45.011.5 19.2 24.5 46.112.0 20.0 25.0 47.312.5 21.0 25.5 48.513.0 21.9 26.0 49.713.5 22.9 26.5 51.014.0 23.8 27.0 52.3
Copper sulfate can be determined by taking the Baumé reading. This gives the combined copper sulfate plussulfuric acid. Subtraction of the ounces of acid leaves the ounces of copper sulfate.This method of obtaining the concentration of copper sulfate plus sulfuric acid is not accurate if otheringredients such as aluminum sulfate are present or if the solution is contaminated with iron.
564
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